TriStar II 3020 Operator's Manual

TriStar II 3020
Operator’s Manual
V1.03
302-42801-01
July 2009
Adobe Acrobat Reader is a registered trademark of Adobe Systems, Inc.
Alconox is a registered trademark of the Alconox Company.
Fomblin is a resistered trademark of Solvay S.A.
Micromeritics is a registered trademark of Micromeritics Instrument Corporation.
Microsoft, Windows, and Windows Vista are registered trademarks of Microsoft Corporation.
© Micromeritics Instrument Corporation 2008-2009. All rights reserved.

The software described in this manual is furnished under a license agreement and may be used or copied only in
accordance with the terms of the agreement.
WARRANTY
MICROMERITICS INSTRUMENT CORPORATION warrants for one year from the date of shipment each instru-
ment it manufactures to be free from defects in material and workmanship impairing its usefulness under normal use
and service conditions except as noted herein.
Our liability under this warranty is limited to repair, servicing and adjustment, free of charge at our plant, of any
instrument or defective parts when returned prepaid to us and which our examination discloses to have been defec-
tive. The purchaser is responsible for all transportation charges involving the shipment of materials for warranty
repairs. Failure of any instrument or product due to operator error, improper installation, unauthorized repair or alter-
ation, failure of utilities, or environmental contamination will not constitute a warranty claim. The materials of
construction used in MICROMERITICS instruments and other products were chosen after extensive testing and
experience for their reliability and durability. However, these materials cannot be totally guaranteed against wear and/
or decomposition by chemical action (corrosion) as a result of normal use.
Repair parts are warranted to be free from defects in material and workmanship for 90 days from the date of
shipment.
No instrument or product shall be returned to MICROMERITICS prior to notification of alleged defect and authori-
zation to return the instrument or product. All repairs or replacements are made subject to factory inspection of
returned parts.
MICROMERITICS shall be released from all obligations under its warranty in the event repairs or modifications are
made by persons other than its own authorized service personnel unless such work is authorized in writing by
MICROMERITICS.
The obligations of this warranty will be limited under the following conditions:
1. Certain products sold by MICROMERITICS are the products of reputable manufacturers, sold under their
respective brand names or trade names. We, therefore, make no express or implied warranty as to such products.
We shall use our best efforts to obtain from the manufacturer, in accordance with his customary practice, the
repair or replacement of such of his products that may prove defective in workmanship or materials. Service
charges made by such manufacturer are the responsibility of the ultimate purchaser. This states our entire liability
in respect to such products, except as an authorized person of MICROMERITICS may otherwise agree to in
writing.
2. If an instrument or product is found defective during the warranty period, replacement parts may, at the discre-
tion of MICROMERITICS, be sent to be installed by the purchaser, e.g., printed circuit boards, check valves,
seals, etc.
3. Expendable items, e.g., sample tubes, detector source lamps, indicator lamps, fuses, valve plugs (rotor) and
stems, seals and O-rings, ferrules, etc., are excluded from this warranty except for manufacturing defects. Such
items which perform satisfactorily during the first 45 days after the date of shipment are assumed to be free of
manufacturing defects.
Purchaser agrees to hold MICROMERITICS harmless from any patent infringement action brought against
MICROMERITICS if, at the request of the purchaser, MICROMERITICS modifies a standard product or manufac-
tures a special product to the purchaser’s specifications.
MICROMERITICS shall not be liable for consequential or other type damages resulting from the use of any of its
products other than the liability stated above. This warranty is in lieu of all other warranties, express or implied,
including, but not limited to, the implied warranties of merchantability or fitness for use.
4356 Communications Drive Norcross, GA 30093-1877 Fax (770) 662-3696
Domestic Sales - (770) 662-3633 Domestic Repair Service - (770) 662-3666

International Sales - (770) 662-3660 Customer Service - (770) 662-3636
TriStar II 3020 Table of Contents
TABLE OF CONTENTS
1. GENERAL DESCRIPTION
Organization of the Manual . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1-1
Conventions . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1-3
Equipment Description. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1-4
Krypton Option . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1-4
Software . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1-5
Vacuum Pump . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1-5
Degasser . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1-6
Internet Access . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1-7
Specifications . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1-8
2. USER INTERFACE
Instrument Components and Connectors . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-1
Front Panel . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-1
Sample Compartment. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-2
Side Panel. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-3
Rear Panel . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-4
Turning the Analyzer On and Off . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-5
Turning the Analyzer On . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-5
Turning the Analyzer Off. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-5
Using the Software. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-6
Shortcut Menus . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-6
Shortcut Keys . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-6
Dialog Boxes and Subdialog Boxes . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-8
Selecting Files . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-11
Selecting Reports . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-13
File Name Conventions . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-14
How-To Videos . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-15
Installation Instructions . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-15
Online Manual . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-17
Using Bookmarks. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-17
Using the Table of Contents, Index, and other Links. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-19
Table of Contents . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-19
Index . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-20
Cross References . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-20
Using the Find Command . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-21
Printing . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-22
Menu Structure. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-23
Main Menu Bar . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-23
Windows Menu . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-24
Help Menu . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-24
Jul 09 i
Table of Contents TriStar II 3020
3. OPERATIONAL PROCEDURES
Specifying Sample Defaults . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-1
Advanced Format . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-1
Basic Format . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-4
Defining Parameter Files . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-6
Sample Tube . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-6
Degas Conditions . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-8
Analysis Conditions . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-9
Adsorptive Properties . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-10
Report Options . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-12
Creating a Sample Information File . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-14
Advanced Format . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-14
Basic and Restricted Formats . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-16
Preparing for Analysis . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-18
Cleaning and Labeling Sample Tubes . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-18
Determining the Sample Mass . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-21
Degassing the Sample. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-23
Installing the Sample Tube . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-24
Installing the Analysis Dewar. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-25
Performing an Analysis . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-27
Standard Analysis . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-27
QuickStart Analysis . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-29
Printing File Contents . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-31
Listing File Statistics . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-33
Exporting Isotherm Data. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-34
Generating Graph Overlays . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-35
Multiple Sample Overlays . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-35
Multiple Graph Overlays . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-38
4. SOFTWARE AND SETUP MODIFICATIONS

Installing the Software . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-1
Using the Setup Program for Other Functions . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-6
Installing Subsequent Software Versions . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-8
Adding an Analyzer . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-9
Ethernet Switch . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-9
Software . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-10
Moving an Analyzer from One Computer to Another Computer. . . . . . . . . . . . . . . . . . . . . 4-11
Moving a Configured Analyzer to a New Computer . . . . . . . . . . . . . . . . . . . . . . . . . . 4-11
Moving a Configured Analyzer to a Computer with an Existing Analyzer . . . . . . . . . 4-15
Removing an Analyzer . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-16
Changing the Analyzer Setup Configuration . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-17
Reinstalling Calibration Files . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-19
Uninstalling the Analysis Program . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-20
ii Jul 09
5. FILE MENU
Description . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-1
Open . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-3
Sample Information . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-4
Advanced . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-5
Basic . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-8
Restricted . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-10
Sample Tube. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-11
Degas Conditions . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-13
Analysis Conditions . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-15
Adsorptive Properties. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-28
Report Options . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-31
Summary Report. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-35
Isotherm Report Options . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-37
BET/Langmuir Surface Area Report Options . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-39
Freundlich Report Options . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-42
Temkin Isotherm . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-44
t-Plot Report Options . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-46
Alpha-S Plot . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-52
f-Ratio Plot . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-55
BJH Adsorption/Desorption Report Options . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-57
Dollimore-Heal Adsorption/Desorption Report Options . . . . . . . . . . . . . . . . . . . . . . . 5-64
Horvath-Kawazoe Report Options . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-65
DFT Pore Size . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-71
DFT Surface Energy. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-74
Dubinin Report Options . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-75
MP-Method Report Options. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-80
Options Report . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-85
Sample Log Report. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-85
Validation Report . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-86
Entered or Collected Data . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-87
Save . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-91
Save As. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-91
Sample and Parameter Files . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-92
t-Curve and Alpha-S Files . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-92
Save All . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-93
Close. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-93
Close All. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-93
Print . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-94
List . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-95
Export. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-96
Format of Data Output . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-97
Convert. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-98
Exit . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-99
6. UNIT MENU
Description . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6-1
Sample Analysis. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6-3
Jul 09 iii
QuickStart . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6-8
Krypton Analysis . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6-11
Blank Analysis . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6-12
Enable Manual Control. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6-14
Show Instrument Schematic . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6-17
Show Status . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6-19
Show Instrument Log . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6-21
Unit Configuration . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6-23
Diagnostics . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6-24
Calibration . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6-27
Zero Pressure . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6-27
Match Transducers . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6-28
Servo Valve. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6-28
Store Instrument Information . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6-29
Save to File . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6-29
Load from File . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6-30
Service Test . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6-30
7. REPORTS MENU
Description . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-1
Start Report. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-3
Close Reports . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-5
Open Report . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-5
SPC Report Options . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-6
Regression Report. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-7
Control Chart . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-11
Heat of Adsorption Report . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-15
Printed Reports . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-19
Header. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-19
Onscreen Reports . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-19
Tool Bar . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-20
Shortcut Menus . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-24
Zoom Feature . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-28
Axis Cross Hair. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-28
Report Examples. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-29
Isotherm Plot. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-30
BET Surface Area Report . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-31
BET Surface Area Plot . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-32
t-Plot Report . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-33
BJH Adsorption: Cumulative Pore Area . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-34
BJH Desorption: Pore Volume Plot . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-35
Dollimore-Heal Desorption: Pore Volume/Area . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-36
Summary Report . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-37
Sample Log Report . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-38
iv Jul 09
8. OPTIONS MENU
Description . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8-1
Option Presentation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8-2
Advanced . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8-3
Basic . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8-4
Restricted . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8-5
Sample Defaults . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8-6
Advanced . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8-6
Basic . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8-10
Units . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8-12
Graph Grid Lines . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8-13
Live Graph . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8-14
Parameter Files Directory . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8-15
Service Test Mode . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8-15
9. TROUBLESHOOTING AND MAINTENANCE

Troubleshooting . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 9-1
Preventive Maintenance . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 9-3
Lubricating Elevator Drive Assembly . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 9-4
Cleaning the Analyzer . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 9-4
Cleaning the Analysis Dewar. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 9-4
Replacing Port Filter and O-ring . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 9-6
Replacing the Sample Tube O-ring . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 9-7
Inspecting and Changing Vacuum Pump Oil. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 9-8
Inspecting the Oil . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 9-8
Changing or Adding Oil . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 9-8
Replacing the Alumina in the Oil Vapor Trap . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 9-11
Changing the Vacuum Pump Exhaust Filter . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 9-15
Performing a Leak Test . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 9-16
Connecting Gases. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 9-19
Guidelines for Connecting Gases to the Analyzer . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 9-19
Disconnecting the Depleted Bottle. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 9-19
Connecting a Replacement Gas Bottle. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 9-21
Cleaning and Verifying the Gas Line. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 9-24
Specifying Gas Ports . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 9-28
Calibrating the System . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 9-29
Zero Pressure . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 9-29
Match Transducers . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 9-30
Servo valve. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 9-30
10. ORDERING INFORMATION
A. FORMS
Sample Data Worksheet. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . A-3
Jul 09 v
B. ERROR MESSAGES
2400 Series . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . B-1
2500 Series . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . B-12
4000 Series . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . B-18
6000 Series . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . B-34
C. CALCULATIONS
Saturation Pressure . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . C-1
Relative Pressure Calculations . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . C-1
Volume Adsorbed Calculations . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . C-3
Free Space. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . C-3
Measured. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . C-3
Calculated . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . C-4
Equilibration . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . C-5
Thermal Transpiration Correction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . C-6
BET Surface Area. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . C-7
Langmuir Surface Area. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . C-9
t-Plot . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . C-10
BJH Pore Volume and Area Distribution . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . C-12
Explanation of Terms . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . C-12
Calculations . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . C-13
Compendium of Variables . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . C-21
Horvath-Kawazoe . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . C-22
Slit Pore Geometry (original HK). . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . C-22
Cylinder Pore Geometry (Saito/Foley) . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . C-23
Sphere Pore Geometry (Cheng/Yang) . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . C-24
Cheng/Yang Correction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . C-25
Interaction Parameter . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . C-26
Additional Calculations . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . C-27
Interaction Parameter Components. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . C-28
Dubinin-Radushkevich . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . C-30
Dubinin-Astakhov. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . C-32
MP-Method. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . C-36
Freundlich Isotherm . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . C-38
Temkin Isotherm. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . C-39
DFT (Density Functional Theory) . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . C-40
The Integral Equation of Adsorption . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . C-40
Application to Surface Energy Distribution . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . C-41
Application to Pore Size Distribution . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . C-41
Performing the Deconvolution . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . C-42
Regularization . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . C-42
SPC Report Variables . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . C-43
Regressions Chart Variables. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . C-43
Control Chart Variables . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . C-43
Summary Report. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . C-45
References. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . C-47
vi Jul 09
D. FREE-SPACE CORRECTION
Measure . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . D-2
Calculate. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . D-2
Enter . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . D-3
E. ETHERNET CONFIGURATION
Configuring the Ethernet Port . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . E-1
Windows XP Professional . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . E-1
Windows Vista . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . E-4
Configuring the Firewall Setting . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . E-7
Windows XP Professional . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . E-7
Windows Vista . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . E-8
F. DFT MODELS
Models Based on Statistical Thermodynamics . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . F-1
Theoretical Background . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . F-1
Molecular Simulation Methods . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . F-2
Molecular Dynamics Method . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . F-2
Monte Carlo Method . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . F-2
Density Functional Formulation. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . F-3
Models Included. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . F-7
Non-Local Density Functional Theory with Density Independent Weights . . . . . . . . F-7
Modified Non-Local Density Functional Theory with Density-Dependent Weights . F-7
Models Based on Classical Theories . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . F-11
Surface Energy . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . F-11
Pore Size. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . F-11
Models Included. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . F-12
Kelvin Equation with Halsey Thickness Curve . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . F-12
Kelvin Equation with Harkins and Jura Thickness Curve . . . . . . . . . . . . . . . . . . . . . . F-12
Kelvin Equation with Broekhoff-de Boer Thickness Curve . . . . . . . . . . . . . . . . . . . . F-13
References . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . F-15
G. MAINTAINING HIGH PURITY GASES

Using Metal Gas Lines. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . G-1
Removing Trapped Air. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . G-1
Purge Method . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . G-2
Evacuation Method. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . G-3
INDEX
Jul 09 vii
TriStar II 3020 Organization of the Manual
1. GENERAL DESCRIPTION
This manual provides a description of the TriStar 3020, its menu options, and operating
instructions. Installation instructions are located on the installation disk included with your
software.
To help you operate the TriStar more efficiently:
• read Chapter 2, User Interface, before operating the analyzer and its software
• use the step-by-step instructions in Chapter 3 when performing common operations
Organization of the Manual

This operator’s manual is organized as follows:
Chapter 1 GENERAL DESCRIPTION

Provides a general description of the TriStar 3020 and its features and
specifications.
Chapter 2 USER INTERFACE

Provides instrument and software interface.
Chapter 3 OPERATIONAL PROCEDURES

Provides step-by-step procedures for the operations performed with the
TriStar 3020.
Chapter 4 SOFTWARE AND SETUP MODIFICATIONS

Provides instructions for installing software updates and for modifying
analyzer setup configurations.
Chapter 5 FILE MENU

Provides a description of the choices available on the File menu.
Chapter 6 UNIT MENU

Provides a description of the choices available on the Unit menu.
Chapter 7 REPORTS MENU

Provides a description of the choices available on the Reports menu.
Apr 08 1-1
Organization of the Manual TriStar II 3020
Chapter 8 OPTIONS MENU

Provides a description of the choices available on the Options menu.
Chapter 9 TROUBLESHOOTING AND MAINTENANCE

Provides user maintenance and service information.
Chapter 10 ORDERING INFORMATION

Provides ordering information for TriStar system components.
Appendix A FORMS
Contains a copy of the Sample Information Worksheet. This form is used to
assist you in obtaining your sample mass.
Appendix B ERROR MESSAGES

Lists the error messages that may be displayed by the software and includes a
cause and action for each.
Appendix C CALCULATIONS
Provides the calculations used by the TriStar program.
Appendix D FREE-SPACE CORRECTION

Provides a discussion of the free-space measurements available with TriStar.
Appendix E ETHERNET CONFIGURATION

Provides information on configuring an ethernet port and specifying firewall
settings.
Appendix F DFT MODELS

Provides information on DFT models.
Appendix G MAINTAINING HIGH PURITY GASES

Provides information on the importance of maintaining high purity gases.
Index INDEX
Provides quick access to a subject matter.
1-2 Apr 08
TriStar II 3020 Organization of the Manual
Conventions
This manual uses the icons shown below to identify notes of importance, cautions, and
warnings.
Notes contain important information pertinent to the subject matter.
Warnings contain information that help you prevent actions that may cause personal
injury.
Cautions contain information that help you prevent actions that may damage the
analyzer or one of its components.
Apr 08 1-3
Equipment Description TriStar II 3020
Equipment Description
The TriStar 3020 is an automated gas adsorption analyzer which contains three ports, allowing
you to analyze up to three samples simultaneously. Also featured is a dedicated port for mea-
suring the saturation pressure (Po) on a continuous basis. Surface areas as low as 0.01 m2/g
can be measured using nitrogen and as low as 0.001 m2/g with the Krypton option. Up to 1000
data points can be collected, allowing you to observe minute details of the isotherm.
You can operate up to four TriStar analyzers with one computer. The TriStar II 3020 system
consists of the TriStar analyzer, a SmartPrep degasser (optional) for preparing samples, a vac-
uum pump, and a computer for entering analysis and report options.
Krypton Option
The Krypton option enables you to measure surface areas as low as 0.001 m2/g using krypton
as the adsorptive. Your TriStar system must be equipped with a 10-mmHg transducer and a
high-vacuum pump to provide this capability. Refer to Ordering Information, page 10-1 for
ordering information.
1-4 Apr 08
TriStar II 3020 Equipment Description
Software
The TriStar 3020 analysis program operates in a Windows® environment. This makes opera-
tion of the TriStar easier and allows you to run other applications while an automatic operation
is in progress.
The report system provided in the analysis program allows you to manipulate and customize
reports in a variety of ways. You can zoom in on portions of the graphs or shift the axes to
examine fine details. Scalable graphs can be copied to the clipboard and pasted into other
applications. Reports can be customized with your choice of fonts and a company logo added
to the report header for an impressive presentation. Refer to Onscreen Reports, page 7-19 for
the options available for reports.
To make it easier for you to obtain information, an online manual is included on the Help
menu. This enables you to access the desired information in just a couple of mouse clicks.
Refer to Online Manual, page 2-17 for additional information and navigation methods. Also
included on the Help menu are a variety of How-To videos. These videos are designed to visu-
ally step you through procedures such as creating sample files, changing the vacuum pump oil
and alumina, etc.
Vacuum Pump
A vacuum pump is required for sample analysis with the TriStar analyzer.
Vacuum pumps used with the TriStar must meet the following criteria. They must:
• be able to achieve vacuums better than 20 µmHg at the instrument inlet
• contain an anti-suckback valve to prevent vacuum pump oil from backing up into the
analyzer in the event of a vacuum pump failure
• contain an NW16 inlet port for connection to the TriStar
An oil-based or oil-free vacuum pump can be used with the TriStar (an oil-free pump is
required if you have the Krypton option installed). Appropriate vacuum pumps are available
from Micromeritics. (Refer to Ordering Information, page 10-1 for ordering information.)
Apr 08 1-5
Equipment Description TriStar II 3020
Degasser
Micromeritics has available the following degassing units for preparing samples:
• SmartPrep 065
The SmartPrep uses flowing-gas to remove adsorbed contaminants from the surface and
pores of your sample. It contains six sample ports, each one independently controlled
for greater flexibility. It contains two serial ports, one for connecting to the computer
and the other available for connecting an additional SmartPrep. In fact, you can connect
up to four SmartPreps, one to the other, allowing the capability of up to 24 preparation
ports at one time.
The SmartPrep also can be controlled through the TriStar application and is the
recommended degassing unit for the TriStar.
• VacPrep 061
The VacPrep degasses up to six samples at up to 400 ºC with either flowing gas or
evacuation.
• FlowPrep 060
The FlowPrep degasses up to six samples at up to 400 ºC with flowing gas.
Refer to Chapter 10, page 10-1 for ordering information.
1-6 Apr 08
TriStar II 3020 Internet Access
Internet Access
Visit www.micromeritics.com to learn more about Micromeritics, our products, and applica-
tions. Our site is user-friendly, easy to navigate, and informative. Its content is summarized
below.
About Micromeritics A brief history of Micromeritics, office locations, awards/cer-

tifications, career opportunities, and a virtual tour of its
headquarters
Products Product information and printable brochures
Applications Application Notes, Product Bulletins, Tech Tips, Technical

Articles/papers, and important application links
Online Catalog Catalog of instruments and accessories, allowing you to place

your order online
News and Press Press releases, Events calendar, microReports, and latest
Micromeritics news updates
Lab Service Provides laboratory tips and access to the Micromeritics Ana-
lytical Services web site
Customer Support Customer support contacts, product registration, instrument

training information, Material Safety Data Sheets, and account
registration
Grant Program Details of the Grant Program established for non-profit orga-
nizations and universities
Contact Us Contact information, office locations, maps and driving direc-

tions to the Micromeritics facility, and registration for the
microReport newsletter
Be sure to browse our site to see the many ways in which we can assist you.
Apr 08 1-7
Specifications TriStar II 3020
Specifications
The TriStar 3020 has been designed and tested to meet the specifications provided below.
Characteristic Specification
Pressure Measurement
Absolute
Range: 0 to 950 mmHg
Resolution: Within 0.05 mmHg
Accuracy: Within 0.5%
Linearity: Within 0.25% of full scale (transducer manufacturer’s
specification)
Relative
P/Po range: 0 to 1.0 P/Po
Resolution: < 10-4
Analysis
Specific Surface Area: From 0.01 m2/g, nitrogen unit

From 0.001 m2/g, krypton unit
Total Surface Area: From 0.1 m2, nitrogen unit
From 0.01 m2, krypton unit
Pore Volume: From 4 x 10-6 cm3/g
Dewar duration: > 24 hours
Adsorptive Gases
Nitrogen unit: Nitrogen; argon, carbon dioxide, or other non-corrosive gases;

butane, methane, or other light hydrocarbon vapors. Oxygen can
also be used only with an appropriate vacuum pump.
Krypton unit: Same as Nitrogen unit, plus the capability to perform krypton
surface area analyses at lower pressures.
The TriStar should be operated in a properly vented environment when using flammable or
toxic gases.
Manifold Temperature
Accuracy: ± 0.25 ºC
Resolution: Within 0.1 ºC
1-8 Apr 08
TriStar II 3020 Specifications
Characteristic Specification
Vacuum System
Nitrogen unit: Must accommodate 20 x 10-3 mmHg or better; uses oil-based or oil-
free vacuum pump
Krypton unit: Must accommodate 0.1 x 10-3 mmHg; oil-free vacuum pump
required
Environment
Temperature: 10 and 35 ºC (50 to 95 ºF), operating;

0 to 50 ºC (0 to 122 ºF), nonoperating
Humidity: 20 to 80% relative, noncondensing
Physical
Height: 74 cm (29 in.)

Width: 40 cm (16 in.)
Depth: 51 cm (20 in.)
Weight: 37 kg (82 lbs)
Electrical
Voltage: 100/120, 220/240 VAC

Power: 150 VA, maximum
Frequency: 50 to 60 Hz
Computer
Minimum Pentium 333 MHz computer (or equivalent)

requirements: 512 megabytes of main memory
20-gigabytes hard drive
Ethernet port (capable of communicating with a 10 base-T
ethernet card)
CD-ROM drive
1024 x 768 video display capability
Windows® XP Professional or Windows Vista® operating system
Apr 08 1-9
TriStar II 3020 Instrument Components and Connectors
2. USER INTERFACE
This chapter contains information to familiarize you with the hardware and software compo-
nents of the TriStar II 3020. It is recommended that you read this chapter before attempting to
operate the TriStar system.
Instrument Components and Connectors
Front Panel
Power indicator Blinks when power is applied to the analyzer; illuminates

when analysis program is initiated and ready for operation.
Sample Compartment Sliding door which encloses the sample compartment.

door
Mar 09 2-1
Instrument Components and Connectors TriStar II 3020
Sample Compartment
Sample ports (three)
Saturation pressure (Po) tube Diagram of port locations
Elevator
Sample ports For installing sample tubes; you can install up to three sample
tubes.
Po tube For measuring the saturation pressure.
Diagram Provides a pictorial representation of port numbers and their

locations.
Elevator Allows placement of the Dewar around the sample and Po

tubes.
2-2 Mar 09
TriStar II 3020 Instrument Components and Connectors
Side Panel
Ethernet connector
RS232 connector
Ethernet connector For connecting the ethernet cable, allowing communication

between the analyzer and the computer.
RS-232 connector Used by service personnel to perform calibration procedures.
Mar 09 2-3
Instrument Components and Connectors TriStar II 3020
Rear Panel
Analysis inlet valves Vacuum Pump connector
Maximum inlet Helium inlet valve

pressure
On/Off switch
Power cord connector
Gas Inlet Valves Inlets V8, V9, and V14 are for analysis gases; inlet V7 is
dedicated to helium.
Vacuum Pump connector For attaching the vacuum pump hose.
On/Off switch For turning the analyzer on and off.
Power connector For connecting the analyzer to the power supply.
2-4 Mar 09
TriStar II 3020 Turning the Analyzer On and Off
Turning the Analyzer On and Off
Turning the Analyzer On
1. Place the computer, monitor, and printer ON/OFF switches in the ON position.
2. Place the TriStar analyzer ON/OFF switch in the ON ( | ) position. The pump will turn on
automatically if it is plugged into the electrical outlet; allow the pump to operate for two
hours before performing analyses.
Turning the Analyzer Off
Always exit the analysis program and Windows before turning off the computer.
Failure to do so could result in loss of data.
1. Select Close from the System menu or Exit from the File menu.
If an analysis is in progress, the following message is displayed:
2459- An Instrument is busy. A delay in restarting this

application could result in loss of new data. Continue
program exit?
Yes No
If you click Yes and the analysis program closes, the analysis continues and data continue
to be collected. Reports that are queued under the Print Manager will print. If, however, a
power failure occurs and an uninterruptible power supply (UPS) is not attached to the
analyzer, the data collected after exiting the analysis program are lost.
2. Place the computer, monitor, and printer ON/OFF switches in the OFF position.
3. Place the TriStar analyzer ON/OFF switch in the OFF position.
Mar 09 2-5
Using the Software TriStar II 3020
Using the Software

The TriStar 3020 analysis program operates in the Windows environment and requires famil-
iarity with standard Windows operations such as using the mouse, menus, and dialog boxes.
While this manual provides brief instructions for such standard operations, you may have to
refer to your Windows documentation or to its online help system to clarify functions which
are specific to Windows.
Shortcut Menus
Shortcut menus (sometimes referred to as context-sensitive menus or pop-up menus) are avail-
able for certain components on the instrument schematic when in manual mode, and for
onscreen graphs and tabular reports. These menus are accessed by selecting the item for which
you want to display its menu and clicking the right mouse button. For example, right-click in a
column of an onscreen report and the following menu is displayed.
Shortcut Keys
Shortcut keys can be used to activate some menu commands. Shortcut keys or key combina-
tions (if assigned) are listed to the right of the menu item. Instead of opening the menu and
choosing the command, simply press the key combination. For example, to open a sample
information file, press F2; the Open Sample Information dialog is displayed.
You can also use shortcut keys to access a menu or any function that contains an underlined
letter by pressing Alt plus the underlined letter in the command. For example, to access the
File menu, press Alt, then F.
Table 2-1 provides a list of the keys available in the TriStar 3020 analysis program.
2-6 Mar 09
TriStar II 3020 Using the Software
Table 2-1. Shortcut Keys
Key(s) Function
F1 Access online operator’s manual
F2 Open a sample information file
Clear the field of existing date (Select Dates dialog)
F3 Open an analysis conditions file
Insert the current date (select Dates dialog)
F4 Open an adsorptive properties file
Display a calendar to choose a date (Select Dates dialog)
F5 Open a report options file
F6 Tile windows
F7 Cascade windows
F8 Start a report
F9 Close all open reports
F10 Generate a Heat of Adsorption report
Alt + F4 Exit the analysis program
Shift + F2 List sample information files
Shift + F3 List analysis conditions files
Shift + F4 List adsorptive properties files
Shift + F5 List report options files
Shift + F9 Access shortcut menu of (1) selected component on instrument
schematic, or (2) onscreen reports
Mar 09 2-7
Dialog Boxes and Subdialog Boxes
Dialog boxes are displayed when an item followed by an ellipsis (...) is selected. Subdialog
boxes are displayed when a push button on a dialog box is selected. Both types of dialogs may
contain one or more of the following:
Dialog box
Subdialog box
Data entry field These fields may be either numeric (numbers only) or
alphanumeric (numbers, letters, or printable characters). If
you make an invalid entry in either of these fields, an error
message occurs.
Alphanumeric field
Numeric fields
2-8 Mar 09
Information bar Some dialog boxes contain information pertinent to the

selected field in an information bar across the bottom of the
dialog. For example, a range is shown for fields in which
numeric entries are required.
Selected field
Displays range for

selected field.
List A list contains selections from which you may choose one or
more items. To select an item on the list: Highlight the
selection, then double-click or press the Spacebar. An item
is selected when it is preceded with a check mark.
Indicates item is
selected.
Push Button A push button is used to display subdialog boxes in which to

enter additional information about the subject matter. For
example, this push button displays a dialog for specifying a
range of dates (explained later in this chapter).
Push buttons also may be used to cause an action. For

example, Cancel closes the open dialog, discarding any
information you may have entered.
Mar 09 2-9
Radio Button Radio buttons are contained within a group box. These
buttons are used to select options; you may choose only one
item.
Check Box Check boxes also are used to select options. You may make
as many selections as you wish.
Drop-down List A drop-down list is indicated by a down arrow to the right of

the field. Drop-down lists contain a list of options from
which you may choose one
Down Arrow
Some of the more commonly used push buttons are:
Browse Displays a dialog which allows you to select a file for the
subject matter.
Replace Allows you to copy file values from an existing file into the
one you are creating. After the values have been copied into
the file, you can edit them as desired. The file from which the
values were copied is not affected and remains intact.
Save Saves the information entered in the open dialog but allows
the dialog to remain open.
2-10 Mar 09
Close Closes the open dialog. If the dialog contains changes that
have not been saved, you are prompted to save them before
the dialog closes.
Selecting Files
Sample information is stored in files and saved under file names. Some dialogs contain a Files
list window, which displays a list of files available for that particular operation. For example,
the Open Sample Information dialog:
Choose a new Status

category to limit the
files displayed in the
Files list box.
Click to specify a
range of dates.
Choose the
drive/directory.
Choose the file

you wish to open.
From the list of files in the Files list window, highlight the file you wish to open and double-
click, or click OK. If you do not see the desired file, it may be in another directory. Go to the
Directories list window and choose the correct drive and/or directory.
You may limit the list of files displayed in the Files list window by choosing one or more of
the following:
• Use wildcard characters in the path name you enter in the File name field.
Wildcard characters such as * and ? can be used to filter file names. For example, you
can limit the list of files displayed to those beginning with 01 by entering 01*.smp.
Mar 09 2-11
• Enter a range of dates. Click Date Range; the Select Dates dialog is displayed.
Select the Show Date Range radio button. This enables the From and To fields allow-
ing you to enter a beginning and ending date. Alternatively, you can double-click in
each field to display a calendar to set a date. The range of dates remains the default until
you change the dates or select Show All Dates.
For convenience, the following function keys are available when the Select Dates dialog
is displayed:
F2 Clears the field

F3 Inserts the current date
F4 Displays a calendar from which to select a date
You can change the date format by using the International Date Format function on the
Windows Control Panel.
• Select a file status from the Status drop-down list. Table 2-2 describes each file status.
Table 2-2. File Status and Description
Status Description
All All sample information files in the specified directory and within
the specified range of dates.
Analyzing Sample information files that are currently being used for
analysis or are in the degassing process.
Complete Sample information files that were used in an analysis that has
been completed.
Entered Sample information files that contain manually entered data.
No analysis Sample information files that have not been used to perform an
analysis.
Prepared Sample information files that have been used in an automatic
degas operation, but not for an analysis.
Preparing Sample information files currently being used in an automatic
degas operation.
2-12 Mar 09
• Navigate to a different directory. The current directory is displayed above the Directo-
ries list window. You can change directories by double-clicking a directory in the
Directories list window, double-clicking [...] to move up one level, or by entering the
desired directory in the File Name field. For example, enter C:\3020\files\sample\*.smp
to display sample files in the 3020\files\sample directory on your local drive.
Displays the current Double-click to move

directory. up one level.
Double-click to open
the listed directory.
Selecting Reports
Reports are selected from the Report Options dialog, or any dialog containing a Selected
Reports list. Simply select (highlight) the report and then double-click, or press the
Spacebar. A report is selected when it is preceded with a check mark (3). Reports are dese-
lected in the same manner.
Indicates a report
is selected.
Mar 09 2-13
File Name Conventions
For sample information files, a default file name (the next available sequence number) and a
default extension display. For Sample tube, Degas conditions, Analysis conditions, Adsorptive
properties, and Report options, only a default extension displays.
The following table shows the file name extensions for the TriStar 3020 analysis program.
Table 2-3. Default File Name Extensions
File Type Extension

Sample information SMP
Sample tube STP
Degas conditions DEG
Analysis conditions ANC
Adsorptive properties ADP
Report options RPO
Export to disk (ASCII) EXP
Report to disk RPT
List to disk LST
Thickness curve THK
Alpha-s curve ALS
The following types are available for reports saved from the
Report window:
Report REP
Spreadsheet XLS
ASCII TXT
2-14 Mar 09
How-To Videos
For your convenience and to make it easier for you to perform common operations, How-To
videos have been included in the software. These videos visually step you through a proce-
dure; for example, one of the How-To videos is designed to assist you in properly preparing
your sample.
These videos are accessible from the Help menu; take a few minutes to view the ones avail-
able. Included in this group of videos is one entitled Using the How-to Videos. This module
provides information and tips on using the videos; you may want to view this one first.
Installation Instructions
Also included, but not accessible from the Help menu, are the System Installation videos used
for initial installation of your analyzer. To access these videos:
1. Open Windows Explorer and navigate to the directory in which you installed the
application; the default directory is win3020 and is the directory shown in this example.
2. Double-click on the system installation directory to display its contents.
Mar 09 2-15
3. Double-click on the file named Menu.exe; the menu for the Installation Instructions is
displayed.
4. Click on the desired procedure to launch the video.
2-16 Mar 09
TriStar II 3020 Online Manual
Online Manual
For your convenience, the Operator’s Manual is available online. You can access the manual
by selecting Help, then Operator’s Manual from the analysis program main menu. The
manual appears in an Adobe® Acrobat® Reader®.
Following are some tips to help you quickly locate the information you need in the manual.
Refer to the Adobe Acrobat Help system (click the Help button on the Acrobat menu) for
more information on the Acrobat features you can use while viewing the manual.
Using Bookmarks
Click the Bookmarks tab to list and access the topics included in the manual.
Bookmarks
Topics
Navigation Pane Topic Pane
You can use the + and − buttons next to topics as they are used in Windows Explorer to
expand or collapse the topic list.
Mar 09 2-17
Online Manual TriStar II 3020
To display a topic, click the topic name in the Bookmarks section. The related information
appears in the topic pane of the window as shown in the following example.
Click bookmark
to display topic.
2-18 Mar 09
Using the Table of Contents, Index, and other Links
Links provide direct access to selected information. All links appear in blue type. Links are
contained in:
• the table of contents

• index entries
• cross-references within the manual
Table of Contents
To display the table of contents, click Table of Contents in the Bookmarks section. When the
table of contents is displayed, you can click an entry to display its associated page. For
example, clicking Using the Software in the table of contents, displays the page containing
information about the software.
Click topic name in

table of contents to
display topic.
Mar 09 2-19
Index
To use the index in the online manual, click the Bookmarks tab, scroll down to INDEX (the
last topic in Bookmarks), then click the + button to expand the index. The letters A through Z
are displayed. Click a letter to display its corresponding index entries as shown in the
following example.
Click a letter to display

its index entries.
After you display the entries, locate the item of interest and click on the page reference to
access the information.
Cross References
Cross-references work in the same manner. In the example below, clicking on the cross-
reference, FILE MENU (shown on the screen in blue type) will display the first page of the
chapter describing the commands found on the File menu.
FILE MENU
Provides a description of the commands available on the File menu.
2-20 Mar 09
Using the Find Command
The Adobe Acrobat Find command provides another method of easily accessing specific
information. For example, suppose you want to know how the Save as command works. You
could select Edit > Find from the Adobe Acrobat menu, then enter Save as in the Find dialog.
The following example shows the results.
Mar 09 2-21
Printing
You can print the entire manual, a selected page, or range of pages. There are several options
for printing. You can:
• Select the printer icon ( ) on the Adobe Acrobat toolbar.
A standard Print dialog is displayed. Select the page(s) to print, then click OK. When using
this option (or the next one), be sure to enter the page number(s) displayed in Adobe
Acrobat; do not use the page number(s) listed in the footer(s) of the manual.
Do not use
number in
Enter
footer of the
this
manual.
number.
• Select File > Print.
A standard Print dialog is displayed. Select the page(s) to print, then click OK.
• Click the Thumbnails tab.
Thumbnails of manual pages are displayed.

a. Click the pages you want to print.
b. Right-click to display a shortcut menu, then select Print Pages.
c. A standard Print dialog is displayed; click OK.
Thumbnails
tab
2-22 Mar 09
TriStar II 3020 Menu Structure
Menu Structure
SmartPrep drop-down
menu displays here if a
SmartPrep unit is being
used with the TriStar.
Main Menu Bar
All functions for the TriStar 3020 are accessed from the main menu bar. Brief descriptions are
provided below; refer to the chapter given in parentheses for a detailed description of the
options contained on that menu.
File Allows you to manage sample and parameter files.

(Chapter 5, FILE MENU)
Unit [n] Enables you to perform analyses, calibrations, and other instrument
operations. (Chapter 6, UNIT MENU)
SmartPrep Displays only if you have a SmartPrep degassing unit installed on the
TriStar. The options contained on this menu are explained in the
SmartPrep operator’s manual.
Reports Enables you to generate, close, and customize reports.

(Chapter 7, REPORTS MENU)
Options Allows you to edit sample defaults, specify your system

configuration, and select data presentation formats.
(Chapter 8, OPTIONS MENU)
Windows Enables you to arrange the windows and icons on your screen. It also
displays the names of all open windows. (this chapter, page 2-24)
Help Displays Help topics. (this chapter, page 2-24)
Mar 09 2-23
Menu Structure TriStar II 3020
Windows Menu
The choices on this menu allow you to arrange your open windows and icons.
Tile Resizes all open windows and arranges them side by side so that the
contents of all open windows are visible.
Cascade Resizes all open windows and arranges them in a stacked fashion.
The active window is positioned on top of the stack. Each window’s
title remains visible, making it easy to select other windows.
Arrange Icons Arranges the symbols for all minimized windows in an orderly
manner.
The Windows menu also displays all open files; the active window is preceded with a check
mark.
Help Menu
Help Provides access to the online operator’s manual and the How-To
videos.
About TriStar 3020 Displays information about the TriStar 3020 analysis program.
2-24 Mar 09
TriStar II 3020 Specifying Sample Defaults
3. OPERATIONAL PROCEDURES
This chapter contains step-by-step procedures for operating the TriStar. It does not provide
detailed descriptions of the fields in the dialogs used to perform these procedures. Chapters 5
though 8 contain details for the dialogs. At the beginning of each procedure, you will find the
location of the dialog used in that procedure.
Specifying Sample Defaults

Sample information files include the information required by the TriStar to perform an analy-
sis and collect data. The TriStar automatically generates sample information file names and
assigns the default values which you specify.
Sample defaults can be specified using the Advanced or Basic format.
Advanced Format
You can move from one set of parameters to another by clicking the parameter tab or by using
Next and Prev. The values you specify in the parameter portions of the sample file (Sample
Tube, Degas Conditions, Analysis Conditions, Adsorptive Properties, and Report Options)
are saved as the defaults for newly created parameter files.
For example, after specifying defaults for a sample file in the Advanced format:
• Select File > Open > Sample Information, then click Yes to create the file, and the
defaults you specify display for all parameters.
• Select File > Open > Analysis Conditions, enter a file name; then click OK, and the
defaults you specify in the Analysis Conditions portion of the Advanced Sample
Defaults dialog display in the fields.
Refer to Advanced, page 8-6 for a detailed description of the fields on this dialog.
Jul 09 3-1
Specifying Sample Defaults TriStar II 3020
1. Select Options > Sample Defaults; the Sample Defaults dialog is displayed.
2. In the Sequence field, specify a default string. This is the number that is incrementally
sequenced and displays in the File name field when you select File > Open > Sample
information.
3. In the field on the right of the Sample line, enter a format for the identification. Be sure to
include the $ symbol if you wish to have the sample file number included as part of the
identification. You can use up to 42 alphanumeric characters.
You can also edit the label (Sample); for example, you may wish to use Sample Material.
You can enter up to 15 characters in this field.
4. Edit the Operator and Submitter lines as desired. Or you may have either (or both) of
these lines omitted entirely by selecting Omit.
5. If bar code information is not applicable, select Omit to omit this field from the sample
information dialog. Or, if you prefer to use this line for some other type of information,
edit the label.
6. You can enter a sample mass or have it calculated automatically; choose the desired
method.
• Enter: enter a default value in the Mass field.
• Calculate: enter default values in the Empty tube and Sample+tube fields
Regardless of which method you choose, the choice can be changed when you create a
sample file.
3-2 Jul 09
7. Enter a default value in the Density field. This value is applicable only when using a
calculated free space.
8. In the Type of Data group box, choose whether you wish to collect data automatically or
enter it manually.
9. If you plan to report statistical process control (SPC) information, enter appropriate
information. These are user-definable parameters that can be entered and tracked along
with other statistical process control data; refer to Sample Defaults, page 8-8 for
additional information on these parameters.
10. After you complete the Sample Information dialog, click on the parameter tabs to open
associated dialogs; specify defaults as desired.
The defaults you specify for parameters serve as the defaults for new parameter files. For
example, the values you specify in the Analysis conditions portion of the sample file
display as the default values for a newly created standalone Analysis conditions file.
11. Click Save, then Close.
Jul 09 3-3
Specifying Sample Defaults TriStar II 3020
Basic Format
Perform the following steps to establish defaults for a sample information file in the Basic for-
mat. The defaults you establish with this format also serve as defaults for files created
using the Restricted format.
When specifying defaults in the Basic format, you will have to select default parameter files.
You may wish to define parameter files before entering sample defaults (refer to Defining
Parameter Files, page 3-6).
Refer to Basic, page 8-10 for a detailed description of the fields on this dialog.
1. Select Options > Sample Defaults; the Sample Defaults dialog is displayed.
2. In the Sequence field, specify a default string. This is the number that is incrementally
sequenced and displays in the File name field when you select File > Open > Sample
information.
3. In the field on the right of the Sample line, enter a format for the identification. Be sure to
include the $ symbol if you wish to have the sample file number included as part of the
identification. You can use up to 42 alphanumeric characters
You can also edit the label (Sample); for example, you may wish to use Sample Material.
You can enter up to 15 characters in this field.
3-4 Jul 09
4. You can enter a sample mass or have it calculated automatically; choose the desired
method.
• Enter: enter a default value in the Mass field.
• Calculate: enter default values in the Empty tube and Sample+tube fields
Regardless of which method you choose, the choice can be changed when you create a
sample file.
5. Enter a default value in the Density field. This value is applicable only when using a
calculated free space.
6. Select the down arrow to the right of the following fields to choose default parameter files:
• Sample Tube
• Degas Conditions
• Analysis Conditions
• Adsorptive Properties
• Report Options
Jul 09 3-5
Defining Parameter Files TriStar II 3020
Defining Parameter Files

The following file types can exist as part of the sample information file, as well as individual
parameter files:
• Sample tube
• Degas conditions
• Analysis conditions
• Adsorptive properties
• Report options
Having these files exist independently allows you to use them over and over again.
Several predefined parameter files are included with the TriStar program. Although these files
may come close to the needs of your laboratory, you may wish to define additional ones. Or
you can use a predefined file as a starting point. You can do this by creating a new file and then
clicking Replace. A dialog is displayed so that you can select the existing parameter file. Then
you can make any changes you need to make and the original file remains unchanged.
Make sure you save these files to the directory specified as the Parameter File directory, or
they will not be included in the drop-down lists on the Basic and Restricted sample informa-
tion dialogs. Unless you have changed the parameter file directory, the software defaults to the
correct directory (refer to Parameter Files Directory, page 8-15 for detailed information).
Parameter files may be created using either the Basic or Advanced format.
Sample Tube
Sample tube files are applicable only when using Calculate as the free-space method.
Refer to Sample Tube, page 5-11 for a detailed description of the fields on this dialog.
Be sure you have performed a blank analysis using the sample tube for which you are creating
a Sample Tube file. You will use the data obtained from the blank analysis in your Sample
Tube file.
1. Selct File > Open > Sample Tube; the Open Sample Tube File dialog is displayed.
2. Enter a name in the File name field, then click OK.
3-6 Jul 09
TriStar II 3020 Defining Parameter Files
3. Click Yes to create the file; the Sample Tube dialog is displayed:
4. Enter a description in the Sample Tube field. Be sure to use an intuitive description so that
you can recognize it easily. Most users enter the serial number of the sample tube and/or
size.
5. Click Load from Sample File; the Open Sample Information File dialog is displayed.
6. Select the file you used in the blank run with this sample tube, then click OK to copy the
data for the warm and cold free space and the non-ideality factor into the Sample Tube
dialog.
7. Select whether a filler rod and/or an isothermal jacket was used in the blank run.
8. If a vacuum seal was used, select the one you used; if not, leave the default of None
selected.
Jul 09 3-7
Degas Conditions
Degas Conditions files contain degassing information for sample preparation. These files are
used only if you are using the SmartPrep Degasser.
Refer to Degas Conditions, page 5-13 for a detailed description of the fields on this dialog.
1. Select File > Open >Degas conditions; the Degas Conditions dialog is displayed.
3. Click Yes to create the file; the Degas Conditions dialog is displayed:
4. Enter a description in the Description field. Be sure to use an intuitive description so that
you can recognize it easily.
5. Enter up to five stages of degassing (soak temperature, ramp rate, and soak time).
3-8 Jul 09
Analysis Conditions
Analysis conditions specify the data used to guide an analysis.
Refer to Analysis Conditions, page 5-15 for a detailed description of the fields on this dialog.
1. Select File > Open > Analysis conditions; the Analysis Conditions dialog is displayed.
3. Click Yes to create the file; the Analysis Conditions dialog is displayed:
4. Enter a description in the Description field. Be sure to use an intuitive description so that
you can recognize it easily.
5. Choose whether you wish to have the isotherm collected by target pressures or in dose
increments. Use the push button(s) adjacent to your choice to specify details.
6. Click Preparation to specify evacuation rate and time, and leak test values.
7. Click Free Space to specify how the free space is to be measured.
8. Click pº and T to specify how the saturation pressure (Po) is to be measured and the
analysis bath temperature.
9. Click Equilibraiton to specify the equilibration times for relative pressure ranges.
10. Click Backfill to choose backfill options.
Jul 09 3-9
Adsorptive Properties
Adsorptive properties provide the adsorptive (analysis gas) characteristics for the analysis.
Refer to Adsorptive Properties, page 5-28 for a detailed description of the fields on this
dialog.
1. Select File > Open > Adsorptive properties; the Open Adsorptive Properties dialog is
displayed.
3. Click Yes to create the file; the Adsorptive Properties dialog is displayed:
4. Enter a description in the Adsorptive field; most users enter the gas and the temperature.
5. Enter the mnemonic for the Adsorptive gas; for example, N2.
6. Click Psat vs. T to view or edit the values in the Psat vs. Temperature table.
3-10 Jul 09
7. Select the Non-condensing Adsorptive option if this file is to be used for a non-
condensing gas.
8. Enter information (or accept the defaults) in the following fields:
Maximum manifold pressure

Non-ideality factor
Density conversion factor
Therm. tran. hard-sphere diameter
Molecular cross-sectional area
9. Select the applicable dosing method; choose From Psat tube for krypton and Normal for
all other gases.
Jul 09 3-11
Report Options
Report options files specify the type of reports which can be generated from an analysis or
from manually entered data. They also contain report details such as axis scale, axis range, and
column headings. These report options files may be used to generate reports automatically at
any time during or after the analysis. Of course, reports generated during analysis can only
report on data collected up to the time of the report.
Report options files may contain tabular reports only, plots only, or both tabular reports and
plots. They may also contain user-defined report tables.
Report options files also may be defined to include overlay options. The TriStar program
enables you to overlay up to eight plots of different samples onto a ninth plot of the same type.
Or you can overlay one plot type onto a different plot type from the same analysis. Refer to
Generating Graph Overlays, page 3-35 for instructions on generating overlays.
Refer to Report Options, page 5-31 for a detailed description of the fields on this dialog.
1. Select File > Open > Report Options; the Open Report Options File dialog is displayed.
3. Click Yes to create the file; the Report Options dialog is displayed:
4. Enter a description (up to 42 characters) in the Description field. Enter an identifier that
gives a more intuitive description of the file’s contents. For example, BJH Adsorption
Report Options.
3-12 Jul 09
5. Select Show report title and enter the title you wish to appear at the top of the report.
Deselect this option if you prefer not to have a report title.
If your company logo exists as a bitmap (bmp) or enhanced metafile (emf), you can
have it display in the report header by selecting Show graphic. Click Browse to select
the file; use the Height and Width fields to specify the size.
6. If you wish to compare the same type of graph from multiple files, click Overlays and
choose the files. Then be sure you edit the graph from the Selected Reports window and
choose Samples from the Overlay drop-down list.
7. The reports that may be generated are listed in the Selected Reports list.
a. Double-click on the reports you wish to include in this file; this places a check mark
before them and indicates they are selected.
b. Click Edit to specify report options; be sure the report is highlighted and selected.
Jul 09 3-13
Creating a Sample Information File TriStar II 3020
Creating a Sample Information File

Whether you choose to create your sample file in advance or at the time of analysis, a sample
information file must be created for each analysis. The sample information file consists of
information groups which, collectively, identify the sample, guide the analysis, and specify
report options.
A sample file may be created in any of the sample presentation formats:
• Advanced. This format provides complete access to all parts of the sample file,
allowing you to edit parameters quickly and conveniently.
• Basic. This format presents a single window from which you select predefined
parameter files. You can also switch to the Advanced format if you wish to view or edit
details.
• Restricted. This format presents a single window from which you select predefined
parameter files. You cannot, however, switch to the Advanced format for editing.
Advanced Format
The Advanced format presents all parts of the sample file in an index card manner. This format
lets you customize your sample file, allowing you quick access to all parameters.
Refer to Advanced, page 5-5 for a detailed description of the fields on this dialog.
1. Select File > Open > Sample Information; the Open Sample Information File dialog is
displayed.
2. Accept the next sequenced file number or enter a new name in the File name field.
3. Click OK, then Yes to create the file; the Sample Information dialog is displayed.
3-14 Jul 09
TriStar II 3020 Creating a Sample Information File
These fields may not

display if omitted in
sample defaults.
4. Enter a description in the Sample field, or edit the one established in sample defaults.
5. In the Operator field, enter the name of the person who will be performing the analysis.
6. In the Submitter field, enter the name of the department, company, etc. submitting the
sample for analysis.
7. Select Enter to enter a value for the sample’s mass (if different from the default value), or
Calculate to have the mass calculated automatically. If you select Calculate, you must
enter weights for the Empty tube and the Tube + sample.
8. Enter a value in the Density field (or accept the default). This value is applicable only
when using a calculated free space.
9. Choose whether you are going to use manually entered data or have data collected.
10. Unless you are gathering statistical process control information, it is unnecessary to enter
parameter values. These are user-definable parameters that can be entered and tracked
along with other statistical process control data; refer to Sample Defaults, page 8-8 for
information on user parameters.
11. After you complete the Sample Information dialog, click on the parameter tabs to open
associated dialogs and edit as desired. Instructions for completing these dialogs are
explained in Defining Parameter Files, page 3-6.
12. After you have completed all parameters, click Save, then Close.
Jul 09 3-15
Creating a Sample Information File TriStar II 3020
Basic and Restricted Formats
The Basic and Restricted formats are the easiest and simplest way to create a sample file. You
simply create your sample information file using predefined parameter files (explained in this
chapter beginning on page 3-6). If more detailed conditions or custom files are required, you
must use the Advanced format (explained on page 3-14).
• If you are using the Basic format, you can switch to the Advanced format when editing
is required.
• If you are using the Restricted format, you cannot edit parameter files.
Refer to Basic, page 5-8 for a detailed description of the fields on this dialog.
1. Select File > Open > Sample Information; the Open Sample Information File dialog is
displayed.
2. Accept the next sequenced file number or enter a new name in the File name field.
3. Click OK; then Yes to create the file; the Basic Sample Information dialog is displayed.
The Restricted dialog

does not contain an
Advanced push
button.
4. Enter a description in the Sample field, or edit the one established in sample defaults.
5. Select Enter to enter a value for the sample’s mass (if different from the default value), or
Calculate to have the mass calculated automatically. If you select Calculate, you must
enter weights for the Empty tube and the Tube + sample.
6. Enter a value in the Density field (or accept the default). This value is applicable only
when using a calculated free space.
3-16 Jul 09
TriStar II 3020 Creating a Sample Information File
7. Click on the down arrow to the right of each of the following fields to choose parameter
files:
• Sample tube
• Degas conditions (if using the SmartPrep degasser)
• Report options
If you have an existing sample file containing the values you wish to use for this file,
click Replace All to choose the file and copy the values into the current file.
Jul 09 3-17
Preparing for Analysis TriStar II 3020
Preparing for Analysis

The table shown here outlines the tasks necessary to properly prepare for an analysis, as well
as the location of the procedure for performing the task. It is best to perform the tasks in the
order given in the table.
Task Name and Location
Clean the sample tube Cleaning and Labeling Sample Tubes, page 3-18
Create the sample file Creating a Sample Information File, page 3-14
Weigh your sample Determining the Sample Mass, page 3-21
Degas your sample Degassing the Sample, page 3-23
Load sample on sample port Installing the Sample Tube, page 3-24
Fill Dewar and check LN2 level Installing the Analysis Dewar, page 3-25
Cleaning and Labeling Sample Tubes
Sample tubes and filler rods must be clean and dry before samples are added and weighed. The
following procedures are recommended. Refer to Table 3-1 for a list of materials needed to
clean and weigh samples.
Table 3-1. Materials Required to Clean and Weigh Sample Tubes
Supplied by Micromeritics Supplied by User
Sample tube Drying oven

Filler rod (if used) Ultrasonic cleaning unit
Sample tube brush Detergent
Stopper for sample tube Rubber gloves or lint-free cloth
Sample tube rack Acetone or isopropyl alcohol
Sample weighing support Safety glasses
Sample data worksheet (copied from Waste container
Appendix A of this manual) Analytical balance
Pipe cleaners
1. Turn on the drying oven used for heating the sample tubes and filler rods and set the
temperature to 110 ºC.
2. Check the reservoir of the ultrasonic cleaning unit to make sure it is clean.
3-18 Jul 09
TriStar II 3020 Preparing for Analysis
3. Using 5 grams of Alconox (or other suitable detergent) per 500 mL of warm water, fill the
reservoir of the ultrasonic unit with enough water to cover the sample tubes and filler rods.
Make sure the detergent is dissolved before placing the sample tubes and filler rods into
the water. If too much detergent is used, it may be difficult to rinse from the sample tubes.
4. Fill the sample tubes with warm water and place them in the reservoir of the ultrasonic
cleaning unit. Place the filler rods in the bowl also. Turn on the ultrasonic cleaning unit for
approximately fifteen minutes.
5. Using rubber gloves, remove the sample tubes and filler rods from the reservoir.
6. Clean the interior of the sample tubes with the brush supplied with the TriStar System.
7. Rinse the sample tubes and filler rods thoroughly with hot water, then with isopropyl
alcohol or acetone.
If isopropyl alcohol or acetone is not available, deionized water may be used to rinse
the sample tubes.
Jul 09 3-19
8. Stand the sample tubes on the sample tube rack and place the filler rods in a basket or in
the rack. Bake in a vacuum oven for two hours.
9. Remove the sample tubes and filler rods from the oven and allow them to cool.
Do not insert the filler rods at this time. Filler rods are inserted just before the sample
tube is installed on the analysis port.
10. Wipe a rubber stopper with a lint-free cloth.
11. Label the sample tube and stopper for identification.
3-20 Jul 09
Determining the Sample Mass
Analysis results are expressed in units of surface area per gram of sample; therefore, it is
important the true sample mass be known. The true mass is best calculated as follows:
• Weigh the Sample Tube Set (sample tube and stopper or seal frit) before degas
• Weigh the Sample Tube Set with sample before degas and subtract from the weight of
the Sample Tube Set
• Weigh the Sample Tube Set with sample after degas and subtract from the weight of the
Sample Tube Set
• Weigh the Sample Tube Set with sample after analysis and subtract from the weight of
the Sample Tube Set
For your convenience, a Sample Data Worksheet for recording the weights and calculating
the mass is included in Appendix A. You may make copies as needed.
Make a copy of the Sample Data Worksheet, then proceed with the instructions provided
below.
1. Write the Sample Tube Identification on the Sample Data Worksheet.
2. Place the sample weighing support on the balance. Tare the balance and allow it to
stabilize at zero (0).
3. Place the sample tube set on the sample weighing support, and place it on the balance.
Jul 09 3-21
4. Record the stabilized weight on the Sample Data Worksheet as Mass for empty sample
tube set. Remove the sample weighing support and sample tube set from the balance.
Do not touch the sample with bare hands while performing the following steps. Doing
so could affect the accuracy of results.
5. Place a sample container on the balance; slowly add the desired amount of sample to the
container.
6. Remove the rubber stopper (or seal frit) from the sample tube.
7. Using the sample tube funnel (provided in the accessories kit), pour the sample from the
weighing container into the sample tube.
Funnel
8. Replace the rubber stopper (or seal frit).
9. Weigh the sample tube set containing the sample; record the value on the Sample Data
Worksheet as Sample tube set plus sample mass (Before Degas).
10. Subtract the Mass for empty sample tube set from the Mass of sample tube set plus sample;
record this value as the Sample mass (Before Degas).
3-22 Jul 09
Degassing the Sample
After the sample has been weighed, use a degassing unit to remove any contaminants which
may have adsorbed to the surface or pores of your sample. Appropriate degassing units are
available from Micromeritics. Refer to Ordering Information, page 10-1 for ordering
information.
If you are using the SmartPrep degasser, a menu will display on the menu bar of the TriStar
application. You can degas your sample using commands on this menu and information you
enter in the Degas Conditions dialog. Refer to the SmartPrep operator’s manual for operating
instructions.
After degassing is complete, perform the following steps:
1. Weigh the sample tube set containing the sample; record the weight on the Sample Data
Worksheet as Sample tube set plus sample mass (After Degas).
2. Subtract the Mass for empty sample tube set (Before Degas) from the Sample tube set plus
sample mass (After Degas) to obtain the sample’s mass; record this value as Sample mass
(After Degas).
Jul 09 3-23
Installing the Sample Tube
To attach a sample tube to a port, follow the steps below.
1. Remove the sample tube stopper.
2. If using a filler rod: hold the sample tube horizontally and carefully slide the filler rod into
the tube.
Do not hold the rod vertically and drop the rod into the tube; this could break the rod
and/or the tube.
3. If using an isothermal jacket, slide the jacket down over the stem of the sample tube until
it touches the bulb of the sample tube.
4. Insert the Po tube into the center hole of the Dewar cover and slide the cover up; make
sure the tapered side of the cover is facing downward.
5. Insert the sample tube through one of the holes in the cover.
O-ring
Ferrrule
Connector Nut
Dewar Cover
6. Place the connector nut, ferrule, and O-ring onto the sample tube stem.
7. Attach the sample tube to the analysis port. Make sure it is fully in the port; secure in place
by screwing the connector nut onto the analysis port. Hand-tighten the connector nut.
8. Slide the Dewar cover upward until it stops.
3-24 Jul 09
Installing the Analysis Dewar
Prepare the analysis Dewar after you have installed the sample tube(s),
Always handle Dewars with care. Any product incorporating a vacuum is a potential
safety hazard and should be treated with caution. Always observe the precautions
listed below.
We recommend the following be observed when handling Dewars containing liquefied gases:
• Protect yourself by wearing 1) goggles (or a face shield), 2) an insulated or rubber

apron, and 3) insulated gloves.
• When pouring liquefied gases from one container to another: 1) cool the receiving
container gradually to minimize thermal shock, 2) pour the liquefied gas slowly to
prevent splashing, and 3) vent the receiving container to the atmosphere.
• Use a plastic stirring rod when stirring substances in a Dewar containing liquefied gases
(or other materials of extremely low temperature). Do not use a glass or metal stirring
rod unless it is coated with some type of protective coating.
• Do not remove the mesh covering from the Dewar flask. This covering is in place so
that you can maintain a secure grip on the Dewar.
• Do not handle heavy objects above the Dewar. If unavoidable, place a protective cover
over the Dewar’s opening. If an object of sufficient weight is accidentally dropped into
the Dewar, shattering may occur.
Install the analysis Dewar as follows:
1. Place the analysis Dewar onto the elevator.
2. Fill the Dewar with the analysis bath liquid (liquid nitrogen) to about 5 cm (2 in.) from the
top.
Incorrect fluid levels can lead to measurement errors. You should check the level of
the bath liquid before each analysis.
3. Insert the dipstick into the Dewar and check the level of the analysis bath liquid.
Condensation should not exceed the Level Indicator mark.
Jul 09 3-25
Level indicator mark

Wetness or frozen
condensation indicates
bath liquid level
4. Allow approximately 30 minutes (for best results) for the temperature of the Dewar to
stabilize with that of the bath liquid. Then recheck the level of the bath liquid; add
additional liquid if necessary.
It is not necessary to allow time for stabilization unless the Dewar has not been in use
for a while.
5. Close the sample compartment door.
3-26 Jul 09
TriStar II 3020 Performing an Analysis
Performing an Analysis
After the sample has been degassed and transferred to the analysis port, you may begin analy-
sis. The TriStar provides two types of analyses from which you may choose:
• Standard - allows you to perform up to three analyses using different analysis

conditions.
• QuickStart - allows you to perform multiple sample analyses using the same analysis
conditions.
Standard Analysis
Refer to Sample Analysis, page 6-3 for a detailed description of the fields on this dialog.
1. Select Unit > Sample analysis; the Analysis dialog is displayed.
2. Click Browse to choose a sample information file to be used for each port you plan to use.
3. The sample identification, sample mass, and sample density contained in the sample
information file are displayed. Verify the sample mass and density. The density value is
applicable only if you are using the Calculate method for the free-space determination.
4. The Po and bath temperature are displayed; these values may be edited if desired.
Jul 09 3-27
Performing an Analysis TriStar II 3020
5. Select Report after analysis to have reports generated automatically when the analysis
completes. Be sure to designate the destination if you choose this option.
6. Click Export after analysis to have isotherm data exported automatically when the
anlaysis completes.
7. Click Start to start the analysis; an analyzing view of the window is displayed so that you
can view data as it is collected. A short delay is encountered before the port status changes
from the Idle state.
8. After the analysis is finished, remove the sample tube and dispose of the sample
accordingly.
Use caution when removing the sample tube if a hanging filler rod is being used. The
sample tube O-ring or Dewar cover may snag the filler rod retaining ring. Loosen the
snag gently; excessive force may break the tip of the filler rod.
3-28 Jul 09
TriStar II 3020 Performing an Analysis
QuickStart Analysis
It is not necessary to prepare sample files in advance when using the QuickStart method. Sam-
ple files are assigned automatically and given default conditions. You can replace file contents
if desired on the second view of the QuickStart dialog.
Refer to QuickStart, page 6-8 for a detailed description of the fields on this dialog.
1. Select Unit > QuickStart analysis; the following dialog is displayed.
2. Enter an identifier for this series of samples.
3. Enter the operator’s name in the Operator field.
4. Select Report After Analysis if you wish to have reports generated automatically after
the analyses. Be sure to specify a destination if you choose this option.
5. Click Export after analysis to have isotherm data exported automatically as analyses are
completed.
6. Click Next; the following dialog is displayed.
Jul 09 3-29
Performing an Analysis TriStar II 3020
File names are assigned automatically and given default conditions. Click Replace All
adjacent to the Sample field if you wish to replace parameter values with those of another
file.
7. Be sure the ports you are using in the analyses are selected.
8. Enter the sample’s mass and density for each port. The density is only applicable if you are
using Calculate as the free-space method.
9. Ensure that the Po value and bath temperature are correct; edit if needed.
10. Click Start to start the analysis; the following actions occur:
• A view of the data collection as it progresses is displayed. A short delay is encountered

before the port status changes from the Downloading state. If desired, you can obtain a
report on the data collected so far by selecting the appropriate Report Port [n] push
button; the report is printed to the screen.
• When the analysis finishes, the first view of the QuickStart dialog is displayed.
11. Repeat steps 5 through 9 to perform additional analyses or click Close to close the
QuickStart dialog.
12. After the analysis is finished, remove the sample tube and dispose of the sample
accordingly.
Use caution when removing the sample tube if a hanging filler rod is being used. The
sample tube O-ring or Dewar cover may snag the filler rod retaining ring. Loosen the
snag gently; excessive force may break the tip of the filler rod.
3-30 Jul 09
TriStar II 3020 Printing File Contents
Printing File Contents

Using the Print command on the File menu, you can print the contents of one or more sample
or parameter files.
Refer to Print, page 5-94 for a detailed description of the fields on this dialog.
1. Select File > Print > (file type); a dialog similar to this one is displayed.
Choose the
destination.
Choose the file(s)

you wish to print.
Click to complete
the printing process.
2. From the Files list, select the file(s) you wish to print. If you plan to print multiple files,
hold down Ctrl while selecting the files.
3. At the Destination field, click the down arrow and choose a destination for file output.
• Printer; the Copies field is enabled allowing you to print up to four copies. Output goes
to the printer specified as the default printer.
• File; the File name field is enabled allowing you to enter a name for the file, or you can
accept the default.
Jul 09 3-31
Printing File Contents TriStar II 3020
4. Click OK, the contents of the requested file(s) is(are) sent to the selected destination; this
example shows a sample information file printed to the Screen.
Header
Close: closes the dialog
Print: prints the report to the default printer
Header: toggles the header on and off
Prev and Next: enabled when the report contains multiple pages allowing you to advance
to other pages
3-32 Jul 09
TriStar II 3020 Listing File Statistics
Listing File Statistics

You can generate a list of the following information on one or more sample or parameter
files:
• File name
• Date the file was created (or last edited)
• Time the file was created (or last edited)
• File identification
• Status
Refer to List, page 5-95 for a detailed description of the fields on this dialog.
1. Select File > List> (file type); a dialog similar to this one is displayed.
Choose the
destination.
Choose the file you

wish to print.
Click to complete
the operation.
2. From the Files list, choose the desired file(s). If you wish to include all files in the list,
leave all files deselected.
3. At the Destination field, click the down arrow and choose a destination for file output.
• Printer; the Copies field is enabled allowing you to print up to four copies. Output goes
to the printer specified as the default printer.
• File; the File name field is enabled allowing you to enter a name for the file, or you can
accept the default.
4. Click OK, a list for the requested file(s) is sent to the specified destination.
Jul 09 3-33
Exporting Isotherm Data TriStar II 3020
Exporting Isotherm Data

Export allows you to copy the isotherm data in a sample information file and export it as
ASCII text. If saved to a File, the data can be imported into applications such as spreadsheets.
The output file consists of four columns containing the elapsed time, absolute pressure, rela-
tive pressure, and specific volume adsorbed.
Refer to Export, page 5-96 for a detailed description of the fields on this dialog.
1. Select File > Export; the Sample Information File Export dialog is displayed.
2. From the Files list box, select the file(s) you wish to export. If you plan to export multiple
files, hold down Ctrl while selecting the desired files.
3. In the Settings group box, choose a Destination for your exported file.
a. If you choose File as the destination, select the file type. Then enter a name in the File
name field or accept the default. If you have selected multiple files, individual files are
exported as their file name. You can also change the destination path if desired.
b. If you choose Printer, the Copies field is enabled; you can print up to four copies.
4. Click OK; the file is exported to the specified destination.
3-34 Jul 09
TriStar II 3020 Generating Graph Overlays
Generating Graph Overlays

Use the graph overlay function when you wish to compare graphically multiple graph options.
Graphical lines are differentiated by the use of varying symbols and reported in a legend on
the report. Overlays may be generated in two ways:
• Multiple Sample Overlays

Overlay up to eight plots of the same type with that of the current plot
• Multiple Graph Overlays

Overlay two different types of plots from one sample. This type of overlay is available
only for
BJH Adsorption/Desorption
DFT Pore Size/Surface Energy
Dollimore-Heal Adsorption/Desorption
Horvath-Kawazoe
M-P Method
You must use the Advanced format for generating overlays. Select Options > Options pre-
sentation > Advanced to access the Advanced mode, or click the Advanced push button on
the Basic Sample Information dialog.
Multiple Sample Overlays
To overlay the same type of graph on multiple samples:
1. Select File > Open > Sample Information to display the Open Sample Information File
dialog.
2. Select a sample on which to overlay graphs of other samples, then click OK; the Sample
Information dialog is displayed.
3. Click the Report Options tab to display the Report Options dialog.
Jul 09 3-35
Generating Graph Overlays TriStar II 3020
4. Choose the type of report from the Selected Reports window; then click Edit.
5. Choose the type of report for which you wish to generate overlays, click Edit, and perform
the steps listed for that report:
If you are overlaying this

type of report.... Then ....
Isotherm Select the desired plot(s) from the Select Reports group
box.
Click Options (becomes enabled when the plot is
selected) adjacent to the selected plot
Select the Overlay samples check box, then click OK.
Click OK again to return to the Report Options dialog..
BET Surface Area Select the Overlay Samples check box.
Langmuir Surface Area
Click OK.
Freundlich
Temkin
t-Plot
Alpha-S
f-Ratio
3-36 Jul 09
If you are overlaying this

type of report.... Then ....
BJH Adsorption Choose the report variable from the Selected Reports
BJH Desorption window, then click Edit.
Dollimore-Heal Adsorption
Click on the down arrow at the Overlay field and choose
Dollimore-Heal Desorption
Samples; then click OK.
MP-Method
Click OK again to close the report variable’s dialog and
return to the Report Options dialog.
6. From the Report Options dialog, click Overlays; the Graph Overlays Samples dialog is
displaed.
7. Click Browse to the right of the Sample [n] field; the Plot Overlay Sample Selection
dialog is displayed.
8. Choose the file containing the graph you wish to overlay, then click OK. You may choose
up to eight files in this manner.
9. After selecting your files, click OK to return to the Report Options dialog.
10. Click Save if you wish to save your selections; you can still generate the overlays even if
you do not wish to save them.
11. Select Reports > Start report; the Start Report dialog with the name of your edited file
highlighted is displayed.
12. Click OK; the Select Reports dialog is displayed.
13. Ensure that the desired graph is selected, then click OK .
Jul 09 3-37
Generating Graph Overlays TriStar II 3020
Multiple Graph Overlays
Multiple graph overlays can only be generated for:
• BJH Adsorption
• BJH Desorption
• DFT Pore Size
• DFT Surface Energy
• Dollimore-Heal Adsorption
• Dollimore-Heal Desorption
• Horvath-Kawazoe
• MP-Method
1. Select File > Open > Sample Information to display the Open Sample Information File
dialog.
2. Select the desired file, then click OK; the Sample Information dialog is displayed.
3. Click the Report Options tab to access the Report Options dialog.
4. Select the type of report on which you wish to have overlays generated; this example
shows BJH Adsorption.
3-38 Jul 09
5. Highlight BJH Adsorption and click Edit; the BJH Adsorption dialog is displayed.
Select the report

variable.
Click to choose the

second report variable.
6. From the Selected Reports window, select the report variable on which you wish to have
another variable overlaid, then click Edit. A dialog similar to this one is displayed.
Displays the first report

variable.
Choose the second variable

from this drop-down list.
7. From the Overlay drop-down list, choose the report variable you wish to overlay, then
click OK.
8. Click OK again to return to the Report Options dialog.
9. Click Save if you wish to save your selections; you can still generate the overlays even if
you do not wish to save them.
10. Select Reports > Start report; the Start Report dialog with the name of your edited file
highlighted is displayed.
11. Click OK; the Select Reports dialog is displayed.
12. Ensure that the desired graph is selected, then click OK.
Jul 09 3-39
TriStar II 3020 Installing the Software
4. SOFTWARE AND SETUP MODIFICATIONS
This chapter provides instructions for:
• Installing the software, beginning on this page

• Using the Setup Program for Other Functions, page 4-6
You can also install the TriStar program for offline data manipulation on a computer other than
the one controlling the analyzer. This allows you to:
• create or edit sample and parameter files

• generate reports on completed sample files
Review the Micromeritics PROGRAM License Agreement for restrictions on the use of
another copy of the analysis program.
Installing the Software

Be sure you have completed the following tasks before installing the software for the first
time.
• Configure the ethernet port the analyzer will use (refer to Configuring the Ethernet
Port, page E-1)
• Disable the firewall setting for the connection between your computer and analyzer
(refer to Configuring the Firewall Setting, page E-7)
• Connect the analyzer to the configured port and turn the analyzer on.
If installing multiple analyzers, connect the ethernet switch to the configured port and
the analyzers to the ethernet switch (refer to Ethernet Switch, page 4-9); turn the
analyzers on.
Install the program as follows:
1. Select Start > Run from the Windows menu bar.
2. Enter the name of the drive designator, followed by analyzersetup.
For example: e:analyzersetup.
Mar 08 4-1
Installing the Software TriStar II 3020
3. Click OK; the Ethernet Introduction dialog is displayed. This screen outlines the steps
that should be completed before installing the software.
If all of the steps have not been completed, click Cancel and perform the steps; then
restart the installation program. Do not proceed with installation until these tasks have
been completed.
4. Click OK; the New Installation dialog is displayed.
The Destination Folder group box displays the amount of current disk space required for
the analysis program, and the directory into which the application will be installed. If you
prefer a different directory for installation, click Browse to select the desired directory.
4-2 Mar 08
The TriStar application should not be installed on a network drive with shared access.
Multiple users cannot operate the application at the same time.
5. Select the check box just below the Destination Folder group box to add an icon to your
desktop; this enables quick access to the analysis program.
6. The TriStar icon is added to the Micromeritics folder by default. If you prefer a different
folder, enter or select one from the drop-down list.
7. The Install this application for All Users check box enables you to allow or prohibit
users other than the installer to access the application.
• Select the check box to allow access for all users logged onto Windows.
• Deselect the check box to allow access for only the user installing the application.
8. Click Next; the Analyzer configuration dialog is displayed.
Mar 08 4-3
Installing the Software TriStar II 3020
a. In the Step 1 group box:
If .... Then ....

you are installing the select the number of analyzers you are installing.
analysis program at
initial installation:
you plan to use the select 0
analysis program for
offline data reduction:
you are moving an select 0 (Refer to Moving an Analyzer from One Com-
analyzer from another puter to Another Computer, page 4-11.)
computer to this one:
b. In the Step 2 group box, enter the serial number(s) for the analyzer(s) you are
attaching to this computer.
9. Click Next; the Ethernet Ports dialog is displayed.
10. Choose one of the following:
If .... Then ....

the port you configured select the port and proceed to the next step.
is listed:
the port you plan to use Click Specify, the Specify Ethernet Port dialog is displayed.
has been configured but Enter the remaining portion of the IP address in the enabled
is not listed: fields, then proceed to the next step.
4-4 Mar 08
11. Click Next; the calibration files are installed.
If you are installing more than one analyzer, the Calibration File Installation dialog
instructing you how to proceed with installation of other calibration files is displayed.
Read the instructions carefully; they are restated here.
a. Remove this setup CD.
b. Insert the CD containing the files for the analyzer serial number requested.
IMPORTANT: To prevent the CD from AutoPlay, hold down the Shift key before
you close the CD door. Do not release the Shift key until the CD light stops blinking.
c. When the CD lights ceases to blink, click Next. After the calibration files are installed,
you will be prompted to reinsert the original setup CD.
The application software is installed after installation of all calibration files.
12. The Installation Complete dialog containing the Readme file will display when
installation is complete. This dialog may also contain other important notices. After
reading the information contained in this dialog, click Finish to close it.
13. Choose one:
If .... Then ....

you are installing the analysis Return to the Installation Instructions menu and con-
program with regard to the tinue with the next procedure.
installation video:
you are installing the analysis Remove the program CD and store in a secure loca-
program independent of the tion. The original program CD contains calibration
installation video and have no files specific to your instrument. Upgrade CDs do not
other operations to perform: contain calibration files. Therefore, it is important that
you maintain your original program CD in a secure
location in the event calibration files need to be
reinstalled.
Mar 08 4-5
Using the Setup Program for Other Functions TriStar II 3020
Using the Setup Program for Other Functions

After initial installation of the analysis program, the application setup program can be used to:
• install software upgrades, page 4-8

• add an analyzer, page 4-9
• move an analyzer from one computer to another computer, page 4-11
• change the analyzer setup (port configuration), page 4-17
• remove an analyzer from the computer, page 4-16
• reinstall calibration files, page 4-19
• uninstall the analysis program, page 4-20
To start the application setup program:
1. Ensure that the analysis program is not operating and the analyzer is idle.
2. Insert the CD into your CD-ROM drive; after a few seconds the menu for the TriStar
installation instructions is displayed.
If Autorun is not enabled on your computer, proceed to Step 4.
Click here to
close the
menu.
3. Click X in the upper right-hand corner to close the installation menu.
4. Select Start from the Status bar, then Run from the start menu.
4-6 Mar 08
TriStar II 3020 Using the Setup Program for Other Functions
5. Enter the drive designator of the CD-ROM drive, followed by setup. For example:
e:setup
Alternatively, you can click Browse, navigate to the CD-ROM drive, and select
setup.exe.
6. Click OK; the setup Welcome screen showing the options available is displayed.
Options
available for
the TriStar
program are
enabled.
7. Select the operation you wish to perform. Procedures for performing each operation are
in subsequent sections.
After the requested operation is completed, the setup Welcome screen is again displayed.
A confirmation message indicating completion of the operation is shown in the lower
section of the dialog.
Indicates status
of last operation
performed.
Mar 08 4-7
8. After you have completed all desired operations, click Exit to close the Welcome screen.
9. Remove the CD and store in a secure location.
Installing Subsequent Software Versions
When you install a software upgrade, the system installs all of the application files and any sta-
tus files that do not already exist on the computer. Existing analyzer status files are not
affected and default and data files are not overwritten. There are three types of subsequent
installation; the software version controlled by the setup program is:
• a later version than the version installed on the computer

• the same version as the version installed on the computer
• an earlier version than the version installed on the computer
The setup program automatically detects which type of installation applies and customizes the
selection in the Setup dialog accordingly.
1. Start the Setup program (refer to Using the Setup Program for Other Functions, page
4-6).
2. Choose the software option; remember, only the applicable option will display:
• Upgrade software to version (number) from version (number)

• Reinstall software version (number)
• Downgrade software to version (number) from version (number)
3. Click Start File Installation; the application installs the software and displays the setup
Welcome dialog.
4-8 Mar 08
Adding an Analyzer
An ethernet switch is required when connecting multiple analyzers. After connecting the eth-
ernet switch, continue with the software section.
Ethernet Switch
An Ethernet switch with a straight-through cable is required when installing multiple

analyzers.
1. Connect the power cord of the Ethernet switch to an appropriate power outlet.
2. Disconnect the ethernet cable of the current analyzer from the computer; do not
disconnect it from the analyzer.
3. Connect one end of the straight-through cable to the Ethernet switch and the other end to
the computer.
4. Connect the ethernet cable of the current analyzer to a numbered port on the Ethernet
switch (do not use the uplink port).
5. Connect one end of the Ethernet cable (for the analyzer you are adding) to the connector
labeled Ethernet on the rear panel of the analyzer and the other end to a numbered port
on the Ethernet switch. Repeat this step for each analyzer you are adding.
The finished configuration should look like the following illustration.
Ethernet switch Be sure cables are not

connected to the uplink port.
6. Turn on the analyzer that was added. Also ensure that the computer and current analyzer
are on.
Mar 08 4-9
Software
1. Insert the analysis program CD for the analyzer you are adding into the CD-ROM drive.
2. Start the Setup program (refer to Using the Setup Program for Other Functions, page
4-6).
3. Select Add an analyzer, then click Next; the Set up analyzer being added dialog is
displayed.
You may see the Ethernet Introduction screen. This information is not applicable since
you are connecting to an ethernet switch which is connected to a port that has been
configured. Click OK to close the screen and proceed.
4. Enter the serial number of the analyzer being added.
5. Click Next; the calibration files are installed and the Welcome screen is displayed.
4-10 Mar 08
Moving an Analyzer from One Computer to Another Computer
Use the instructions in this section to move a configured analyzer (along with its status, cali-
bration, and log file) from one computer (Source PC) to a different computer (Destination
PC). This operation does not move sample or parameter files. Use a file management program
such as Explorer or a backup/restore utility to move these types of files.
Moving a Configured Analyzer to a New Computer
This section provides steps for moving a configured analyzer to a computer that does not have
an analyzer installed.
If the analysis program is already installed on the destination computer, begin with
Step 2.
1. Install the analysis program on the destination computer (refer to Installing the
Software, page 4-1). Be sure to select 0 as the number of instruments on the Analyzer
Configuration screen; all related instrument information will be transferred in the Move
operation.
2. Start the application setup program on the source computer (refer to Using the Setup
Program for Other Functions, page 4-6).
3. Select Move an analyzer from one PC to another PC, then click Next; the Move
analyzer operation dialog is displayed.
Mar 08 4-11
4. Select Source PC, then click Next; the following dialog is displayed.
5. From the drop-down list in the Step 1 group box, select the analyzer that is to be moved
from this computer.
6. In the Step 2 group box, click Browse to select a location for storing the status,
calibration, and log files associated with the source computer. If possible, the location
should be a shared network drive. If this is not possible, select a local folder and then use
a transfer utility to copy its contents from the Source PC to the Destination PC.
Sample and parameter files are not copied and moved with the analyzer. Use a file
management program such as Explorer or a backup/restore utility to move these files.
7. Click Next; the files are copied to the specified location and the setup Welcome screen is
displayed.
8. Start the Setup program on the destination computer.
9. Select Move an analyzer from one PC to another PC; the Move analyzer operation
dialog is displayed (shown on previous page).
4-12 Mar 08
10. Select Destination PC, then click Next; the Ethernet Introduction screen is displayed.
This screen outlines the steps that should be completed to configure the ethernet port to
which the analyzer is connected to on the computer.
If these tasks have not been completed, click Cancel and complete them; then restart the
setup program. Do not proceed until the ethernet port in the computer has been
configured.
11. Click OK; the Move analyzer information dialog to this PC dialog is displayed.
12. In the Step 1 group box, enter the serial number of the unit you are moving to this
computer.
13. In the Step 2 group box, click Browse to choose the location of the files that were stored
previously from the Source computer.
Mar 08 4-13
14. Click Next; the files are transferred and the Ethernet Ports dialog is displayed.
Select the desired ethernet port.
15. Click Next; the setup Welcome screen is displayed.
16. Turn on the analyzer and start the analysis program.
4-14 Mar 08
Moving a Configured Analyzer to a Computer with an Existing Analyzer
This section provides steps for moving a configured analyzer to a computer that already has
the analysis program and a configured analyzer installed, this being the second analyzer. When
installing two analyzers on one computer, additional hardware is required. Refer to Adding an
Analyzer, page 4-9.
1. Perform Steps 2 through 7 (steps for Source computer) of the procedure Moving an
Analyzer from One Computer to Another Computer, page 4-11.
2. Disconnect the Ethernet cable of the analyzer from the Source computer (or Ethernet
switch). Reconnect the cable to the Ethernet switch for the Destination computer. You
must use a switch when attaching multiple analyzers. Refer to Ethernet Switch, page 4-9
for configuring ethernet connections using a switch.
3. After ethernet connections have been established, return to page 4-12 and begin with Step
8 (steps for Destination computer). You will not see the Ethernet Ports dialog (Step 13)
since an ethernet port has already been assigned.
4. Turn on both analyzers and start the analysis program.
Mar 08 4-15
Removing an Analyzer
You can remove an analyzer from the computer as follows. When you remove an analyzer, the
status files are removed as well.
1. Start the Setup program. Refer to Using the Setup Program for Other Functions, page
4-6.
2. Select Remove an analyzer, then click Next; the Remove an analyzer dialog is
displayed.
3. From the drop-down list, choose the serial number of the analyzer you wish to remove.
This operation removes the selected instrument from the list of attached instruments.
It does not remove calibration and status files associated with the analyzer, nor does it
remove sample and parameter data files.
4. Click Remove; the analyzer is removed and the Welcome screen is displayed.
4-16 Mar 08
Changing the Analyzer Setup Configuration
This option allows you to change the ethernet port being used by the analyzer(s). For example
if the current ethernet port malfunctions, you would use this option to move the analyzer to
another ethernet port.
Be sure that the ethernet port you are switching to has been configured and the firewall setting
between the computer and the analyzer is turned off. Refer to Configuring the Ethernet Port,
page E-1 and Configuring the Firewall Setting, page E-7.
4-6.
2. Select Change analyzer setup, then click Next; the Ethernet Introduction screen is
displayed. This screen outlines the steps that should be completed to configure the
ethernet port to which the analyzer will be connected.
If these tasks have not been completed, click Cancel and complete them; then restart the
setup program. Do not proceed until the ethernet port in the computer has been
configured.
Mar 08 4-17
3. Click OK; the Ethernet Ports dialog is displayed.
If .... Then ....

the port you plan to select the port and proceed to the next step.
use is listed:
the port you plan to Click Specify, the Specify Ethernet Port dialog is
use has been config- displayed.
ured but is not listed: Enter the remaining portion of the IP address in the
enabled fields, then proceed to the next step.
5. Click Next; the change is completed and the Welcome screen is displayed.
4-18 Mar 08
Reinstalling Calibration Files
Calibration files specific to the analyzer are contained on the original program CD; they are
not contained on an update CD. It is important that you store your original program CD in a
safe location. CDs containing calibration files will always end with a suffix of 99. Update CDs
end with a suffix of 00.
Reinstall calibration files as follows:
1. Using the CD containing the appropriate calibration files, start the Setup program. Refer
to Using the Setup Program for Other Functions, page 4-6.
2. Select Re-install calibration files for an analyzer, then click Next:
If .... Then ....

you have only one the calibration files are installed and the Welcome screen
analyzer installed is displayed.
you have multiple ana- select the appropriate analyzer, then click Next; the cali-
lyzers installed, a bration files are installed and the Welcome screen is
dialog enabling you to displayed.
choose the desired
analyzer is displayed.
Mar 08 4-19
Uninstalling the Analysis Program
You can remove the analysis program as follows. When you perform this operation, the appli-
cation removes the analysis program, status files, analyzer setup files, and resulting empty
directories. It does not remove data files.
4-6.
2. Select Uninstall, then click Next; the Uninstall dialog is displayed.
3. Click Uninstall; the Select Uninstall Method dialog is displayed.
4-20 Mar 08
• Automatic: click Next; the system uninstalls the software automatically and the setup
Welcome dialog is displayed.
• Custom: click Next; a series of dialogs is displayed, allowing you to choose the files
you wish to uninstall. After all files are selected and uninstalled, the setup Welcome
Mar 08 4-21
TriStar II 3020 Description
5. FILE MENU
The File menu contains options which allow you to manage sample and parameter files.
Description
Listed below are brief descriptions of the File menu options. Detailed descriptions follow this
section.\
Open Opens an existing sample or parameter file, or enables you to create a

new one. Page 5-3.
Save Saves the file in the active window. Page 5-91.
Save As Saves the file in the active window as a different name. You also can
use this option to save a subset of the sample file as a parameter file.
Page 5-91.
Save All Saves all open files. Page 5-93.
Close Closes the file in the active window. Page 5-93.
Close All Closes all open files. Page 5-93.
Print Prints the contents of a sample or parameter file. Page 5-94.
Mar 09 5-1
Description TriStar II 3020
List Generates a list of certain information for sample or parameter files.

Page 5-95.
Export Exports the isotherm data contained in a sample file. Page 5-96.
Exit Exits the analysis program. Page 5-99.
5-2 Mar 09
TriStar II 3020 Open
Open
Open enables you to open an existing sample information or parameter file, or to create a new
one.
Regardless of which file type you select, a dialog similar to the one shown here is displayed.
Does not display for

parameter files.
File name For sample information files, this field contains the next
sequenced file name generated by the analysis program.
For parameter files, the file name displayed includes an

asterisk (*) and a default extension as follows:
*.STB for sample tubes

*.DEG for degas conditions
*.ANC for analysis conditions
*.ADP for adsorptive properties
*.RPO for report options
If you are creating a new file, enter a name in the File name
field. If you are editing an existing file, select a file from the
list.
Refer to Selecting Files, page 2-11 for a description of the other fields on this dialog.
Mar 09 5-3
Open TriStar II 3020
Sample Information
Sample information files contain information used to control the analysis. Therefore, every
analysis must be linked with a sample information file before the analysis can proceed. A
sample information file is comprised of the following:
• Sample identification
• Sample tube parameters
• Degas conditions (if using automatic degassing)
• Report options
• Entered or collected (appears after analysis is complete) data
Parts of the sample information file can also exist as parameter files which are separate from
the sample information file itself. Having these files exist independently allows you to use
them as many times as you wish. For example, if you typically use the same analysis condi-
tions for many of your analyses, you can create an analysis conditions file containing those
conditions. Then when you create your sample file, select that file for your analysis conditions.
Once it becomes part of the new sample file, you can edit it in any way you wish without
changing the file from which it was copied.
Sample information files are presented in three formats: Advanced, Basic and Restricted.
Specify or change your format by selecting Options > Option presentation.
• Advanced
Presents all parts of the sample information file in a single, index card tabbed dialog.
• Basic
Presents the entire sample information file in a single dialog.
• Restricted
Presents the sample information file in a single dialog similar to the Basic format with
certain functions disabled.
5-4 Mar 09
Advanced
When you open an existing sample information file or create a new one using the Advanced
format, all parts of the sample file are displayed in a tabbed dialog. The Advanced format
allows you to customize sample files. Refer to Advanced Format, page 3-14 for step-by-step
instructions for creating an Advanced sample information file.
A Collected Data tab

displays here when
analysis is complete.
An Entered Data tab

displays if you choose
Manually entered
allowing you to enter
the data.
The prompts for the Sample, Operator, Submitter, and Bar Code fields may be customized
by selecting Options > Sample defaults. Refer to Sample Defaults, page 8-6 for instructions
on customizing these prompts.
Sample Displays the default file description or the description of the

file you are opening. You may enter a new description or edit
the existing one.
You can use up to 50 alphanumeric characters.
Operator Enter the name of the operator who will be performing the
Submitter analysis and the name of the person (or department)
submitting the sample for analysis.
You may use up to 40 alphanumeric characters
Mar 09 5-5
Bar Code This field enables you to enter bar code information. If bar
code information is not used, you can use this field to enter
additional information about the sample; for example, you
may wish to enter the lot number of your sample.
This field will also accept data from a bar code reader.
Mass You can enter a sample mass or have the mass calculated
automatically.
Enter Enables the Sample Mass field allowing you to enter a value.
Calculate Enables the Empty tube and Sample + tube fields, allowing
you to enter appropriate values. These values are used to cal-
culate the mass of the sample,
Mass sample = Mass sample + tube – Mass tube
Density This value is used only for the Calculated free-space

method; it is ignored for other methods.
Use 0.000 for a blank analysis.
Type of Data Choose whether data are to be collected automatically by the

analysis program or manually entered.
If you choose Manually entered, an “Entered” tab is added

so that you may enter the desired data. You cannot enter data
if you are creating the file on a computer that is not attached
to the analyzer.
User Parameters These fields are used primarily for SPC (Statistical Process
Control) reporting. However, they can be used for other data
as well. You may wish to enter specific analysis conditions
or sample criteria. These parameters print on the Options
report. Select Options > Sample Defaults to specify the
parameters you wish to report. The parameter(s) you specify
replace the User Parameter label(s).
If desired, you can have these fields omitted from the sample
information file (refer to Sample Defaults, page 8-6).
5-6 Mar 09
Add Log Entry Displays the Add Log Entry dialog.
Enter information pertinent to the sample file. For example, if

you are not using the SmartPrep for automatic degassing, you
may wish to enter external degassing information. Any
information you enter here is printed as part of the sample log
report. You may make multiple entries by selecting this push
button as many times as you wish.
Replace All Allows you to copy an existing sample file’s values into the
sample information file you are creating. A dialog is
displayed so that you may select the desired file. Click OK;
the values are copied into the new file automatically. You
may edit the values in the new file; the file from which they
were copied remains unchanged. This replaces all parameters
of the entire sample information file, excluding any collected
data.
Each of the individual tabbed dialogs contains a Replace push button if you wish only
to replace specific parameters and not the entire file contents.
Comments Enter comments about the sample or its analysis conditions.

Comments entered here are printed in the header of the
reports.
Save Saves the information you have specified for this sample file.
Close Closes the dialog. If changes have been made in the dialog
and have not been saved, you will be prompted to save before
the dialog closes.
Basic Displays the sample information file in the basic format.
Mar 09 5-7
Basic
When you open an existing sample information file or create a new one using the Basic for-
mat, all parts of that file are contained on a single dialog. With the Basic format, you can
quickly create a sample information file using previously defined parameter files. This format
also allows you to switch to the Advanced format to view or edit parameters. Refer to Basic
and Restricted Formats, page 3-16 for step-by-step instructions for creating a Basic sample
information file.
Sample Displays the default file description (new files) or the

description in the file you are opening. You may enter a new
description or edit the existing one.
You may use up to 50 alphanumeric characters.
Mass You can enter a sample mass or have the mass calculated
automatically.
Enter Enables the Sample Mass field allowing you to enter a value.
you to enter appropriate values. These values are used to cal-
culate the mass of the sample,
5-8 Mar 09
Density Enter the density of the sample to be analyzed. This value is

used only for the Calculated free-space method; it is ignored
for other methods.
Use 0.000 when performing a blank analysis.
Sample Tube The drop-down lists for these fields contain previously
Degas Conditions defined files; those included with the analysis program as
Analysis Conditions well as any you may have created specifically for your
Adsorptive Properties laboratory.
Report Options
Degas Conditions files are pertinent only if you are using the
SmartPrep for degassing samples.
Add Log Entry Displays a dialog so that you may enter pertinent information
relating to the sample file. For example, if you are not using
automatic degassing, you may wish to enter external
degassing information. Any information you enter here is
printed as part of the sample log report. You may make
multiple entries by selecting this push button as many times
as you wish.
Replace All Alllows you to copy the values from all parameters of an
existing sample file into the one you are creating. A dialog is
were copied remains unchanged.
Save Saves the information you have specified for this sample file.
Close Closes the dialog. If a file containing unsaved changes is

open, you are prompted to save before the dialog closes.
Advanced Displays the sample information file in the advanced format,

allowing you to view or edit parameters.
Mar 09 5-9
Restricted
A third format is provided to control access to some portions of the sample information file.
The Restricted format displays in the same manner as the Basic presentation format.
This format displays in the

same manner as the Basic
format; however, it does not
allow you to switch to the
Advanced format.
The fields on this dialog are identical to the ones on the Basic Information dialog except that
this dialog does not contain an Advanced push button allowing you to switch to the
Advanced format. This format is also password-protected, preventing the operator from
making changes to file parameters. Refer to Restricted, page 8-5 for additional information
on the Restricted format.
Restricted presentation is ideal for laboratories in which standard analysis procedures are
established by a lab manager, while one or more lab technicians actually perform the analyses.
The lab manager can create independent parameters files containing standard sets of operating
conditions, then the operator(s) can use Restricted mode for daily operations, selecting the
standard parameter files from the drop-down lists.
5-10 Mar 09
Sample Tube
This dialog allows you to store sample tube information. Before creating a Sample Tube file,
you should perform a blank analysis (no sample) using the sample tube.
A sample tube file can be created as an independent parameter file or as part of the sample
information file.
Be sure to save this file to the directory you specified as the Parameter files directory
if it is to be included in the drop-down list on the Basic and Restricted Sample
Information dialogs (see Parameter Directory in Chapter 8).
Sample Tube Contains the description of the current file.
If this is a new file, this field contains the description you

specified as the default. You can enter a new description or
add to the existing one if desired.
Replace Use this push button to replace the values of the current file
with those from an existing file. The Open Sample Tube
dialog is displayed, allowing you to choose a file. After the
values are copied into the current file, you can edit them as
desired.
Warm free space Displays the warm free space for the current file.
Cold free space Displays the cold free space for the current file.
Mar 09 5-11
Non-ideality factor Displays the non-ideality factor determined during the blank
analysis.
Use isothermal jacket Select this option if an isothermal jacket is to be used in the
analysis.
An isothermal jacket is used to maintain a constant

temperature profile along the sample tube stem during an
extended analysis (more than 1 or 2 hours).
Use filler rod Select this option if a filler rod is to be used in the sample
tube.
A filler rod is used to reduce the stem free-space volume,

resulting in reduction of free-space error.
Vacuum seal type If the sample tube is to be transferred under vacuum to the
analysis port, select the seal type to be used. If not, leave
None selected.
Load From Sample File Click this push button to choose the sample file that was used
in the blank analysis. The data for the Warm and Cold free
spaces, the port volume, and the non-ideality factor will be
copied into the sample tube file.
5-12 Mar 09
Degas Conditions
This dialog is used when using the SmartPrep Degasser for degassing your sample. If you are
not using the SmartPrep, you can use the dialog to record information used with a different
degassing unit.
Information dialogs (see Parameter Directory in Chapter 8).
Description If you are opening an existing file, this field contains the
description.
If this is a new file, enter a description; at least one character

is required.
Replace Allows you to copy the values of an existing degas conditions

file into the file you have open. A dialog is displayed so that
you may select the desired file. Click OK; the values are
copied into the new file automatically. You may edit the
values in the new file; the file from which they were copied
remains unchanged.
Conditions Table Allows you to enter up to five stages of degas conditions
Mar 09 5-13
Soak Temperature Enter the temperature at which the sample is to soak while
flowing gas.
Ramp Rate Enter the rate at which the temperature is to change when
advancing to the soak temperature.
Soak Time Enter the amount of time to soak the sample.
Insert Inserts a row into the conditions table. A row is inserted

above the selected line; the cursor moves to the new line.
Delete Deletes the selected row from the conditions table.
Clear Clears all the table of all but one entry; one entry is required.
The rows do not have to be selected.
5-14 Mar 09
Analysis Conditions
This dialog is used to specify the analysis conditions for your sample. An analysis conditions
file can be created as an independent parameter file or as part of the sample information file.
Information dialogs (see Parameter Files Directory, page 8-15).
Description If you are opening an existing file, this field contains the
description.
If you are creating a new file, enter a description; at least one

character is required.
Replace Allows you to replace the values in the current analysis

conditions file with those from an existing file. A dialog is
the values are copied into the new file automatically.
Isotherm Collection The choices in this group box allow you to specify how you
wish to have isotherms collected.
Mar 09 5-15
Target Pressures Select this option to have isotherms collected by specifying

target pressures. When you select this option, Pressures and
Options (directly to the right of this field) become enabled.
Select each push button to verify or edit data.
Pressures Displays the Entered Pressures dialog.
Edit the existing pressure table or clear the table and enter a
new pressure table.
A pressure table is a table of relative pressure points (and

possibly calculation assignments) at which data (isotherms)
are to be collected. The relative pressures may span the entire
range of 0.00000001 to 0.995 P/Po. There must be one
adsorption branch followed optionally by one desorption
branch.
Several analysis conditions files containing complete pres-

sure tables are included with the TriStar software. These files
(and all other parameter files) can be edited. If you want to
use any of these files, it is recommended that you use the
Save As option on the File menu to save the file as a different
name; then make your changes.
5-16 Mar 09
Pressures The pressure table for automatically collected data includes

the pressure points for data collection and (when Use calcu-
(continued) lation assignments is selected) identifies calculations
through which the data are processed.
Insert Range
Displays the Insert Pressure Range dialog.
This dialog allows you to specify the starting pressure, the

ending pressure, the number of points to insert within the
specified range, and whether you wish to have linear or geo-
metric progression.
Choose Linear to insert evenly spaced points into your table.
Choose Geometric from low pressure to insert geometri-

cally spaced points from the low pressure range. For
example, if you wish to insert 5 points with a 0.01 starting
pressure and a 0.16 ending pressure, the following points are
inserted into the table:
0.01
0.02
0.04
0.08
0.16
Mar 09 5-17
Pressures Choose Geometric towards saturation to insert geometri-

cally spaced points from the saturation pressure. For
(continued) example, if you wish to insert 5 points with a 0.99 starting
pressure and a 0.84 ending pressure, the following points are
inserted into the table:
0.99
0.98
0.96
0.92
0.84
Insert Predefined
Displays the Insert Predefined Pressures dialog.
Choose predefined pressure points for surface area, t-Plot

micropore and/or BJH adsorption/desorption.
Click on the down arrow of each field to choose the desired

set of points. You can also specify Adsorption/desorption
total pore volume and saturation.
Insert
Inserts a row into the pressure table. A row is inserted above
the selected line; the cursor moves to the new line.
Delete
Deletes the selected row.
Clear
Clears all entries from the table. The rows do not have to be
selected.
5-18 Mar 09
Options Allows you to specify target pressure options; the Target

Pressure Options dialog is displayed.
First Pressure Fixed Dose

Select this option to have the sample dosed with a specified
amount of gas until the first pressure point is reached. This
initial dosing quickly meets the adsorptive demand of the
sample.
The first point on the pressure table is the threshold value.

Once this first pressure point is reached, points are equili-
brated and recorded in accordance with the specified pressure
table.
You may wish to use this mode if you are performing a stan-
dard nitrogen analysis of microporous or highly mesoporous
materials such as catalysts. If the first pressure table point is
low, and you expect the gas uptake of the sample to be high,
choosing this mode can shorten the time required to reach the
first point on the pressure table.
Maximum volume increment

Select this option to specify when additional data points are
to be collected between target pressures in regions of high
adsorption. When the maximum increment has been adsorbed
since the last collected data point, another point is equili-
brated and collected.
When using this option, reaching pressure points exactly is

not important; therefore, the tolerances should be set
relatively large (10 mmHg and 10% or so) for proper
functioning of the algorithm. The pressure table should also
have several points scattered over the region of interest.
During desorption, this field is treated as a maximum volume

“decrement” value.
Mar 09 5-19
Options Absolute pressure tolerance

Relative pressure tolerance
(continued)
These values are used to determine how close the actual
pressure must be to each target pressure from the pressure
table. At lower pressures the relative tolerance value is lower,
and at higher pressures the absolute tolerance value is lower.
For example:
Experiment 1: you have an absolute tolerance of 5 mmHg, a

relative tolerance of 5%, and a target pressure of 40 mmHg;
5% of 40 mmHg is 2 mmHg. Since 2 mmHg (relative toler-
ance) is lower than 5 mmHg (absolute tolerance), 2 mmHg is
used. Therefore a minimum pressure of 38 mmHg (40 - 2)
must be attained to collect data for a target pressure of 40
mmHg.
Experiment 2: you have an absolute tolerance of 5 mmHg, a

relative tolerance of 5%, and a target pressure of 200 mmHg;
5% of 200 mmHg is 10 mmHg. Since 5 mmHg (absolute tol-
erance) is lower than 10 mmHg (relative tolerance), 5 mmHg
is used. Therefore a minimum pressure of 195 mmHg (200 -
5) must be attained to collect data for a target pressure of 200
mmHg.
Normally, surface area measurement points are widely

spaced, and the resulting measurement is not very sensitive to
the precise location of points so wider tolerances may be
used. Unnecessarily tight tolerances lengthen the analysis.
Dose Increments In this form of dosing, there is no predefined pressure table.

The sample is dosed repeatedly with a fixed amount of gas
and isotherm points are collected after equilibrating each
dose. Each entry in the table defines how much to dose for a
segment of the isotherm.
5-20 Mar 09
Options Displays the Dose Increments dialog.
Insert or edit target ranges for up to 10 dose increments.
The current specified dose increments are displayed. The

ending relative pressure and the dose amount (entered or as
the fraction of the previous volume adsorbed) for each target
range are shown.
Insert Displays the Dose Increment Edit dialog.

Edit
Ending pressure
Enter the desired ending pressure of this segment.
Dose increment
Select this option to have the sample dosed with a specified
amount of gas for each isotherm point taken.
Mar 09 5-21
Insert Percent of previous

Edit Select this option to have the sample dosed with a percentage
of the volume adsorbed during the previous interval of the
(continued)
table. For example if in the previous segment 5 cm3 STP of
gas was adsorbed and you enter 40% in this field, this seg-
ment will dose 2 cm3 STP for each isotherm point taken.
This feature is disabled for the first entry of the dose

increment table.
Delete Deletes the selected range.
Clear Clears the table of all entries except one; one entry is
required.
Absolute pressure Select this option to specify pressure targets in mmHg, mbar,
dosing or kPa instead of relative pressure. This option is typically
selected when using adsorptives at analysis conditions above
the critical point of the gas; for example, H2 adsorption on
carbon at liquid nitrogen temperature.
Preparation Displays the Analysis Preparation dialog.
Fast evacuation Select this option for samples (such as pellets) that do not
fluidize or shed particles during evacuation.
Evacuation rate These fields are enabled when Fast evacuation is not
Unrestricted evac. from desired, allowing you to enter an evacuation rate and the
pressure at which unrestricted sample evacuation is to begin.
5-22 Mar 09
Evacuation time Enables you to enter the length of time for preliminary
evacuation, which takes place prior to the free-space
measurement.
Leak test Enables the system to check for system leaks or sample
outgassing before the analysis.
The leak test seals the sample tube and monitors the pressure.
If the pressure rises more than 0.15 mmHg, the analysis does
not proceed and you are notified with a message. While leak
testing slightly increases analysis time, it prevents the
continuation of analysis and collection of erroneous data if a
leak exists.
When you select this option, the Leak test duration field is
enabled so that you can specify how long the pressure is to be
monitored.
Use TranSeal Select this option if you are using the TranSeal to transfer the
sample from the preparation port to the analysis port under
vacuum.
Free Space Displays the Free Space dialog, allowing you to specify the
type of free-space measurement you wish to use.
Refer to Appendix D, page D-1 for a discussion of free-space

methods.
Mar 09 5-23
Measure Measures the free space automatically over the sample prior
to data collection.
Lower Dewar for evacuation

Lowers the Dewar during evacuation.
Evacuation time
Enter the time you wish to allow for evacuation after the free-
space measurement.
Outgas test
Checks the system for sample outgassing after the free-space
measurement. The outgas test seals the sample tube and mon-
itors the pressure. If the pressure rises more than 0.025
mmHg within the time specified in the Outgas test duration
field, outgassing is present. If outgassing is found, the test
repeats up to nine times with a 30-minute evacuation time
between each test. If the 10th test fails, the analysis does not
proceed and you are notified of its cancellation. Outgas test-
ing slightly increases analysis time, but it prevents
continuation of analysis and collection of erroneous data if
outgassing is present.
Enter Enables the Warm free space and Cold free space fields so
that you may enter the free space manually.
The warm free space is the sample tube gas capacity mea-
sured at room temperature.
The cold free space is the sample tube gas capacity measured
with the Dewar raised.
Calculate Select this option to have the free-space measurement

calculated using the sample and tube parameters.
If you choose this option for a tube in which there is no

sample, be sure to enter 0 in the Density field.
5-24 Mar 09
pº and T Displays the pº and Temperature Options dialog.
This dialog provides six options for obtaining the saturation

pressure (pº) and analysis bath temperature. Clicking on each
option prompts you for the entry of related parameters in the
lower portion of the dialog.
Option Prompts for...

1 the analysis bath temperature.
This method measures the pº on a continuous basis;

enabling you to measure every data point without
slowing down the analysis.
2 an analysis bath temperature.
This method measures the pº on a continuous basis

and over the sample, then adjusts the measured pº in
the sample tube to agree with the pº over the
sample.
3 a pº and analysis bath temperature, or
an analysis bath temperature only (when Absolute

pressure dosing is selected on the Analysis condi-
tions dialog).
This method uses the values you enter in the fields.
Mar 09 5-25
Option Prompts for...

4 a psat gas.
If this is a Krypton analysis, be sure to select the

Krypton @ 77.35 K SOLID option from the drop-
down list.
Click Psat vs T to edit the values of the Psat vs T

table if desired. Editing the values in the current
table does not affect the ones of the original table.
5 an analysis bath temperature and an estimate for the
initial pº.
This method measures the pº over the sample. After

the pº is measured, the value is reapplied to all data
points.
6 an analysis bath temperature.
This method calculates the pº at the time of analysis

using the temperature you enter.
Options 1, 2, and 5 cannot be used for krypton analyses.
If you have selected From Psat tube (for krypton analysis)

on the analysis dialog and a pº option other than 3, 4, or 6
was selected , an error message is displayed when you
attempt to start the analysis.
Equilibration Displays the Equilibration dialog.
Does not
display when
Absolute
dosing is
selected.
5-26 Mar 09
Relative Pressure The relative pressure for which the equilibration interval will
(P/Po) be applied.
Equilibration The number of seconds between successive pressure readings

interval during equilibration. At least 11 pressure readings for each
equilibration are required to obtain an accurate reading of the
pressure changes.
• Long equilibration intervals tend to lengthen analyses,

but improve data integrity.
• Short equilibration intervals produce a faster analysis but

may reduce the accuracy of data.
Minimum The value entered in this field determines the minimum

equilibration delay number of seconds required before equilibration can occur
at P/Po> = 0.995 for a relative pressure greater than or equal to 0.995.
This field does not display if you select Absolute pressure

dosing on the analysis conditions dialog.
Backfill Displays the Sample Backfill Options dialog, allowing you to

select options for backfilling the sample tube at the start and
end of an analysis.
Mar 09 5-27
Adsorptive Properties
This dialog allows you to specify the characteristics of the gases used in the TriStar system. An
Adsorptive properties file can be created as an independent parameter file or as part of the
sample information file.
Adsorptive If this is a new file, this field contains the name of the default
adsorptive gas. Enter a description for the adsorptive gas for
which you are creating the file.
Mnemonic The mnemonic name for the adsorptive gas; for example, N2
for nitrogen, CO2 for carbon dioxide, etc.
Non-condensing Select this option if this file is for a non-condensing gas

Adsorptive (adsorptive). You must also select the Absolute pressure
dosing option on the Analysis Conditions dialog when you
select Non-condensing Adsorptive.
When you select this option, the Density conversion factor

field and the Psat vs. T push button become disabled.
5-28 Mar 09
Maximum manifold The maximum gas pressure allowed in the manifold.

pressure
Non-ideality factor Enter a factor to compensate for the forces of attraction

between molecules in a real gas.
Density conversion Enter the density conversion factor. The density conversion
factor factor is determined by obtaining the ratio of the gas volume
(STP) to the liquid volume.
Therm. tran. hard-sphere The thermal transpiration hard-sphere diameter.

diameter
Molecular The molecular cross-sectional area.

cross-sectional area
Replace Allows you to replace the values in the current adsorptive

properties file with those from another file. A dialog is
were copied remains unchanged.
Psat vs. T Displays the Psat vs. Temperature dialog for the adsorptive
gas; this example shows for Nitrogen.
This table contains saturation pressures and their correspond-

ing temperatures. The table may include as many as ten
entries; at least two are required.
Mar 09 5-29
Psat vs. T Edit the table by moving the cursor to the desired saturation
pressure or temperature and entering a different value. Points
(continued) always have to be in an ascending order. If you try to add a
point which is less than the previous one, you will receive an
error message.
Insert Inserts a new row. A row is inserted above the selected line;
the cursor moves to the new line.
Delete Deletes the selected row.
Dosing Method Select the manner in which the sample tube is dosed.
Select From Psat tube for krypton.
Select Normal for all other gases.
5-30 Mar 09
Report Options
This dialog allows you to specify report options for a new file or to edit an existing one. A
report options file can be created as an independent parameter file or as part of the sample
information file.
Description If you are editing an existing file, this field displays a

description of the report options file. You may change the
name if you wish.
If this is a new file, the default report options description is

displayed. Enter a name for this file.
Mar 09 5-31
Show report title Enables you to enter a title for your report.
If this is a new file, the title you specified as the default is dis-
played. You can accept the default title or enter a new one.
You can enter up to 50 alphanumeric characters.
If you deselect this option, a title will not display on the

report.
Show graphic Select this option to have a graphic display above the report
title. The graphic can be in a bitmap (bmp) or an enhanced
metafile (emf) format. For example, you may wish to display
your company logo.
Click Browse to choose the graphic, then use the Height and
Width fields to specify a size. This image can be edited from
the report window.
Replace Allows you to replace the values in the current report options
file with those from an existing file. A dialog is displayed so
that you may select the desired file. Click OK; the values are
copied into the new file automatically. You may edit the
values in the new file; the file from which they were copied
remains unchanged.
5-32 Mar 09
Overlays Displays the Graph Overlay Samples dialog.
Choose the sample files you wish to overlay onto selected

plots.
Click Browse to the right of the Sample [n] field to choose a

file. You may select up to eight files. Use the Clear push but-
ton to clear the field of its entry.
After choosing your file(s), be sure to select the Overlay

samples option for each report type you plan to overlay.
Refer to Generating Graph Overlays, page 3-35 for instruc-
tions on generating overlays.
Apply thermal Select this option to correct for the temperature-induced

transpiration correction pressure difference between the manifold and the chilled
sample tube. This option is most significant for pressures less
than approximately 1.0 mmHg. Never use filler rods in the
sample tube when applying correction for thermal
transpiration.
Always use thermal transpiration when performing

micropore analyses.
Inside diameter of Enabled when you select Apply thermal transpiration

sample tube correction, so that you may enter the inside diameter of the
sample tube.
Mar 09 5-33
Selected Reports Contains a list of available reports:
• Summary
• Isotherm
• BET Surface Area
• Langmuir Surface Area
• Freundlich
• Temkin
• t-Plot
• Alpha-S Method
• f-Ratio Method
• BJH Adsorption
• BJH Desorption
• Dollimore-Heal Adsorption
• Dollimore-Heal Desorptioin
• Horvath-Kawazoe
• DFT Pore Size
• DFT Surface Energy
• Dubinin
• MP-Method
• Options
• Sample Log
• Validation
Refer to Selecting Reports, page 2-13 for information on

selecting reports.
Edit Displays an associated dialog for the selected report. Editing

options for available reports are shown in subsequent
sections.
You cannot edit the Options and Sample Log reports.
5-34 Mar 09
Summary Report
The summary report provides a condensed listing of selected data results. Click Edit for Sum-
mary report options; the Summary Report Options dialog is displayed.
The choices on this dialog allow you to choose the types of data to include in the Summary
report.
If you choose Adsorption or Desorption total for Pore Volume data, the P/Po field is enabled
so that you can enter the relative pressure at which to calculate the total pore volume. If Use
calculation assignments (Collected Data screen) is not selected, the isotherm is interpolated
to this value and that point used for the Total pore volume calculation. Otherwise, the point
selected with calculation assignment is used.
This dialog also enables you to specify Pass/Fail criteria for up to four parameters.
Select All Selects all choices on the dialog.
Deselect All Deselects all choices on the dialog.
Mar 09 5-35
Pass/Fail Selection Displays the parameter you selected on the Pass/Fail Options
dialog.
Pass/Fail Displays the Pass/Fail Optioins dialog so that you can choose
a parameter on which to specify pass/fail criteria.
Upper/Lower Select these options to specify upper and lower limits for the
selected parameter; a valid range for the selected field is
displayed in the information bar.
You can leave the range open by deselecting one of the limits.
For example; if you wish to leave the upper limit open,
deselect the Upper check box and specify a value only for
the Lower limit.
Each of these fields has a message line in which you can

enter advice to the operator if a failure occurs. You may enter
up to 120 characters in each field.
5-36 Mar 09
Isotherm Report Options
The isotherm report indicates adsorption (up to saturation pressure) and desorption (down
from saturation pressure) of a gas by a solid held at constant temperature.
Select Reports Lists the types of reports offered.
Choices: Tabular Report, Linear plot, Logarithmic plot,

Linear Absolute plot, Logarithmic Absolute plot
Pressure Composition plot
Options Displays the related Plot Options dialog; this example shows
the dialog for the Linear plot.
All plot dialogs contain the same options.
You can plot the graphs as a curve, points, or both.
Mar 09 5-37
Options Select Overlay samples to overlay data from the current plot
with data from other samples. The other sample files are
(continued) selected by clicking Overlays on the Report Options dialog.
Autoscale options enable you to have the X- and/or Y-axes

automatically scaled.
Linear X-axes begin at zero, and logarithmic X-axes begin at

an appropriate value. Y-axes begin at zero. The system uses
the highest values collected during analysis as the ending
points for axes ranges.
If you choose not to autoscale data, the From and To fields

are enabled, allowing you to specify a range. Data collected
outside these ranges are not included in the plot.
The value entered in the To field must be greater than the

value entered in the From field.
The X-axis fields show the relative pressure.The Y-axis fields

show the quantity of gas adsorbed
Tabular Options Enables you to have Run Time and/or Time Between Points
reported. Run time reports the time elapsed from the
beginning of the analysis to the finish. Time between points
reports the time relapsed between each point.
Also enables you to report Weight % when plotting pressure

composition.
Plot Options Enables you to choose the type of isotherm you wish to plot.
You can plot the adsorption and/or the desorption isotherm.
Volume Adsorbed Enables you to choose the manner in which the volume
adsorbed is reported. These data are reported by default as
Per Gram (cm3/g). However, you can choose to report data
Per BET Surface Area (cm3/m2) or Per Other Surface
Area (m2/g). If the latter field is selected, a field is enabled
allowing you to enter a value.
Weight The Adsorbate Molecular Weight field is enabled when you

choose Pressure Composition plot, allowing you to enter the
molecular weight of the adsorbate.
This plot is useful for plotting pressure as a function of

Weight % adsorbed; for example, H2 adsorbed on carbon.
5-38 Mar 09
BET/Langmuir Surface Area Report Options
• The BET calculation obtains the sample surface area value by determining the
monolayer volume of adsorbed gas from the isotherm data. Refer to BET Surface
Area, page C-7 for additional information.
• The Langmuir calculation determines the surface area of a sample by relating the
surface area to the volume of gas adsorbed as a monolayer. Refer to Langmuir Surface
Area, page C-9 for additional information.
The Langmuir and BET Surface Area dialogs include the same fields; the operating instruc-
tions for both are the same.
Displays as Langmuir
Surface Area Report
Options if the Langmuir
report is being edited.
Tabular report Select this option to have a tabular report of the plotted data.
BET (or Langmuir) Generates a traditional BET (Langmuir) surface area plot that
Transform plot is used to determine monolayer volume and BET C constant.
BET (or Langmuir) Uses the BET (Langmuir) monolayer volume and constant to
Isotherm plot produce an isotherm.
Overlay samples Allows you to overlay data of the selected type from the
current plot with data from other samples. The other samples
are selected by clicking Overlays on the Report Options
screen.
Mar 09 5-39
Autoscale x-axis Select these options to have the X- and/or Y-axes scaled
Autoscale y-axis automatically.
Both X- and Y-axes begin at zero; the system uses the highest
values collected during analysis as the ending points. If you
choose not to autoscale data, the From and To fields are
enabled, allowing you to enter the ranges.
The X-Axis Range fields show the relative pressure.
The Y-Axis Range fields show the quantity of gas adsorbed.
From/To fields Enabled when you choose not to autoscale data (deselect the
Autoscale option), allowing you to specify the beginning and
ending ranges of the X- and/or Y-axis. Data collected outside
these ranges are not included in the plot. The values entered
in the To field must be greater than the value entered in the
From field.
Pressures Displays the Report Relative Pressure Table dialog so that

you may edit or enter relative pressure points.
Does not display

for Langmuir.
• If Use calculation assignments is not selected on the

collected/Entered dialog, the isotherm is interpolated to
these pressure points, and those interpolated values are
used in the BET calculations.
• If Use calculation assignments is selected, collected

data are used.
5-40 Mar 09
Insert Predefined Displays the Surface Area Report Pressure Selection dialog,
allowing you to select predefined points.
Choices: None, 1 Point, 3 Point, 5 Point,

5 Point Low Pressure
Does not display for the Langmuir report.
Insert Inserts a row into the table above the selected line; the cursor
moves to the new line.
Clear Removes all but the one required entry from the table. The
rows do not have to be selected. A warning message request-
ing confirmation is displayed before the table is cleared.
Mar 09 5-41
Freundlich Report Options
The Freundlich isotherm is an empirical isotherm that is used to model low-pressure adsorp-
tion data. It can also be applied to model some micropore isotherms.
Refer to Freundlich Isotherm, page C-38 for information on report calculations.
Specify monolayer In this field, enter the monolayer capacity of the sample.
capacity
Absolute pressure range Allows you to enter a pressure range when calculation
assignments are not requested.
Tabular report Select this option to have a tabular report of the pressure
points generated.
Transform plot Plots the log(p) vs log(Q) in a straight line.
5-42 Mar 09
Isotherm plot Plots the absolute pressure vs quantity adsorbed. Shows best
fit line.
Overlay samples Choose this option to overlay Freundlich isotherm data from
the current file with the same type of data from other samples
(files). The desired files are chosen by clicking Overlays on
the Report Options dialog.
Autoscale x-axis Select these options to have the X- and/or Y-axis scaled
values collected during analysis as the ending points.
are enabled, allowing you to enter the ranges.
The X-axis shows the log of absolute pressure and the Y-axis
shows the quantity of gas adsorbed.
these ranges are not included in the plot.
Mar 09 5-43
Temkin Isotherm
The Temkin isotherm is used to model adsorption data where the heat of adsorption drops lin-
early with increasing coverage.
Refer to Temkin Isotherm, page C-39 for information on report calculations.
Specify monolayer In this field, enter the monolayer capacity of the sample.
capacity
Specify differential Enter the differential heat of adsorption at zero surface

heat of adsorption at coverage. This allows inclusion of all Temkin constants.
zero surface coverage
Absolute pressure Allows you to enter a pressure range when calculation

range assignments are not requested.
Tabular report Select this option to have a tabular report of the pressure
points generated
5-44 Mar 09
Transform plot Plots a linear form of the Temkin isotherm.
Temkin Isotherm plot Overlays the Temkin isotherm with the analysis data.
Overlay samples Choose this option to overlay Temkin isotherm data from the
current file with the same type of data from other samples
(files). The desired files are chosen by selecting Overlays on
the Report Options dialog.
Autoscale x-axis Select these options to have the X- and/or Y-axis scaled
The X-axis shows the natural log of absolute pressure and the
Y-axis shows the quantity of gas adsorbed.

Mar 09 5-45
t-Plot Report Options
The t-Plot calculation allows quantitative analysis of the area and total volume ascribed to
micropores. Matrix area, the area external to micropores, is directly determined and often
proves to be a valuable way of characterizing complex mixed materials.
Refer to t-Plot, page C-10 for information on report calculations.
Thickness Curve Presents the type of thickness curves available.
• Reference
• Kruk-Jaroniec-Sayari
• Halsey
• Harkins and Jura
• Broekhoff-de Boer
• Carbon Black STSA
You can also apply the Frenkel-Halsey-Hill thickness curve

using the Halsey option, and entering the appropriate values
in the equation. Use Edit to edit the values in the equation.
Edit Displays the equation for the type of thickness curve selected
so that you may view or edit the values.
5-46 Mar 09
Reference Displays the Entered t-Curve dialog allowing you to define a

t-curve by entering the relative pressure and thickness values.
This table can also be created in another application if desired

and imported into this dialog using Open. When creating the
table in another application, the file must be saved as ASCII
text with a THK extension. Use a two-column format with
the relative pressures in the first column and the thickness
values in the second column. Columns must be separated by a
space (or a tab).
Open
Allows you to import the values from an existing thickness
curve (THK) into this table. One predefined curve is shipped
with the analysis program and is found in the Referenc
directory. The Referenc directory is defaulted when you
select this push button.
After the values are copied into the table, you may edit them
if desired. Editing these values will not affect the file from
which they were copied.
Save As
Enables you to save the current table of values as a thickness
curve. After the table is saved you can use Open to import
the values (see above)
Clear
Clears the table of all but one entry; one entry is required
Mar 09 5-47
Kruk-Jaroniec-Sayari Displays the Kruk-Jaroniec-Sayari Thickness Equation

dialog.
The values shown in the above dialog are the defaults; you
can edit them if desired.
Halsey Displays the Halsey Thickness Equation dialog.
The Halsey method is sometimes referred to as Frenkel-

Halsey-Hill. The values shown in the above dialog are the
defaults; you can edit them if desired.
Refer to t-Plot, page C-10 for more information.
5-48 Mar 09
Harkins and Jura Displays the Harkins and Jura Thickness Equation dialog.
You can edit the values for the numerator, first element of the
denominator, and exponent.
Broekhoff-de Boer Displays the Broekhoff-de Boer Thickness Equation dialog.
You can edit the values for the multiplier, numerator, and
exponent.
Carbon Black STSA Displays the Carbon Black STSA Thickness Equation dialog.
All coefficients can be edited.
Mar 09 5-49
Surface Area group box Allows you to choose the surface area value used for
thickness calculations. You can use BET (most commonly
used), Langmuir, or enter one of preference.
Pressure Range Displays the Report Relative Pressure Range dialog so that
you may specify minimum and maximum relative pressures
to use with this report.

Collected/Entered dialog, all of the nonoutlier points of
the collected data within the specified range are used for
calculating the data for this report.

data points which are assigned to this report type are
used.
Fitted Thickness Range Provides two fields, allowing you to enter the minimum and
maximum thicknesses you wish to include in the thickness
curve.
The values entered for the thicknesses can be expressed in

angstroms or nanometers. Select Options > Units to specify
desired units.
Surface area correction This value corrects for surface areas that are not smooth and
factor brings the values for BET surface area and micropore surface
area into accordance. For most samples, the default value of
1.000 is adequate.
Tabular report Select this option to have a tabular report generated.
t-Plot Select this option to have a graphical representation of data.
5-50 Mar 09
Overlay samples Allows you to overlay data from the current sample file with
data from other sample file(s). The other sample file(s) are
chosen by clicking Overlays on the Report Options screen.

The value entered in the To field must be greater than the

value entered in the From field.
The X-Axis Range fields show the relative pressure
Mar 09 5-51
Alpha-S Plot
The Alpha-S plot converts the standard adsorption isotherm into a dimensionless isotherm
using the quantity adsorbed at a relative pressure of 0.4.
Table Provides two columns for entering the relative pressure (first
column) and the alpha-s values (second column).
This table can also be created in another application if desired

and imported into this dialog using Open. When creating the
table in another application, the file must be saved as ASCII
text with an ALS extension. Use a two-column format with
the relative pressures in the first column and the alpha-s
values in the second column. Columns must be separated by a
space (or a tab).
Insert Inserts a row above the selected row. A row cannot be

inserted if the value in the selected row is at its lowest value;
values must be strictly increasing. For example, in the table
shown above, the default value is 0.000000001. Therefore
you must use Ctrl + Down arrow to insert rows.
5-52 Mar 09
Clear Clears the table of all but one entry; one entry is required.
Open Allows you to import the values from an existing alpha-s

curve (ALS) into the table. One predefined curve is shipped
with the analysis program and is located in the Referenc
directory. The Referenc directory is defaulted when you click
this push button. After the values are copied into the table,
you may edit them if desired. Editing these values will not
affect the file from which they were copied.
Save As Enables you to save the current table of values under a file
name.
Fitted alpha-S Range Provides two fields for entering the minimum and maximum
relative pressures from which the fit will be determined.
Ref. surface area Enables you to enter the surface area from the reference
curve. This value is used to calculate the sample surface area.
Relative pressure range Provides two fields for entering a pressure range when
calculation assignments are not used.
Tabular report Choose this option to have a tabular report generated
Alpha-S Plot Choose this option to have the data plotted as a graph.
data from other sample files. The other sample files are
chosen by clicking Overlays on the main Report Options
screen.

Mar 09 5-53
these ranges are not included in the plot. The value entered in
the To field must be greater than the value entered in the
From field.
The X-Axis Range fields show the relative pressure.
5-54 Mar 09
f-Ratio Plot
The f-Ratio report allows you to take the measured isotherm and normalize it using a reference
isotherm.
Reference Isotherm Displays the sample file you choose as a reference. You
should always choose a file containing an isotherm measured
from a non-porous sample of the same material as the current
sample.
Browse Click to choose the sample file you wish to use as a reference
for the isotherm.
Relative pressure range Allows you to enter a pressure range when calculations
assignments are not used.
Tabular report Choose this option to have a tabular report generated The
tabular report contains four columns: relative pressure,
quantity adsorbed for the isotherm of interest, quantity
adsorbed for the reference isotherm, and the ratio of the
quantities adsorbed.
f-Plot Choose this option to have the data plotted as a graph.
Mar 09 5-55
data from other sample files. The other sample files are
chosen by clicking Overlays on the Report Options screen.

From/To fields Enabled when you choose not to autoscale the axis, allowing
you to enter a range.
5-56 Mar 09
BJH Adsorption/Desorption Report Options
The BJH calculation determines the mesopore volume/area distribution which accounts for
both the change in adsorbate layer thickness and the liquid condensed in pore cores. You can
generate BJH reports from both adsorption and desorption data.
Or BJH Desorption
Report Options
Does not display

on the Desorption
dialog.
The BJH Adsorption and Desorption dialogs include the same fields; the operating
instructions for both are the same.
Thickness Curve Presents the type of thickness curves available.
• Reference
• Kruk-Jaroniec-Sayari
• Halsey
• Harkins and Jura
• Broekhoff-de Boer
• Carbon Black STSA
The choices in this group box allow you to choose the type
of thickness curve you wish to use; you can also edit values
in the equation, if desired.
An incomplete pore distribution may be generated if you select a thickness curve

which is not a good match for the sample being analyzed.
Mar 09 5-57
Edit Displays the equation for the type of thickness curve selected.
Refer to t-Plot Report Options, page 5-46 for an explanation
of the dialogs associated with this push button.
Minimum BJH Enter the minimum diameter (radius or width) of pores you
(diameter, radius, wish to have included in the BJH reports. The value entered
or width) in this field must be less than the value entered in the
Maximum BJH field.
Maximum BJH Enter the maximum diameter (radius or width) of pores you
(diameter, radius, wish to have included in the BJH reports. The value entered
or width) in this field must be greater than the value entered in the
Minimum BJH field.
Fraction of pores open During adsorption calculations, the software assumes that all
at both ends pores are closed at one end. Sometimes a percentage of pores
may be open at both ends, causing disagreement in the
adsorption and desorption data or in the values for total vol-
ume and total BJH pore volume. In this field, you may enter
the fraction of pores open at both ends to compensate for this
error.
This field is not shown on the BJH Desorption Report

Options dialog.
Adsorptive Displays the BJH Adsorptive Options dialog.
The recommended adsorptives and their values are shown.

You may specify up to six additional adsorptive/adsorbate
property factor combinations.
5-58 Mar 09
Adsorptive The adsorbate property factor is the combination of constants

in the numerator of the BJH equation which is specific to the
(continued) type of gas used. Adsorbate property factors may be specified
in angstroms or nanometers. Select Options > Units to
specify units.
Smooth differentials Smooths all differential calculations, eliminating variations

in the differential computation caused by noise in the input
data.
Cumulative Reports Select Larger to report the total volume found in pores larger
than the current pore size. This is the traditional way in which
BJH data are displayed.
Select Smaller to report the total volume found in pores

smaller than the current pore size.
you may enter the range of pressures to use with this report.

Collected/Entered dialog, all of the non-outlier points of
calculating the data for this report

used.
Selected Reports Contains a list of available BJH reports:
• Tabular Report
• Cumulative Pore volume
• dV/d* Pore Volume
• dV/dlog(*) Pore volume
• Cumulative Pore Area
• dA/d* Pore Area
• dA/dlog(*) Pore Area
* = width, radius, or diameter
You can measure pore width (w), pore radius (R), or pore
diameter (D) for BJH reports. Select Options > Units to
choose the desired measurement.
Mar 09 5-59
Selected Reports Choose a report by double-clicking on the report name or

highlight the report name and press the Spacebar. A report is
(continued) selected when it is preceded with a check mark. Reports are
deselected in the same manner.
Edit Allows you to edit the selected report. Editing options for
available reports are shown in the following sections.
Tabular Report
Click Edit for the BJH Adsorption/Desorption tabular report to specify the method of data
reduction; the BJH Adsorption (or Desorption) Tabular Report Options dialog is displayed.
Fixed pore size table Specify exact pore sizes for which volume or area data are
reported. Only the pore sizes within the specified range are
reported.
When you select this option, the Table push button is enabled
so that you may enter or edit a fixed pore size table.
Collected points Includes all relative pressure points collected by the system
5-60 Mar 09
Columns Displays the BJH Adsorption (or Desorption) Tabular Report

Column Options dialog.
The default column title appears next to the column number.

Each column includes a drop-down list of the data types
available for inclusion in the report. You can measure pore
width, pore radius, or pore diameter.
Table Enabled when you choose Fixed pore size table. Displays the
BJH Adsorption (or Desorption) Fixed Pore Size Table dialog
so that you may enter or edit a fixed pore size table.
The fixed pore size table must contain a minimum of two

points and may include as many as 1000. The points must be
strictly decreasing.
Mar 09 5-61
Insert Inserts a row into the pressure table. The row is inserted
above the selected row and the cursor moves to the new row.
Delete Deletes the selected row from the pressure table.
Clear Clears all points from the pressure table; none have to be
selected.
Plot Options
Click Edit for BJH Adsorption/Desorption plots to specify plotting methods and to customize
plots. A dialog similar to the following is displayed when you select a BJH plot
Plot curve Plot data as a curve, points, or both.

Plot points
X-axis Lists the scale options for the x-axis.
Linear/Logarithmic Choose whether you wish to have the X-axis on a

logarithmic or linear scale.
5-62 Mar 09
Autoscale Select this option to have the x-axis scaled automatically.

The lowest and highest values collected during analysis are
used as the beginning and ending points.
When you deselect this option, the adjacent fields are

enabled so that you can specify beginning and ending
values.
Data ranges are displayed in the information bar across the

bottom of the dialog when a cursor is in a numerical data
field.
Y-axis Lists the options for the y-axis.
Variable Choose the desired variable for the Y-axis.
Overlay Displays a list of overlay choices. You may choose to

overlay the current plot with data from other samples or with
other plots from this sample.
Autoscale Select this option to have the y-axis scaled automatically.

The lowest and highest values collected during analysis are
used as the beginning and ending points.
When you deselect this option, the adjacent fields are

enabled so that you can specify beginning and ending
values.

bottom of the dialog when a cursor is in a numerical data
field.
Mar 09 5-63
Dollimore-Heal Adsorption/Desorption Report Options
You can generate DH reports from both adsorption and desorption data.
Or Dollimore-Heal
Desorption Report
Options
The options for Dollimore-Heal reports are the same as those for the BJH reports with the
exception of BJH Correction and Adsorptive properties; this item is not applicable to DH
reports. Refer to BJH Adsorption/Desorption Report Options, page 5-57 for a description
of the fields on this dialog.
5-64 Mar 09
Horvath-Kawazoe Report Options
Pore Geometry Select the option in this group box which best represents the
physical geometry of the micropores in the sample material.
If you choose Sphere, interaction parameters are disabled.
Refer to Horvath-Kawazoe, page C-22 for information on

report calculations.
Apply Cheng/Yang Allows you to apply the Cheng/Yang correction to the pore
correction size analysis. This correction substitutes the Langmuir
equation of state for Henry’s Law in the Horvath-Kawazoe
derivation (see Appendix C, page C-25 for calculations).
Smooth differentials Smooths the differential calculations, eliminating variations

in the differential computation caused by noise in the input
data.
Mar 09 5-65

Collected/Entered dialog, all of the nonoutlier points of
calculating the data for this report.

used.
Interaction Parameter Select one of the options in this group box to determine
which interaction parameter is used during report generation.
These options are disabled when you choose Sphere as the

pore geometry.
Computed The interaction parameter is calculated using the parameters

on the Horvath-Kawazoe Physical Properties dialog. You can
click Properties to view or edit these parameters. Each time
you change one of the parameters, the interaction parameter
is recalculated. Refer to Interaction Parameter, page C-26
for the formula for computing the interaction parameter.
Entered The value you enter in the adjacent field will be used.
Properties Use this push button to view or edit the constants (used
during report generation) describing the physical properties
of the adsorbent and adsorptive; the Horvath-Kawazoe
Physical Properties dialog is displayed.
5-66 Mar 09
Properties
(continued)
These options are disabled if Entered is selected as the inter-

action parameter.
Adsorbent Group Box Contains the parameters for the sample. If you select
Computed for the interaction parameter, all fields are
enabled and can be edited if desired. If you select Entered,
only the values in the Diameter and Diameter at zero
energy fields may be edited.
Description
The name of the adsorbent used in the analysis. Click on the
down arrow to make a new selection. Each time you change
the selection, the values for that adsorbent are displayed in
the appropriate fields.
Diameter
The diameter of the sample atom.
Diameter at zero energy

The diameter of an atom at zero interaction energy,
(2/5)1/6 x diameter.
Polarizability
The polarizability of the adsorbent.
Magnetic susceptibility
The magnetic susceptibility of the adsorbent.
Density
The density per unit area of the adsorbent
Mar 09 5-67
Adsorptive Group Box Contains the parameters for the adsorptives (provided with
the software and/or user-defined). If you select Computed
for the interaction parameter, all fields are enabled and can be
edited if desired. If you select Entered, only the values in the
Diameter and Diameter at zero energy fields may be
edited.
Mnemonic
The mnemonic name of the adsorptive gas in use.
Click on the down arrow to make a new selection. Each time

you change the selection, the values for that adsorptive
display in the appropriate fields. If no parameters have been
defined, the default values are displayed.
Diameter
The diameter of the adsorptive atom.
Diameter at zero energy

The diameter of an atom at zero interaction energy,
(2/5)1/6 x diameter.
Polarizability
The polarizability of the adsorptive.
Magnetic susceptibility
The magnetic susceptibility of the adsorptive.
Density
The density per unit area of the adsorptive.
Selected Reports Lists the available Horvath-Kawazoe reports. Choose a report

by double-clicking on the report name or highlight the report
name and press the Spacebar. A report is selected when it is
preceded with a check mark.
The following reports are available:
• Tabular Report
• Cumulative Pore Volume
• dV/dw Pore Volume
Edit Allows you to edit the selected report.
5-68 Mar 09
Tabular Report Options
Displays the Horvath-Kawazoe Tabular Report Column Options dialog so that you can select
the type of data to display in each column.
The default column title displays next to the column number. Each column includes a drop-
down list of the types of data to include in the report.
Plot Options
Selecting a Horvath-Kawazoe plot option from the Horvath-Kawazoe Report Options dialog
enables you to specify the plotting method used for your report and to customize the plot. Plots
for Cumulative Pore Volume and dV/dw Pore Volume are available.
When you select either of these plots from the Horvath-Kawazoe Report Options dialog, a dia-
log like the following is displayed.
Mar 09 5-69

Plot points
X-axis options Choose Autoscale to have the x-axis scaled automatically.

The X-axis begins at zero and the system uses the highest
value collected during analysis as the ending point.
If you deselect Autoscale, the adjacent fields are enabled so

that you may enter a beginning and ending value. Data
collected outside these ranges are not included in the plot.
X-axis range fields show pore radius or diameter in

angstroms or nanometers.

bottom of the dialog when the cursor is in a numerical data
entry field.
Y-axis options Click on the down-arrow at the Variable field to choose a

variable for the Y-axis.
Click on the down-arrow at the Overlay field to overlay the

plot with data from other samples.
Choose Autoscale to have the y-axis scaled automatically.

Y-axes begin at zero. The system uses the highest value
collected during analysis as the ending point.
If you deselect Autoscale, the corresponding fields are

enabled so that you may enter a beginning and ending value.
Data collected outside these ranges are not included in the
plot.
Y-axis range fields show the quantity of gas adsorbed

entry field.
5-70 Mar 09
DFT Pore Size
Type Drop-down list containing the types of models available;

DFT or Classical.
DFT models are based on the density functional theory.

Classical models are based on the Kelvin equation and
thickness for determining the pore size distribution. Refer to
Appendix F, page F-1 for a discussion on models.
Refer to DFT (Density Functional Theory), page C-40 for

information on report calculations.
Geometry Drop-down list containing pore shapes available; Slit or

Cylinder.
Models Lists the models that meet the criteria specified and which
match the adsorbate and temperature of the sample data.
The models display in alphabetical order with the first one

automatically selected; you may select any one desired.
If the list is empty, there were no models that meet the

selected criteria.
Mar 09 5-71
• If Use calculation assignments is not selected on the Col-

lected/Entered dialog, all of the nonoutlier points of the
collected data within the specified range are used for calcu-
lating the data for this report.
• If Use calculation assignments is selected, collected data

points which are assigned to this report type are used.
Regularization These choices enable you to choose the extent of smoothing

you wish to have applied to your data, or your can choose
None.
If you choose Entered, its field is enabled allowing you to

enter a number giving a relative weight for the smoothing
during deconvolution. Larger values produce more
smoothing.
Reports to Generate Displays the types of reports available.
• Tabular Report
• Isotherm table
• Cumulative area graph
• Incremental area graph
• Differential area graph
• Cumulative volume graph
• Incremental volume graph
• Differential volume graph
• Log goodness of fit graph*
• Goodness of fit graph*
Graph details can be edited by selecting the Edit push button.
*These graphs cannot be edited.
5-72 Mar 09
Edit Use this push button to edit details of a selected graph; a dia-
log like the following is displayed.
Displays the type of

graph you are
editing.
This push button is disabled for tables and Goodness of Fit

graphs.
Plot Type Enables you to choose the manner in which you wish to
display plotted data; as a curve or as a histogram.
Autoscale Options Select these options to have the axes scaled automatically.
If you deselect one or both of these options, you must enter a

range in the related Axis Range fields which become enabled
automatically.
Overlay This drop-down list contains the type of overlays available

for the current graph.
Choose Samples to overlay the same type of graph as the

current one from other data reductions. Then select Overlays
on the Report Options dialog to choose your files (explained
on page 5-33).
Axis Range The fields in this group box become enabled when you dese-
lect Autoscale, allowing you to specify beginning and ending
values for the X- and/or Y-axis. Data collected outside these
ranges are not included in the plot.
Valid ranges for a selected field are displayed in the informa-

tion bar across the lower portion of the dialog.
The X-axis displays the energy and the Y-axis displays the
area.
Mar 09 5-73
DFT Surface Energy
The fields on the DFT Surface Energy dialog are identical to those on the DFT Pore Size dia-
log with the following exceptions:
Geometry drop-down list Is not applicable to the Surface Energy report and, therefore,
does not display on its dialog.
Reports to Generate Displays the types of reports available.
• Tabular report
• Isotherm table
• Cumulative area graph
• Incremental area graph
• Differential area graph
• Log goodness of fit graph
• Goodness of fit graph
Graph details can be edited by selecting the Edit push button.
Refer to the previous section for the DFT Pore Size report beginning on page 5-71 for infor-
mation on the fields contained on this dialog.
5-74 Mar 09
Dubinin Report Options
Report Type Allows you to specify the type of report you wish to generate.
At least one type of report must be selected.
Select Radushkevich to generate the Radushkevich report.
Select Astakhov to generate the Astakhov report. With this

choice, you may select Optimize exponent. If you do not
select this option, the Exponent field is enabled so that you
can enter a value.
Refer to Dubinin-Astakhov, page C-32 and Dubinin-

Radushkevich, page C-30 for information on report
calculations.
Fitted relative Allows you to specify minimum and maximum limits on

pressure range relative pressures included in the line fit. Data collected
outside these limits are not included in the line fit.
Mar 09 5-75
Adsorptive Allows you to specify up to ten adsorptive/affinity coefficient

(beta) combinations. The Dubinin Adsorptive Options dialog
is displayed.


used.
Selected Reports Lists the available Dubinin reports. Choose a report by

double-clicking on the report name or highlight the report
name and press the spacebar. A report is selected when it is
preceded with a check mark.
• Dubinin Tabular Report

• Transformed Isotherm
• dV/dw Pore Volume (Astakhov only)
5-76 Mar 09
Selecting Tabular Report from the Dubinin Report Options dialog enables you to customize
your report with up to six columns of data for Astakhov reports and up to five columns of data
for Radushkevich reports. The Dubinin Tabular Report Column Options dialog is displayed.
The default column title appears next to the column number. Each column includes a drop-
down list of the data types to include in the report.
The value for n (shown in column 5) is the optimized exponent if Optimized Astakhov expo-
nent is selected on the Dubinin Report Options dialog. If not, then the value for n is the
entered exponent value.
Mar 09 5-77
Transformed Isotherm Plot Options
Selecting Transformed Isotherm from the Dubinin Plot Option dialog enables you to restrict
the line fit to a portion of the isotherm. The Dubinin Transformed Isotherm Plot Options dia-
log is displayed.
Overlay Samples Select this option to overlay the current plot with data from
other samples. Then click Overlays on the Report Options
dialog to choose the sample files.
Autoscale x-axis Select these options to have the X- and/or Y-axes

Autoscale y-axis automatically scaled. Both axes begin at zero; the system
uses the highest values collected during analysis as the
ending points for axis ranges.
If you choose not to autoscale data for either (or both) axis,
the corresponding fields are enabled so that you may enter a
beginning and ending value.
The X-axis shows the quantity of gas adsorbed at standard

temperature and pressure.
The Y-axis shows the log of relative pressure.

entry field.
5-78 Mar 09
Pore Volume Options
When you select dV/dw Pore Volume from the Dubinin Report Options dialog, the Dubinin
dV/dw Pore Volume Options dialog is displayed.

Plot points
Overlay samples Select this option to overlay data from other samples. Then
click Overlays on the Report Options dialog to choose the
files.
Autoscale x-axis Select these options to have the X- and/or Y-axes

Autoscale y-axis automatically scaled. Both axes begin at zero; the system
uses the highest values collected during analysis as the
ending points.
If you choose not to autoscale data for either (or both) axis,
the corresponding fields are enabled so that you may enter a
beginning and ending value. Data collected outside these
ranges are not included in the plot.

entry field.
Mar 09 5-79
MP-Method Report Options
Pore size can be expressed in Angstroms or nanometers. Select Options > Units to
specify the desired unit.
Thickness Curve Select the thickness curve type from this group box. You
must choose either the Halsey equation or the Harkins-Jura
equation. Use Equation to edit the values in the equation.
Refer to MP-Method, page C-36 for information on report

calculations.
Harkins and Jura Displays the Harkins and Jura Thickness Equation dialog.
You can edit the values for the numerator, first element of the
denominator, and exponent.
5-80 Mar 09
Halsey Displays the Halsey Thickness Equation dialog.
You can edit the values for the multiplier, numerator, and
exponent.
Equation Displays the equation for the type of thickness curve selected.
Selected Reports Lists the available MP-Method reports. Choose a report by

double-clicking on the report name or highlight the report
name and press the spacebar. A report is selected when it is
preceded with a check mark (3).
• MP Tabular Report
• dA/dw Pore Area
The data for these reports are measured in pore width only.
Edit Enables you to edit the selected report.


used.
Mar 09 5-81
Selecting Tabular Report from the MP-Method Report Options dialog enables you to cus-
tomize your report with up to six columns of data. The MP-Method Tabular Report Column
Options dialog is displayed.
The default column title appears next to the column number for columns three through six.
Each of these columns includes a drop-down list of the data types to include in the report. The
following data types are available:
• Incremental Pore Volume

• cumulative Pore volume
• dV/Dw Pore volume
• Incremental Pore Area
• dA/dw Pore Area
Columns 1 and 2 are fixed and cannot be edited.
The MP-Method reports hydraulic radius only. If you select Pore size in diameter from
the Unit Selection dialog, pore size in radius will be reported.
5-82 Mar 09
Plot Options
Selecting an MP-Method plot option from the MP-Method Report Options dialogs enables
you to specify the plotting method used for your report and to customize the plot. The follow-
ing plots are available:

• dA/dw Pore Area
When you select any of the plots from the MP-Method Report Options dialog, a dialog similar
to the following one is displayed. The fields on all dialogs are the same.

Plot points
X-Axis Choose Autoscale to have the x-axis scaled automatically.

The X-axis begins at zero and the system uses the highest
values collected during analysis as the ending point.
If you deselect Autoscale, the corresponding fields are

plot.

entry field.
Mar 09 5-83
Y-Axis
Variable Click on the down-arrow to choose a variable for the Y-axis.
Overlay You can use the choices in this drop-down list to overlay
plots. You can choose a different type of plot for the current
sample to overlay with the listed Variable, or you can choose
Samples to overlay the variable plot with the same type of
plot from other samples. Click Overlays on the Reports
Options dialog to choose the samples.
Autoscale Choose this option to have the y-axis scaled automatically.

Y-axes begin at zero. The system uses the highest values
collected during analysis as the ending points for axes ranges.
If you deselect this option, the corresponding fields are

plot.
Y-axis range fields show the volume of gas adsorbed.

entry field.
5-84 Mar 09
Options Report
The Options report is a subset of the contents report; it provides pertinent information for the
following:
• Sample tube
• Degas conditions
• Free space
• Po and temperature
• Equilibration
• Isotherm collection
Sample Log Report
The Sample Log report displays the following:
• Manual control operations performed during analysis

• Information entered using Add Log Entry on the sample file editor
• Warnings and/or errors which occurred during analysis
Mar 09 5-85
Validation Report
Use this report to have your data examined by the software to determine if the results are
within typical ranges.
If the data for any report(s) you selected for validation are determined to be out of range, a
warning is displayed and suggestions are given for corrective action. This information is also
detailed in the report and plotted on the graph as a unique plot symbol.
5-86 Mar 09
Entered or Collected Data
If you select Manually Entered on the Advanced view of the Sample information dialog, an
Entered tab is added enabling you to enter the data.
If you select Automatically collected, a Collected tab is added after the analysis is
completed.
Mar 09 5-87
Pressure table For collected data, columns for the following are displayed:
• absolute pressure
• relative pressure
• quantity adsorbed
• outliers (if Use calculation assignments is not selected)
• calculation assignments for each requested report option

(if Use calculation assignments is selected)
For entered data, columns for the following are displayed:
• absolute or relative pressure, depending on the selection

in the Pressures group box
• quantity adsorbed
Insert Enabled for entered data. Inserts a row into the pressure table.
Delete Enabled for entered data. Deletes the selected row.
Clear Enabled for entered data. Clears the table of all but one entry;
one is required.
Use calculation If selected, allows you to assign the points for each report
assignments type.
If deselected, each report (with the exception of Langmuir

and BET) uses a range of pressures as selected in the report
options. The Langmuir and BET reports interpolate to
entered relative pressures on the report options.
The outlier points can be selected so that they will not be

reported.
5-88 Mar 09
Pº and T Displays the Pº and T dialog.
This dialog allows you to edit the Po measurement and

analysis bath temperature.
Free Space Displays the Free Space dialog, allowing you to edit free-
space values.
This dialog also shows the isotherm for the analysis. The
isotherm is redrawn each time values are edited.
You can also customize parts of the isotherm plot, as well as

zoom in for finer detail. Right-click in the graph area to
display a shortcut menu displaying the options available.
Refer to Shortcut Menus, page 7-24.
Mar 09 5-89
Measured Displays the Warm and Cold free-space values if Measured

was chosen as the Free-space method for the analysis; these
values cannot be edited..
Entered Enables the Warm, Cold, and Non-ideality Factory fields

so that you may enter the values manually.
The warm free space is the sample tube gas capacity

measured at room temperature.
The cold free space is the sample tube gas capacity measured
with the Dewar raised.
The non-ideality factor compensates for the forces of

attraction between molecules in a real gas.
Calculate Select this option to have the free-space measurement

calculated using the sample conditions and sample tube
parameters.
Port volume Displays the volume for the port used in the blank analysis.
5-90 Mar 09
TriStar II 3020 Save
Save
Save enables you to save any changes you have made to the file in the active window. The file
is saved under its current name.
Save As
Save As enables you to:
• save a sample or parameter file in the active window under a different name. This
option is useful for making a duplicate copy of a file that you can modify as desired
without changing the original one. The original file remains open when you use this
function, so be sure to open the new file before making any changes.
• save a subset (parameter) of the sample file in the active window as a standalone
parameter file. For example, select Analysis Conditions from the Save As menu to
create a standalone parameter file of the analysis conditions portion of the active sample
file.
• save as an ASCII file the relative pressures and corresponding thicknesses (t-Curve).
These data are derived by dividing the condensed volume of adsorptive by the selected
surface area. The density conversion factor in the adsorptive properties file is used to
convert quantity adsorbed to volume of condensed adsoptive.
• save as an ASCII file the relative pressures and resulting quantities adsorbed (Alpha-S).
These data are derived by dividing the isotherm by the quantity adsorbed at 0.4 relative
pressure.
Mar 09 5-91
Save As TriStar II 3020
Sample and Parameter Files
A dialog similar to the one shown below is displayed when you select Sample Information,
Sample Tube, Degas Conditions, Analysis Conditions, Adsorptive Properties, or Report
Options.
Indicates the type

of file being saved.
Enter a file name (up to eight characters) in the File name field; the appropriate extension is
appended automatically when you click OK. The new file is saved as specified, but does not
remain in the active window. Be sure to open the new file before making any changes to the
file.
t-Curve and Alpha-S Files
The same type of dialog shown above is also displayed when you select t-Curve or Alpha-S.
However, before you receive this dialog for t-Curve, the Save As t-Curve dialog is displayed.
This dialog allows you to choose the surface area for the sample.
5-92 Mar 09
TriStar II 3020 Save All
Save All
Save All enables you to save all open files under their current names. This option provides a
faster way to save all open files at one time and avoids having to perform a Save operation on
each individual file.
Close
Close enables you to close the file in the active window. The following message is displayed if
changes have been made to the file:
(File name) has been changed. Save changes before

closing?
Yes No Cancel
Yes saves any changes and closes the active window.

No discards any changes and closes the active window.
Cancel returns you to the open file.
Close All
Close All enables you to close all open files under their current names. The following message
is displayed for each file in which changes have been made:
(File name) has been changed. Save changes before

closing?
Yes No Cancel
Yes saves any changes and closes the active window.

No discards any changes and closes the active window;.
Mar 09 5-93
Print TriStar II 3020
Print
Print enables you to print the contents of one or more sample or parameter files to the printer,
screen, or to a file. For example, if you choose Analysis Conditions, you will receive the
parameters used for all analysis conditions associated with the file(s). The print dialog is com-
mon to all file types.
Indicates the type of

file you are printing.

parameter files.
File name The name of the file you select from the Files list box is
copied to this field.
Copies Enabled when Printer is selected as the print destination,

allowing you to print up to four copies
Destination Select the destination. You may print to a printer, the screen,
or to a file.
File name Enabled when you select File as the destination. A default
file name (the same name as the sample file) appears if you
choose only one file; you can use the default name or enter
another one.
If you select multiple files, the default displays as *.RPT;

each file will be exported as its original file name with the
RPT extension.
Refer to Selecting Files, page 2-11 for an explanation of the remaining fields on this dialog.
5-94 Mar 09
TriStar II 3020 List
List
List enables you to generate the following information on a selected sample or parameter file.
• File name
• Date the file was last edited
• Time the file was last edited
• File identification
• File status
The List dialog is common to all file types.
Indicates the type of

file on which statistics
have been requested.

parameter files.
The behavior of the List dialog is the same as the Print dialog; refer to Print, page 5-94 for an
explanation of the fields on this dialog.
You may request a list of multiple files by holding down Ctrl while selecting files. If no files
are selected, a list is generated for all files.
Mar 09 5-95
Export TriStar II 3020
Export
Export allows you to copy the isotherm data in a sample information file and reformat it in an
ASCII format acceptable to other programs, such as spreadsheets.
The output file consists of four columns containing the elapsed time, absolute pressure, rela-
tive pressure, and specific quantity adsorbed (see example on next page).
You may export multiple files by holding Ctrl while selecting the files.
Select File > Export; the Export Sample File dialog is displayed.
File name The name of the file you select from the Files list box is
copied to this field.
Destination You can export data to a printer, to the screen, or to a File.
• If you select Printer, the Copies field is enabled allow-

ing you to print up to four copies.
• If you select File, the File Type and File name fields are
enabled.
5-96 Mar 09
TriStar II 3020 Export
File Type You can export data in a spreadsheet format (XLS) or as a

text file (TXT).
File name Allows you to specify a name for your exported file, or you
may accept the default. The default name is the name of the
sample file appended with the appropriate extension.
Refer to Selecting Files, page 2-11 for an explanation of the remaining fields on this dialog.
Format of Data Output
This example shows the format of the output file for exported data.
Description
Operator
Submitter
Sample mass
Type of Data*
Elapsed time Absolute pressure Relative pressure Specific quantity

adsorbed
*0 = automatically collected
1 = entered (relative pressures)
2 = entered (absolute pressures)
Mar 09 5-97
Convert TriStar II 3020
Convert
Convert enables you to convert StarDriver files (MGD extension) to a format compatible with
the TriStar 3020 analysis program. The only files that will display in the Files window are
those with the MGD extension.
Files window Displays the StarDriver files in the current directory (the
current directory is shown just above the Directories
window). Refer to page 2-13 for information on navigating to
other directories.
Destination Displays the current directory and the name of the selected
file with an SMP extension. If you wish to save the file in a
different directory, be sure to enter (or navigate to) the
desired directory. You can choose multiple files by holding
down Ctrl while selecting the files.
Date Range These options are explained in Selecting Files on page 3-6.
Files
Directories
5-98 Mar 09
TriStar II 3020 Exit
Exit
Exit enables you to exit the TriStar analysis program. Select File > Exit from the main menu.
If an analysis is in progress, it will continue until completion; analysis data are collected and
stored in an embedded controller.
• If a window containing a modified file is open, the following message is displayed:
Modifications have been made to (file name). Do you want

to save the modifications?
Yes No Cancel
Yes saves any changes and exits the analysis program.

No abandons any changes and exits the analysis program.
• If an analysis is in progress, the following message is displayed:
CAUTION: Sample analysis is in progress. If you exit the

program, analysis will continue to completion, but the data
are not saved to disk until the program is restarted. Do you
want to exit the program?
Yes No
Yes exits the analysis program.

No leaves the analysis program active and allows the analysis to finish.
Although data are stored in an embedded controller when you exit the program, data
are not saved to disk until you restart the program and save the data. If a power failure
occurs and the analyzer does not have an Uninterruptible Power Supply (UPS), any
unsaved data are lost.
• If a report is in progress, the following message is displayed:
CAUTION: Reports are being generated. If you exit the

program these reports will be canceled. Do you want to
cancel reports and exit the program?
Yes No
Yes cancels the reports and exits the analysis program.

No leaves the analysis program active and allows the reports to finish.
Mar 09 5-99
6. UNIT MENU
The Unit menu contains the options for the operations which can be performed with the
TriStar 3020. The main menu will contain a Unit menu for each attached analyzer. For exam-
ple, if you have two attached analyzers, the main menu contains two Unit menus. The status
displays associated with each unit are displayed in different colors. The unit number and the
serial number also are displayed in the title bar of the operational windows. This is especially
convenient if you have more than one analyzer attached to the same computer.
The Unit menu does not appear on the menu bar if the analysis program is being used
for offline data operations on a computer other than the one controlling the analyzer.
Description
Listed below are brief descriptions of the Unit menu options. Detailed descriptions are found
later in this chapter.
Sample Analysis Allows you to perform up to three analyses using different

analysis conditions. Page 6-3.
QuickStart Analysis Allows you to perform multiple sample analyses using the
same analysis conditions, allowing you to create sample files
at the time of analysis. Page 6-8.
Mar 08 6-1
Krypton Analysis Enables you to perform a krypton analysis. Page 6-11.
Blank Analysis Enables you to perform a blank analysis. Page 6-12.
Enable Manual Control Allows you to control the system manually. Page 6-14.
Show Instrument Displays the analyzer’s schematic. Page 6-17.

Schematic
Show Status Displays the status window. Page 6-19.
Show Instrument Log Displays a log of recent analyses, calibrations, and error
messages. Page 6-21.
Unit Configuration Displays software version, hardware configuration, and

calibration information. Also allows you to enter mnemonic
names for port gases. Page 6-23.
Diagnostics Enables you to perform predefined diagnostics. Page 6-24.
Calibration Enables you to perform certain instrument calibrations. The

options on this menu are enabled only with the direction of a
Micromeritics service representative. Page 6-27.
Service Test Enables you to perform certain troubleshooting procedures.

This option is enabled only with the direction of a
Micromeritics service representative. Page 6-30.
6-2 Mar 08
TriStar II 3020 Sample Analysis
Sample Analysis
Use this mode of operation to schedule analyses which have different analysis conditions or
report options. You can schedule up to three analyses at a time.
You can continue to schedule analyses by clicking Next (appears after the first series of analy-
ses are finished) on the analyzing view of the Analysis dialog.
Samples cannot be removed from or added to ports until the full set of analyses has completed.
Select Unit > Sample analysis; the Analysis dialog is displayed.
View Allows you to choose the view you wish to display in the
window.
Operation displays the current mode of operation.
Instrument Schematic displays a schematic of the TriStar

system. Refer to Show Instrument Schematic, page 6-17
for additional information.
Instrument Log displays a list of recent analyses,

calibrations, and errors or messages. Refer to Show
Instrument Log, page 6-21 for additional information.
Mar 08 6-3
Sample Analysis TriStar II 3020
Close Valves Enabled when analysis is complete, allowing you to close all
sample port valves immediately; otherwise the valves close in
approximately five minutes.
Port [n] This field is blank until you choose a file to use for the
analysis on this port.
Browse Click this push button to select a sample information file for
the current; the Open Sample Information dialog is displayed.
You can choose an existing file or accept the next sequenced
number to create a new; default values will apply.
Clear Clears the information displayed for this port.
Sample Displays the identification of the selected sample file or the

default description if creating a new one; this field may be
edited if desired.
Mass Displays the value specified in the sample file; enter the mass
for the current sample..
Density Displays the density of the sample specified in the sample

information file; this, too, may be edited if needed. This value
is applicable only when using the calculated free-space
method.
Po Enabled if you have selected Entered for the Po

measurement for at least one file. Enter the Po value, or edit
the current one.
Bath temperature Enter the temperature for the analysis bath.
6-4 Mar 08
Report After Analysis Allows you to have a report generated automatically after the
analysis; displays the Report Settings dialog so that you may
specify output options.
Export After Analysis Allows you to have isotherm generated automatically after
the analysis; displays the Export Settings dialog so that you
may specify output options.
Start Starts the analysis; displays an analyzing view of the

Analysis dialog.
Mar 08 6-5
Sample Analysis TriStar II 3020
Port activity
Status window
This view also displays port activity as well as the status

window.
Skip Skips an analysis; visible only when an analysis is in

progress. The Skip dialog is displayed so that you may
choose the port(s) containing the analysis you wish to skip.
A check box is included for each port on which an analysis is

being performed. This example shows only one port being
used.
Suspend Suspends an analysis; visible only when an analysis is in

progress. A dialog similar to the one shown above is
displayed so that you may choose the port(s) containing the
analysis you wish to suspend.
6-6 Mar 08
Resume Resumes a suspended analysis; visible only when an analysis

is suspended. A dialog similar to the one shown above is
analysis you wish to resume.
Report [n] These push buttons allow you to generate reports on data
collected at that time for the sample in the respective port.
The reports are printed to the screen only.
Cancel Cancels an analysis; enabled only when an analysis is in

progress. A dialog similar to the one shown above is
analysis you wish to cancel.
Start On this view of the Analysis dialog, this push button changes
to Next when analyses are finished.
Next Returns you to the first view of the Analysis dialog so that
you may schedule additional analyses.
Close Closes the Analysis dialog.
Mar 08 6-7
QuickStart TriStar II 3020
QuickStart
Use this mode of operation to analyze samples of the same type using the same analysis condi-
tions, adsorptive properties, and report options. You may schedule up to three analyses at a
time.
You can continue to schedule analyses by clicking Next (appears after the first series of analy-
ses are finished) on the analyzing view of the Analysis dialog.
Select Unit > QuickStart analysis to display the QuickStart dialog.
View Allows you to choose the view you wish to display in the
window.
Operation displays the current mode of operation.
Instrument Schematic displays a schematic of the TriStar

system. Refer to Show Instrument Schematic later in this
chapter for additional information.
Instrument Log displays a list of recent analyses,

calibrations, and errors or messages. Refer to Show
Instrument Log later in this chapter for additional
information.
Close Valves Allows you to ensure that all valves are closed before
analysis is started. After analysis begins, this push button is
disabled.
6-8 Mar 08
TriStar II 3020 QuickStart
Sample ID Enables you to enter a name for the current series of samples.
Operator Enables you to enter the operator’s name, or some other

appropriate identifier.
Report Options This group box allows you to have a report generated
automatically after each analysis. You can specify a
destination and, when Printer is selected, the number of
reports to be printed.
If you choose File, the File name field is enabled. You can
accept the default name or enter a new one.
Export Options Enables you to have isotherm data exported automatically

after analyis.
Next Advances you to the second view of the QuickStart dialog.
This view of the QuickStart dialog allows you to specify sample information for the current set
of samples.
The behavior of this dialog is the same as the Analysis dialog; refer to Sample Analysis, page
6-3 for a description of the fields on this dialog.
Mar 08 6-9
QuickStart TriStar II 3020
Port [n] Enables you to select the port(s) being used in the analyses.
Sample tube Enables you to select the sample tube file you wish to use;
applicable only if you have selected the calculated method
for measuring the free space.
Start Starts the analysis; displays an analyzing view of the

Analysis dialog.
This view contains data collection for each analysis, as well

as port information. Refer to the previous section for an
explanation of the push buttons contained on this dialog.
When analyses are complete, the second view of the dialog

again is displayed, allowing you to quickly start the next set
of samples.
6-10 Mar 08
TriStar II 3020 Krypton Analysis
Krypton Analysis
This option enables you to perform up to three krypton analyses at the same time.
Use the following guidelines for performing krypton analyses:
• All analyses must use krypton gas; if a gas other than krypton is specified, an error
message is displayed.
• From Psat tube must be selected as the Dosing Method (Adsorptive Properties
dialog); an error message is displayed if this has not been selected.
• Samples cannot be removed from or added to ports until the full set of analyses has
completed.
The fields on this dialog are the same as for those on the Analysis dialog; refer to Sample
Analysis, page 6-3 for a description of the fields on this dialog.
Mar 08 6-11
Blank Analysis TriStar II 3020
Blank Analysis
A blank analysis is used for obtaining sample tube parameters when using a calculated free
space. A blank analysis can also be used for diagnostic purposes.
The behavior of this dialog is the same as the Analysis dialog; refer to Sample Analysis, page
6-3 for a description of the fields on this dialog.
Port [n] Enables you to choose the port(s) you are using for a blank
analysis. Displays the file name assigned to the blank analy-
sis on the current port. File names are assigned automatically
and contain appropriate conditions for performing a blank
analysis.
Replace All Click this push button to replace the values of the current file
with those of an existing file. Appropriate default conditions
for a blank analysis are contained in the assigned file. How-
ever, if you require a different set of conditions, you can use
this push button to copy them into the assigned file.
6-12 Mar 08
TriStar II 3020 Blank Analysis
Sample Enables you to enter an identification for the blank analysis.
Use the dollar sign to have the automatically generated file

name appear in the identification. For example, if you enter $
Blank Analysis Jan 2008 in the Sample field for Port 1 in
the dialog shown above, BK1-000 Blank Analysis Jan 2008
will display as the identification in printed reports.
The assigned file name will display wherever you place the $
sign within the identification.
Mar 08 6-13
Enable Manual Control TriStar II 3020
Enable Manual Control

Select this option to control certain components of your system manually. The instrument
schematic must be visible to use this option. If it is not visible, select Unit [n] > Show Instru-
ment Schematic.
Servo valve
Elevator
When manual control is enabled, the valve symbols change color on the monitor screen to
indicate their status.
Green = open
Yellow = closed
Each component that can be manually controlled has a shortcut menu displaying the opera-
tions available for that particular component. These menus may be accessed by selecting the
desired component, then clicking the right mouse button once, or pressing Shift + F9.
The options available for the components on the instrument schematic are:
Valves 1 through 15 Open, Close, Pulse
Open and Close open and close the valves. You may also
open and close the valves by double-clicking on the valve or
by pressing the Spacebar while the valve is selected.
Pulse quickly turns the valve on and off, allowing the opera-
tion to proceed in small increments. You may also pulse the
valve by pressing P while the valve is selected.
6-14 Mar 08
TriStar II 3020 Enable Manual Control
Table 6-1. System Valves
Valve(s) Description
1 through 3 Sample ports
4 Po port
5 Isolation valve
6 Isolation valve
7 Helium port
8 and 9 Analysis gas ports
10 Vacuum
11 through 13 Unrestricted vacuum for sample ports
14 Analysis gas port
15 10-mmHg isolation valve (displays
only if the Krypton option is installed).
Unmarked Servo
Servo Valve Set, Close
Set displays the Servo Valve Settings dialog so that you may
choose to dose or evacuate and specify a target pressure. You
may also display this dialog by pressing Spacebar while the
servo valve is selected.
Close closes the servo valve. You may also close the servo
valve by pressing Spacebar while the servo valve is selected.
Mar 08 6-15
Enable Manual Control TriStar II 3020
Elevator Raise, Lower, Stop
Raise and Lower raise and lower the elevator. You may also
raise and lower the elevator by double-clicking in the elevator
area or pressing Spacebar while the elevator area is selected.
Stop stops the elevator at its current position. You may also
stop the elevator by double-clicking in the elevator area or
pressing Spacebar while the elevator area is selected.
These components are for informational purposes only; they cannot be controlled manually.
Represents the sample tube.
Represents the pº (saturation pressure) tube.
6-16 Mar 08
TriStar II 3020 Show Instrument Schematic
Show Instrument Schematic

Select this option to display a schematic of the analyzer. Refer to the previous section for an
explanation of the components contained on the instrument schematic.
Displays only if the Krypton option is installed.
Even when manual control is not enabled, you still can determine the state of the valves by
their color.
Green = open
White = closed
If you wish to change the state of a valve, you must enable manual control.
A tool bar has been included on the instrument schematic, making it convenient and easy to
perform commonly used operations.
Open Sample File Displays the Open Sample Information dialog, enabling you
to open and view or edit a sample file. Refer to Sample
Information, page 5-4 for detailed information.
Start Report Displays the Start Report dialog so that you can choose a
sample file on which to generate report data. Refer to Start
Report, page 7-3 for detailed information.
Mar 08 6-17
Show Instrument Schematic TriStar II 3020
Start Analysis Displays the Analysis dialog so that you can start an analysis,
or analyses. Refer to Sample Analysis, page 6-3 for detailed
information.
QuickStart Analysis Displays the QuickStart dialog so that you can begin a series
of analyses. Refer to QuickStart, page 6-8 for detailed
information.
SPC Control Chart Displays the Control Chart dialog so that you can specify
options for generating an SPC Control Chart report. Refer to
Control Chart, page 7-11 for detailed information.
6-18 Mar 08
TriStar II 3020 Show Status
Show Status
Select this option to show only the status window of the analyzer.
If you have multiple instruments attached to your computer, the status bar for each
instrument is displayed in a different color.
The status window shows the current status for each port.
You may wish to use this option if:
• You have an automatic operation in progress and you wish to edit a sample file. This
way, you can keep up with the status of your operation while performing another task.
• You have multiple units attached to your computer. You can select Show Status on each
unit menu and have the status for all units displayed at one time.
The Status window, like the instrument schematic, includes a tool bar of commonly used
operations.
Open Sample File Displays the Open Sample Information dialog, enabling you
to open and view or edit a sample file. Refer to Sample
Information, page 5-4 for detailed information.
Start Report Displays the Start Report dialog so that you can choose a
sample file on which to generate report data. Refer to Start
Report, page 7-3 for detailed information.
Start Analysis Displays the Analysis dialog so that you can start an analysis,
or analyses. Refer to Sample Analysis, page 6-3 for detailed
information.
Mar 08 6-19
Show Status TriStar II 3020
QuickStart Analysis Displays the QuickStart dialog so that you can begin a series
of analyses. Refer to QuickStart, page 6-8 for detailed
information.
SPC Control Chart Displays the Control Chart dialog so that you can specify
options for generating an SPC Control Chart report. Refer to
Control Chart, page 7-11 for detailed information.
6-20 Mar 08
TriStar II 3020 Show Instrument Log
Show Instrument Log

Displays a log of recent analyses, calibrations, and errors or messages. By default, this infor-
mation is logged for a 7-day period for analyses and a 30-day period for messages and
calibrations. You may change the time for which this information is retained in the Unit sec-
tion of the WIN3020.INI file.
You can choose the type of information to display in the window by selecting only the desired
item(s). For example, select only the Analysis option to display analysis information:
Mar 08 6-21
Show Instrument Log TriStar II 3020
Analysis These options allow you to choose which entries to display in

Calibration the window.
Message
Add Log Entry Enables you to make an entry in the instrument log that
cannot be recorded automatically through the application
software. For example, you may change the port filter. The
field adjacent to the push button allows you to enter the
operation; the push button is enabled when you make an
entry in the field, allowing you to add the entry.
Report Displays the Log Report Settings dialog so that you can
specify report output options.
Use the Start Date field to specify a date at which to start the
printout. You can specify a date using one of the following
methods:
• Press F2 to clear the field so that you can enter a date
• Double-click in the field (or press F4) to display a calen-

dar to choose a date
• Press F3 to insert the current date
The Copies field is enabled when you select Printer as the

destination, enabling you to print up to four copies.
Choose the report destination in the Destination field. If you

choose File as the destination, the File name field is enabled,
allowing you to enter a name for the printed file (or you may
accept the default).
6-22 Mar 08
TriStar II 3020 Unit Configuration
Unit Configuration
Select this option to display hardware/software configurations, calibrations, and gas selections
of the connected analyzer. When you select this option from the Unit menu, the Unit Configu-
ration dialog is displayed.
Configuration Displays the IP address used by the analysis program and the
serial number of the selected analyzer. Also enables you to
view details of the boards installed in the analyzer.
Software Versions Displays the software versions of the MICBIOS, controller,

and TriStar 3020 analysis program.
Gas Selections Enables you to specify the mnemonic names for the analysis
gas(es). Gas inlet valves V8, V9, and V14 are designated for
analysis gases; V7 is dedicated to the free-space
measurement which uses Helium (He). You can enter up to
three characters.
Servo Valve Displays the date the servo valve was last calibrated.
Calibration group boxes The remaining group boxes display calibration information
for their respective component.
Mar 08 6-23
Diagnostics TriStar II 3020
Diagnostics
This option enables you to clean and verify gas lines when connecting or changing a gas
(refer to Cleaning and Verifying the Gas Line, page 9-24 for step-by-step instructions). This
option also allows you to perform diagnostic tests which your service representative may
request. The data generated from these tests may be insignificant to you as a user, but can be
very helpful to your service representative. Your service representative can view the results
and may be able to resolve the problem, eliminating downtime and repair costs.
These tests generate files to the 3020\Service\userdiag directory. Your service representative
will request that you E-mail or fax the files to him so that he may examine them.
When you select Unit [n] > Diagnostics, the Service Test dialog is displayed:
View Allows you to view the current operation, the instrument

schematic, or the instrument log in the Service Test dialog.
Operation is the appropriate choice for tests.
Test Contains a list of diagnostic tests. These tests will always

include the latest revision letter at the end of the test name.
Sequence Displays the test file number. This number is assigned auto-
matically and incrementally sequenced by the software each
time a test is performed. This also serves as the name of the
file that is generated to the userdiag directory, and will be
appended with SVT. For example, the name of the file for
the test shown in the above dialog is 0006.SVT.
6-24 Mar 08
TriStar II 3020 Diagnostics
Report after test Select this option to have a report generated automatically
after the test; page 6-9 provides an explanation of output
options.
If you do not select this option, you can still have a report
generated from the report window.
Cancel Cancels the test.
Next Begins the test; displays the next view of the Service test
dialog. The second view of the Service test dialog may con-
tain a single pane or two panes, depending on the test
selected.
Report (field) Contains a list of the reports that will be generated during
this test.
Item [n] Lists the data in the two panes. Item 1 is the upper pane and
Item 2, the lower pane.
Report (push button) Enables you to generate a report.
Cancel Cancels the test.
Mar 08 6-25
Diagnostics TriStar II 3020
The following push buttons become enabled when the test is complete.
Repeat Repeats the test; not applicable for this test.
Next Returns you to the first view of the Service Test window.
Close Closes the dialog.
6-26 Mar 08
TriStar II 3020 Calibration
Calibration
This option allows you to perform system calibrations. Some calibrations are disabled and can
be accessed only when using the Service Test Mode with the assistance of your service repre-
sentative. .
Zero Pressure
Use this option to evacuate the manifold and zero the selected transducers. The Calibrate Pres-
sure Offset dialog is displayed.
Choose the transducer(s) you wish to have offset to zero. Be sure to install a sample tube on
the selected ports. Click Start; a dialog indicating evacuation is in progress is displayed. When
evacuation is complete, the dialog closes automatically.
Mar 08 6-27
Calibration TriStar II 3020
Match Transducers
Use this option to zero and match the selected transducers to the main manifold transducer.
Choose the transducer(s) you wish to have matched. Be sure to install a sample tube on the
selected ports. Click Start; a progress dialog is displayed. When the operation is complete, a
confirmation dialog is displayed; click OK to close the dialog.
Servo Valve
Use this option to calibrate the servo valve to the manifold pressure transducer. The servo
valve should always be recalibrated after a pressure calibration has been performed. The Cali-
brate Servo Valve dialog is displayed.
The only action required here is to click Start. The servo valve is then used to fill and equili-
brate the manifold, first to approximately 760 mmHg and then to approximately 50 mmHg.
The pressure transducer readings (previously calibrated) at these points are used to calibrate
the servo set point. Status messages are displayed during this procedure and a confirmation
dialog is displayed when the operation is finished; click OK to close the dialog.
6-28 Mar 08
TriStar II 3020 Calibration
Store Instrument Information
This option enables you to store calibration information in a text file, allowing you to view cal-
ibration parameters. When you select this option, the information is stored and a dialog giving
the location of the saved file is displayed.
Make a note of the location, then use a utility such as Notepad to open the file.
Save to File
Use this dialog to save the current calibration settings to a file that you can reload; the Select
Calibration File dialog is displayed.
File name The default for naming calibration files is the serial number,
then the next sequenced number. For example in the dialog
shown above, the number has defaulted to 201-002.CAL,
where 201 represents the instrument serial number and 002
represents the second calibration file saved.
You can enter a different name if you wish; up to eight

characters.
Mar 08 6-29
Service Test TriStar II 3020
Load from File
Displays the Select Calibration File dialog (shown above) so that you can load a different cali-
bration file. When you choose a file and click OK, the following dialog is displayed.
This error message states that changing your calibration may affect the performance of your
instrument. If you click Yes to continue, the selected file is loaded and a backup of the current
calibration is saved as (SN)last.cal allowing you to reload the settings using the backup file.
Although a backup file is created, it is recommended that you save the current calibration set-
tings using the Save to File command before loading another file. A backup file is written over
each time a new one is created. The Save to File function saves the file permanently.
Service Test
Certain service tests are included in the operating program, but can be performed only with
the assistance of a trained Micromeritics service representative. These tests are designed to
provide your service representative with instrument readouts, as well as to assist him in trou-
bleshooting potential problems and, perhaps, eliminating unnecessary repair services. This
service strategy allows you to conduct expert tests in less time than it would take to be prop-
erly trained in servicing the instrument.
This option is enabled only when the analysis program is operating in Service Test mode
(refer to Service Test Mode, page 8-15 for additional information).
6-30 Mar 08
7. REPORTS MENU
This chapter describes the commands on the Reports menu; it also contains examples of
reports.
Reports can be generated for data:
• collected on a sample that has completed analysis
• collected on a sample that is currently being analyzed (includes only the information
collected up to the time of the report)
• that is manually entered
Description
Listed below are brief descriptions of the commands contained on the Reports menu. Detailed
descriptions follow this section.
Start Report Allows you to generate a report on a completed sample

analysis or on the data collected thus far for an analysis in
progress. Page 7-3.
Close Reports Closes all open report windows. Page 7-5.
Open Report Enables you to open a report that was saved from the report
window. Page 7-5.
SPC Report Options Allows you to specify the sample data to be included in SPC
reports. Page 7-6.
Mar 08 7-1
Regression Report Allows you to generate a regression report. Page 7-7.
Control Chart Allows you to generate a control chart report. Page 7-11.
Heat of Adsorption Allows you to generate a heat of adsorption report.

Page 7-15.
7-2 Mar 08
TriStar II 3020 Start Report
Start Report
Select this option to generate a report on a sample analysis; the Start Report dialog is
displayed.
File name The name of the sample file you select from the Files list
window is copied to this field. If you select multiple files, the
last one selected is displayed. If you have a sample file open,
its name defaults to this field.
• If you select multiple files on which to have reports gen-

erated, the reports specified in each sample file are
printed to the output destination.
• If you choose a single file, the Select Reports dialog con-

taining the available reports is displayed.
Mar 08 7-3
Start Report TriStar II 3020
Status This drop-down list determines what type of sample files are
displayed in the Files list window in the specified directory
for all dates, or within the specified range of dates (using
Date Range push button). Refer to Table 2-2. File Status
and Description, page 2-12 for a description of status types.
Date Range Displays the Select Dates dialog so that you may specify a
range of dates. Refer to Selecting Files, page 2-11 for a
description of this push button.
Copies Enabled when the Printer destination is chosen, enabling

you to print up to four copies of the selected report(s).
Destination Enables you to print to a printer, to the screen, or to a file.
If you select Screen, reports are displayed onscreen, allowing

flexibility in manipulating and customizing reports. Refer to
Printed Reports, page 7-19 for detailed information.
If you select File, the tabular reports of the requested file are
converted to a text file which can be viewed with a text editor
or other text file manipulation tool.
File name Enabled when you select File as the destination. Allows you
to enter a name, or you may accept the default.
Files list box Displays a list of the available sample files for the choice
shown in the Status field and within the range of dates
specified in the Select Dates dialog.
Directories Displays a list of available drives and directories. The drive

and directory last accessed is displayed immediately above
the Directories list box.
7-4 Mar 08
TriStar II 3020 Close Reports
Close Reports
This option enables you to close all open report windows at one time. This avoids having to
select close on each report window. This option is unavailable if reports are being generated.
Open Report
This option enables you to open a report that was saved from the Report window; the Report
window opens with an Open dialog positioned on top.
Report Window
After you navigate to the desired directory, select your file, and click Open, your saved report
is displayed in the Report window.
Mar 08 7-5
SPC Report Options TriStar II 3020
SPC Report Options
When you select SPC Report Options, the SPC Report Options dialog is displayed.
The SPC Calculations dialog lists the variables available for SPC reporting. You can check as
many as desired. However, for efficiency, it is best to select only the variables you actually
intend to us. All variables selected must be computed for each sample file used in an SPC
report.
Click More on this dialog to display the SPC Calculations dialog.
The options on this dialog allow more detailed reports.
7-6 Mar 08
TriStar II 3020 Regression Report
Regression Report
Select this option to generate a regression report. The regression report is used to determine
the interdependency between two variables. Up to three dependent variables (Y-axis) may be
plotted against a single independent variable (X-axis). The degree of correlation between the
variables also is reported. The graphs for the regression report are scaled so that all three fit
on a single page. If you choose less than three, the graphs are scaled to fill most of the page.
Show report title Select this option to have a title display on your report.
Accept the default or enter a new title. You can enter up to 40
alphanumeric characters.
Deselect this option to omit the report title.
Show graphic Select this option to have a graphic display above your report
title. For example, you may wish to display your company
logo. The graphic must be a bitmap (bmp) or enhanced
metafile (emf).
Click Browse to choose the file, then use the Height and
Width fields to specify a size. This image can be edited in the
report window (when printed to the screen), or removed if
desired.
Mar 08 7-7
Regression Report TriStar II 3020
X- and Y-Axes Allows you to designate the X- and Y-axes variables. Click
Variable fields on the down arrow to display a list of variables. The variables
in this list are the ones you specified in the SPC report
options dialog.
With this option, you can plot the regression of up to three Y-

axis variables against the X-axis variable. The X-axis
specifies the independent variable for the regression, while
the Y-axes provide the dependent variables.
Axis Range Enables you to specify the beginning and ending values for
the X- and Y-axis ranges. Data collected outside these ranges
are not included in the plot. These fields are disabled if you
choose Autoscale.
Autoscale Allows you to have the X- and/or Y-axes scaled

automatically.
Recalculate archived Select this option to have archived SPC values recalculated.
SPC results This ensures that any changes made to the SPC Report
Options are included in the new report; however, it does
lengthen the time required to generate the report.
Tabular report Enables you to generate tabular, as well as graphical, data of

the included samples. A tabular report contains the numeric
values contributed by each sample.
Label data Allows you to label the points on the plot to correspond with
the values in the sample files.
Samples Displays the Regression Report Sample Selection dialog,

allowing you to choose the sample files you wish to have
reported.
7-8 Mar 08
TriStar II 3020 Regression Report
File name Use this field to limit the files displayed in the Available Files
pane. For example; enter g*.smp to display only the files
beginning with a g.
Status This drop-down list determines the type of sample files that
display in the Available Files pane in the selected directory
for all dates, or within the specified range of dates (using
Date Range push button). Refer to Table 2-2. File Status
and Description, page 2-12 for an explanation of the Status
types.
Date Range Displays the Select Dates dialog so that you can specify a
range of dates. Refer to Selecting Files, page 2-12 for an
explanation of this push button.
Use all files in Select this option to include all files from the selected
this directory directory in the report.
Directories Lists the current directory. Use the directory window to

navigate to a different directory. Refer to Selecting Files,
page 2-13 for information on selecting different directories.
Mar 08 7-9
Regression Report TriStar II 3020
Add Moves the selected file in the Available Files pane to the
Selected Files pane. Alternatively, you can simply double-
click on the desired file(s). You can select multiple files by
holding down Ctrl while making your selections. You can
include up to 200 sample files.
Remove Removes the selected file from the Selected Files pane and
places it back into the Available Files pane.
Save As Default Saves the current definition of the report as the default.
Report Settings The options in this group box enable you to choose output
criteria.
The Copies field is enabled when you choose Printer as the

destination, enabling you to print up to four copies of the
report.
Report Generates the report.
7-10 Mar 08
TriStar II 3020 Control Chart
Control Chart
This option enables you to generate a control chart report which plots the changes in a
statistic.
Show report title Select this option to have a title display on your report.
Accept the default or enter a new title. You can enter up to
40 alphanumeric characters.
Deselect this option to omit the report title.
Show graphic Select this option to have a graphic display above your report
title. For example, you may wish to display your company
logo. The graphic must be a bitmap (bmp) or enhanced meta-
file (emf).
Click Browse to choose the file, then use the Height and
Width fields to specify a size. This image can be edited in
the report window (when printed to the screen), or removed
if desired.
Mar 08 7-11
Control Chart TriStar II 3020
X-axis Order By Enables you to choose the order in which X-axis statistics
are placed. You can have them placed by Time, File name,
Date, Minutes, or Days.
Time places the files on the graph at numerical points in the

order of the date/time the files are analyzed.
File name places the files on the graph at numerical points

in alphanumeric order.
Date places the files on the graph at points representing the

actual date/time the files are analyzed.
Minutes places the files on the graph at points representing

the minutes that have elapsed from the first file placed on the
list, which is the earliest-analyzed file.
Days places the files on the graph at points representing the

number of days that have elapsed from the first file placed
on the list, which the earliest-analyzed file.
Graph [n] Displays the Control Chart Graph [n] Options dialog,
allowing you to define the Y-axis of each graph.
Statistic This drop-down list displays the SPC variables selected on

the SPC Report Options dialog. The variable you choose will
be plotted against time.
7-12 Mar 08
TriStar II 3020 Control Chart
Autoscale Allows you to have the Y-axis scaled automatically. If you

wish to specify a range, deselect this option and enter a range
in the From and To fields.
Center Line Displays placement options for the variable’s optional value.
Choose Entered to specify placement of the line.
Limit Lines Displays the options available for limiting lines. You can
have the lines placed at some multiple of the standard
deviation or at specified positions (Entered).
When you select Entered, the High limit and Low limit
fields are enabled, allowing you to enter appropriate values.
Tabular report Allows you to generate tabular, as well as graphical, data of

the included samples. A tabular report contains the numeric
values contributed by each sample.
Recalculate archived Select this option to have archived SPC values recalculated.
SPC results This ensures that any changes made to the SPC Report
Options are included in the new report. It also lengthens the
time required to generate the report.
Samples Displays the Control Chart Sample Selection dialog, allowing

you to choose the sample files on which you wish to report.
Mar 08 7-13
Control Chart TriStar II 3020
Samples This dialog functions in the same manner as the Regression

Report Sample Selection Dialog explained earlier in this
(continued) chapter. Refer to page 7-8 if you need assistance on the fields
of this dialog.
Save as Default Saves the current definition of the report as the default.
Report Settings The options in this group box enable you to choose output
criteria.
The Copies field is enabled when you choose Printer as the

destination, enabling you to print up to four copies of the
report.
7-14 Mar 08
TriStar II 3020 Heat of Adsorption Report
Heat of Adsorption Report

The isosteric heat of adsorption is an important parameter for characterizing the surface heter-
ogeneity and for providing information about the adsorbent and the adsorption capacity.
Multiple adsorption isotherms are obtained on the same sample using the same adsorptive but
at different temperatures to obtain the heat of adsorption.
This option allows you to choose the sample files, define the quantities, and generate a Heat of
Adsorption report; the Heat of Adsorption dialog is displayed.
Table Contains the files you choose; also lists the quantity
adsorbed.
Add Samples Displays the Select Samples dialog so that you can choose
desired files.
Remove Samples Removes the selected sample from the list. If no samples are
selected, the last one is removed.
Clear Samples Removes all samples from the list.
Mar 08 7-15
Heat of Adsorption Report TriStar II 3020
Edit Quantities Displays the Edit Quantities Adsorbed dialog so that you can
specify the range of surface coverage to include in the heat of
adsorption report.
Quantity Adsorbed Allows you to enter the points.

table
Insert Range Displays the Insert Quantity Range dialog.
This dialog allows you to specify the starting and ending

quantities adsorbed, as well as the number of points to insert
within the specified range.
Insert Inserts a row above the selected row.
7-16 Mar 08
TriStar II 3020 Heat of Adsorption Report
Clear Clears the entire table of all entries except one; one is
required.
Load Table Allows you to import a previously saved table.
Save Table Allows you to save the current table as a file (QNT
extension).
Report Settings The options in this group box allow you to choose report
criteria.
Show report title Choose this option to have a title display in the header of
your report; use the adjacent field to enter the title.
Show graphic This option allows you to have a graphic appear in your title;
for example, you may wish to show your company logo. You
can use a bitmap or an enhanced metafile.
Use the Height and Width fields to define a size.
Tabular report Select this option to have data generated in a tabular format.
Isostere plot Select this option to generate a graph showing quantities of

gas adsorbed vs. the temperature.
Heat of adsorption Select this option to generate the Heat of Adsorption data in a
plot graphical format.
Copies Enabled when you choose Printer as the destination,

allowing you to print up to four copies of your report(s).
Destination Enables you to choose a destination for your reports.
File name Enabled when you choose File as the destination, allowing
you to enter a name (or you can accept the default).
Open Enables you to open a previously saved report.
Mar 08 7-17
Heat of Adsorption Report TriStar II 3020
Save Saves the current report.
7-18 Mar 08
TriStar II 3020 Printed Reports
Printed Reports
Header
All printed reports (either to the screen or to a printer) contain a header displaying file
statistics.
If specified, the report header can also contain a graphic (such as a company logo) and a title.
• Tabular and graphical reports contain sample and instrument statistics such as date and
time of analysis, analysis conditions, and so forth.
The headers for these reports also contain notes of any changes to the sample file that
occur after analysis.
• Summary report headers contain the same type of information displayed in tabular and
graphical reports with the exception of notes.
Onscreen Reports
The report window containing onscreen reports provides many options for customizing and
manipulating reports:
• a tool bar
• shortcut menus
• zoom feature
• axis cross hairs
When reports are printed to the screen, they are printed in a window like the one shown below.
Each requested report is listed in the Reports window on the tool bar; they are also indicated
by selectable tabs across the top of the report header. To view a specific report, select its tab or
select the report in the Reports window and click Show.
Mar 08 7-19
Printed Reports TriStar II 3020
Tabs display for each type of report you generate.
Header
List of reports
requested.
Options or
Tool Bar
Displays
graphical
(or tabular)
data.
Tool Bar
Reports Contains a list of all requested reports.
Show Shows the selected report in the report window. If the report
has been hidden, it and its associated tab will become
visible.
7-20 Mar 08
Delete Deletes the selected report. A deletion confirmation dialog is

displayed since this function cannot be undone. The deleted
report(s) will have to be regenerated if deleted in error.
Hide Hides (removes) the selected report from the report window.
The report’s associated tab is also removed.
Open Allows you to open a previously saved report file.
Print Displays a print dialog so that you can choose an appropriate

printer for report output. A list of available reports is
displayed in the window on the right side of the dialog.
For convenience in selecting which reports to print, push

buttons are provided beneath the report window. Or, you can
make your selection by clicking on the desired reports.
Current selects the report displayed in the report window.
Shown selects only the shown reports; any nonhighlighted

reports indicate they are hidden. You can still select hidden
reports from this window to print.
All selects all reports, including those that may have been
hidden.
Clear clears all selections.
Mar 08 7-21
Save Saves all reports of the currently open file in a report format
using the same name as the sample file, only with an rep
extension. If you wish to specify a name and/or specific
reports to save, use the Save As push button.
Save As Saves all or specified reports from the currently open file.
The push buttons displayed on this dialog perform in the
same manner as the print dialog (explained above).
Reports can be saved in three different formats:
Report system (*.rep): Saved in a format which allows you

to reopen the file using the Open push button on the Report
window tool bar.
Spreadsheet (*.xls): Saved in a format which can be

imported into most spreadsheet programs.
Ascii Text (*.txt): Saved in ASCII text which can be

imported into programs accepting this type of file.
Default Style Displays the Default Style dialog so that you can specify
default parameters for report fonts and curve properties.
Font Contains a list of report elements for which the font can be
edited. Simply highlight the desired element and click Edit; a
font dialog is displayed so that you can specify the desired
font and attributes.
Curve The items in this group box enable you to specify a thickness
for report curves and, when using histograms, the type of fill
to apply.
7-22 Mar 08
Graph border line Enables you to specify a thickness for the border of the graph.
thickness
Load Loads the last saved defaults.
Save Saves the changes as the defaults. If you do not click Save,
the changes will apply to the current report set only. The next
reports will revert to the defaults.
Close Closes the dialog and applies the changes. If you clicked
Save, the changes become the defaults. If you did not click
Save, the changes apply to the current report only.
Close Closes the report window.
Mar 08 7-23
Shortcut Menus
Shortcut menus are accessed when you right-click on the tabular or graphical portion of a
report.
Tabular Reports
Resize column Displays a dialog so that you can specify the width of the
selected column (in inches).
Rename column Displays a dialog so that you can edit the name of the
selected column. Use to insert line feeds.
Move column Allows you to move the location of the selected column to
the left or to the right.
Align column Enables you to right-align, left-align, or center the data in the
selected column.
Hide column Displays a list of all columns, enabling you to select the one
you wish to hide.
Show column Displays a list of all hidden columns, enabling you to select
the one you wish to have shown again.
Column font Displays a Font dialog, allowing you to change font attributes
for the tabular data in the current report.
7-24 Mar 08
Header font Displays a Font dialog, allowing you to change font attributes
for column headers in the current report.
Edit title Allows you to edit the table title and font.
Copy table as text Enables you to copy the entire table (column headers and
data) and then insert it into another program. Columns are
tab-delimited, allowing easy alignment.
Graphs
Autoscale Autoscales all axes of the graph. This function is useful for
returning to a full view after having zoomed in.
Show curve Shows any curve(s) that has been hidden. This option is
disabled (greyed) if no curves have been hidden.
Hide curve Hides (removes from view) any unwanted curve(s)
Mar 08 7-25
Edit curve Displays the Curve Properties dialog, allowing you to edit
curve properties.
Title Displays the title of the curve you are editing.
Style Drop-down list containing styles in which collected data can

be displayed.
Choices: Curve, Histogram, Points, Curve and Points
Curve group box Contains options for curves and points. You can edit the
curve interpolation, the style of curve and/or points, as well
as the pen color. The options in this group box are disabled if
Histogram is chosen in the Style drop-down list.
Histogram group box Allows you to specify the type of fill as well as the color if
Histogram is chosen as the style for collected data.
7-26 Mar 08
Edit axis Displays the Axis Properties dialog, allowing you to edit axis
properties.
Edit legend Displays the Legend Properties dialog, allowing you to edit
the placement of the legend.
Edit title Displays the Title Properties dialog, allowing you to edit the
current graph’s title and font.
Copy as metafile Copies the graph and places it on the clipboard, allowing you
to paste it into other applications accepting Windows
metafiles.
Copy as text Copies the data used to generate the graph as a series of tab-
delimited columns of text.
Mar 08 7-27
Zoom Feature
A zoom feature is included with the report system so that you can zoom in to examine fine
details. To use this feature, simply hold down the left mouse button and drag the mouse cursor
(drawing a box) across the area you wish to view; then release the button. The enlarged area
immediately fills the graph area. Right-click in the graph area and choose Autoscale from the
shortcut menu to return to the normal view
Axis Cross Hair
A cross-hair function is available so that you can view axis coordinates. To use this feature,
simply left-click in the desired area of the graph.
X-axis position
Point of coordination Y-axis position
Right-click in the graph area and choose Autoscale or Redraw from the shortcut menu to
remove cross-hair lines and return to the normal view. Alternatively, you can click outside of
the graph area.
7-28 Mar 08
TriStar II 3020 Report Examples
Report Examples
The remainder of this section contains samples of some of the reports which may be generated
by the TriStarII 3020 Analysis Program. Most of the reports can be varied through entries on
the report options dialogs.
Mar 08 7-29
Report Examples TriStar II 3020
Isotherm Plot
7-30 Mar 08
BET Surface Area Report
Mar 08 7-31
BET Surface Area Plot
7-32 Mar 08
t-Plot Report
Mar 08 7-33
BJH Adsorption: Cumulative Pore Area
7-34 Mar 08
BJH Desorption: Pore Volume Plot
Mar 08 7-35
Dollimore-Heal Desorption: Pore Volume/Area
7-36 Mar 08
Summary Report
Mar 08 7-37
Sample Log Report
7-38 Mar 08
8. OPTIONS MENU
The commands on the Options menu allow you to configure the system to your laboratory’s
requirements and specify defaults for sample and parameter files.
Description
Listed below are brief descriptions of the commands on the Options menu. Detailed descrip-
tions follow this section.
Option presentation Allows you to display the sample file dialog in either Basic,
Advanced, or Restricted format. Page 8-2.
Sample defaults Allows you to specify defaults for the parameters contained
in the sample information and parameter files. Page 8-6.
Units Allows you to choose the types of units to use for

measurement, pressure, and temperature. Page 8-12.
Graph Grid Lines Enables you to choose the types of grid lines to display for
the X- and Y-axes. Page 8-13.
Live Graph Enables you to choose the variable for the X-axis during data
collection. Page 8-14.
Parameter files directory Allows you to specify a location for the predefined parameter
files used by the Basic and Restricted formats. Page 8-15.
Service Test Mode Enables you to perform certain troubleshooting procedures

under the direction of a Micromeritics service representative.
Page 8-15.
Mar 09 8-1
Option Presentation TriStar II 3020
Option Presentation
The sample editing dialogs for the TriStar 3020 analysis program may be presented in three
different formats: Advanced, Basic, or Restricted.
Each format displays sample information and menu options differently.
• Advanced: displays all parts of the sample information file in a tabbed dialog as in an
index card file. Clicking on each tab opens an associated dialog. Use this format to edit
parameter files or create customized sample files.
• Basic: displays the sample file and parameter files in a single dialog. Use this format to
create sample files using previously created parameter files.
• Restricted: displays in the same manner as the Basic format. This format also is used to
create sample files using previously created parameter files. However, you cannot
switch to the Advanced format to edit parameters. You must also use a password for
entering and exiting this format.
8-2 Mar 09
TriStar II 3020 Option Presentation
Advanced
The Advanced format presents all parts of the sample information file in a tabbed dialog. For
example, if you wish to open or create a sample file using the Advanced format, the following
If you are opening com-

pleted file, thisdialog also
contains a tab for Col-
lected Data.
The Advanced format is used to create customized sample files — easily and quickly. Simply
click on the tabs to display its associated dialog. You can also switch to the Basic format, if
desired, by clicking Basic. Refer to Advanced, page 5-5 for a detailed description of this
dialog.
Mar 09 8-3
Option Presentation TriStar II 3020
Basic
The Basic format presents the sample information file and its parameter files in a single dialog.
For example, if you wish to open or create a sample information file using the Basic format,
the dialog is displayed in this manner.
The Basic format is used to create sample information files using previously defined parame-
ter files. You can easily switch to Advanced format, if desired, by clicking Advanced. Refer to
Basic, page 5-8 for a detailed description of this dialog.
8-4 Mar 09
TriStar II 3020 Option Presentation
Restricted
The Restricted format is identical to the Basic format, except that certain menu options are dis-
abled, and you cannot switch to the Advanced format. This format is password-protected and
is typically used in laboratories where analysis conditions must remain constant, for example,
in the pharmaceutical industry.
Does not contain the

Advanced push button
allowing access to
parameter files.
When you select Restricted, a dialog requesting a password is displayed:
Any password (up to 31 characters) can be used to enable the Restricted format. The same
password, however, must be used to exit the Restricted format. For example, if you enter
“password” to enable the Restricted format, then you must use “password” to exit. If you for-
get the password, open the system INI file and navigate to the Private section. The current
password will be shown immediately following “OptionPresentationPassword.” Make a note
of the password, exit the INI file, and enter the password where requested. Do not attempt to
delete the password in the INI file.
Mar 09 8-5
Sample Defaults TriStar II 3020
Sample Defaults
This option allows you to specify default parameters for sample information files and parame-
ter files. You can specify default values using the Advanced or Basic format.
Advanced
When you select Sample Defaults while in the Advanced format, the Sample Defaults dialog
is displayed. The values you specify for parameters of the Advanced sample information file
serve as the parameter file defaults. For example, the values specified for the Analysis Condi-
tions portion of the Advanced sample file display as the defaults for a newly created Analysis
Conditions file..
Sequence Specify a default sequence for the sample file name. The
number you specify is sequenced incrementally each time
you create a sample file. It is the number that appears in the
File name field when you select File > Open > Sample
information.
• Use numbers, letters, or other printable characters, such

as dashes. Do not use special characters such as * or ?.
At least three numbers must be included.
• Use up to eight characters.
8-6 Mar 09
TriStar II 3020 Sample Defaults
Sample Allows you to enter an additional identification that provides

more information than the sample file name alone.
In the field on the left, edit the prompt for Sample if you
wish. For example, you may prefer to use Test or Material.
The maximum number of characters is 20.
In the field on the right, specify a format for the sample

identification.

as dashes.
• Maximum number of characters is 42, plus the $ symbol.
• Include the automatically generated file name as part of

the identification by using the $ symbol where you want
the sequence number to appear.
For example, if the sequence number is 000-001, enter

the sample identification as follows:
Lab #25 - $
The resulting sample identification for the first sample

information file would be:
Lab #25 - 000-001
and the second:
Lab #25 - 000-002, and so on.
Operator Allow you to enter the name (or other identification) of the
Submitter operator performing the analysis and the name of the person,
department, customer, etc. that submitted the sample for
analysis.
The fields on the left can be edited to display something

other than Operator and Submitter if you like.
The fields on the right allow you to specify default names or

titles.
• Include the automatically generated file name as part of

the identification by using the symbol $ where you want
the sequence number to appear. Refer to the example in
the previous section.
Mar 09 8-7
Operator • Maximum number of characters for the prompt is 20.

Submitter
• Maximum number of characters for the identification is
(continued) 42, including the $ symbol.
• Omit this item entirely from the sample information file

by selecting Omit.
Mass You can choose to enter a sample mass or have the mass auto-
matically calculated. Regardless of which option you choose
for your default, you can change it in the sample file.
Enter Enables the Sample Mass field allowing you to enter a

default value.
you to enter default values. These values are used to calculate
the mass of the sample,
Density Enter a default density. If there is a material you analyze quite

often, you may wish to use its default in this field. This value
can be edited in the sample information file.
Type of Data Choose the manner in which you typically display data.
User Parameters The fields in this group box are used primarily for SPC (Sta-
tistical Process Control) reporting. They are used to specify
characteristics of the sample or its manufacturing process.
Once specified, these parameters display on the sample edi-

tor and in the SPC Sample Options dialog (accessed through
the SPC Report Options dialog).
These fields can also be used to record analysis conditions or

sample information so that it can be printed on the Summary
report.
Select Omit if you do not wish to use these fields; this will
prevent them from displaying on the sample information dia-
log.
8-8 Mar 09
Comments Allows you to enter comments about the sample or its

analysis conditions. Anything you enter in this window is
printed in the report header.
Add Log Entry Allows you to enter comments about the sample or its
analysis conditions. Anything you enter using this option
appears in the Instrument Log Report; it does not display in
the report header.
Replace All Allows you to replace the contents of all parameter files
contained in the current default sample file with those from
an existing sample file. For example, you may have an
existing sample file that contains most (or all) of the
parameters that you wish to use. You can select this push
button, choose the file, and then OK. All parameter files of
the file you choose are copied into the sample defaults dialog.
You can even change the values in these files (if needed)
without affecting the file from which they were copied.
Click on each remaining tab of the Advanced Sample dialog to complete sample defaults and
establish parameter defaults. Refer to the following sections if you need assistance on the
fields of these dialogs.
• Sample Tube, page 5-11

• Degas Conditions, page 5-13
• Analysis Conditions, page 5-15
• Adsorptive Properties, page 5-28
• Report Options, page 5-31
Mar 09 8-9
Basic
When you select Sample Defaults while using the Basic format, the Sample Defaults dialog is
displayed. The values you specify for the Basic format also apply to the Restricted format..
Sequence Specify a default sequence for the sample file name. The
number you specify is sequenced incrementally each time
you create a sample file. It is the number that appears in the
File name field when you select File > Open > Sample
information.

as dashes. Do not use special characters such as * or ?.
At least three numbers must be included.
• Use up to eight characters.
Sample Allows you to enter an additional identification that provides

more information than the sample file name alone.
• In the field on the left, edit the prompt for Sample if you
wish. For example, you may prefer to use Test or Mate-
rial. The maximum number of characters is 20.
• In the field on the right, specify a format for the sample

identification.

as dashes.
8-10 Mar 09
Sample • Maximum number of characters is 42, plus the $ symbol.
(continued) • Include the automatically generated file name as part of

the identification by using the $ symbol where you want
the sequence number to appear.
For example, if the sequence number is 000-001, enter

the sample identification as follows:
Lab #25 - $
The resulting sample identification for the first sample

information file would be:
Lab #25 - 000-001
and the second:
Lab #25 - 000-002, and so on.
Mass You can choose to enter a sample mass or have the mass auto-
matically calculated. Regardless of which option you choose
for your default, you can change it in the sample file.
Enter Enables the Sample Mass field allowing you to enter a

default value.
you to enter default values. These values are used to calculate
the mass of the sample,
Density Enter the density of the material you are analyzing.
Sample tube Each parameter contains a drop-down list containing

Degas conditions predefined parameter files, some of which were included
Analysis conditions with the software. Choose the file you wish to use as the
Adsorptive properties default.
Report options
Mar 09 8-11
Units TriStar II 3020
Replace all Allows you to replace all parameters of the default sample
file you are creating with parameters from an existing sample
file. For example, you may have an existing sample file that
contains most (or all) of hte parameters that you wish to use.
You can click this push button, choose the file, and then OK.
All parameters ofthe file you choose are copied into
thesample defaults dialog. You can edit the values if desired
without changing the file from which they were copied.
Save Saves the specified defaults.
Units
This menu command displays the Units Selections dialog which allows you to choose the
manner in which to display data on reports.
8-12 Mar 09
TriStar II 3020 Graph Grid Lines
Graph Grid Lines

Graph Grid Lines enables you to choose the type(s) of grid lines to show on your reports; the
Graph Grid Lines dialog is displayed.
X-Axis Enables you to choose Major and/or Minor lines to

Y-Axis display in printed reports for the Logarithmic and Linear
scales.
If you deselect these items (remove the check marks),

your report will not display grid lines.
Grid Line Style Allows you to choose the type of grid line to display if
grid lines are being shown.
Mar 09 8-13
Live Graph TriStar II 3020
Live Graph
This option enables you to choose the variable for the x-axis during data collection. You can
also choose to correct for thermal transpiration which should always be selected for micropore
analyses (refer to page 5-33 for additional information on thermal transpiration).
8-14 Mar 09
TriStar II 3020 Parameter Files Directory
Parameter Files Directory

This option allows you to select the location for the predefined parameter files displayed in the
drop-down lists on the Basic and Restricted Sample Information dialogs. The current directory
specified for parameter files is displayed above the directory window.
When you select this option, the Parameter File Directory Selection dialog is displayed.
The directory specified here is the one you should use when creating parameter files to be
included in the drop-down lists on the Basic and Restricted sample information dialogs. It is
where the software goes to obtain the files for the drop-down lists. The default directory is
param and includes several parameter files supplied with the analysis program. If you specify
a different directory, these files will not be included in the drop-down lists unless you copy (or
move) them to the new directory.
If you wish to continue to use the param directory for parameter files, it will display as the
default when saving parameter files.
Service Test Mode

Certain service tests are included in the TriStar operating program. These tests, however, can
be performed only with the assistance of a trained Micromeritics service representative. When
you select Options > Service Test Mode, a dialog prompting you to enter a password is dis-
played. This password is supplied by your service representative. You will be unable to
perform these tests without his guidance.
After Service Test Mode has been enabled, the tests are accessible from the Unit menu.
Mar 09 8-15
TriStar II 3020 Troubleshooting
9. TROUBLESHOOTING AND MAINTENANCE
The TriStar system has been designed to provide efficient and continuous service. However,
certain maintenance procedures should be followed to obtain the best results over the longest
period of time. This chapter includes maintenance procedures and calibration procedures.
Troubleshooting
Most operational problems are caused by:
• Leaks (commonly around the sample tube O-ring at the analysis port)
• Sample weighing errors
• Use of too much analysis bath fluid in the Dewar at the start of an analysis
• Entry of incorrect system volume for analysis
• Impure gas supply
Always check these first when expected analysis results are not obtained. Some common oper-
ational problems, which are not indicated on the video monitor screen, and their respective
causes and solutions are provided in the following table.
What Happened Why What To Do
Analysis Dewar cannot Elevator that moves Dewar is Check for possible obstruction to
be raised (or lowered). stuck. elevator movement.
Vacuum pump is noisy. Sample tube connector is loose. Tighten fitting. Replace O-ring.
Sample tube O-ring is worn or Replace O-ring. Refer to
cracked. Replacing the Sample Tube O-
ring, page 9-7
Sample tube is cracked. Replace with new sample tube.
No sample tube loaded on a Install plug or empty sample

selected port. tube.
Gas inlet valve open while With manual control enabled, use
vacuum valve open. the instrument schematic to close
gas inlet valve.
Analysis valves cannot Cable from computer to the Make sure the cable is connected
be operated. instrument is loose. properly.
Mar 08 9-1
Troubleshooting TriStar II 3020
What Happened Why What To Do
Sample is not within There may be a leak into or out of Refer to Performing a Leak
specifications. the manifold. Test, page 9-16.
Gas may be contaminated. Perform a blank analysis. If

results are okay, perform a
reference material analysis.
Incorrect type of gas line. Be sure your gas line is all metal;
it is best to use the one shipped
with the instrument. Do not use
polymer gas lines or flexible gas
lines that may be internally
coated with a polymer.
Elevator is noisy. The elevator screw may need Contact your Micromeritics
greasing. Service Representative.
9-2 Mar 08
TriStar II 3020 Preventive Maintenance
Preventive Maintenance
The table below lists the preventive maintenance procedures you should complete to keep
your analyzer operating at peak performance. Instructions for each procedure follow the table.
Micromeritics also recommends that you have preventive maintenance procedures and cali-
bration performed by one of our service representatives every 12 months.
Maintenance Required Frequency
Check and clean Dewar, page 9-4 Weekly
Replace port filters and O-rings, page 9-6 Every 3 to 6 months
Replace sample tube O-ring, page 9-7 As required or every 3 to 6 months
Inspect and change vacuum pump fluid*, page 9-8 As required or every 3 to 6 months
Replace alumina in oil vapor traps*, page 9-11 As required
Clean the outside of the analyzer, page 9-4 As required or every 6 months
Test analyzer for leaks, page 9-16 As required or every 12 months
Replace vacuum pump exhaust filter, page 9-15 As required or every 12 months
Replace diaphragm in vacuum pump (if an oil-free Every 12 months

pump is used)**
*Oil-sealed vacuum pumps only.
**For oil-free pumps only: After 12 to 18 months of operation, the diaphragm in the pump
will wear out and the pump becomes completely inoperable. To prevent any instrument
downtime due to an inoperable pump, it is recommend that you have the diaphragm replaced
by a Micromeritics Service Representative every 12 months.
Mar 08 9-3
Preventive Maintenance TriStar II 3020
Lubricating Elevator Drive Assembly
The elevator screw should not require lubricating; it is lubricated before it leaves the factory. If
your elevator starts to vibrate or become noisy when traveling, contact your Micromeritics
Service representative for disposition.
Cleaning the Analyzer
The exterior casing of the analyzer may be cleaned using a clean cloth, dampened with isopro-
pyl alcohol (IPA), a mild detergent, or a 3% hydrogen peroxide solution. Do not use any type
of abrasive cleaner.
Do not allow liquid to penetrate the casing of the analyzer. Doing so could result in
damage to the unit.
Cleaning the Analysis Dewar
When handling Dewars, be sure to observe the Dewar precautions outlined in

Installing the Analysis Dewar, page 3-25.
Ice and suspended frost particles may accumulate in the bottom of an analysis port Dewar. Par-
ticles or deposits exceeding 1/4 in. (0.64 cm) in depth may jam between the bottom of the
sample tubes and the bottom of the Dewar, causing the Dewar not to raise fully. Accumula-
tions of fine particles impede liquid nitrogen circulation around the bottom of the sample
tubes. This causes the sample temperature to be slightly higher which, in turn, can cause pore
volume measurement errors in those samples exhibiting high isotherm slope above 0.97 rela-
tive pressure.
Accumulated ice is likely to melt and form a pool of water in the Dewar if all liquid nitrogen
evaporates. The water must be removed; otherwise it will solidify when liquid nitrogen is
added and could press on the bottom of the sample tube causing breakage.
To ensure problems do not develop due to ice accumulation, check the Dewar after each use.
Clean the Dewar on a weekly basis.
1. Remove the sample tubes from the analysis ports.
2. Select Unit [n] > Show Instrument Schematic to display the instrument schematic, then
Unit [n] > Enable Manual Control.
9-4 Mar 08
3. Right-click on the elevator icon and select Lower to lower the elevator to its lowest
position.
4. Remove the Dewar and pour the liquid nitrogen from the Dewar into an appropriate
cryogenic container.
Do not pour liquid nitrogen directly into a sink. Doing so may cuase drain pipes to
burst.
5. Rinse the Dewar with warm water to melt any ice accumulation which may remain in the
Dewar, then dry thoroughly.
Mar 08 9-5
Replacing Port Filter and O-ring
A 20-µm filter (frit) is located in each analysis port. If the filter is contaminated, the contami-
nant may adsorb or desorb during analysis, affecting the results. A contaminated filter on the
analysis port may be indicated by a leak or by a free-space reading much lower than normal.
A contaminated filter should be replaced as follows:
1. Select Unit [n] > Show Instrument Schematic, then Unit [n] > Enable Manual
Control.
2. Right-click on the valve for the desired port and choose Close to close the valve.
3. Using a wrench, remove the sample tube fitting from the port. Pry out the filter and
O-ring.
20-µm filter (frit)
O-ring
Sample Tube fitting
To avoid degassing problems, the filter and O-ring should be clean and should not be
touched with bare hands.
4. Replace the filter and O-ring. Carefully reassemble the sample tube fitting and reinstall on
the sample port. Tighten by hand, then with a wrench to prevent leaks.
9-6 Mar 08
Replacing the Sample Tube O-ring
It is important to maintain a vacuum-tight seal near the top of the sample tube stem. If an O-
ring becomes worn or cracked, it does not provide a good seal and will need to be replaced.
Before removing (or installing) a sample tube, ensure that the port valve is closed.
Observe the instrument schematic to verify valve status.
1. Holding the sample tube firmly with one hand, loosen the sample tube connector nut by
turning counterclockwise.
Be careful not to let the sample tube connector nut drop onto the bottom of the tube as
it may break the tube.
2. Carefully pull the sample tube down until it is free from the port. You may have to grasp
the sample tube with both hands.
O-ring
Ferrrule
3. Remove the O-ring from the top of the sample tube and replace it with a new one.
If the O-ring remains inside the sample port, you may use a pair of tweezers or needle-
nose pliers to remove it.
4. After the new O-ring is in place, insert the sample tube back into the sample port until it is
fully seated.
5. Slide the sample tube connector nut up the tube (the ferrule and O-ring will move along
with the connector nut). Then, turning clockwise, hand-tighten the connector nut to the
sample connector.
Mar 08 9-7
Inspecting and Changing Vacuum Pump Oil
This procedure is also shown in one of the How-To videos located on the
Help menu.
The oil in the vacuum pump should be changed every three months, when the efficiency of the
vacuum pump declines (requiring increased time to reach vacuum levels), or if it becomes dis-
colored. The oil is easily inspected to determine if a change is necessary.
Inspecting the Oil
View the vacuum pump oil through the oil-level window. The oil level should be midway
between the indicators on the oil-level window. Oil in good condition is clean, clear or light in
color, and transparent.
Oil-level window
• Change the oil if it has darkened

• Add oil if it is below the midway level
Changing or Adding Oil
Always drain the vacuum pump while the pump is warm and disconnected from the
power source.
Use oil supplied by Micromeritics, or refer to the vacuum pump manual for other acceptable
oils.
1. Unplug the vacuum pump from the power source.
9-8 Mar 08
2. Loosen the wing nut on the clamp at the top of the oil vapor trap. Swing the clamp open
and remove the trap from the hose.
3. Grasp the handle on top of the vacuum pump and place it on a work table.
4. Drain the used oil:
If you are adding oil, skip this step and continue with Step 5.
a. Place a waste container under the drain spout.
b. Remove the plug from the drain spout; allow the oil to drain into the waste container.
d. Replace the drain plug.
Mar 08 9-9
5. Remove the plug from the oil-fill port.
Oil-fill port
6. Slowly add oil to the port until the level is midway between the indicator lines in the oil-
level window.
Midway level
Do not allow oil to rise above the midway position. Doing so may cause oil to splash
into the oil filter and contaminate it.
7. Check the washer or O-ring used at the oil-filling port; replace if necessary.
8. Insert the oil-fill plug and turn counterclockwise to tighten.
9. Check the alumina in the oil vapor trap. If most of the pellets are no longer white, replace
the alumina in the oil vapor trap before reattaching the vacuum pump. Refer to Replacing
the Alumina in the Oil Vapor Trap, page 9-11 for instructions.
10. Reconnect the vacuum pump hose.
11. Reconnect the power cord to the power source.
12. Allow the pump to run a few hours (overnight if possible) to eliminate air and moisture
from the fresh fluid and to produce efficient vacuum operations.
9-10 Mar 08
Replacing the Alumina in the Oil Vapor Trap
The activated alumina in the oil vapor trap becomes saturated during use. The alumina should
be inspected periodically and replaced when most of the alumina pellets are no longer white.
Do not perform the following procedure on used alumina. The resultant oil vapors may
cause a fire or an explosion.
1. Loosen the wing nut on the clamp at the bottom of the oil vapor trap. Swing the clamp
open and remove the trap.
2. Remove one end fitting from the trap body; dispose of the used alumina in an appropriate
manner.
3. Wash the trap body with a detergent-based soap. Rinse with water, then with isopropyl or
ethyl alcohol. Set the trap aside and allow to dry thoroughly.
Exposure of the trap body to oil vapor may cause small cracks on the inside surface of
the trap body. Under normal circumstances, these cracks will not cause problems or
leaks.
Mar 08 9-11
4. Prepare fresh alumina as follows:
a. Preheat the oven to 300 °C.
b. Pour approximately 180 grams of fresh alumina into a glass or metal container for
(approximately 250 mL if a graduated beaker is used). Place the container in the
oven.
c. Bake the alumina for two hours.
d. Remove the baked alumina from the oven and allow it to cool until luke warm. A
desiccator may be used to speed the cooling process.
5. Using a small spatula, gently pry the O-ring from the end fittings of each end of the trap
body.
6. Inspect the O-rings.
• If dusty, clean with a lint-free tissue.

• If damaged, replace with a new O-ring.
7. Screw one of the end fittings onto the trap body.
9-12 Mar 08
8. Be sure the trap body is dry and the alumina is lukewarm; pour the alumina pellets into the
trap until they are level with the top of the trap body.
9. Screw the other end fitting back onto the trap and tighten securely by hand.
10. Lightly tap both ends of the trap body on the work surface. This will remove any
remaining dust from the pellets.
11. Make sure the centering ring is in place on the intake port.
12. Place the trap on the centering ring.
Centering Ring
Mar 08 9-13
13. Open the clamp and place it around the flange of the intake port and the flange of the trap.
Swing the clamp fastening screw toward the intake port until it fits into the slot in the
other half of the clamp. Tighten the wing nut securely by hand.
14. Reconnect the hose from the analyzer to the oil vapor trap.
a. Place the clamp around the flange of the vacuum pump hose and vapor trap.
b. Swing the cslamp fastening screw around until it fits into the slot on the other half of
the clamp. Tighten the wing nut securely by hand.
15. Plug the pump power cord into the power source.
16. Allow the pump to run a few hours (overnight if possible) to eliminate air and moisture
from the fresh oil and to produce efficient vacuum operations.
9-14 Mar 08
Changing the Vacuum Pump Exhaust Filter
The gases used by the TriStar 3020 are exhausted by the vacuum pump. An exhaust filter is
installed on the exhaust port of oil-filled pumps. The filter minimizes the release of oil vapor
and should be replaced when it becomes so saturated with oil that it is ineffective.
Exhaust filters are used to minimize the release of oil vapors. The gases are diluted
substantially upon release from the vacuum pump. However, it may be desirable in
some locations to provide a fume hood for protection from hazardous gases and
vapors released into the work area.
1. Loosen the wing nut of the clamp at the vacuum pump exhaust port. Swing the clamp
away from the exhaust port and remove it.
2. Remove and discard the exhaust filter; do not remove the centering ring.
3. Make sure the centering ring is in place on the exhaust port.
4. Place the new filter on the centering ring.
5. Open the clamp and place it around the flange of the exhaust port and the flange of the
exhaust filter. Swing the clamp fastening screw toward the exhaust port until it fits into the
slot in the other half of the clamp. Tighten the wing nut securely by hand.
Mar 08 9-15
Performing a Leak Test
Your service representative may request that you perform a leak test to determine if there is a
leak in your system. This test generates a report that your service representative will request
that you send to him for observation.
The following types of information are displayed during the test:
• Prompts on preparing the instrument for the test

• Approximate time period of the test
• Prompts in which an operator response is required
1. Select Unit [n} > Diagnostics; the Service Test dialog is displayed.
2. Click the down arrow to the right of the Test field and select System Leak Test Rev.
[latest revision letter].
3. Ensure that Report after test is selected and that Screen is chosen as the destination.
9-16 Mar 08
4. Click Next; the second view of the Service Test dialog is displayed.
Data will be inserted into the pane as collected.
5. After the test is finished, a dialog stating the test is complete is displayed.
6. Click OK to close the dialog, then click Close on the test dialog to close the test.
7. When you close the test, a report is generated automatically to the screen.
Mar 08 9-17
8. Click Save as; the Save As dialog is displayed.
9. Accept the default name displayed in the File name field, then click Save to return to the
report window.
10. Click Close to close the report window.
11. E-mail the report file to your service representative.
9-18 Mar 08
TriStar II 3020 Connecting Gases
Connecting Gases
This procedure is also shown in one of the How-To videos located on the
Help menu.
Guidelines for Connecting Gases to the Analyzer
Use these guidelines when installing regulators and gas lines:

• Place gas bottles close to the analyzer. Using gas line extenders on gas bottles located in
remote areas may degrade gas quality and reduce pressure.
• Use a retaining strap (or other appropriate tether) to secure the gas bottle.
• Carefully route the gas lines from the bottle to the analyzer, avoiding overlapping or
entangling gas lines.
• Label the gas line at the instrument inlet for proper identification and maintenance.
• Ensure that the gas bottle is closed before connecting to the analyzer.
The instructions below describe a typical installation. Some configurations require additional
components, such as regulator expansion kits, when one gas source will be used for several
operations or when the gas bottle cannot be located close to the analyzer.
In order to use oxygen with the TriStar, your analyzer must be equipped with an
oxygen-compatible vacuum pump that uses Fomblin® (or a suitable equivalent) pump
oil, or a dry pump. Failure to use the proper vacuum system could result in hazardous
conditions including fire and personal injury.
Disconnecting the Depleted Bottle
1. Close the gas bottle shut-off valve, then open the regulator shut-off valve.
Gas Bottle
shut-off valve
Regulator
shut-off
valve
Mar 08 9-19
Connecting Gases TriStar II 3020
2. Both gauges should read at or near zero; if not, disconnect the gas line from the regulator
and allow the pressure to purge from the lines.
3. Use an appropriate wrench to loosen the nut at the regulator/gas bottle connection, then
remove the regulator from the bottle.
You do not have to disconnect the gas line from the regulator or the instrument.
4. Replace the protective cap on the depleted bottle, disconnect the retaining strap, and
remove the bottle from its current location.
9-20 Mar 08
Connecting a Replacement Gas Bottle
Move the replacement bottle close to the instrument and tether it into place.
When connecting hazardous gases, be sure to vent properly and follow the safety
procedures established for your lab.
A power failure or loss of cryogen can result in dangerous pressures in the sample
tube. The TriStar uses pressure relief valves to vent this pressure into the instrument
cabinet and return the instrument to a safe condition. When using toxic or flammable
gases, additional venting of the cabinet may be required.
1. Use an appropriate cylinder wrench to remove the protective cap from the replacement
bottle.
2. Attach the gas regulator to the connector on the gas bottle. Hand-tighten the nut, then use
an appropriate wrench to tighten an additional 3/4 turn.
Do not overighten the fitting; doing so may cause a leak.
3. Check for leaks at the high-pressure side of the regulator and in the connector.
HIgh-pressure Gauge
Gas Bottle
Shut-Off valve
Regulator
Regulator connector nut
Control knob
Mar 08 9-21
a. Turn the regulator control knob fully counterclockwise.
b. Slowly open the gas bottle shut-off valve, then close it.
c. Observe the pressure on the high-pressure gauge.
• If the pressure is stable, proceed with the next step.

• If the pressure decreases, tighten the regulator connector nut until it becomes stable.
4. Purge the air from the lines.
Gas Bottle
Shut-Off valve
Regulator
Shut-Off
valve
a. Turn the regulator shut-off valve counterclockwise to open.
b. Open the gas bottle shut-off valve to flow gas.
c. Close the regulator shut-off valve to stop flow.
d. Close the gas bottle valve.
5. Set the instrument pressure.
Low-pressure Gauge
Regulator
Gas Bottle
Shut-Off
Shut-Off valve
valve
Regulator
Control knob
a. Turn the regulator control knob clockwise until the low-pressure gauge reads 15 psig
(103 kPag).
b. Open the regulator shut-off valve.
9-22 Mar 08
c. Open the gas bottle shut-off valve and flow gas for 10 to 30 seconds.
d. Close the gas bottle shut-off valve.
6. If you disconnected the gas line to the instrument inlet, reconnect it now.
7. Verify that the line for the newly connected gas is clean; refer to Cleaning and Verifying
the Gas Line, page 9-24.
8. If you connected the same gas as the one you removed, you are ready to resume operation.
If you connected a different gas than the one you removed, you must specify the change;
refer to Specifying Gas Ports, page 9-28.
Mar 08 9-23
Cleaning and Verifying the Gas Line
You should always clean the gas lines and verify there are no leaks at the connections after you
connect a gas bottle. This test examines the gas line from the instrument to the gas bottle, then
from the instrument to the regulator shut-off valve. A report is generated at the completion of
the test verifying that it has passed or failed. Causes and corrective action for a failure are
provided.
Before beginning, confirm that the state for valves and the low-pressure gauge are as follows:
Low-pressure gauge
14 - 15 psig
Gas Bottle Shut-Off valve

CLOSED
Regulator Control knob

OPEN
Regulator Shut-Off valve
OPEN
1. Select Unit [n} > Diagnostics; the Service Test dialog is displayed.
2. Click the down arrow to the right of the Test field and select Clean and Verify Gas Line
[port number] Test Rev. [latest revision letter].
3. Ensure that Report after test is selected and that Screen is chosen as the destination.
Be sure Report after

test is selected and
Screen is the
destination.
9-24 Mar 08
4. Click Next; the second view of the Service Test dialog is displayed. On this dialog a series
of messages is displayed. These messages are of the following types:
• Informative; for example, advising how long the test will take or how long before you
will be required to open or close a valve. Read the message and click OK to proceed.
• Operator response; for example, you will be asked to open and close regulator and gas
bottle valves (depicted below). Perform the task first, then click OK.
Low-pressure gauge

5. After the test is finished, a dialog stating the test is complete is displayed; click OK to
close the dialog.
6. A report is generated automatically to the screen.
Observe the Slope field on the Instrument to Regulator Shut-off Valve -1 report; it
should display Passed, indicating that the gas line from the instrument to the regulator is
clean and leak-free.
If Failed is shown, a leak is indicated between this connection. Check the connections
from the instrument to the gas regulator valve. Tighten as necessary, then try the test again.
Mar 08 9-25
7. Click the Instrument to Gas Bottle Shut-off Valve - 2 tab to display its report.
Observe the Slope field; it should display Passed, indicating that the gas line from the
instrument to the gas bottle is clean and leak-free.
If Failed is shown, a leak is indicated between this connection. Check the connections
from the regulator shut-off valve to the gas bottle shut-off valve. Tighten as necessary,
then try the test again.
8. Click the Gas Pressure Test - 3 tab to display its report.
9-26 Mar 08
Passed should display in the Minimum field, indicating that all valves are in the proper
state for operation.
If Failed is shown, one or more valves is not in the proper position; set the valves as
shown below and ensure the appropriate pressure is displayed on the low-pressure gauge.
Low-pressure gauge
14 - 15 psig

OPEN

OPEN
OPEN
If you wish to run the test again, be sure to close the gas bottle valve before starting the
test.
9. Click Close to close the test report.
10. Click Close on the test dialog to close the test.
Mar 08 9-27
Specifying Gas Ports TriStar II 3020
Specifying Gas Ports

The TriStar 3020 has gas inlets for up to three analysis gases and a dedicated inlet for helium.
The gases you connect to the inlets must be specified in the analysis program. If you change
gases on one of the inlets, be sure to access the Unit Configuration dialog and make the change
there as well. It is very important that the analysis program be kept informed of any change in
gases.
1. Select Unit [n] > Unit Configuration; the Unit Configuration dialog is displayed.
2. In the Gas Selections group box, enter the mnemonic for the gas(es) you have attached to
the gas inlets.
3. Click OK to save the selections and close the Unit Configuration dialog.
9-28 Mar 08
TriStar II 3020 Calibrating the System
Calibrating the System

A calibration file was created specifically for your analyzer and included with your accesso-
ries. Reinstalling Calibration Files, page 4-19 describes how to install this file. It is not
necessary to recalibrate your system unless you suspect that it may be out of calibration. Cer-
tain calibrations are not allowed unless performed under the direction of a Micromeritics
service representative; those calibrations are greyed on the Calibration menu.
You can review calibration details of your analyzer by selecting Unit > Unit configuration.
The following calibrations can be performed without the assistance of a service representative:
• Zero pressure
• Match transducers
• Servo valve
Zero Pressure
This command enables you to evacuate the system and zero the transducers.
1. Install a blank sample tube on each applicable port.
2. Select Unit [n] > Calibration > Zero pressure; the Calibrate Pressure Offset dialog is
displayed.
3. Ensure that all transducers are selected, then click Start. The dialog closes automatically
when calibration is complete.
Mar 08 9-29
Calibrating the System TriStar II 3020
Match Transducers
This command enables you to zero and match the selected transducers to the main manifold
transducer.
Be sure that a sample or Po tube is installed on each selected port before clicking Start.
Servo valve
Make sure the pressure transducer has been calibrated before performing this
procedure. Select Unit > Unit configuration and view the calibration information.
Contact your service representative if calibration dates are not listed.
1. Select Unit [n] > Calibration > Servo valve; the Calibrate Servo Valve dialog is
displayed.
2. Click Start; the dialog closes when calibration is complete.
9-30 Mar 08
TriStar II 3020 Ordering Information
10. ORDERING INFORMATION
The TriStar 3020 Analysis System components and accessories can be ordered using one of
the following methods:
• Call our Customer Service Department at (770) 662-3636

• Access our web site at www.micromeritics.com
• Contact your local sales representative
When ordering, please use the information provided below to place your order.
Part Number Item and Description

065-00000-00 SmartPrep 065, Windows interface allowing programmable ramp and
soak rates; degasses up to six samples with flowing gas
060-00030-00 FlowPrep 060, degasses up to six samples at up to 400 ºC with flowing
gas
061-00030-00 VacPrep 061, degasses up to six samples at up to 400 ºC; uses flowing
gas or evacuation by vacuum (evacuation requires a vacuum pump and a
regulator)
302-33002-00 Krypton Option; adds 10-mmHg transducer and high-vacuum pump,
enabling you to perform krypton analyses (service-installed).
062-00000-11 Vacuum pump with built-in anti-suckback valve, 100/120 VAC, includes
hose kit
062-00000-23 Vacuum pump with built-in anti-suckback valve, 220/240 VAC, includes
hose kit
062-33002-00 Oil Vapor Trap; includes alumina and instructions
004-16830-00 Activated alumina, 500 grams; for oil vapor trap
003-22617-00 Valve, solenoid, 24 VDC 10-32 Mt, 0.025-in. orifice, for standard
evacuation (Valves 1 through 10)
003-22626-00 Valve, solenoid, 24 VDC 10-32 Mt, 0.060-in. orifice, for fast evacuation
(Valves 11, 12, and 13)
004-62230-58 CGA 580 fitting, 30 psig (He, N2)
004-62230-32 CGA 320, 30 psig (CO2)
004-33601-00 Expansion Kit; adds an additional outlet to the gas regulator
004-33602-00 Pressure Relief Kit; prevents excessive gas pressure in the event of
regulator failure (not to be used with toxic gases)
004-16833-00 Reference Material, Carbon black, ~ 30.6 m2/g, 10 g
004-16821-00 Reference Material, Silica alumina, ~ 215 m2/g,10 g
Jul 09 10-1
Ordering Information TriStar II 3020

004-16818-00 Reference Material, Glass, ~ 5.8 m2/g, 10 g
004-16816-00 Reference Material, Alumina, ~ 0.25 m2/g, 15 g; for krypton analysis
003-63801-01 Cable, ethernet straight-thru
004-25549-00 Reducer, 1/8-in. tube x 1/4-in. tube
290-25846-00 Gas inlet line, 1/8 in. x 6 ft long, copper
290-25846-01 Gas inlet line, 1/8 in. x 16 ft long, copper
240-14855-00 Rack, sample tube
240-25853-00 Funnel, sample tube
240-25901-00 Dip stick; for checking liquid nitrogen level in Dewar
302 -33601-00 Sample Tube Kit, 1/4-in; includes six each sample tubes, O-rings, and
plastic caps; three each isothermal jackets, filler rods, and ferrules; and a
Dewar cover
stoppers; three each isothermal jackets, filler rods, and ferrules; one
sample tube brush; and a Dewar cover
stoppers; three each isothermal jackets, filler rods, and ferrules; one
sample tube brush; and a Dewar cover
302-61001-00 Sample tube, 1/4-in. stem OD; for analyzing powdered samples where
free-space management (with a filler rod inserted) is critical
302-61001-01 Sample tube, 3/8-in. stem OD; for analyzing any type of sample
302-61001-02 Sample tube, 1/2-in. stem OD; for analyzing larger pieces of granular or
pelleted samples
302-61002-00 Sample tube, 1/4-in. stem OD, flat bottom
302-25812-00 Isothermal jacket, for 1/4-in sample tube
302-25812-01 Isothermal jacket, for 3/8-in. sample tube
302-25812-02 Isothermal jacket, for 1/2-in. sample tube
302-25821-00 Hanging filler rod, for 1/4-in. sample tube
302-61005-02 Filler rod, for 1/2-in. sample tube when using the Seal Frit
004-25466-00 O-Ring, Buna-N size 010; for sample port and 1/4-in. sample tube
004-25022-00 O-Ring, Buna-N size 012; for 3/8-in. sample tube
004-25469-00 O-Ring, Buna-N size 014; for 1/2-in. sample tube
10-2 Jul 09
TriStar II 3020 Ordering Information

300-31802-02 Dewar cover, for 1/4-in. and 3/8-in. sample tubes
300-31802-03 Dewar cover, for 1/2-in. sample tube
004-54104-00 Brush, for cleaning sample tubes
300-25825-00 Ferrule, for 1/4-in. sample tube
004-27046-00 Frit, 40 µm, for sample port
004-32004-00 Stopper, rubber, for 3/8- and 1/2-in. sample tubes
004-32604-08 Cap, plastic, for 1/4-in. sample tube
302-33607-00 Seal Frit Kit; includes three seal frits, nine openers, three filler rods,
installation tool and instructions
260-25890-00 Seal Frit assembly
300-32800-00 Support, sample weighing
300-25861-20 Dewar, 2.75 liters
004-27040-00 Filter, for vacuum pump exhaust
004-16003-01 Oil, vacuum pump, 1 Liter
200-25879-00 Funnel, for filling vacuum pump with oil
302-42801-00 Operator’s manual, TriStar 3020
202-33024-00 DataMaster Program; allows you to generate classical or micropore data
reductions
Jul 09 10-3
TriStar II 3020 Appendix A
A. FORMS
This appendix contains the following form:
• Sample Data Worksheet
Copy and use this form as needed.
Mar 08 A-1
Sample Data Worksheet
Use this worksheet to record the values necessary to calculate the sample mass.
Sample Tube Identification:_________________________________
Sample Mass
NOTE: Record all values in grams.

Before Degas After Degas After Analysis
A. Mass for empty sample tube set: ____________
B. Sample tube set plus sample mass: ____________ _____________ ____________
C. Sample mass (B - A): ____________ _____________ ____________
Degas Information
Degas apparatus: ____________________________________________

Temperature (ºC): ____________________________________________
Time (hours): ____________________________________________
Actual time started: ____________________________________________
Actual time finished: ____________________________________________
Degas notes: ________________________________________________________________________

___________________________________________________________________________________
___________________________________________________________________________________
___________________________________________________________________________________
___________________________________________________________________________________
TriStar II 3020 Appendix B
B. ERROR MESSAGES
Error messages for the are listed numerically. If the Action response instructs you to contact
your service representative, record the error message and make backup copies of any files
involved in the operation.
The 1000-series error message, used primarily for software testing, are not included in
this appendix. These errors should not occur during normal operation. If you receive a
1000-series message, contact your service representative after making backup copies
of nay files involved in the operation.
2400 Series
2401- FATAL ERROR: (error message)
Cause: An internal processing and/or hardware error has occurred during com-
munication with the analyzer.
Action: Contact your service representative if you continue to receive this mes-
sage.
2430- Error accessing file (file name), error code = (number).
Cause A: Media may be damaged.
Action A: Clean the media drive. If this does not eliminate the problem, attempt
operation using a backup copy of the file.
Cause B: Hard disk may be damaged.
Action B: Contact your service representative.
Cause C: A software error occurred when the file was accessed.
Action C: Contact your service representative.
Cause D: The name specified contains one or more invalid characters.
Action D: Enter a valid filename (refer to your operating systems manual).
Mar 08 B-1
Appendix B TriStar II 3020
2431- Error writing file (file name), error code = (number).
Cause: The hard disk does not have enough space left to perform the opera-
tion.
Action: Copy files not used regularly from the hard disk to diskette, delete
them from the hard disk, and then try the operation again
2432- Invalid response from MMI ‘FILE_READ’ request.
Cause: An internal processing and/or hardware error has occurred.
Action: Contact your service representative if you continue to receive this error
message.
2433- New entries have been found in this directory. Refresh the directory
information?
Cause: Several TriStar 3020 files (sample information, analysis conditions,

adsorptive properties, or report options) have been added to this direc-
tory by some function other than the TriStar 3020 program.
Action: Select Yes to update the directory information with data from each new
file. This operation may take a minute.
Select No if you do not want to spend the time updating the directory
information. This option may be feasible if a large number of files have
been copied into the directory and you know the name of the file you
wish to access.
2434- File (file name) — Subset # (number) wrote wrong amount of data.
message.
B-2 Mar 08
2436- Path specification (path name) is invalid.
Cause: You entered an invalid path name and/or extension.
Action: Type a valid path name (including the proper extension) and press
Enter.
2437- File (file name) does not exist.
Cause: You entered a file specification that does not exist.
Action: Enter an existing file specification or select a file name from the list
box.
2438- Disk drive (letter): is inaccessible.

2439- Could not register file.
2440- Subset not found.
2441- Seek within file failed.
2442- Bad header in subset file.
2443- Subset owner denied access.
2444- Not a valid file format.
2445- Subset wrote the wrong amount of data.
2446- Error reading data.
2447- Error writing data.
Cause: An unexpected error occurred when you tried to access a data file.
Action: Contact your service representative.
2448- File directory (path name) is invalid. Resetting to the installation directory.
Cause: A working directory specified in the .INI file is invalid. The directory
may have been deleted or moved to a different location.
Action: The installation directory will be substituted. The next time you open a
file, use the Directories list to move to the correct directory.
2449- This field does not contain a valid file specification.
Cause: You entered an invalid file name.
Action: See the description of file naming conventions in your Windows man-
ual and re-enter the name.
Mar 08 B-3
2450- Sample Defaults may not be edited while this operation is in progress. Do you
wish to save and close the Sample Defaults edit session?
Cause: You are in the process of initiating an automatic analysis (an analysis in
which sample files are created using the defaults) while editing the
defaults.
Action: Finish your edit session of the defaults and close the dialog. Then
restart the automatic analysis.
2452- Attempt to write MICATTR.DIR in read only mode. (file name)

2453- Attempt to append MICATTR.DIR in read only mode. (file name)
Cause: The Read-Only attribute is turned on in the application’s

MICATTR.DIR file (this file exists in each folder containing sample or
parameter files).
Action: Use Windows Explorer to access the folder containing the

MICATTR.DIR file and disable the Read-Only option.
2454- Too many selections for a print-to-file operation. Only the first (number) selec-
tions will be processed. Please reselect the remainder.
2455- Too many selections for an export-to-file operation. Only the first (number)
selections will be processed. Please reselect the remainder.
Cause: You selected too many files for this operation.
Action: Select only the number of files specified in the message.
2456- Insufficient file handles available. Application cannot continue.
Cause: You have more than 50 files open at the same time.
Action: Refer to the manual for your operating system and set the limit for
open files to 50 or greater.
B-4 Mar 08
2457- Results cannot be displayed. More than (number) windows are currently dis-
playing or printing results.
Cause: You have too many windows open in the application.
Action: Close some of the open windows.
2458- An instrument is performing a critical operation. Wait a few moments before

exiting the application.
Cause: You are attempting to exit the application while the instrument is per-
forming a critical operation. This operation must be completed before
the application can be stopped.
Action: Wait a short time and attempt to stop the application again.
2459- An instrument is busy. A delay in restarting this application could result in loss
of new data. Continue with program Exit? (Yes, No)
Cause: You are attempting to exit the application while an analysis is in

progress. While this is possible, the data collected while the application
is inactive will not be permanently recorded until the application is re-
started. A power failure to the instrument could cause some data to be
lost.
Action: If you are not concerned with the potential for loss of data should a
power failure occur, click Yes to continue; otherwise click No.
2460- Fatal Communications error on (Unit n - S/N: nnnn)
Cause: There was a fatal error in communication between the application and
the software in the instrument. All displays for that instrument will be
closed.
Action: Ensure that the analyzer is connected to the computer on the commu-
nications port configured in the Setup program. Stop the TriStar 3020
software and then restart it. If this error persists, contact your service
representative.
Mar 08 B-5
2461- No instruments are in operation. This application will unconditionally

terminate.
Cause: At least one instrument must be active for the application to operate.
The initialization of all of the instruments configured with the Setup
program has failed. The application stops.
Action A: Usually this message is preceded by another message giving the reason
for the instrument’s failure to initialize. See the instructions for that
message.
Action B: Ensure that the instrument is attached to the computer on the commu-
nications port configured with the Setup program. Verify that the
instrument has the power switch in the ON position and that the light
on the front panel is illuminated. If the application continues to fail in
its attempts to initialize the instrument, contact your service represen-
tative.
2477- Unit n - S/N: nnnn did not properly initialize.
Cause: The software was unable to initialize this instrument; this is usually
caused by one of the conditions listed in the error messages above.
Action: Correct the problem as described above, then restart the application.
2478- Error copying sequential data segment.
Cause: An internal processing and/or hardware error occurred while accessing

a portion of a sample file.
Action: Confirm that the media being accessed does not contain errors; for
example, you may wish to use a utility such as ScanDisk. Contact your
service representative if you continue to receive this error message.
B-6 Mar 08
2479- (Unit n; Serial nn) The instrument is busy performing an operation of which this
application is unaware. Do you want to cancel? (Yes, No)
Cause: During initialization of the application, the status of the analyzer was
found to be in a different state than expected.
Action: Click Yes to cancel the operation in process, allowing the analyzer to
reset and continue with initialization.
Click No to cancel the initialization process.
If you continue to get this message, verify that files in the application
directory structure are not being changed or removed.
2480- File <name> cannot be analyzed. It is currently being edited.
Cause: You are trying to start an analysis using a file that is open for editing.
Action: Finish editing the file, save and close it, then start the analysis.
2481- Error accessing the sample information file <name>.
Cause: An unexplained error prevents you from accessing this file.
Action: The hard disk drive may be corrupt. Run diagnositics.
2482- File cannot be opened for writing. It is already in use.
Cause: You attempted to open a file that is currently being used (either by this
application or another).
Action: Locate the application using the file (in the Micromeritics application,
use the Windows menu item to get a list of all windows, one of which
may contain this file).
Mar 08 B-7
2483- An analysis cannot be performed on (file name). It is open for editing and con-
tains errors.
Cause: You attempted to use a sample file containing errors that is currently
open.
Action: Go to the window containing the file, correct the errors, and save it.
2484- The edit session for <name> must be saved before the analysis. Save
changes and continue with the analysis? (yes, no)
Cause: You are trying to start an analysis using a file that contains unsaved
changes and is open for editing.
Action: Select Yes to save the changes and proceed with the analysis; select No
to cancel the analysis and continue editing the Sample Information file.
2485- The service test file has an invalid status and cannot be used for this analysis.
Cause: The selected service test file has a status other than No Analysis.
Action: Select a different service test file or create a new one and use Replace
All to copy parameters from the file you originally selected.
2486- Could not construct (name) report type. Program will terminate.
Cause A: You may not have full rights to the application’s folders and files.
Action A: Contact your system administrator to have full rights granted.
Cause B: An internal processing and/or hardware error has occurred.
Action B: Contact your service representative if you continue to receive this error
message.
B-8 Mar 08
2487- Could not start report generator. Error code (number). Program will
terminate.
message.
2488- File (file name) cannot be opened for editing. It is already in use.
Cause: The file you specified is being used in another edit operation.
Action: Check the Windows list to locate the other edit session.
2489- File (file name) cannot be opened for writing. It is already in use.
Cause: The file you specified in a Save As operation is already open for edit.
Action: Select a different file for the Save As operation.
2490- No ‘.INI’ file present. Application will terminate.
Cause: The ASCII file containing initialization information and system

options information used during program startup does not exist.
Action: Run the TriStar 3020 Setup program, select Change analyzer setup,
and create the control file used by the TriStar 3020.
2491- Highlighted fields contain errors. Please correct the errors before closing dia-
log box.
Cause: The highlighted fields contain invalid entries. You will not be able to
close the dialog box until you correct the errors.
Action: Check the entries, correct the errors, and close the dialog box.
2492- This field’s entry is invalid.
Cause: The highlighted field contains an invalid entry.
Action: Check the entry and correct the error.
Mar 08 B-9
2493- An entry is required for this field.
Cause: This field requires a valid entry for you to proceed.
Action: Enter or select an appropriate value.
2494- Value is out of the valid range.
Cause: The value you entered in the highlighted field is outside the valid range
of values.
Action: Check the entry and enter or select an appropriate value.
2495- Value is out of the valid range. Enter a value between (value) and (value).
Cause: The value you entered in the highlighted field is outside the valid range
of values.
Action: Check the entry and enter or select a value within the indicated range.
2496- Invalid number.
Cause: The number you entered in the highlighted field is invalid.
Action: Check the entry and enter or select a valid number.
2497- This field contains an invalid character.
Cause: You entered an invalid character in the highlighted field.
Action: Check the entry and enter valid characters.
2498- The requested change to the Sample’s status is invalid at this time.
Cause: A request to change the file’s status (for example, from automatically
collected to manually entered) could not be done.
message. Record the name of the sample file in which the problem
occurred.
B-10 Mar 08
2499- Sequence number must contain at least 3 digits.
Cause: You tried to enter a sequence number that did not contain at least three
digits.
Action: Enter a sequence number that contains at least three digits.
Mar 08 B-11
2500 Series
2500- All sample file names that can be created using the sequence number pattern
already exist. You may want to modify the next sequence number.
Cause: No more sample information files can be created using the currently
entered file name sequence number.
Action: Select Options > Sample defaults and enter another sequence number.
2501- System resources have reached a dangerously low level. Please close some
windows to avoid the loss of data.
Cause: A large number of windows are open and consuming the system
resources available to all applications.
Action: Close one or more windows on the screen. Contact your service rep-
resentative if you continue to receive this error message.
2502- Error writing to file (name) during print. Error code: (number).
Cause: An error occurred in the file being written to during a print operation.
Action: Ensure that there is sufficient space on the drive containing the file.
2503- Error converting file (file name). Could not create DIO intermediate file.
Cause A: Insufficient space is available on the hard disk. The DIO file is placed
in the directory specified by the TEMP environment variable.
Action A: Determine if there is sufficient space on the drive where the TEMP
directory is located.
Cause B: An internal processing and/or hardware error has occurred.
Action B: Contact your service representative if you continue to receive this error
message.
B-12 Mar 08
2504- Cannot create output file for sample (sample name).
Cause: Insufficient space may be available on the hard disk.
Action: Ensure that sufficient space is available. Contact your service repre-
sentative if you continue to receive this error message.
2506- (sample file) Output device (name) is not installed. Printing cannot be
accomplished.
Cause: The selected output device is not installed in Windows.
Action: Select a different output device in the System Configuration dialog

box. Install the device using the Control Panel - Printers operation.
2508- (sample file) Overlay file (name) was not found. It will not be included in the
reports.
Cause: The specified overlay file could not be found.
Action: Ensure that the file specified as an overlay does exist.
2509- (sample file) Error opening file (name): (error). Reports cannot be produced.
Cause: An error occurred while the program was opening a file necessary to
the report operation.
Action: Use the name given in the error message to investigate. Contact your
service representative if you continue to receive this error message.
Mar 08 B-13
2510- (sample file) Error parsing reports from file (name). Reports cannot be
produced.
Cause A: One or more data entry fields in the sample file may contain an invalid
character (such as a single quote or double quotes).
Action A: Review the data entry fields and remove the invalid character.
Cause B: The system was unable to create the usual temporary files during the
report, possibly due to insufficient disk space.
Action B: Check the space available on the hard disk.
Cause C: An internal processing error occurred.
Action C: Contact your service representative.
2511- Print job (name) has been cancelled due to insufficient disk space. Delete
unnecessary files and restart the report.
Cause: The disk drive does not have enough space for the temporary file
required by the Windows Print Manager. Therefore, printing of the
requested report has been canceled.
Action: Delete unnecessary files from the disk. You will require at least five
megabytes of free space for normal operation.
2512- Print job (name) cancelled.
Cause: The requested print job was canceled at your request.
Action: None required.
2513- Unable to read the calibration file (file name).
Cause: You selected an invalid calibration file or one that cannot be read.
Action: Be sure the media containing the calibration file has no problems.
B-14 Mar 08
2514- Unable to write the calibration file (file name).
Cause: An attempt to Save calibration data has failed due to possible media
problems.
Action A: Be sure the media you want to Save the file to has no problems.
Action B: Choose an alternate media to Save the calibration data.
2515- Warning: Changing the calibration information will affect the performance of
the instrument. Only qualified service personnel should do this. Do you wish to
proceed?
Cause: You have started the process of performing a calibration operation.
Action: Calibration operations should only be done by or under the direction of

qualified service personnel.
2516- Warning: Keeping a backup copy of the calibration data is recommended by

Micromeritics. Would you like to do so now?
Cause: You have performed a calibration operation; a backup copy is recom-

mended.
Action: Perform a calibration Save operation.
2517- Canceling this dialog will reset the calibration state to what it was when this
dialog was first opened. Are you sure you want to cancel?
Cause: You have not accepted the calibration you performed.
Action: If the calibration operation was successful, press Accept.
2521- Unable to program controller.
Cause: A hardware malfunction has occurred.
Action: Contact your local Micromeritics service representative.
Mar 08 B-15
2522- Invalid controller application file.
Cause: The application’s control file has been corrupted or deleted.
Action: Reinstall the TriStar analysis program.
2523- Programming the controller failed.

2524- CRC check failed on programming controller.
2525- Unknown error programming controller.
2526- Controller download was not successful.
2527- Controller CRC error on boot block.
2528- Controller DRAM error.
2529- Controller Com1: error.
2530- Controller Com2: error.
2531- Controller debug port error.
message.
2532- The instrument contains a different software version. Do you want to reset it?
Cause: The application has discovered a different version of software operat-

ing in the analyzer.
Action: If there are no analyzers other than the TriStar connected to the com-
puter, select Yes and allow the updated software to load.
2533- Analyzer initialization failed.
message.
B-16 Mar 08
2534- Error opening file (name) for printing. Error code: (number).
Cause: An error occurred in the selected file for print output.
Action: Ensure that sufficient space is available on the drive containing the file.
2548- System status (n)
Cause: There was a problem establishing communication with the analyzer.
Action: Ensure that the communications cable is seated firmly in the ethernet
slot at the analyzer connection and the computer connection.
If you continue to get this message, contact your Micromeritics service

representative.
2549- Error accessing online manual file (code #).
Cause: The operator’s manual file could not be located.
Action A: Reinstall the application.
Action B: Copy the contents of the manual folder on the setup CD to the appli-
cation directory.
2550- Attempts to acquire the instrument’s status timed out.
Cause: There was a problem establishing communication with the analyzer.
Action: Ensure that the communications cable is seated firmly in the ethernet
slot at the analyzer connection and the computer connection.
If you continue to get this message, contact your Micromeritics service

representative.
Mar 08 B-17
4000 Series
4000- Memory Allocation Error.
4001- Error Smoothing Data.
Cause: An internal processing and/or hardware error occurred during report

generation.
message.
4002- Thermal Transpiration correction had no effect.
Cause: The Thermal transpiration correction option was selected on the

Report Options dialog. However, the correction did not change any
pressure by more than one percent.
Action: Deselect this option to disable this message. This correction is only
meaningful for very low pressures.
4003- Error Converting Pressures.

4004- Error Computing Volume Adsorbed.

generation.
message.
4005- Pressures were not smoothed. Not enough pressures below 0.10 P/Po.
Cause: The Smooth pressures below 0.10 P/Po option was selected on the
Report Options dialog. There must be at least 10 pressures within this
range for smoothing to occur.
Action: Deselect this option to disable this message.
B-18 Mar 08
4006- Report Type Not Found.

4007- Error Processing Report.

generation.
message.
4008- Report requested on sample file with no data points.
Cause: You selected a file for reporting which contains no collected data.
Action: Select another file which contains collective data and restart the report.
4010- Summary Report was not included in the Selected Reports.
Cause: You did not select a plot or a table for any of the Selected Reports in
the Report Options dialog; you selected the reports only to generate an
entry in the summary. However, the Summary was not included in the
Selected Reports.
Action: Select a plot or table in one or more of the Selected Reports, and/or add
the Summary to the Selected Reports.
4014- File (name) is not a valid file for conversion.
Cause: The file selected for conversion is not a valid file.
Action: Select only files that have been created by TriStar 3000 or Gemini pro-
grams.
4015- Error creating export file for sample <sample file name>.
Cause: A file error occurred during creation of an export output file.
Action: The output file name may be invalid. Ensure that the target directory
exists. Ensure that the target diskette is not full or write protected. The
target disk drive may be damaged or inoperative. Verify that other files
may be created on the same drive. Contact your service representative
if you continue to receive this error message.
Mar 08 B-19
4016- Sample <sample file name> has no data for export to ISO/DFT.
Cause: The file selected for export has a status of No Analysis. No export file
will be created.
Action: Select a file which contains analysis data.
4017- Damage to the instrument will result if the sample has not been manually evac-
uated. Have you evacuated the sample?
Cause: You did not select Backfill sample at start of analysis on the Sample
Backfill Options dialog. The sample tube is normally at atmospheric
pressure when an analysis is started, and it must be backfilled before
the analysis begins to prevent sample material from being drawn into
the manifold.
Action: If you have manually evacuated the sample tube, select Yes. If you
have not, select No and then either perform a manual evacuation or go
to the Sample Backfill Options dialog and select Backfill sample at
start of analysis.
4020- Disabling this option may damage the instrument. Are you sure that the sample
should not be backfilled?
Cause: You did not select Backfill sample at start of analysis on the Sample
Backfill Options dialog. The sample tube is normally at atmospheric
pressure when an analysis is started; it must be backfilled before the
analysis begins to prevent sample material from being drawn into the
manifold.
Action: If you want to manually evacuate the sample prior to the start of the
analysis, select Yes. Otherwise, select No, go to the Sample Backfill
Options dialog, and select Backfill sample at start of analysis.
4023- The file <name> cannot be prepared for analysis. It is open for editing and con-
tains errors.
Cause: You are trying to start an analysis using a file that contains errors and is
open for editing.
Action: Finish editing this file, save and close it, then start the analysis.
B-20 Mar 08
4026- Cannot calculate Dubinin-Astkahov: bad least squares data.
Cause: Less than two selected data points are within the fitted pressure range.
Action: Edit the calculation assignments on the Collected Data dialog, or

change the fitted pressure range on the Dubinin report options dialog.
4027- Fewer than two sample files have data suitable for heat of adsorption reports.
Cause: Less than two of the sample files you selected for heat of adsorption
reports contain appropriate data.
Action: Edit the Quantity Adsorbed table, or select other sample files.
4028- Dubinin calculations cannot be performed because the affinity coefficient of

the analysis gas is zero.
Cause: Dubinin values could not be calculated because the affinity coefficient
of the analysis gas is zero.
Action: Access the Dubinin Report Adsorptive options in the sample file and
enter an appropriate value for the analysis gas.
4029- At least two fitted data points are needed for Alpha-S calculations.
Cause: Fewer than two data points fall within the selected Alpha-s range.
Action: Edit the calculation assignments or the fitted Alpha-s range, or use a
different reference curve.
4030- Preparations failed in primary data.
Cause: Appropriate data were not available to generate the report.
Action: This message was preceded by a different error message; refer to the
cause/action of the preceding message.
Mar 08 B-21
4031- Not enough points with a relative pressure in the range (n,n)
Cause: Fewer than two data points selected for the Dubinin report falls within
the selected relative pressure range.
Action: Edit the calculation assignments or the fitted relative pressure range.
4032- Some summary reports could not be produced because they require the
Micropore option.
Cause: Some of the summary reports you requested were not produced
because you do not have the micropore option installed.
Action: Edit the summary report and deselect the micropore options.
4033- Not enough points to generate Dubinin Tabular Report.
Cause: There are fewer than two valid data points available for the Dubinin
tabular reports.
Action: Examine the calculation assignments in the Collected Data dialog of

the sample file. You must have at least two micropore pressures
selected for inclusion in the Dubinin report.
4034- Fewer than 2 points available for Dubinin calculations.
Cause: There are fewer than two valid data points available for Dubinin
reports in one of the sample files selected for overlaying.
Action: Examine the calculation assignments in the Collected Data dialog of

the sample file. You must have at least two micropore pressures
B-22 Mar 08
4035- Cannot calculate optimized Astakhov exponent: Not enough points with a rel-
ative pressure in the range [(pressure), (pressure)].
Cause: There are fewer than two valid data points in the relative pressure
range specified. Astakhov reports will not be produced.
Action: Examine the calculation assignments in the Collected Data dialog for
the sample file. You must have at least two pressures in the given range
4036- Fewer than 2 points available for Horvath-Kawazoe calculations.
Cause: You must select at least two data points for inclusion in the Horvath-
Kawazoe analysis on the Collected Data dialog. No report will be pro-
duced.
Action: From the Collected Data dialog, select the data points to be analyzed.
4037- Computations failed while processing the primary data set. No reports will be
produced.
Cause: The preparation of data for reporting could not be successfully com-
pleted. No Horvath-Kawazoe reports will be produced. This message
will always be preceded with another one containing additional infor-
mation.
Action: Refer to the number of the error message which preceded this one for
an explanation.
4038- Fewer than 2 points available for the Langmuir Qm computation. Cheng/Yang
correction will not be applied.
Cause: The Cheng/Yang correction to the Horvath-Kawazoe equation requires

the value of the monolayer volume as calculated from the Langmuir
equation. The isotherm must include at least two points above 0.02 rel-
ative pressure for the Langmuir equation to be applied.
Action: The analysis will be performed without the Cheng/Yang correction.

Deselect Apply Cheng/Yang correction on the Horvath-Kawazoe
Report Options dialog to prevent this message from appearing on
future reports.
Mar 08 B-23
4039- The isotherm does not meet the constraints of the Cheng/Yang assumption.
Cheng/Yang correction will not be applied.

equation. The isotherm does not correlate to the Langmuir assumption
with a coefficient of 0.98 or more. The correction is not applicable to
this isotherm or to the range of the data points selected.
Action A: The analysis will be performed without the Cheng/Yang correction.

Deselect Apply Cheng/Yang correction on the Horvath-Kawazoe
Report Options dialog to prevent this message from appearing on
future reports.
Action B: Generate the Langmuir report for the same data points selected for the
Horvath-Kawazoe report. If the Langmuir correlation coefficient can
be brought above 0.98 by removing some points at high relative pres-
sure, remove them and reproduce the Horvath-Kawazoe reports.
4040- The value of Qm computed from the Langmuir equation is too low. The pore
size will not be computed for all data points.

equation. The computed value is less than the volume adsorbed at the
largest relative pressure included in the analysis. The correction is not
applicable to this isotherm or to the range of the data points selected.
Action: The analysis will be performed and the Cheng/Yang correction will be
applied to all points with a volume adsorbed less than the value of Vm.
The pore size will not be calculated for data points with an invalid vol-
ume adsorbed. Deselect Apply Cheng/Yang correction on the Horvath-
Kawazoe Report Options dialog to clear this message.
B-24 Mar 08
4041- Cheng/Yang correction is inappropriate for some P/Po.
Cause: The Cheng/Yang correction is usually inappropriate for any P/Po above
the isotherm knee. In some instances, the computed pore sizes may
decrease above the knee. While it is possible to include these relative
pressures (usually above 0.1 P/Po) in the analysis, the computed pore
sizes for these pressures are usually meaningless.
Action: Change the data points selected for the Horvath-Kawazoe report to
include only relative pressures at or below the knee of the isotherm, or
change the Horvath-Kawazoe report options so that the Cheng/Yang
correction is not applied.
4042- 0.0 cannot be a starting or ending pressure for a geometric progression from
low pressure.
Cause: You selected to generate a pressure table from a geometrically pro-

gressing range.
Action: Change the 0.0 entered value.
4043- 1.0 cannot be a starting or ending pressure for a geometric progression toward
saturation.
Cause: You selected to generate a pressure table from a geometrically pro-

gressing range.
Action: Change the 1.0 entered value.
4044- Points in the Langmuir report pressure table lie outside the collected data.
Cause: Calculation assignments are not being used and more than one of the
report pressure table points is above the range of the collected data, and
more than one is below.
Action: Change the report pressure table to be more consistent with the col-
lected data.
Mar 08 B-25
4045- Points in the report pressure table lie outside the collected data.
Cause: Calculation assignments are not being used and more than one of the
report pressure table points is above the range of the collected data, and
more than one is below.
Action: Change the report pressure table to be more consistent with the col-
lected data.
4046- (file name) could not be opened for reading.
Cause: A thickness curve file could not be opened.
Action: If the problem persists, restart your computer and optionally perform a
media integrity check (using ScanDisk).
4047- Warning: An error occurred while reading (file name).
Cause: An error happened during a read operation of a thickness curve file.
Action: If the problem persists, restart your computer and optionally perform a
media integrity check (using ScanDisk).
4048- Warning: An error occurred while restoring the heat of adsorption report editor.
Cause: The state of the heat of adsorption report editor could not be restored.
Default settings will be used.
Action: No action.
4049- The sample (file name) does not have enough data. A minimum of two adsorp-
tion points is required.
Cause: A sample file has been included in the Heat of Adsorption report that
does not have enough data.
Action: Remove the file from the selected file list.
4050- None of the requested quantities adsorbed is within the range of the collected
B-26 Mar 08
data of more than one sample file.
Cause: The Heat of Adsorption report failed because the specified quantities
are not within the range of the collected data.
Action A: Edit the quantities adsorbed so that they are within the range of the col-
lected data, or select other sample files.
4051- The sample (file name) does not have any data in the range of the requested
quantities adsorbed.
Cause: The sample’s data cannot be interpolated to any of the quantities

adsorbed.
Action: Edit the quantities adsorbed so that they are within the range of the col-
lected data.
4052- Fewer than two points are selected for this report.
Cause: At least two points are required for the BET calculations.
Action: Edit the calculation assignments for the BET report.
4053- At least two data points must be selected for t-Plot calculations.
Cause: At least two points are required for the t-Plot calculations.
Action: Edit the calculation assignments for the t-Plot report.
4054- Fewer than two data points are inside the fitted thickness range.
Cause: At least two points must be within the fitted thickness range for the t-
Plot calculations.
Action A: Edit the calculation assignments for the t-Plot report.
Action B: Edit the fitted thickness range in the t-Plot report editor.
Mar 08 B-27
4055- A positive BET surface area was not calculated.
Cause: Fewer than two points were assigned to the requested surface area cal-
culation in the collected data table.
Action A: Assign more points to the surface area calculation.
Action B: Select a different surface area in the t-Plot report editor.
4056- A positive Langmuir surface area was not calculated.
Cause: Fewer than two points were assigned to the requested surface area cal-
culation in the collected data table.
Action A: Assign more points to the surface area calculation.
Action B: Select a different surface area in the t-Plot report editor.
4057- At least two data points are needed for Freundlich calculations.
Cause: Less than two data points have been selected for the Freundlich report;
at least two are required.
Action: Select Freundlich points on the Collected Data dialog. If calculation

assignments are not being used, edit the Freundlich Report options,
Absolute pressure range in the sample file.
4058- At least two data points are needed for Temkin calculations.
Cause: Less than two data points have been selected for the Temkin report; at
least two are required.
Action: Select Temkin points on the Collected Data dialog. If calculation

assignments are not being used, edit the Temkin Report options,
Absolute pressure range in the sample file.
Cause: You have selected at least one point with a negative pressure value to
include in the Temkin report.
Action: Negative pressure points void Temkin calculations. Open the sample
file and click the Collected Data tab. Locate the negative value(s) in
the Temkin column and deselect it(them).
B-28 Mar 08
4059- Fewer than 2 points available for MP-Method calculations.
Cause: At least two points are required for the MP-Method calculations.
Action: Edit the calculation assignments for the MP-Method report.
4060- Sample (file name) contains no data points.
Action: An attempt was made to save a sample without collected data as a t-

curve or alpha-S curve.
Cause: Repeat the save as t-curve or save as alpha-S operation after opening a
sample that has collected data.
4061- The t-curve must contain at least 2 points.
Cause: At least two points are required in a thickness curve definition.
Action: Edit the thickness curve.
4062- Error during report generation.
Cause: An internal processing error has occurred.
Action: Contact your Micromeritics service representative.
4063- The data requested on this report are not available.
Cause: There is no information in the sample log to report.
Action: You selected a sample file for which no instrument operations have
been used. Select a sample file with a status of Prepared, Preparing,
Analyzing, or Complete to obtain a valid sample log report.
Mar 08 B-29
4067- No data points are within the range of pressures in the reference isotherm.
Cause: Thre are no collected data points within the range of pressures in the
reference isotherm.
Action: Select data points that are in the range of the reference isotherm, or
select a more appropriate reference isotherm.
4068- No points were selected for the f-Ratio report.
Cause: The collected data column for the f-Ratio report does not have any
points selected.
Action: Edit the collected data dialog and select points for the f-Ratio report.
4070- Unable to load deconvolution model (name).
Cause: For some reason, the list of available models was corrupted, therefore,
the model selected could not be loaded for the deconvolution.
Action: Exit the program and reinstall the software, then try again.
4071- The selected pressures points do not form a valid set for deconvolution.
Cause: The data points selected for analysis do not contain enough informa-
tion to allow a DFT data reduction.
Action A: Edit data points in the table of the Collected Data dialog, or select
another sample file. At least two points with strictly increasing pres-
sures and volumes adsorbed are required for a DFT Plus data reduc-
tion.
Action B: Edit the pressure range on the DFT report options dialog.
B-30 Mar 08
4072- The range of pressures selected is too small to deconvolute using this model.
Cause: A null result was found using the selected model.
Action: Edit data points in the table of the Collected Data dialog, or select
another sample file. At least two points with strictly increasing pres-
sures and volumes adsorbed are required for a DFT data reduction.
4073- The analysis gas (name) does not match the model gas (name).
Cause: The model assumes a specific gas and the sample file uses a different
one.
Action: Select a model that assumes the same gas.
4074- The analysis temperature (nn) does not match the model temperature (nn).
Cause: The temperature for the selected model did not match the analysis tem-
perature.
Action: Select a different model.
4075- The models cannot be located in the models folder. Reinstall the software.
Cause: The models could not be located. They may have been inadvertently
deleted or moved.
Action: Reinstall the software.
Mar 08 B-31
4077- Cannot get surface area for: (file name)
Cause: The Isotherm report for the named overlay file has Per gram selected
for the Volume Adsorbed, and the Isotherm report for the primary file
has a surface area option selected for the Volume Adsorbed.
Action A: Edit the Isotherm report for the named overlay file and select a surface
area option for Volume Adsorbed.
Action B: Click Overlays on the Report options dialog of the primary file and
remove the named overlay file from the list.
4078- Slope and Y-Intercept cannot be determined from the selected points.
Cause: The Langmuir report cannot be generated from the selected points.
Action: Edit the calculation assignments in the Langmuir column on the

Collected Data dialog.
4079- Points found with negative pressure values will not appear on the graph.
Cause: Collected data contains negative pressure values.
Action: Negative pressure points are automatically removed from isotherm

graphs. If you wish to have negative pressure values appear on the
graph: Open the sample file and click the Collected Data tab.
Deselect Use calculation assignments and then select the points with
negative pressures as Outliers.
4400- The communications port specified for the SmartPrep(s) is not physically
installed in the Control Module. Cannot initialize.
Cause: The communications port associated with this unit was not valid.
Action: Run the setup program and set up the unit on a valid port.
B-32 Mar 08
4401- The communications port specified for the SmartPrep(s) is already in use. Can-
not initialize.
Cause: The communications port associated with this instrument is in use by

some other program in the system.
Action: Close the other program to release the port. Restart the TriStar 3020
application.
4402- The communications port specified for the SmartPrep(s) cannot be accessed.
Cannot initialize.
4403- Cannot communicate with SmartPrep Unit n - S/N: nn.
Cause: The communications port associated with this unit was not valid.
Action: Run the setup program and set up the unit on a valid port.
4404- The application version of the SmartPrep Unit n - S/N: nn is invalid.
Cause: The controller software running on the designated instrument is

invalid.
Action: Use the SmartPrep setup program to download the proper controller
software to the instrument, or contact a service representative if
unavailable.
4405- Fatal communications error with SmartPrep Unit n - S/N: nn.
Cause: There was a fatal error in the serial communications between the appli-
cation and the SmartPrep Instrument Controller. All displays for that
SmartPrep will be closed.
Action: Ensure that the SmartPrep is properly chained to the computer on the
communications port configured in the Setup program. Stop and re-
start the application. If this error persists, contact your service repre-
sentative.
Mar 08 B-33
6000 Series
6000- An error occurred while loading the application control information. Data entry
cannot be performed. (Code number)
Cause: An error occurred accessing the control information disk file required
by this application.
Action: The disk drive may have failed or be corrupt. Run diagnostics on the
disk drive.
6002- File cannot be opened for writing.
Cause: You attempted to save to a file that is marked as “read-only.” Files can
be marked automatically as read-only when they are transferred from a
CD to the application directory.
Action A: Use Windows Explorer to access the folder containing the file and dis-
able the Read-Only option.
Action B: Enter a different name to save the file.
6003- Unable to read the calibration file (number).
Cause: Your attempt to load a previously saved calibration file was unsuccess-
ful.
Action: Make sure the file exists, and that you have entered the file name cor-
rectly, then try again.
6004- Unable to write the calibration file (number).
Cause: Your attempt to save the calibration to a separate file was unsuccessful.
Action: Make sure that the disk is not full or write-protected, then try again.
B-34 Mar 08
6005- The sample has an invalid status and cannot be used for this analysis.
Cause: You selected a sample file with a status other than No Analysis or Pre-
pared.
Action: Select a sample file with a status of No Analysis or Prepared.
6008- At least one sample must be selected to proceed.
Cause: You attempted to start an analysis without selecting any sample files.
Action: Select at least one file, then start the analysis.
6010- This sample requires a different adsorptive and cannot be analyzed at the same
time as the other samples.
Cause: You selected a sample file for analysis that requires a different adsorp-
tive gas than the sample files selected for the other ports.
Action: Select only sample files to be analyzed with the same adsorptive and
perform the analysis. Then perform the analysis with the other adsorp-
tive.
6011- The adsorptive required by this analysis is not available on this instrument.
Cause: You attempted to start an analysis with an adsorptive that is not con-
nected to the instrument, or has not been designated in the software.
Action A: Make sure that the adsorptive is connected to the instrument. Then
select Unit [n] > Unit configuration to tell the application that the gas
is connected.
Action B: Select only sample files for which the analysis gas is available.
6015- Cannot read the sample tube properties parameter file.
Cause: The sample tube file you selected on the QuickStart screen cannot be
read.
Action: Select a different file.
Mar 08 B-35
6016- Dosing manifold from valve (number) failed.
Cause A: The maximum time was exceeded before the target pressure point was
reached. The nitrogen regulator may be set too low or turned off.
Action A: Set the analysis gas regulator to 10 psig (0.7 bar), then resume the anal-
ysis.
Cause B: The analysis gas bottle is empty.
Action B: Connect a new analysis gas bottle, then resume the analysis.
6017- Leak test failed on port (number).
Cause: With the sample port valve closed, the sample pressure increased by
0.15 mmHg before the leak test duration was completed.
Action: Check sample tube fitting and ensure that it is securely attached to the
port, then restart the analysis.
6018- Volume dosed exceeded 1000 cm3 STP. Analysis is canceled.
Cause: There is a problem with the analyzer’s calibration.
Action: Use the Setup program to reinstall the calibration files. If the problem
persists, contact y our Micromeritics service representative.
6019- Elevator failed to reach upper/lower limit switch.
Cause A: There is an obstruction in the elevator path.
Action A: Clear all obstructions and restart the analysis.
Cause B: Ice is present in the bottom or the neck of the Dewar, preventing the
elevator from rising completely.
Action B: Check the Dewar; remove ice and restart the analysis.
Action C: Contact your service representative if results for Actions A and B

failed.
B-36 Mar 08
6020- Warning, servo valve performance is out of specification.
Cause: The servo valve tried to dose to a pressure but was unable to reach it
within specification. The analysis will continue.
Action: At the next appropriate time, calibrate the servo valve to bring it back
within specification (refer to Chapter 9).
6021- Servo calibration failed.
Cause A: The maximum time was exceeded before the target pressure point was
reached. The nitrogen regulator may be set too low or turned off.
Action A: Set the analysis gas regulator to 10 psig (0.7 bar), then resume the anal-
ysis.
Cause B: The analysis gas bottle is empty.
Action B: Connect a new analysis gas bottle, then resume the analysis.
6022- This file already selected for the analysis.
Cause: You tried to choose a file for the analysis on this port which has been
selected for another port.
Action: Choose a different file.
6023- The instrument (number) is not calibrated.
Cause: The TriStar application is in the process of initializing the instrument

and is unable to locate the calibration files.
Action A: Click OK. Select Unit [n] > Calibration > Load from File and select
a file containing calibration data..
Action B: Click OK. Close the application and use the Setup program to reinstall
calibration files.
Mar 08 B-37
6024- Evacuation failed.
Cause: While attempting to zero the pressure transducers, the instrument was
unable to evacuate to a pressure of less than 1 mmHg. This may be due
to a leak or a bad calibration.
Action A: Check the sample tube fitting and ensure that it is securely attached to
the port.
Action B: Use the Setup program to reinstall the calibraiton files..
6026- Psat gas is not condensing.
Cause A: The working Dewar does not contain enough bath liquid.
Action A: Refill the Dewar and try the operation again.
Cause B: The Psat gas is contaminated.
Action B: Replace the Psat gas supply.
Cause C: The Psat tubing from the regulator to the instrument is contaminated.
Action C: Pump out the tubing.
6027- There is no nitrogen attached to the unit.
Cause: You attempted a calibration requiring nitrogen, but the software does
not recognize that nitrogen is attached.
Action: Be sure that a nitrogen gas bottle is installed at one of the analysis
ports, then Select Unit > Unit configuration and enter N2 for the
appropriate valve.
B-38 Mar 08
6028- The backfill gas required by this analysis is not available on this instrument.
6029- The Po gas required by this analysis is not available on this instrument.
Cause: You attempted to start an analysis with a gas that is not connected to
the instrument, or has not been designated in the software.
Action A: Make sure the gas is connected to the instrument. Then select Unit [n]
> Unit configuration to tell the application that the gas is connected.
6030- Dosing method choice is invalid. The Krypton analysis requires that Adsorptive
Properties “Dosing Method” is set to “From Psat tube.”
Cause: You selected a file for a krypton analysis that has Normal selected for
the Dosing Method. Normal is for standard analyses only.
Action: Open the sample file and change the Dosing Method to From Psat
tube or select a different file for the analysis.
6031- Dosing method choice is invalid. The analysis requires that Adsorptive Prop-
erties “Dosing Method” is set to “Normal.”
Cause: You selected a file for a standard analysis that has From Psat tube
selected for the Dosing Method. From Psat tube is for krypton anal-
yses only.
Action: Open the sample file and change the Dosing Method to Normal or
select a different file for the analysis.
6038- At least one report item must be selected. Press Cancel if you do not want a
report.
Cause: You selected a sample file on which to generate reports but there were
no reports selected.
Action: Open the file and select at least one report.
Mar 08 B-39
6040- Failed to reach pressure dosing through servo. Calibration canceled.
Cause A: There was insufficient gas pressure to calibrate for matching transduc-
ers. The gas is not connected or the tank is almost empty.
Action A: Be sure the gas is connected properly and assigned correctly in the Unit
Configuration dialog. Replace the tank if necessary.
Cause B: The gas valve is not working properly.
Action B: Contact your Micromeritics service representative.
6041- Servo Calibration failed.

6042- Master pressure transducer calibration failed. Offset is out of range.
6043- Port 1 pressure transducer calibraiton failed. Offset is out of range.
6044- Port 2 pressure transducer calibration failed. Offset is out of range.
6045- Port 3 pressure transducer calibration failed. Offset is out of range.
6047- 10-torr pressure transducer calibration failed. Offset is out of range.
6048- Master pressure transducer calibration failed. Scale is out of range.
6049- Port 1 pressure transducer calibration failed. Scale is out of range.
6052- Po pressure transducer calibration failed. Scale is out of range.
6053- 10-torr pressure transducer failed. Scale is out of range.
Cause: There is a problem with the analyzer’s calibration.
Action: Use the Setup program to reinstall the calibration files. If the problem
persists, contact your Micromeritics service representative.
B-40 Mar 08
TriStar II 3020 Appendix C
C. CALCULATIONS
This appendix contains the calculations used in the TriStar program.
Saturation Pressure
Saturation pressure (Po) is selected on the Po and Temperature Options dialog. It may be
entered or measured in the Po tube or on port 3.
• If entered, Po = user-entered value
• If measured, Po = equilibrated pressure reading after saturating Po tube or the sample

tube
Relative Pressure Calculations

If Po was measured at intervals in the Po tube and several data points were collected in the
interval:
• For points taken before the previous Po measurement,
( Po 2 – Po 1 ) × ( T I – To 1 )
Po I = Po 1 + -----------------------------------------------------------
-
( To 2 – To 1 )
• For points taken after the previous Po, use the previous Po:
PoI = Po1
If Po was entered, use the entered Po:
PoI = PoE
Calculate relative pressure for the Ith data point:
P
P rel1 = -------1-
Po I
Mar 08 C-1
Appendix C TriStar II 3020
where
PoI = saturation pressure for the Ith data point (mmHg)

Po1 = most previous measured saturation pressure before Ith data
point (mmHg)
Po2 = first measured saturation pressure after the Ith data point (mmHg)
PoC = calculated Po
PoE = entered saturation pressure (mmHg)
TI = time when the Ith data point was taken (minutes)
To1 = time when Po1 was measured (minutes)
To2 = time when Po2 was measured (minutes)
PrelI = relative pressure for the Ith data point (mmHg)
PI = absolute pressure for the Ith data point, taken at equilibrium (mmHg)
C-2 Mar 08
Volume Adsorbed Calculations
Free Space
Measured
Measured free-space volumes are calculated using the following equations:
V MAN P
- × -----1 – 1 × T STD
V FW = -----------
T MAN P2
P
V FC = V FW ⎛ -----2⎞
⎝ P 3⎠
V FC – V FW
V BATH = -----------------------
-
T BATH
1 – --------------
T AMB
where:
P1 = system manifold pressure before dosing helium onto sample (mmHg)

P2 = system manifold pressure after dosing helium onto sample (mmHg)
P3 = sample pressure after raising Dewar and equilibrating with helium (mmHg)
TSTD = standard temperature (273.15 K)
TAMB = approximate room temperature (298 K)
TMAN = system manifold temperature before dosing helium onto sample (K)
VMAN = manifold volume (cm3)
VFC = volume of free space, cold (cm3 at standard temperature)
VFW = volume of free space, warm (cm3 at standard temperature)
VBATH = portion of cold free space at analysis bath temperature: used in non-ideality
correction (cm3 at standard temperature)
TBATH = analysis bath temperature (K)
Mar 08 C-3
Calculated
The calculated free space is determined by subtracting the gas capacity of the volume occu-
pied by the sample from the measured free space of the empty tube.
T STD
V FW = V WB + ∆V – V S × -----------
-
T AMB
T STD
V FC = V CB + ∆V – V S × -------------
-
T BATH
where
VFW = calculated warm free space

VFC = calculated cold free space
VWB = warm free space of the empty tube
VCB = cold free space of the empty tube
∆V = VP - VPB
VP = volume of the port used for analysis
VPB = volume of the port used for the blank analysis
VS = sample mass/density
C-4 Mar 08
Equilibration
Equilibration is reached when the pressure change per equilibration time interval (first
derivative) is less than 0.01% of the average pressure during the interval. Both the first
derivative and average pressure are calculated using the Savitzky-Golay1 convolution method
for polynomial functions. The equations below are those used to compute weighted average
and first derivative, respectively, for the 6th point of an 11-point window.
– 36 ( P 11 + P 1 ) + 9 ( P 10 + P 2 ) + 44 ( P 9 + P 3 ) + 69 ( P 8 + P 4 ) + 84 ( P 7 + P 5 ) + 89 ( P 6 )
P AVG = -------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------
-
429
5 ( P 11 – P 1 ) + 4 ( P 10 – P 2 ) + 3 ( P 9 – P 3 ) + 2 ( P 8 – P 4 ) + ( P 7 – P 5 )
P CHG = ----------------------------------------------------------------------------------------------------------------------------------------------------------
-
110
P CHG
P PCPI = 100% -----------
-
P AVG
where the numerical constants are from the Savitzky-Golay convolution arrays, and
PAVG = average pressure (mmHg)

PCHG = change in pressure (mmHg)
PPCPI = percent change per interval
PI = Ith pressure reading taken at equilibrium intervals (mmHg)
If a non-zero value that is too small is entered for the maximum equilibration time,
the points are collected before equilibration is reached.
If PAVG is greater than 0.995 times the current Po, equilibration will not take place
until the Minimum equilibration delay for P/Po 0.995 has expired, in addition to the
standard equilibration criteria.
Mar 08 C-5
Thermal Transpiration Correction
During data reduction, thermal transpiration correction is applied to the data if the user
selected Thermal transpiration correction from the Report Options dialog. Starting with the
first collected pressure, the following calculations are performed until the pressure ratio (PC/
P) is greater than or equal to 0.99.
P × SD × MD
2
Y = ----------------------------------- × 10
3
2.33 × T
µ = 1 + G × Y-
----------------------
1+H×Y
1
F = -----------------------------------------------------
-
(α × Y ) + (β × Y) + µ
2
⎧ T ABT⎞ 0.5⎞ ⎫
PC = ⎨ 1 – F – ⎛ F ⎛ ---------- ×P
⎝ ⎝ T RM ⎠ ⎠ ⎬
⎩ ⎭
where:
P = equilibrated collected pressure measured by gauge at temp TRM (mmHg)

SD = inside diameter of sample tube (mm), from the Report Options dialog
MD = thermal transpiration hard sphere diameter of gas (Å), from the Adsorptive
Properties dialog
T = average temperature [TABT + TRM] / 2 (K)
α = Weber’s coefficient, 0.033
β = Weber’s coefficient, 0.245
G = Weber’s coefficient, 2.5
H = Weber’s coefficient, 2
TABT = analysis bath temperature (K), from the Po and Temperature Options dialog
TRM = room temperature (298 K)
PC = corrected equilibrated pressure at temperature TABT (mmHg)
F,Y,µ = intermediate values for subsequent calculations
C-6 Mar 08
BET Surface Area
For each point designated for surface area calculations, the BET2 transformation is calculated
as follows:
P rel1
B 1 = ---------------------------------------------
-
( 1.0 – P rel1 ) × N ads1
where BI is in units of g/cm3 STP.
A least-squares fit is performed on the (PrelI ,BI) designated pairs where PrelI is the
independent variable and BI is the dependent variable. The following are calculated:
a. Slope (S g/cm3 STP)
b. Y-intercept (YINT g/cm3 STP)
c. Error of the slope (SERR g/cm3 STP)
d. Error of the y-intercept (YIERR g/cm3 STP)
e. Correlation coefficient (Cc)
Using the results of the above calculations, the following can be calculated:
BET Surface Area (m2/g):
CSA × ( 6.023 × 10 )
23
SA BET = --------------------------------------------------------------------------------------------------------------------
-
( 22414 cm STP ) × ( 10 nm /m ) × ( S + Y INT )
3 18 2 2
where
CSA = analysis gas molecular cross-sectional area (nm2), user-entered on the

Adsorptive Properties dialog
BET C value:
S + Y INT
C = ------------------
-
Y INT
Mar 08 C-7
Volume of the Monolayer (cm3/g STP):
1 - = ------------------
V M = ------------------- 1 -
C × Y INT S + Y INT
Error of the BET Surface Area (m2/g):

2 0.5
SA BET × ( S ERR + YI ERR )
2
BET ERR = --------------------------------------------------------------------
-
Y INT + S
C-8 Mar 08
Langmuir Surface Area

For each point designated for surface area calculations, the Langmuir3 transformation is cal-
culated as follows:
P rel
L I = -----------I
N adsI
where LI is in units of g/cm3 STP
A least-squares fit is performed on the (PrelI, LI) designated pairs where PrelI is the indepen-
dent variable and LI is the dependent variable. The following are calculated:
a. Slope (S g/cm3 STP)
b. Y-intercept (YINT g/cm3 STP)
c. Error of the slope (SERR g/cm3 STP)
d. Error of the y-intercept (YIERR g/cm3 STP)
Langmuir Surface Area (m2/g):
CSA × ( 6.023 × 10 )
23
SA LAN = -----------------------------------------------------------------------------------------------
( 22414 cm STP ) × ( 10 nm /m ) × S
3 18 2 2
where
CSA = analysis gas molecular cross-sectional area (nm2), user-entered on the

Adsorptive Properties dialog
Volume of the Monolayer (cm3/g STP):
1
V M = ---
S
Langmuir b Value:
b = ( Y INT ) ( V M )
Error of the Langmuir Surface Area (m2/g):
SA LAN × S ERR
LAN ERR = -------------------------------
S
Mar 08 C-9
t-Plot
For each point designated for t-Plot4 calculations, the following calculations are done:
Thickness for the Ith point (Å):
HP3
HP2
t I = HP1 × -------------------- (Halsey5)
ln ( P relI )
or
HJP3
HJP1
t I = ------------------------------------------- (Harkins and Jura6)
HJP2 – log ( P relI )
or
t I = STSA1 ( P rel1 ) + STSA2 ( P rel1 ) + STSA3

2
where:
tI = thickness for Ith point

HP1 = Halsey parameter #1
HJP1 = Harkins and Jura parameter #1
STSA1 = statistical thickness surface area parameter #1
PrelI = relative pressure for the Ith point (mmHg)
A least-squares analysis fit is performed on the (tI, NadsI) data pairs where tI is the indepen-
dent variable and NadsI is the dependent variable. Only the values of tI between tMIN and
tMAX, the minimum and maximum thickness, are used. The following are calculated:
a. Slope (S cm3/g-Å STP)
b. Y-intercept (YINT cm3/g STP)
c. Error of the slope (SERR cm3/g-Å STP)
C-10 Mar 08
d. Error of the Y-intercept (YIERR cm3/g STP)
External Surface Area (m2/g):
( S cm /g – A STP ) × ( 10 A/m ) × ( D cm liquid/cm STP )

3 10 3 3
SA EXT = -------------------------------------------------------------------------------------------------------------------------------------------------------
-
F × ( 10 cm /m )
6 3 3
where
F = surface area correction factor, user-entered on the t-Plot Report Options dialog
D = density conversion factor, user-entered on the Adsorptive Properties dialog
Micropore Surface Area (m2/g):
SA µP = SA TOT + SA EXT
where SATOT is the BET surface area if the user enabled the BET report exclusively, or Lang-
muir surface area if the user enabled the Langmuir report exclusively. If neither report has
been selected, SATOT is the BET surface area value calculated using a set of default
parameters.
Micropore Volume (cm3 liquid/g):
V µP = ( Y INT cm /g STP ) × ( D cm liquid/cm STP )

3 3 3
Mar 08 C-11
BJH Pore Volume and Area Distribution

For adsorption data, the relative pressure and volume adsorbed data point pairs collected dur-
ing an analysis must be arranged in reverse order from which the points were collected during
analysis. All calculations are performed based on a desorption model, regardless of whether
adsorption or desorption data are being used.
The data used in these calculations must be in order of strictly decreasing numerical value.
Points which do not meet this criterion are omitted. The remaining data set is composed of
relative pressure (Pr), volume adsorbed (Va) pairs from (Pr1, Va1) to (PrN, VaN) where (PrN =
0, VaN = 0) is assumed as a final point. Each data pair represents an interval boundary (or de-
sorption step boundary) for intervals i=1 to i=N-1 where N = total number of (Pr, Va) pairs.
Generally, the desorption branch of an isotherm is used to relate the amount of adsorbate lost
in a desorption step to the average size of pores emptied in the step. A pore loses its con-
densed liquid adsorbate, known as the core of the pore, at a particular relative pressure related
to the core radius by the Kelvin7 equation. After the core has evaporated, a layer of adsorbate
remains on the wall of the pore. The thickness of this layer is calculated for a particular rel-
ative pressure from the thickness equation. This layer becomes thinner with successive
decreases in pressure, so that the measured quantity of gas desorbed in a step is composed of
a quantity equivalent to the liquid cores evaporated in that step plus the quantity desorbed
from the pore walls of pores whose cores have been evaporated in that and previous steps.
Barrett, Joyner, and Halenda8 developed the method (known as the BJH method) which incor-
porates these ideas. The algorithm used on the TriStar 3000 is an implementation of the BJH
method.
Explanation of Terms
A pore filled with condensed liquid nitrogen has three zones:
a. The core - evaporates all at once when the critical pressure for that radius is reached;
the relationship between the core radius and the critical pressure is defined by the
Kelvin equation.
b. The adsorbed layer - composed of adsorbed gas that is stripped off a bit at a time
with each pressure step; the relationship between the thickness of the layer and the
relative pressure is defined by the thickness equation.
C-12 Mar 08
c. The walls of the cylindrical pore - the diameter of the empty pore is required to
determine the pore volume and pore area. End area is neglected.
pore
a
d
s
o
r c
b o wall
e r
d e
l
a
y
Insignificant e
compared to r
core length
Calculations
The volumes adsorbed (Va) are converted to the liquid equivalent volumes (V1, cm3/g):
VI I = ( Va I ) ( D )
where D is the Density Conversion Factor from the Adsorptive Properties dialog.
The relative pressure (Pr1) is assumed to be close to unity so that substantially all the pores in
the sample are filled.
The corresponding Kelvin core radius is calculated. Only pores smaller than this size will be
included:
–A
Rc I = ----------------------------------------
-
( 1 + F ) [ ln ( Pr I ) ]
where
A = adsorbate property factor (the BJH Adsorptive Options dialog)

F = fraction of pores open at both ends (from the BJH Adsorption Report Options
dialog or the BJH Desorption Report Options dialog); assumed to be zero for
desorption
This radius will be adjusted for the thickness of the adsorbed layer during subsequent calcu-
lation steps.
Mar 08 C-13
The thickness of the remaining adsorbed layer at this relative pressure is calculated:
HP3
HP2
Tw 1 = HP1 ------------------
ln ( Pr 1 )
where
HP1, HP2, and HP3 are Halsey Parameters 1, 2, and 3 (respectively) from the Halsey Thick-
ness Equation dialog.
These calculations illustrate the use of the Halsey thickness equation. If the Harkins/Jura
equation was selected, substitute the following wherever the thickness equation appears:
HJ3
HJ1
Tw 1 = --------------------------------------
HJ2 – log ( Pr 1 )
where
HJ1, HJ2, and HJ3 are Harkins-Jura Parameters 1, 2, and 3 (respectively) from the Harkins-
Jura Thickness Equation dialog.
The following calculations (a-c) are made for each relative pressure interval based on the
increment of volume desorbed during that interval. The variable I refers to the interval num-
ber, that is I=1 for the first interval from Pr1 to Pr2, and so on. J refers to each previous
interval during which new pores were found. K refers to the total number of intervals in
which new pores have been found. K is also the number of lines reported on the BJH table for
collected data.
a. The thickness of the adsorbed layer at the end of the interval is calculated as follows:
HP3
HP2
Tw I + 1 = HP1 ------------------------
ln ( Pr I + 1 )
(For the last pressure interval from the lowest PrI to zero relative pressure, TwI+1 = 0.)
For the first pressure interval, there are no previously opened pores so the volume
desorbed from walls of previously opened pores is zero (Vd1 = 0), and the remainder
of Step (a) is skipped.
The change in thickness of the wall layer due to desorption from previously opened
pores is calculated:
∆Tw = Tw 1 – Tw I + 1
C-14 Mar 08
The annular cross-sectional area of the wall layer desorbed is calculated for all pre-
viously opened pores:
CSA J = π [ ( Rc j + ∆Tw ) – Rc j ] ( 10 cm /A )
2 2 – 16 2 2
The total volume of gas desorbed from walls of previously opened pores is
calculated:
Vd I = ∑ ( Lp J ) ( CSAaJ ) for all previously opened pores
where LPJ = length of previously opened pores as calculated in Step b(2).
b. The physical processes occurring for this pressure interval are determined as follows:
(1) If VdI is greater than the current increment of volume desorbed (VlI - VlI+1),
desorption from walls only is occurring. Total surface of walls exposed thus far
(cm2/g) is calculated as follows:
∑ π ( LPJ ) ( Davg ) ( 10 cm/A ) for all previously opened pores

–8
SA W = J
where
DavgJ = weighted average pore diameter calculated below in Step b(2).
A new layer thickness (∆Tw) that will not overcompensate for the actual volume
desorbed in this interval is calculated:
( V1 I – V1 I + 1 ) ( 10 A/cm )
8
∆Tw = --------------------------------------------------------------
SAw I
Since no cores are evaporated in this pressure interval, no new pores are revealed.
Thus no ending Kelvin radius and average pore diameter are calculated for this
interval. Note that this means the report may have fewer tabulated intervals on
the collected data report than experimental pressure intervals.
(2) If VdI is less than the volume increment desorbed during this interval
( Vl 1 – Vl l + 1 ) , the remaining volume is due to new pores with core evaporation
taking place in this interval. K, the number of intervals with new pores exposed,
is increased by 1. (For the interval from the lowest Pr1 to zero relative pressure,
no new pore volume is calculated and the rest of Step b is skipped.)
Mar 08 C-15
The volume desorbed from newly opened pores in this interval is calculated as
follows:
Vc I = ( VI I – VI I + 1 ) – Vd I
The Kelvin radius for the end of the interval is calculated as follows:
–A
Rc K + 1 = -----------------------------------------------
( 1 + F ) [ ln ( Pr I + 1 ) ]
All new pores opened in this interval are represented by one pore having a
length-weighted average pore diameter and a corresponding length sufficient to
account for the required volume of adsorbate. The weighted average pore diam-
eter is calculated as follows:
( 2 ) ( Rc K + Rc K + 1 ) ( Rc K ) ( Rc K + 1 )
D avgK = ------------------------------------------------------------------------------
2 2
-
Rc K + Rc K + 1
DavgK is the diameter of a pore which would have a surface area that is the aver-
age of the areas for pores radius RcK and RcK+1, if its length was the mean of the
lengths at those radii.
The relative pressure corresponding to is calculated as follows:
–1 – 2A
P avgK = ln -----------------------------------
( 1 + F ) ( D avgK )
The thickness of the adsorbed layer at this pressure is calculated as follows:
HP3
HP2
Tw avgK = HP1 ----------------------
ln ( P avgK )
The decrease in thickness of the wall layer by desorption from the walls of new
pores during the lower portion of the pressure interval is calculated as follows:
∆Td = Tw avgK – TW I + 1
The cross-sectional area of the newly opened pores is calculated as follows:

2
Davg
CSAc K = ----------------K + ∆Td ( 10 cm /A )
– 16 2 2
2
C-16 Mar 08
The length of the newly opened pores is calculated as follows:
Vc I
LP K = ----------------
-
CSAc K
c. Pore diameters and radii are adjusted for the change in thickness of the adsorbed wall
layer during this interval. If new pores were opened during this interval, the average
diameter is adjusted by the change in layer thickness during the second portion of the
desorption interval as follows:
D avgKnew = D avgKold + 2 ( ∆Td )
The layer thickness change during the whole interval is added to diameters of previ-
ously opened pores as follows:
D avgJnew = D avgJold + 2 ( ∆ Tw )
(not including DavgK)
The layer thickness change desorbed during this interval also is added to the radii
corresponding to the ends of the pressure intervals as follows:
Rc Jnew = Rc Jold + ∆Tw
for all except RcK+1.
Steps a to c are repeated for each pressure interval.
After the above calculations have been performed, the diameters corresponding to the
ends of the intervals are calculated as follows:
Dp J = 2 ( Rc J )
for all RcJ including RcK+1.
The remaining calculations are based on DP(I), Davg(I), and LP(I). These calculations
are only done for Davg(I) values that fall between the Minimum BJH diameter and the
Maximum BJH diameter specified by the operator on the BJH Adsorption Report
Options dialog or the BJH Desorption Report Options dialog.
1) Incremental Pore Volume (VpI, cm3/g):
D avg 2 16
Vp I = π ( Lp I ) -----------I 10 cm /A
2 2
2
Mar 08 C-17
2) Cumulative Pore Volume (VpCUM(1), cm3/g):
VP CUM( 1 ) = ∑ VpJ for ( J ≤ 1 )

3) Incremental Surface Area (SAI, m2/g):
SA I = π ( LP I ) ( 10 m/cm ) ( D avgI ) ( 10 m/A )

–2 – 10
4) Cumulative Surface Area (SACUM(I), m2/g):
SA CUM10 = ∑ SAJ for J ≤ 1

5) dV/dD pore volume (dV/dDI, cm3/g-A):
VP I
dV/dD I = -----------------------------
-
Dp I – Dp I + 1
6) dV/dlog(D) pore volume (dV/dlog(D)I, cm3g):
Dp I ⎞
dDv/d log ( D ) I = VP I / log ⎛ --------------
-
⎝ Dp I + 1⎠
7) dA/dD pore area (dA/dDI, m2/g-A):
SA I
dA/dD I = -----------------------------
-
Dp I – Dp I + 1
8) dA/dlog(D) pore area [dA/dlog(D)I, m2/g]:
Dp I ⎞
dA/d log ( D ) I = SA I / log ⎛ --------------
-
⎝ Dp I + 1⎠
C-18 Mar 08
For fixed pore size tables (if selected), the following calculations are performed:
1) Average Fixed Pore Size (DFavgJ, A):
Dp FJ + Dp FJ + 1
DF avgJ = ---------------------------------
2
calculated for all intervals in the fixed pore size table.
For the intervals with between the Minimum BJH diameter and the Maximum
BJH diameter.
2) Cumulative Pore volume (VpFCUMI, cm3/g):
VpF CUMI = INTERP ( DpF I + 1 )
where INTERP(x) is the value interpolated from the function X = DpJ+1 and Y =
VPCUMJ, using an AKIMA semi-spline interpolation.
3) Incremental Pore Volume (VpFI, cm3/g):
VpF I = VpF CUMI – VpF CUMI – 1
where VpFCUM0 = 0.
4) Cumulative Surface Area (SAFCUMI, m2/g):
SAF CUMI = INTERP ( DpF I + 1 )
where INTERP(x) is the value interpolated from the function X = DpJ+1 and Y =
SACUMJ.
5) Incremental Surface Area (SAFI, m2/g):
SAF I = SAF CUMI – SAF CUMI – 1
where SAFCUM0 = 0.
Mar 08 C-19
6) dV/dD pore volume (dV/dDpFI, cm3/g-A)):
dV/dDpF I = INTERP ( DpF I + 1 )
where INTERP(x) is the value interpolated from the function X = DavgJ and Y =
dV/dDJ.
7) dV/dlog(D) pore volume [dV/dlog(DpF)I, cm3/g]:
dV/d log ( D pF I ) = INTERP ( DpF I + 1 )
dV/dlog(D)J.
8) dA/dD pore area (dA/dDpFI, m2/g-A):
dA/dDpF I = INTERP ( DpF I + 1 )
dA/dDJ.
9) dA/dlog(D) pore area [dA/dlog(DpFI), m2/g]:
dA/d log ( D pF I ) = INTERP ( DpF I + 1 )
dA/dlog(D)J.
C-20 Mar 08
Compendium of Variables
Va = quantity adsorbed expressed as a volume (cm3/g STP)

Vl = liquid equivalent volume of volume adsorbed (cm3/g)
D = density conversion factor from the Adsorptive Properties dialog
(cm3/cm3 STP)
Pr = relative pressure
Dp = pore (or core) diameter (A)
Rc = Kelvin radius (A) of core
A = adsorbate property factor; from the BJH Adsorptive Options dialog
F = fraction of pores open at both ends; from the BJH Adsorption Report
Options dialog or the BJH Desorption Report Options dialog
∆Tw = thickness of adsorbed layer desorbed during interval (A)
Tw = thickness of remaining adsorbed wall (A)
HP1, HP2, and HP3 are Halsey Parameters from the Halsey Thickness Equation dialog.
HJ1, HJ2, and HJ3 are Harkins and Jura Parameters from the Harkins/Jura Thickness Equa-
tion dialog.
STSA1, STSA2, and STSA3 are STSA parameters from the STSA Thickness Equation
dialog.
Vd = volume of gas desorbed from walls of previously opened pores (cm3/g)

Davg = average pore diameter (A)
CSAa = annular cross-sectional area of the desorbed layer (cm2)
CSAc = cross-sectional area of opening of newly opened pores (cm2)
SAw = total surface area of walls exposed (cm2/g)
∆Td = thickness of layer desorbed from walls of newly opened pores (A)
Vc = volume desorbed from cores of newly opened pores (cm3/g)
Lp = length of pore (cm/g)
Mar 08 C-21
Horvath-Kawazoe
A relative pressure lower limit is determined such that L-d0 never equals zero. All pressure
points less than this limit are discarded. For each collected relative pressure point, values of L
are chosen in an iterative manner, and the relative pressure (P/Po) determined by solving one
of the following equations:
• Slit Pore Geometry (original Horvath-Kawazoe)

• Cylinder Pore Geometry (Saito/Foley)
• Sphere Pore Geometry (Cheng/Yang)
Slit Pore Geometry (original HK)
When you use the original Horvath-Kawazoe9 method, the following equation is solved for
each value of P. The value of L is determined when the solved-for relative pressure is within
0.1% of the collected absolute pressure.
K IP × 10 JA /J cm
32 4 4
σ σ σ σ
4 10 4 10
P
ln ------- = ------- × -------------------------------------------------
- × -----------------------------
- – -----------------------------
- – --------------- + --------------
-9
σ × ( L – 2 × d0 )
RT 4
3 × ( L – d0 ) 9 × ( L – d0 ) 3 × d0 9 × d0
Po 3 9 3
where
K = Avogadro’s number (6.023 x 1023)

R = gas constant (8.31441 x 107 ergs/mole K)
T = analysis bath temperature (K), from an entered or calculated
value on the Po and Temperature Options dialog
ZS + ZA
σ = gas solid nuclear separation at zero interaction energy (Å), ----------------
-
2
where:
ZS = sample equilibrium diameter at zero interaction energy (Å) from the
Horvath-Kawazoe Physical Properties dialog
ZA = zero interaction energy diameter from the Horvath-Kawazoe Physical

Properties dialog
DA + DS ( A )
d0 = -----------------------------
-
2
where:
DA = molecular diameter (Å) from the Horvath-Kawazoe Physical
Properties dialog
DS = diameter of sample atom (Å) from the Horvath-Kawazoe Physical

dialog
L = pore width (nucleus to nucleus) (Å)
C-22 Mar 08
P = equilibrium pressure (mmHg)

Po = saturation pressure (mmHg)
IP = interaction parameter (10-43 ergs-cm4) from the Horvath-Kawazoe Report
Options dialog
Cylinder Pore Geometry (Saito/Foley)
When you use the Saito-Foley10 method, the following equation is solved for each value of P.
The value of L is determined when the solved-for relative pressure is within 0.1% of the
collected absolute pressure.
∞
3 πK IP × 10 JA /J cm
32 4 4
d 2k ⎧ 21 d 10 d 4⎫
ln ⎛ -------⎞ = --- ------- × ------------------------------------------------- ------------ ⎛ 1 – -----0⎞ × ⎨ ------ α k ⎛ -----0⎞ – β k ⎛ -----0⎞ ⎬
P 1
⎝ Po⎠ 4 RT 4
-× ∑ k + 1⎝ rp⎠ ⎝ rp ⎠ ⎝ rp⎠
d0 k=0
⎩ 32 ⎭
where
K = Avogadro’s number (6.023 x 1023)

T = analysis bath temperature (K), from an entered or calculated
value on the Po and Temperature Options dialog
IP = interaction parameter (10-43 ergs-cm4) from the Horvath-Kawazoe Report
Options dialog
DA + DS ( A )
d0 = ---------------------------
-
2
where:
DA = molecular diameter (Å) from the Horvath-Kawazoe Physical
Properties dialog
dialog
2
αk = ⎛ –-------------------
4.5 – k⎞
- α ,α = 1.0
⎝ k ⎠ k–1 0
2
βk = ⎛ –-------------------
1.5 – k⎞
- β ,β = 1.0
⎝ k ⎠ k–1 0
L
rp = radius of the cylindrical pore, ---
2
Mar 08 C-23
Sphere Pore Geometry (Cheng/Yang)
When you use the Cheng/Yang11 method, the following equation is solved for each value of
P. The value of L is determined when the solved-for relative pressure is within 0.1% of the
collected absolute pressure.
6 ( N 1 ε 12 + N 2 ε 22 )L × 10 J A /J cm
* * 3 32 4 4
ln ⎛ -------⎞ = ---------------------------------------------------------------------------------------------------
P
-
⎝ Po⎠ RT ( L – d )
3
0
d 6 1 d 12 1
– ⎛ -----0⎞ ⎛ ------ T 1 + --- T 2⎞ + ⎛ -----0⎞ ⎛ ------ T 3 + ------ T 4⎞
1 1
⎝ L ⎠ ⎝ 12 8 ⎠ ⎝ L ⎠ ⎝ 90 80 ⎠
where

T = analysis bath temperature (K), from an entered or calculated value on the Po
and Temperature Options dialog
DA + DS ( A )
d0 = ---------------------------
-
2
where:
DA = molecular diameter (Å) from the Horvath-Kawazoe Physical Properties
dialog
dialog
N1 = 4π L2 NS, where NS = number of sample atoms/cm2 at monolayer
N2 = 4π (L - d0)2 NA, where Ns = number of gas molecules/cm2
6 × MC × α S × α A
2
AS
e*12 = -----------
-6 , where A S = --------------------------------------------
-
4d S αS αA
----- + ------
χS χA
3 × MC × α A × χ A
2
AA
ε*22 = -------------
-6 , where A A = --------------------------------------------
-
4D A 2
1 1
T1 = -------------------3 – -------------------3
(1 – S) (1 + S)
T2 = ------------------ 1 -
1 - – ------------------
(1 + S) (1 – S)
2 2
C-24 Mar 08
T3 = ------------------ 1 -
1 - – ------------------
(1 – S) (1 + S)
9 9
T4 = ------------------ 1 -
1 - – ------------------
(1 + S) (1 – S)
8 8
L–d
where S = --------------0
L
Cheng/Yang Correction
This factor corrects for the nonlinearity of the isotherm. It adds an additional term to the
equations for the different geometrics:
ln ⎛ -------⎞ = G ( L ) – 1 – --- ln ⎛ ------------⎞

P 1 1
⎝ Po⎠ θ ⎝ 1 – θ⎠
where
G(L) = one of the Horvath-Kawazoe equations given above

θ = degree of void filling; θ is estimated by first computing the monolayer
capacity (Vm) with the Langmuir equation over the range of data points from
relative pressure 0.02 to 0.2 or the maximum relative pressure included in the
Horvath-Kawazoe analysis. θ is computed as the volume adsorbed over Vm.
Mar 08 C-25
Interaction Parameter
The interaction parameter (IP) results from the following calculations:
The Kirkwood-Muller dispersion coefficients -
6 × MC × α S × α A
2
A S = --------------------------------------------
-
αS αA
----- + ------
χS χA
3 × MC × α A × χ A
2
A A = --------------------------------------------
-
2
where
MC2 = kinetic energy of electron (0.8183 x 10-6 erg)

αS = polarizability of sample atoms (cm3)
αA = polarizability of gas molecule (cm3)
χS = diamagnetic susceptability of sample atom (cm3)
χA = diamagnetic susceptability of gas molecule (cm3)
IP = ( N A × A A ) + ( N S × A S )
where:
NA = number of gas molecules/cm2 at monolayer from the Horvath-Kawazoe

Physical Properties dialog
NS = number of sample atoms/cm2 from the Horvath-Kawazoe Physical Properties
dialog
Refer to Interaction Parameter Components later in this Appendix for recommended

values.
C-26 Mar 08
Additional Calculations
Based on the previous calculations, the following can be calculated:
Adjusted Pore Width (Å):

(Shell to Shell)
AL I = L I – DS
Cumulative Pore Volume (cm3/g):
V CUMI = V I × D
where
D = density conversion factor (cm3 liquid/cm3 STP) on the Adsorptive Properties

dialog
dV/dD Pore Volume (cm3/g-Å):
dV V CUMI – V CUMI – 1
--------- = -------------------------------------
-
dD I AL I – AL I – 1
Median Pore Width (Å):
V CUM
V HALF = --------------N
2
log ( D G ) – log ( D L )
D MED = 10 log ( D L ) + [ log ( V HALF ) – log ( V L ) ] × ---------------------------------------------
-
log ( V G ) – log ( V L )
where
VCUMN = total cumulative pore volume (VCUMI) for points designated for Horvath-
Kawazoe calculations
VHALF = 50% of total cumulative pore volume
VL = cumulative pore volume (VCUMI) for first point less than VHALF
VG = cumulative pore volume (VCUMI) for first point greater than VHALF
DL = pore width (LI) that corresponds to VL
DG = pore width (LI) that corresponds to VG
Mar 08 C-27
Interaction Parameter Components
Table C-1. Interaction Parameters
Interaction
Bath Parameter
Temperature Calculated
Gas (K) Sample Type Value*
Argon 87.3 Carbon (Ross/Olivier value) 2.61
Carbon (Horvath/Kawazoe value) 5.89
Zeolite 3.19
Carbon 298.15 Carbon (Ross/Olivier value) 4.20
Dioxide Carbon (Horvath/Kawazoe value) 9.20
Zeolite 5.08
273.15 Carbon (Ross/Olivier value) 4.34
Zeolite 5.22
194.65 Carbon (Ross/Olivier value) 4.72
Zeolite 5.60
Nitrogen 77.15 Carbon (Ross/Olivier value) 2.84
Zeolite 3.49
*The interaction parameter is entered in the Horvath-Kawazoe Report Options dialog in the
following field:
Interaction parameter: (calculated value) x 10-43 ergs-cm4
The following values were used to calculate the values in Table C-1.
Carbon-Graphite Zeolite
DS = 3.40 DS = 3.04
NS = 3.845 x 1015 NS = 3.75 x 1015
χS = 1.05 x 10-29 (Ross/Olivier) χS = 1.94 x 10-29
13.5 x 10-29 (Horvath/Kawazoe, implicit) αS = 0.85 x 10-24
αS = 1.02 x 10-24
Nitrogen Argon
DA = 3.00 DA = 2.95
ΝA = 6.71 x 1014 ΝA = 7.608 x 1014
χA = 3.6 x 10-29 χA = 3.22 x 10-29
αA = 1.76 x 10-24 αA = 1.63 x 10-24
C-28 Mar 08
Carbon Dioxide
DA = 3.23
NA = 4.567 x 1014 (25 ºC)
5.45 x 1014 (0 ºC)
7.697 x 1014 (-78 ºC)
χA = 5.0 x 10-29
αA = 2.7 x 10-24
DA values are from van der Waal’s constant.

NA values are from liquid densities.
χ and α values are derived from data found in Ross and Olivier12.
The physical parameters referenced in Saito/Foley are as follows:
Aluminophosphate Aluminosilicate
DS = 2.60 DS = 2.76
NS = 1.48 x 1015 Ns = 1.31 x 1015
χS = 1.3 x 10-29 χS = 1.3 x 10-29
αS = 2.5 x 10-24 αS = 2.5 x 10-24
Mar 08 C-29
Dubinin-Radushkevich
The Dubinin-Radushkevich13 equation is as follows:
B×T
2 2
log ( V ) = log ( Vo ) – --------------- × log Po
-------
β P
where:
V = volume adsorbed at equilibrium pressure (cm3/g STP)

Vo = the micropore capacity (cm3/g STP)
Po = saturation vapor pressure of gas at temperature T (mmHg)
B = a constant
β = the affinity coefficient of analysis gas relative to Po gas
(for this application β is taken to be 1)
T = analysis bath temperature (K), from the Po and Temperature Options
dialog
For each point designated for Dubinin-Radushkevich calculations, the following calculations
are done:
LV = log (V)
2
LP = log ⎛ -------⎞
Po
⎝ P⎠
The intercept, log(Vo) can be found by performing a least-squares fit on the (LP,LV) desig-
nated pairs where LP is the independent variable and LV is the dependent variable. Assuming
the adsorption of gas is restricted to a monolayer, Vo is the monolayer capacity. Based on this
assumption, the following are calculated:
a. Slope (S cm3/g STP)
b. Y-intercept (YI cm3/g STP)
c. Error of the slope (SERR cm3/g STP)
d. Error of the y-intercept (YIERR cm3/g STP)
C-30 Mar 08
Monolayer Capacity (cm3/g STP):
Vo = 10YI
Error of Monolayer Capacity (cm3/g STP):
VoERR = Vo x (10YIERR - 1.0)
Micropore surface area (m2/g):
σ × Vo × ( 6.023 × 10 )
23
SDP = --------------------------------------------------------------------
22414 cm × ( 10 nm /m )
3 18 2 2
where
σ = molecular cross sectional area of gas (nm2) from the Adsorptive

Properties dialog
Mar 08 C-31
Dubinin-Astakhov
The Dubinin-Astakhov equation is a follows:
N N
RT Po
log ( V ) = log ( Vo ) – --------- × log -------
βE 0 P
where
V = volume adsorbed at equilibrium pressure (cm3/g STP)

Vo = the micropore capacity (cm3/g STP)
Po = saturation vapor pressure of gas at temperature T (mmHg)
T = analysis bath temperature (K)
R = the gas constant (0.0083144 kJ/mol)
E0 = characteristic energy (kJ/mole)
N = Astakhov exponent, may be optimized or user entered from the Dubinin
Report Options dialog
β = the affinity coefficient of the analysis gas relative to the Po gas, from the
Dubinin Adsorptive Options dialog
For each point designated for Dubinin-Astakhov calculations, the following calculations are
done:
LV = log(V)
N
Po
LP = log -------
P
A least-squares fit is performed on the (LP,LV) designated pairs where LP is the independent
variable and LV is the dependent variable. If the user selected Yes for the Optimize Asta-
khov Exponent prompt, a systematic search for the optimum value of N is conducted by
recalculating the linear regression and selecting the value of N that gives the smallest stan-
dard error of the y-intercept. The exponent N is optimized to within 10-4. If the optimum
value for N is not found in this range, an exponent of 2 is used. The following are calculated:
a. Slope (S cm3/g STP)
b. Y-intercept (YI cm3/g STP)
c. Error of the slope (SERR cm3/g STP)
d. Error of the y-intercept (YIERR cm3/g STP)
f. Optimized Astakhov exponent (N)
C-32 Mar 08
Monolayer Capacity (cm3/g STP):
V0 = 10YI
Micropore Volume (cm3/g):
WI = (VI x D)
where
D = density conversion factor (cm3 liquid/cm3 STP) from the Adsorptive

properties dialog
Limiting Micropore Volume (cm3/g):
W0 = (V0 x D)
where
D = density conversion factor (cm3 liquid/cm3 STP) from the Adsorptive

Properties dialog
Error of Limiting Micropore Volume (cm3/g):
W0ERR = W0 x (10YIERR - 1.0)
Characteristic Energy (KJ/mole):
2.303 × R × T
E = ------------------------------------
-
β ( 2.303 × S )
1/N
Modal Equivalent Pore Diameter (Å):

1/3
⎧ 3N 1/N
10 nm /A ⎫
3 3 3
D MODE = 2 × ⎨ ---------------- × ---------------------------- ⎬
⎩ 3N + 1 β ⋅ Eo ⎭
where
β = affinity coefficient of the analysis gas relative to the Po gas from the
Dubinin Adsorptive Options dialog
Mar 08 C-33
Maximum Differential Pore Volume (cm3/g-Å):
This value is also known as frequency of the mode12
1/3N
β ⋅ E0 1/3
× exp ⎛ – ---------------- ⎞
dV - 3N + 1 3N + 1
---------------- Max = 0.5 × ( 3N + 1 ) × W o × ---------------- × ---------------------------
-3
dD mode 3N 3
10 nm /A
3 ⎝ 3N ⎠
Mean Equivalent Pore Width (Å):

3 3 3 1/3
10 nm /A
----------------------------
β ⋅ E0
D MEAN = 2 × --------------------------------------
-
⎛ 3N +
Γ ----------------
1 ⎞
⎝ 3N ⎠
Micropore surface area (m2/g):

1/3
E
× Γ ⎛ ----------------⎞
3N + 1
SDA = 1000 × 2.0 × W 0 × -----0
k ⎝ 3N ⎠
Γ is calculated by a polynomial approximation over the domain 0 ≤ x ≤ 1 as follows:
Γ(x+1) = 1+b1x + b2x2 + b3x3 + b4x4 + b5x5 + b6x6 + b7x7 + b8x8 + ε(x) | ε(x) | ≤ 3 x
10-7
where
b1 = -0.57719 1652
b2 = 0.98820 5891
b3 = -0.89705 6937
b4 = 0.91820 6857
b5 = -0.75670 4078
b6 = 0.48219 9394
b7 = -0.19352 7818
b8 = 0.03586 8343
and where
x + 1 = ⎛ ----------------⎞
3N + 1
⎝ 3N ⎠
C-34 Mar 08
Equivalent Pore Diameter (Å):

3 3 3 N 1/3N
– ⎛ ----------------------------⎞
10 nm /A
⎝ β ⋅ E0 ⎠
D i = 2 × -----------------------------------------
ln ( W i ) – ln ( W 0 )
dV/dD Pore Volume (cm3/g-Å):
3 3 3 N
D –( 3N + 1 ) 3 3 3 N
D –3N
× ⎛ -----i⎞ × exp – ⎛ ---------------------------- ⎞ × ⎛ -----i⎞
dV 10 nm /A 10 nm /A
-------- = 0.5 × W 0 × 3N × ----------------------------
dD i β ⋅ E0 ⎝ 2⎠ ⎝ β ⋅ E0 ⎠ ⎝ 2⎠
Mar 08 C-35
MP-Method
For each point designated for MP-method14 calculations, the following calculations are done:
Thickness for the Ith point (Å):
HP3
HP2
t I = HP1 × -------------------- (Halsey5)
ln ( P relI )
or
HJP3
HJP1
t I = ------------------------------------------- (Harkins and Jura6)
HJP2 – log ( P relI )
where:
tI = thickness for Ith point

PrelI = relative pressure for the Ith point (mmHg)
With the (tI,VI) data pairs, the Akima semi-spline interpolation method is used to interpolate
volume adsorbed values based on thickness values that are evenly spaced 0.2 Angstrom apart
starting at the first outlier point. Outliers are defined as those points have the maximum
instantaneous slope within an iteratively shrinking subset of all points. The remaining pore
surface area calculation result is the slope of the line defined by two consecutive interpolated
points. The slopes of each pair of consecutive points from the origin to the last point must be
monotonically decreasing and non-negative. With the interpolated points set the following
can be calculated:
Average pore hydraulic radius (Å):
tI + tI – 1
R I = -----------------
-
2
C-36 Mar 08
Remaining pore surface area for the Ith point (m2/g):
( V I – V I – 1 ) × ( D × 10 m /cm )
–6 3 3
S I = ------------------------------------------------------------------------------
-
( t I – t I – 1 ) × 10 m/A
– 10
where
D = density conversion factor (cm3 liquid/cm3 STP) on the Adsorptive Properties

dialog
Incremental pore surface area occluded for the Ith point (m2/g):
S INCI = S I – 1 – S I
Cumulative pore surface area occluded for the Ith point (m2/g):
S CUMI = S INCI + S INCI – 1 + … + S INC1
dA/dR pore surface area for the Ith point (m2/g-Å):
dA S INCI
-------- = -----------------
-
dR I tI – tI – 1
Incremental pore volume occluded for the Ith point (cm3/g):
V INCI = ( S INCI × 10 cm /m ) × ( R I × 10 cm/Å )

4 2 2 –8
Cumulative pore volume occluded for the Ith point (cm3/g):
V CUMI = V INCI + V INCI – 1 + … + V INC 1
dV/dR pore volume for the Ith point (cm3/g-Å):
dV V INCI
-------- = -----------------
-
dR I tI – tI – 1
Mar 08 C-37
Freundlich Isotherm
The Freundlich isotherm has the form:
Q 1/m
------- = CP
Qm
where
Q = quantity of gas adsorbed

Qm = quantity of gas in a monolayer
C = temperature-dependent constant
m = temperature-dependent constant
The pressure is absolute; typically, m > 1. In terms of quantity adsorbed,
1/m
Q = Q m CP
Taking the log of both sides yields:
1
log Q = log Q m C + ---- log P
m
C-38 Mar 08
Temkin Isotherm
The Temkin isotherm has the form,
Q RT
------- = --------- ln ( A 0 P )
Qm q0 α
where
Q = quantity of gas adsorbed

Qm = quantity of gas in a monolayer
q0 = the differential heat of adsorption at zero surface coverage
A = a0 exp {-q0/RT}, where α0 and a0 are adjustable constants
In terms of quantity adsorbed,
RTQ
Q = --------------S ln A 0 + ln ⎛ -------⎞
P
q0 α ⎝ Po⎠
Thus, the plot of the natural log of absolute pressure vs. quantity adsorbed yields a straight
line with slope RTQm/q0 and intercept (ln A) RTQm/q0α.
Mar 08 C-39
DFT (Density Functional Theory)
The adsorption isotherm is known to convey a great deal of information about the energetic
heterogeneity and geometric topology of the sample under study. The data of physical adsorp-
tion have been used for many years as the basis for methods to characterize the surface area
and porosity of adsorbents. Real solid surfaces rarely approach ideal uniformity of structure.
It is accepted that in general, the surface of even a nonporous material presents areas of
greater or lesser attraction for adsorbed molecules.
This energetic heterogeneity greatly affects the shape of the adsorption isotherm with the
result that simple theories such as the Langmuir and BET formulas can, at best, give only
approximate estimates of surface area. Porous solids virtually are never characterized by a
single pore dimension, but instead exhibit a more or less wide distribution of sizes. The
observed adsorption isotherm for a typical material is therefore the convolution of an adsorp-
tion process with the distribution of one or more properties which affect that process. This
was first stated mathematically by Ross and Olivier12 for the case of surface energy distribu-
tion and has become known as the integral equation of adsorption.
The Integral Equation of Adsorption
In a general form for a single component adsorptive, the integral equation of adsorption can
be written as
Q ( p ) = ∫ da db dc…q ( p, a, b, c… ) f ( a, b, c… ) (1)
where
Q(p) = the total quantity adsorbed per unit weight at pressure p,

a,b,c,... = a set of distributed properties,
f(a,b,c,...) = the distribution function of the properties, and
q(p,a,b,c,...) = the kernel function describing the adsorption isotherm on unit
surface of material with fixed properties a,b,c,...
Equation (1), a Fredholm integral of the first kind, is a member of a class of problems known
as ill-posed, in that there are an infinite number of functional combinations inside the integral
that will provide solutions. Even when the kernel function is known, experimental error in the
data can make solving for even a single distribution function a difficult task. Solving for mul-
tiple distribution functions requires more data than provided by a single adsorption isotherm.
C-40 Mar 08
Application to Surface Energy Distribution
Under certain conditions, an energetically heterogeneous surface may be characterized by a

distribution of adsorptive energies. The conditions are that the sample is not microporous, i.e.,
that adsorption is taking place on essentially a free surface with no pore filling processes at
least to about 0.2 relative pressure. Secondly, that each energetically distinct patch contributes
independently to the total adsorption isotherm in proportion to the fraction of the total surface
that it represents. This condition is satisfied if the patches are relatively large compared to an
adsorptive molecule, or if the energy gradient along the surface is not steep. In mathematical
terms, this concept is expressed by the integral equation of adsorption in the following form.
Q ( p ) = ∫ dε q ( p, ε ) f ( ε ) (2)
where
Q(p) = the experimental quantity adsorbed per gram at pressure p,

q(p,e) = the quantity adsorbed per unit area at the same pressure, p, on
an ideal free surface of energy e, and
f(e) = the total area of surface of energy e in the sample.
The exact form of the energy-dependent term depends on the form of the model isotherms
expressed in the kernel function and is provided in the model description.
Application to Pore Size Distribution
Similarly, a sample of porous material may be characterized by its distribution of pore sizes.
It is assumed in this case that each pore acts independently. Each pore size present then con-
tributes to the total adsorption isotherm in proportion to the fraction of the total area of the
sample that it represents. Mathematically, this relation is expressed by
Q ( p ) = ∫ dH q ( p, H ) f ( H ) (3)
where
Q(p) = the experimental quantity adsorbed at pressure p,

q(p,H) = the quantity adsorbed per unit area at the same pressure, p, in an
ideal pore of size H, and
f(H) = the total area of pores of size H in the sample.
Numerical values for the kernel functions in the form of model isotherms can be derived from
modern statistical mechanics such as density functional theory or molecular simulations, or
can be calculated from one of various classical theories based on the Kelvin equation. Several
types are found in the models library.
Mar 08 C-41
Performing the Deconvolution
The integrations in equations (2) and (3) are carried out over all surface energies or pore sizes
in the model. The functions q(p,e) and q(p,H), which we call the kernel functions, are con-
tained in numeric form as model isotherms. Because, in general, there is no analytic solution
for equation (1), the problem is best solved in a discrete form; the integral equation for any
distributed property Z becomes a summation:
Q(p) = ∑ q ( p, Z i ) f ( Z i ) (4)
i
Given a set of model isotherms, q(p,Z), from a model chosen from the models library and an
experimental isotherm, Q(p), contained in a sample information file, the software determines
the set of positive values f(Z) that most nearly, in a least squares sense, solves equation (4).
The distributed property, surface energy or pore size, is then displayed on the Report Options
dialog as a selection of tables or graphs.
Regularization
DFT allows a selectable regularization (also referred to as smoothing) constraint to be applied

during the deconvolution process to avoid over-fitting in the case of noisy data or ill-fitting
models. The method used is based on co-minimization of the second derivative of the distri-
bution. The relative weight given to this term is determined by the value of the regularization
parameter, which is set on the DFT Pore Size or Surface Energy dialog and also is shown in
the header of reports. The value of the regularization parameter varies from zero (for no sec-
ond derivative constraint) to ten (indicating a weight equal to minimizing the residuals), or
even larger. When the distribution and residuals obtained change little with the value of the
regularization parameter, it indicates that the chosen model provides a good representation of
the data. Conversely, a large sensitivity to the regularization parameter might indicate inade-
quate data or a poor choice of model to represent the data.
C-42 Mar 08
SPC Report Variables
Regressions Chart Variables
The line of best fit for the Regression Chart is calculated by the usual Least Squares methd.
(Refer to BASIC Scientific Subroutines Vol II, by F.R. Ruckdeschel, Copyright 1981 BYTE
Publications/McGraw Hill, p. 16.) If there is only a single point or all N points have the same
x-value, there can be no line of best fit in the standard form.
Σx
XAve = ---------i
N
Σy
YAve = ---------i
N
Σ ( x i – XAve ) ( y i – YAve )
Slope = --------------------------------------------------------------
Σ ( x i – XAve )
2
The coefficient of Correlation for this line is also calculated in the usual way. (Refer to Math-
ematical Handbook for Scientists and Engineers, by Granino A. Korn and Theresa M. Korn,
Copyright 1961, 1968 McGraw Hill, Sec. 18.4.)
Σ ( x i – XAve )
2
σx = ------------------------------------
N
Σ ( y i – YAve )
2
σy = -----------------------------------
-
N
Σ ( x i – XAve ) ( y i – YAve )
Cov ( x, y ) = --------------------------------------------------------------
N
Correlation Coefficient = Cov ( x, y )

-----------------------
σx σy
Control Chart Variables
Σy
Mean = ---------i
N
Σ ( y – Mean )
2
StdDev = ------------------------------------
N–1
Mar 08 C-43
CoefVar = StdDev
-------------------
Mean
PlusNSig = Mean + n ⋅ StdDev
MinusNSig = Mean – n ⋅ StdDev
C-44 Mar 08
Summary Report
The following calculations and the results of previous calculations (as noted) are used to gen-
erate the summary report:
a. Single-point Surface Area (m2/g)
[ Va × ( 1 – Pr ) ] × CSA × ( 6.023 × 10 )
23
S 1PT = ------------------------------------------------------------------------------------------------
-
22414 cm STP × 10 nm /m
3 18 2 2
where
Pr = pressure closest to 0.3 of the relative pressure points designated for surface area
calculations.
Va = volume corresponding to Pr
b. Multipoint Surface Area
See BET Surface Area Calculations
c. Langmuir Surface Area
See Langmuir Surface Area Calculations
d. t-Plot Micropore Surface Area
See t-Plot calculations
e. t-Plot External Surface Area
f. BJH Cumulative Adsorption
g. BJH Cumulative Desorption
h. Adsorption Total Pore Volume
i. Desorption Total Pore Volume
j. t-Plot Micropore Pore Volume
k. Dubinin-Radushkevich Micropore Surface Area
See Dubinin-Radushkevich calculations
Mar 08 C-45
l. Dubinin-Radushkevich Monolayer Capacity
See Dubinin-Radushkevich calculations
m. Dubinin-Astakhov Micropore Surface Area
See Dubinin-Astakhov calculations
n. Dubinin-Astakhov Micropore Volume
See Dubinin-Astakhov calculations
o. MP-Method Cumulative Surface Area of Pores
MPSTOT = SCUMI, (see MP-method Calculations) for the last collected data point used
in the MP-method Calculations, and the range of hydraulic pore radii over which the
cumulative surface area was computed.
p. MP-Method Cumulative Pore Volume of Pores
MPVTOT = VCUMI, (see MP-method calculations) for the last collected data point used
in the MP-method calculations, and the range of hydraulic pore radii over which the
cumulative pore volume was computed.
q. Average Pore Hydraulic Radius (A)
MPV TOT
× 10 m /cm × 10 Å/m
–6 3 10
MP DAVER = --------------------
MPS TOT
C-46 Mar 08
References
1. Savitzky, A. and Golay, M.J.E., Anal. Chem. 36, 1627 (1964).
2. Brunauer, S.; Emmett, P.H.; and Teller, E., J. Am. Chem. Soc. 60, 309 (1938).
3. Langmuir, I., J. Am. Chem. Soc. 38, 2267 (1916); J. Am. Chem. Soc. 40, 1361 (1918);
Phys. Rev 8, 149 (1916).
4. deBoer, J.H., et al, J. Catalysis 3, 32, 38, 44, 268 (1964); J. Catalysis 4, 319, 643, 649
(1965); Cranston, R. and Inkley, F., Adv. Catalysis 9, 143 (1957).
5. Halsey, G., J. Chem. Phys. 16, 931-937 (1948).
6. Harkins, W.D. and Jura, G., J. Chem. Phys. 11, 431 (1943).
7. Kelvin, J. (published under the name of Sir William Thomson), Phil. Mag. 42, 448-452
(1871).
8. Barrett, E.P.; Joyner, L.S.; and Halenda, P.P., J. Am. Chem. Soc. 73, 373-380 (1951).
9. Horvath, G. and Kawazoe, K., J. Chem. Eng. Japan 16(6), 470 (1983).
10. Saito, A. and Foley, H.C., AlChE Journal 37(3), 429 (1991).
11. Cheng, Linda S. and Yang, Ralph T., Chemical Engineering Science 49(16), 2599-2609
(1994).
12. Ross and Olivier, J.P., “On Physical Adsorption,” J. Wiley and Sons, New York (1964).
13. Dubinin, M., Carbon 21, 359 (1983); Dubinin, M., Progress in Surface and Membrane
Science 9, 1, Academic Press, New York (1975); Dubinin, M. and Astakhov, V., Adv.
Chem. Ser. 102, 69 (1971); Lamond, T. and Marsh, H., Carbon 1, 281, 293 (1964); Medek,
J., Fuel 56, 131 (1977); Polanyi, M., Trans. Faraday Soc. 28, 316 (1932); Radushkevich,
L., Zh. fiz. Kemi. 33, 2202 (1949); Stoeckli, H., et al, Carbon 27, 125 (1989).
14. Mikhail, R., Brunauer, S. and Bodor, E., J. Colloid and Interface Sci. 24, 45 (1968).
Mar 08 C-47
TriStar II 3020 Appendix D
D. FREE-SPACE CORRECTION
Free space is that volume of the sample tube which is unoccupied by the sample. The quantity
of gas dosed into the sample tube is calculated from the difference in pressures in the manifold
before and after the dose is delivered. The quantity of gas adsorbed by the sample is calculated
by subtracting the quantity of gas remaining in the free space of the sample tube after equilib-
rium is established from the quantity of gas originally dosed into the sample tube. Free space
must be determined accurately to obtain a precise value for quantity adsorbed.
Static-volumetric systems such as the TriStar consist basically of a gas manifold joined to a
sample tube by an isolation valve. The manifold section has connections for an absolute pres-
sure transducer, a temperature gauge, and a vacuum system. It also has inlets for the adsorptive
gas and helium. A Dewar flask containing a cryogenic liquid (usually LN2 at approximately 77
K) is situated so that it can be raised to immerse most of the sample tube. Two temperature
zones exist within the sample tube when immersed in the cryogenic bath: a warm zone (the
volume above the liquid level and near ambient temperature) and a cold zone (the volume
below the liquid level at cryogenic temperature). Not only must the total free-space volume be
determined, but it also is necessary to determine the quantity of gas residing within the “cold”
zone since a nonideality correction must be applied to only that quantity of gas.
The total quantity of gas in the partly immersed sample holder cannot simply be determined
using n = PV/RT because temperature is not constant over the total volume, but instead is dis-
tributed as two temperature zones with a steep temperature gradient between them. A
convenient method for resolving this problem is to derive two factors which, for the existing
temperature profile, can be multiplied by the prevailing pressure to reveal the molar volume of
gas contained in the cold zone and the total quantity residing in the free volume of the
immersed sample holder (the cold free space).
The TriStar system provides the following methods for free-space determination:
• Measure
• Calculate
• Enter
Mar 08 D-1
Appendix D TriStar II 3020
Measure
Generally, this method, although requiring a little more time (approximately 10 minutes) is the
most preferred one for determining free space. It is simple, automatic, requires very little
information, and essentially is error-proof. With this method, the instrument first evacuates
the manifold and sample tube (containing sample), then isolates the sample tube by closing the
valve. Then the manifold is charged with helium, the pressure measured, and the valve opened
allowing the helium to expand into the sample tube at ambient temperature. Again the pressure
is measured.
The Dewar is raised and the sample tube is cooled to cryogenic temperature. Again pressure
drops; when pressure has equilibrated, the value is recorded. Warm and cold free spaces are
calculated from (1) system volume, (2) system, ambient, and bath temperatures, and (3) mea-
sured pressures. From these, the value of the portion of cold free space at cryogenic
temperature which requires correction for nonideality can be determined.
This method may be undesirable if:
• Helium is unavailable; free-space determination by the TriStar requires the use of

helium
• Analysis speed is a major factor; a helium free-space measurement of 10 to 15 minutes

is required
• Your sample tends to absorb and retain helium for a prolonged period of time or if it
adsorbs helium
Calculate
This method is the most rapid and efficient way of compensating for free space. You must
ensure the following is accomplished:
• Perform a blank analysis on the sample tube

• Load the blank analysis file data into the sample tube file
• Indicate whether a filler rod is being used (found on the Sample Tube dialog)
• Enter the analysis bath temperature (foudn on the Po and Temperature dialog)
• Enter the sample mass and density (found on the Sample Information dialog)
D-2 Mar 08
TriStar II 3020 Appendix D
Enter
This method allows you to enter predetermined values for the warm and cold free spaces. The
values to enter may be obtained in one of two ways:
• A pre-analysis free-space calibration of the sample tube containing sample
• The total free space of an empty sample tube is measured and the displacement of the
sample calculated from its mass and density and subtracted from the total free space
In either procedure, ensure that the level (or, in cases where the Isothermal Jacket is used, the
effective level) of the cryogen bath on the sample tube is the same when the analysis is per-
formed as it was when gathering data for free-space calculations.
Mar 08 D-3
TriStar II 3020 Appendix E
E. ETHERNET CONFIGURATION
Your computer and analyzer communicate by means of an ethernet connection. This

appendix contains instructions for ensuring that the ethernet connection operates properly.
The sample screens shown in this appendix are Microsoft operating system
screens, which may be subject to change. The screens are included for reference
purposes only.
Configuring the Ethernet Port
This section contains instructions for configuring an ethernet port in either Microsoft®
Windows XP Professional or Windows Vista. The instructions do not apply to any other
operating system.
Depending on your desktop settings, you may have to access the dialogs in this
procedure in a different manner. Refer to your Windows help system if you need
assistance.
Windows XP Professional
1. Select Start > Settings > Network Connections from the Status bar at the bottom of
the screen; the Network Connections dialog is displayed.
Apr 08 E-1
Appendix E TriStar II 3020
2. Double-click the appropriate Local Area Connection, which is actually the ethernet
port; the Local Area Connection Status dialog is displayed.
If no Local area connections are displayed, Windows did not detect an ethernet
port. Contact your system administrator.
3. Click Properties; the Local Area Connection Properties dialog is displayed.
4. Scroll to Internet Protocol (TCP/IP) and make sure a check mark appears in the box
to the left of the item. If it does not, click on the box to insert a check mark.
Make sure Internet

Protocol (TCP/IP)
is checked
E-2 Apr 08
5. Select Internet Protocol (TCP/IP) to highlight it, then click Properties; the Internet
Protocol dialog is displayed.
6. Click Use the following IP address, then enter the following in the IP address fields:
192 168 77 100.
After entering 77 in this field,

use the right arrow key on
your keyboard to advance to
the next field.
7. The following numbers should display in the Subnet mask field: 255.255.255.0. If
these numbers are not displayed, enter them.
8. Leave all other fields in the dialog blank.
9. Click OK to return to the Local Area Connection Properties dialog, then OK on this
dialog to return to the Local Area Connection Status dialog.
10. Click Close to close the Local Area Connection Status dialog.
Apr 08 E-3
Windows Vista
assistance.
1. Select the Windows icon from the Status bar at the bottom of the screen, then select
Control Panel.
2. Double-click on Network and Sharing Center; a dialog similar to this one is

displayed.
Click here
3. Click Manage network connection from the Tasks list on the left side of the window,
then click Local Area Connection for your analyzer on the dialog that displays. You
should see a dialog similar to this one.
E-4 Apr 08
4. Click Properties; the Local Area Connection Properties dialog is displayed.
5. Highlight Internet Protocol Version 4, then click Properties; the Internet Protocol
Version 4 Properties dialog is displayed.
6. Click Use the following IP address, then enter the following in the IP address field:
192 168 77 100. Use the right arrow key to advance to the fourth field.
After entering 77 in this field,

use the right arrow key on
your keyboard to advance to
the next field.
7. The following numbers should display in the Subnet mask field: 255.255.255.0. If
these numbers are not displayed, enter them.
8. Leave all other fields in the dialog blank.
Apr 08 E-5
9. Click OK to close the Internet Protocol Version 4 dialog.
10. Then click OK or the X in the upper right-hand corner of the remaining dialogs and
windows to close them.
E-6 Apr 08
Configuring the Firewall Setting

An ethernet firewall typically is enabled by default for the Windows XP and Windows
Vista operating systems. Windows operating systems prior to these versions did not have
firewalls. To prevent an initialization failure when running the Micromeritics software,
you must turn off the firewall option between your computer and the analyzer. You must
also do this for any third-party firewalls you may have installed (refer to the firewall
software manual or contact your system administrator for instructions).
assistance.
Windows XP Professional
Perform the following steps to disable the ethernet firewall for the instrument connection:
1. Select Start > Settings > Control Panel from the Status bar at the bottom of the
screen; the Control Panel window is displayed.
2. Double-click the Windows Firewall icon; the Windows Firewall dialog is displayed.
3. Click the Advanced tab; a list of network connections is displayed.
4. Click the check box next to the connection assigned to your analyzer to clear the
check mark, then click OK.
Apr 08 E-7
Windows Vista
1. Select the Windows icon from the Status bar at the bottom of the screen, then select
Control Panel.
2. Double-click on Network and Sharing Center.
Click here
3. Double-click Windows Firewall; the Windows Firewall dialog is displayed.
Highlighted green when

on and red when off.
Note that the Windows Firewall statement is highlighted with green, indicating the
Firewall is turned on.
E-8 Apr 08
4. Click Change Settings; a dialog requesting permission to continue is displayed. Click

Continue; the Windows Firewall Settings dialog is displayed.
5. Click the Advanced tab, then OK; a list of network connections is displayed.
6. Click the check box next to the connection assigned to your analyzer to clear the
check mark, then click Apply. Click OK to close the dialog.
7. Click the X in the upper right-hand corner of the remaining associated windows to
close them.
Apr 08 E-9
TriStar II 3020 Appendix F
F. DFT MODELS
Theories are developed by scientists in an attempt to explain a class of observed behavior. In

the experimental physical sciences, theories are often expressed in terms of a model that can
be visualized and described mathematically. Early models of physical adsorption were quite
simple, both conceptually and mathematically, for very practical reasons — hand computa-
tions were required. Today we can explore complex models that describe adsorption systems
on the atomic scale of size and sub-picosecond time frame. This is not because scientists are
smarter, but because of available tools. The DFT models are created by classical approaches
to adsorption as well as models based on modern statistical thermodynamics.
Models Based on Statistical Thermodynamics

Included in this group are methods that model the adsorption system in terms of forces acting
between individual molecules.
Theoretical Background
Traditional adsorption theories attempt to describe experimental adsorption isotherms with an

isotherm equation containing a small number of parameters. At a minimum, these parameters
include the extent of the surface, such as the monolayer capacity (Vm), and the molar inten-
sity of the gas-surface interaction, such as the Langmuir “K” constant or the BET “C”
constant. In some equations, additional parameters take into account the lateral interaction of
adsorbed molecules with each other. Other theories, such as the Dubinin-Astakhov approach,
also include parameters for the effect of adsorbent porosity.
Instead of this classical kinetic or phenomenological approach, we can use a molecular-based

statistical thermodynamic theory that allows us to relate the adsorption isotherm to the micro-
scopic properties of the system: the fluid-fluid and fluid-solid interaction energy parameters,
the pore size, the pore geometry, and the temperature.
The following example is given so that you may understand how such a theory is constructed.
A clean sample of a solid material containing slit-shaped pores of a single width is placed in
an evacuated space. It is kept at a fixed temperature as a known quantity of pure argon gas is
admitted into the space surrounding the sample. The pressure within the space is recorded
over time. In this situation, the pressure falls rapidly from its initial value and gradually
approaches a steady reading, called the equilibrium pressure. The amount adsorbed corre-
sponds to the quantity of gas effectively removed from the gas phase by the solid surface. A
graph that plots amount adsorbed versus equilibrium pressure is called an adsorption
isotherm.
Under such conditions, the argon atoms that randomly enter the pore space feel the presence
of the solid surface as the action of an external attractive force (the dispersion forces or Van
der Waal’s forces) and spend more time near the surface. As a result, the space near the sur-
face acquires a greater average density of argon atoms than regions farther removed.
Mar 09 F-1
Appendix F TriStar II 3020
If the equilibrium distribution of the gas atoms near the surface could be described as a func-
tion of pressure and the molecular properties of the components of the system, then a model
could be constructed for the adsorption isotherm for the system. Modern physical chemistry
provides several ways to calculate this distribution. All these methods are based on the fun-
damental thermodynamic law that such a system adopts a configuration of minimum free
energy at equilibrium. Also needed is a description of the pairwise interaction energy between
atoms, U(s), commonly given by a Lennard-Jones potential:
σ 12 σ 6
U ( s ) = ⎛ ---⎞ – ⎛ ---⎞
⎝ s⎠ ⎝ s⎠
where
ε = a characteristic energy of the adsorptive,

σ = the diameter of the adsorptive molecule, and
s = the separation distance.
Molecular Simulation Methods
Two simulation techniques are commonly used to determine the distribution of gas molecules
in a system in equilibrium: the molecular dynamics method and the Monte Carlo method.
Both of these are used as reference methods because their results are considered exact.
Molecular Dynamics Method
In the molecular dynamics method, the position and velocity of individual gas particles are
calculated over time at very short intervals. This method takes into account both the forces
acting between the gas particles themselves and those acting between the gas particles and the
atoms of the simulated surface. As the simulated particles collide with each other and with the
surface, the average concentration of particles in the space near the surface is calculated; this
calculation yields the amount of gas adsorbed.
This method can be thought of as a way to determine the chronological record of the move-
ment of each particle in the system using time steps of 10-14 seconds. Although the
mathematics are simple, the number of calculations required for a system of even a few hun-
dred particles is astronomical and challenges even the fastest computers.
Monte Carlo Method
In the Monte Carlo method, determination of the system equilibrium distribution begins with
an assumption (which may be only approximate) about the initial configuration of particles in
the system. The system is “equilibrated” through a process of randomly selecting one particle
and conditionally moving it a random distance in a random direction.
If the move results in a configuration of lower total energy, then the move is completed and
another particle is randomly selected to be moved.
F-2 Mar 09
If the move results in a configuration of higher energy, a probability for that event is calcu-
lated, and a random number between zero and one is generated. If the generated number is
smaller than the probability of the event, then the move is accepted; otherwise, another par-
ticle is selected and the process is repeated. This process continues until the average total
energy of the system no longer decreases; at this point, average configuration data are accu-
mulated to yield the mean density distribution of particles in the system.
Monte Carlo simulations require considerable less computation time than molecular dynamic
simulations and can yield the same results; however, neither method provides a really prac-
tical way to calculate complete isotherms.
Density Functional Formulation
Density functional theory offers a practical alternative to both molecular dynamic and Monte
Carlo simulations. When compared to reference methods based on molecular simulation, this
theory provides an accurate method of describing inhomogeneous systems yet requires fewer
calculations. Because the density functional theory provides accuracy and a reduced number
of calculations, it is the basis embodied in the DFT models.
The system being modeled consists of a single pore represented by two parallel walls sepa-
rated by a distance H. The pore is open and immersed in a single component fluid
(adsorptive) at a fixed temperature and pressure. Under such conditions, the fluid responds to
the walls and reaches an equilibrium distribution. In this condition (by the definition of equi-
librium), the chemical potential at every point equals the chemical potential of the bulk fluid.
The bulk fluid is a homogenous system of constant density; its chemical potential* is deter-
mined by the pressure of the system using well-known equations. The fluid near the walls is
not of constant density; its chemical potential is composed of several position-dependent con-
tributions that must total at every point to the same value as the chemical potential of the bulk
fluid.
As noted previously, at equilibrium, the whole system has a minimum (Helmholtz) free
energy, known thermodynamically as the grand potential energy (GPE). Density functional
theory describes the thermodynamic grand potential as a functional of the single-particle den-
sity distribution; therefore, calculating the density profile that minimizes the GPE yields the
equilibrium density profile. The calculation method requires the solution of a system of com-
plex integral equations that are implicit functions of the density vector. Since analytic
solutions are not possible, the problem must be solved using iterative numerical methods.
Although calculation using these methods still requires supercomputing speed, the calculation
of many isotherm pressure points for a wide range of pore sizes is a feasible task. The com-
plete details of the theory and the mathematics can be found in the papers listed under
References at the end of this appendix.
The following graphs and accompanying text illustrate the results of using density functional
theory to predict the behavior of a model system.
*Chemical potential may be thought of as the energy change felt by a probe particle when it is inserted
into the system from a reference point outside the system. It can also be defined as the partial derivative
of the grand potential energy with respect to density (or concentration).
Mar 09 F-3
Figure F-1 shows the density profile for argon at a carbon surface as calculated by density
functional theory for a temperature of 87.3 K and a relative pressure of about 0.5.
Figure F-1. Density Profile for Argon on Carbon at 87.3 K and a Relative Pressure of 0.5
This figure represents a cross-section of the region near the surface. Note the layerwise dis-
tribution of adsorbate; the first monolayer is sharply defined and a third layer can be
distinguished. The area under the profile curve represents the amount adsorbed per unit area
at this pressure. The positions of the maxima are separated by a distance determined by the
size of the adsorptive atom.
Given the density profile, the amount adsorbed at the stated pressure can be easily calculated
as the integral over the profile. Repeating this calculation over a range of pressures yields the
adsorption isotherm for the model. If the value of H is very large, the isotherm obtained cor-
responds to that of an external, or free, surface. If H is smaller, a range of pressures is reached
where two minima exist for the grand potential, showing the presence of two metastable
phases having different density distributions but the same chemical potential. The phase with
the lower GPE is the stable one. As the pressure is increased, a point is reached where the
other phase becomes the stable one. This phase transition reflects condensation of adsorbate
in the pore; the pressure at which it occurs is called the critical pore-filling pressure. This
pressure is analogous to the condensation pressure predicted by the Kelvin equation in the
classical model of pore filling.
Figure F-2 shows how the profiles change with pressure for a model pore with H = 40 Ang-
stroms. The insets show the density profiles for the corresponding points of the isotherm.
F-4 Mar 09
Figure F-2. Model Isotherm for Argon at 87.3 K in a 40 Å Slit in a Carbon Substrate
The profiles show the density distribution from one wall to the center of the slit; the other half
of the distribution is a mirror image of the profile shown.
As the pressure is first increased from zero, almost all the adsorbed atoms occupy a position
close to the surface.
• Inset a shows the profile corresponding to point a on the isotherm where the surface is
about half covered.
• At point b, the first layer is so full that it is more favorable for atoms to start a new
layer.
• At point c, a third layer is forming. Point c, for this size slit, is the critical pore-filling
pressure. In inset c, the profile shows the density decreasing to near zero (actually the
bulk gas density) at 4 or 5 molecular diameters from the surface.
• Inset d shows the profile converging on a density similar to that of bulk liquid argon in
the center of the pore, indicating a phase transition.
Note that the adsorption isotherms for pores larger than the one shown in Figure F-2 is iden-
tical up to point c. The lower branch of the isotherm simply continues to a higher pressure for
larger pores. This trend is illustrated in Figure F-3, where isotherms for some larger size pores
are shown. It is clear that pore size is uniquely characterized by a corresponding critical pore-
filling pressure. At large pore sizes, density functional theory produces results for the critical
filling pressures that are in good agreement with those produced by the Kelvin equation.
Mar 09 F-5
Figure F-3. Model Isotherms for Some Larger Pore Widths Argon on Carbon at 87.3 K
Figure F-4 shows model isotherms for pores in the micropore size range. Note the logarithmic
scale for pressure.
Figure F-4. Model Isotherms in the Micropore Size Range of Pore Width
Argon on Carbon at 87.3 K
F-6 Mar 09
Pores of 4 Å width, barely larger than the argon atom (3.38 Å), fill at pressures below 1 mil-
litorr. Pores below 15 Å fill before a monolayer is completed on the surface of the larger
pores. In the micropore size range, the pore volume fills more gradually with pressure and the
total shape of the isotherm is important in characterizing the pore size.
Models Included
Non-Local Density Functional Theory with Density Independent Weights
N2 - DFT Model
AR - DFT Model
Geometry: Slit
Substrate: Carbon (graphite)
Category: Porosity
Method: Nitrogen at 77 K; Argon at 87 K
Using the methods of non-local density functional theory, two sets of isotherms have been
calculated to serve as kernel functions for the characterization of porous solids from adsorp-
tion data. The model isotherms are stored in binary format files. These models assume a slit-
like pore geometry. The pore size range from 4.0 to 4000 Å is covered in 91 classes in a geo-
metric progression. The class intervals are rounded to the nearest 0.02 molecular diameters. A
model for the free or external surface is included to account for unfilled pores. Each of the 92
model isotherms has been calculated at 181 pressure points from near 1x10-6 to near 1.00 rel-
ative pressure.
These models are identical to those supplied with the original DOS version of DFT software.
Some slight difference from the DOS results may be noted when they are applied to the same
data due to improvements in the deconvolution algorithm and better regularization of the cur-
rent software.
Modified Non-Local Density Functional Theory with Density-Dependent

Weights
N2 - Modified Density Functional
Geometry: Free surface

Substrate: Surface energy
Method: Nitrogen at 77K
Using the modified Tarazona prescription described by Olivier (refer to References, refer-
ences 3 and 4), model isotherms were calculated for a wide range of adsorptive energies to a
relative pressure of 0.6. The model makes no provision for pore filling in the micropore
region. If the sample solid contains small mesopores, the isotherm data should be truncated
(using the Select Data Points dialog box) to a suitably low relative pressure to avoid trying to
fit this region; mesopore filling reports as a large area of low energy in the calculated distri-
bution of adsorptive potential.
Mar 09 F-7
The surface energy is reported in terms of the effective Lennard-Jones interaction parameter,
e, for the adsorptive/adsorbent pair divided by Boltzmann’s constant. The units are therefore
degrees Kelvin.
N2 - Cylindrical Pores - Oxide Surface

AR - Cylindrical Pores - Oxide Surface
Geometry: Cylinder
Substrate: Oxide
Category: Porosity
Method: Nitrogen at 77 K; Argon at 87 K
Model isotherms were calculated using a combination of statistical mechanical calculations

and experimental observations for macroporous silicas and MCM-41 mesoporous silicas as
well as zeolites. The pore-filling pressures were determined as a function of the pore size
from adsorption isotherms on MCM-41 materials characterized by X-ray and other tech-
niques. The variation of the pore fluid density with pressure and pore size has been accounted
for by density functional theory calculations. The N2 model reports pore sizes ranging from
3.8 to 387 Angstroms and the AR model from 3.8 to over 500 Angstroms.
Reference: M. Jaroniec, M. Kruk, J.P. Olivier, and S. Koch, “A New Method for the
Accurate Pore Size Analysis of MCM-41 and Other Silica-Based Mesoporous
Materials,” Proceedings of COPS-V, Heidelberg, Germany (1999)
N2 – Cylindrical Pores – Pillared Clay Surface (Montmorillionite)
Geometry: Cylinder
Substrate: Crystalline Silicate
Category: Porosity
Method: Nitrogen at 77 K
Model isotherms were calculated using a combination of statistical thermodynamic Non-

Local Density Functional Theory (NLDFT) calculations and experimental isotherms for ref-
erence samples of montmorillionite.The construction method for the hybrid models was
analogous to that described in the first reference below (Jaroniec et al,1999). The additional
references add additional theoretical details as well as examples of the application of the
model to pillared clay catalysts.This model reports pore widths from 3.8 to 387 Angstroms.
F-8 Mar 09
References: Mietec Jaroniec, Michal Kruk, James P. Olivier and Stefan Koch, “A New
Method for the Characterization of Mesoporous Silicas,” Proceedings of
COPS-V, 1999, Studies in Surface Science, Vol 128, Characterization of
porous Solids V , Unger, et al, Eds, Elsevier, Amsterdam, 2000.
James P. Olivier and Mario L. Occell, “Surface Area and Microporosity of a

Pillared Interlayered Clay (PILC) from a Hybrid Density Functional Theory
(DFT) Method,” The Journal of Physical Chemistry B; 2001, 105(3),
623-629.
M. L. Occelli, J. P. Olivier, J. A. Perdigon-Melon, and A. Auroux, “Surface

Area, Pore Volume Distribution, and Acidity in Mesoporous Expanded Clay
Catalysts from Hybrid Density Functional Theory (DFT) and Adsorption
Microcalorimetry Methods,” Langmuir 2002, 18, 9816-9823.9b
James P. Olivier, “The Importance of Surface Heterogeneity in Developing

Characterization Methods.” 6th International Symposium on the Character-
ization of Porous Solids, Studies in Surface Science and Catalysis 144,
Elsevier, 2002.
James P. Olivier and Mario L. Occelli, “Surface Area and Microporosity of

Pillared Rectorite Catalysts from a Hybrid Density Functional Theory
Method,” Microporous and Mesoporous Materials 2003, 57, 291-296.
C02 - DFT Model
Geometry: Slit
Substrate: Carbon
Category: Porosity
Method: Carbon dioxide at 273 K
Model isotherms were calculated, using the non-local prescription of Tarazona, employing
molecular parameters derived from the known bulk properties of carbon dioxide.
AR - Modified Density Functional Model
Geometry: Free Surface

Substrate: Any
Category: Surface energy
Method: Argon at 87 K
This model was produced in the same manner as the N2 Modified Density Functional model
listed earlier, except applicable to argon adsorbed at 87.3 K.
Mar 09 F-9
N2 - Tarazona NLDFT, Esf = 30.0K
Geometry: Cylinder
Substrate: Oxide
Category: Porosity
Model isotherms were calculated using the prescriptions of Tarazona for density dependent
weighting functions and a cylindrical pore geometry. The wall potential used is /k = 30 K,
typical for a silica or alumina surface.
This model file is particularly useful for sizing zeolites or zeolite containing materials that
have substantial micropore volume. The reported pore size range is 3.8 to 387 Angstroms.
Reference: P. Tarazona, Phys. Rev. A 31: 2672 (1985).

Idem, Phys. Rev. A 32: 3148 (1985).
P. Tarazona, U. M. B. Marconi, and R. Evans, Mol. Phys. 60: 573 (1987).
F-10 Mar 09
Models Based on Classical Theories

Both surface energy distribution and pore size distribution may be evaluated using classical
approaches to model kernel functions for use with equation (1) of the DFT Theory in the cal-
culations appendix. Be aware that the deconvolution method only provides a fitting
mechanism; it does not overcome any inherent shortcomings in the underlying theory.
Surface Energy
The use of classical theories to extract adsorptive potential distribution is mostly of historical
interest. At a minimum, the equation must contain a parameter dependent on adsorption
energy and another dependent on monolayer capacity, or surface area. This is sufficient to
permit the calculation of the set of model isotherms that is used to create a library model. The
Langmuir equation has been used in the past, as have the Hill-deBoer equation and the
Fowler-Guggenheim equation. All of these suffer from the fact that they only describe mono-
layer adsorption, whereas the data may include contributions from multilayer formation.
Pore Size
It is well established that the pore space of a mesoporous solid fills with condensed adsorbate
at pressures somewhat below the prevailing saturated vapor pressure of the adsorptive. When
combined with a correlating function that relates pore size with a critical condensation pres-
sure, this knowledge can be used to characterize the mesopore size distribution of the
adsorbent. The correlating function most commonly used is the Kelvin equation. Refinements
make allowance for the reduction of the physical pore size by the thickness of the adsorbed
film existing at the critical condensation pressure. Still further refinements adjust the film
thickness for the curvature of the pore wall.
The commonly used practical methods of extracting mesopore distribution from isotherm
data using Kelvin-based theories, such as the BJH method, were for the most part developed
decades ago and were designed for hand computation using relatively few experimental
points. In general, these methods visualize the incremental decomposition of an experimental
isotherm, starting at the highest relative pressure or pore size. At each step, the quantity of
adsorptive involved is divided between pore emptying and film thinning processes and
exactly is accounted for. This computational algorithm frequently leads to inconsistencies
when carried to small mesopore sizes. If the thickness curve used is too steep, it finally will
predict a larger increment of adsorptive for a given pressure increment than is actually
observed; since a negative pore volume is non-physical, the algorithm must stop. Conversely,
if the thickness curve used underestimates film thinning, accumulated error results in the cal-
culation of an overly large volume of (possibly nonexistent) small pores.
The use of equation (1) represents an improvement over the traditional algorithm. Kernel
functions corresponding to various classical Kelvin-based methods have been calculated for
differing geometries and included in the list of models.
Mar 09 F-11
Models Included
Kelvin Equation with Halsey Thickness Curve
N2 - Halsey Thickness Curve
Geometry: Slit
Substrate: Average
Category: Porosity
The kernel function is calculated using the Halsey equation with standard parameters:
– 5.00 1/3
t = 3.54 ⎛⎝ ----------------------⎞⎠
ln ( P/Po )
The nitrogen properties used in the Kelvin equation are:
Surface tension = 8.88 dynes cm-1

Molar density = 0.02887 g cm-3
N2 - Halsey Thickness Curve
Geometry: Cylinder
Substrate: Average
Category: Porosity
The calculation is the same as above except that cylindrical geometry is assumed.
Reference: G. Halsey, J. Chem. Phys 16, 931 (1948)
Kelvin Equation with Harkins and Jura Thickness Curve
N2 - Harkins and Jura Thickness Curve
Geometry: Slit
Substrate: Average
Category: Porosity
The kernel function is calculated using the Harkins and Jura equation with standard
parameters:
F-12 Mar 09
1/2
t = ⎛ ---------------------------------------------⎞
13.99
⎝ 0.034 – log ( P/Po )⎠

N2 - Harkins and Jura Thickness Curve
Geometry: Cylinder
Substrate: Average
Category: Porosity
The calculation is the same as above except that cylindrical geometry is assumed.
References: W. D. Harkins and G. Jura, J.A.C.S. 66, 1366 (1944)
J. H. DeBoer et al., J. Colloid and Interface Sci. 21, 405 (1966)
Kelvin Equation with Broekhoff-de Boer Thickness Curve
N2 - Broekhoff-de Boer Model
Geometry: Slit
Substrate: Average
Category: Porosity
The kernel function is calculated using the Broekhoff-de Boer equation with standard
parameters:

N2 - Broekhoff-de Boer Model
Geometry: Cylinder
Substrate: Average
Category: Porosity
Mar 09 F-13
The calculation is similar to the above except that cylindrical geometry is assumed, and the
film thickness depends on pore size (see reference).
Reference: Specifically, equations 20 and 21 in: J.C.P. Broekhoff and J.H. de Boer, “The
Surface Area in Intermediate Pores,” Proceedings of the International Sym-
posium on Surface Area Determination, D.H. Everett, R.H. Ottwill, eds., U.K.
(1969)
F-14 Mar 09
References
The papers listed below provide additional information on DFT models:
1. “Determination of Pore Size Distribution from Density Functional Theoretic Models of

Adsorption and Condensation within Porous Solids,” J.P. Olivier and W.B. Conklin,
Micromeritics Instrument Corp; presented at the International Symposium on the Effects
of Surface Heterogeneity in Adsorption and Catalysts on Solids, Kazimierz Dolny, Poland
(July 1992).
2. “Classification of Adsorption Behavior: Simple Fluids in Pores of Slit-shaped

Geometry,” Perla B. Balbuena and Keith E. Gubbins, Fluid Phase Equilibria, 76, 21-35,
Elsevier Science Publishers, B.V., Amsterdam (1992).
3. “Modeling Physical Adsorption on Porous and Nonporous solids Using Density

Functional Theory,” J.P. Olivier, Journal of Porous Materials, 3, 9-17 (1995).
4. “The Determination of Surface Energetic Heterogeneity Using Model Isotherms

Calculated by Density Functional Theory,” J.P. Olivier; presented at the Fifth
International Conference on the Fundamentals of Adsorption, Pacific Grove, CA (1995).
Mar 09 F-15
TriStar II 3020 Appendix G
G. MAINTAINING HIGH PURITY GASES
The TriStar was designed to measure accurately the surface area of all types of materials. It is
important that the gases (nitrogen or helium) used for these measurements be of highest purity,
especially when analyzing low surface area samples. Three ways to ensure high purity gases
are to always maintain:
• thoroughly purged gas pressure regulators

• non-permeable gas lines
• leak-free connections
Impure gas is strongly indicated, for example, if a series of measurements on a low surface
area material yields decreasing specific surface areas with decreasing quantities of sample.
The TriStar uses very small amounts of helium; therefore any residual air in the regulator can
distort results of subsequent analyses for quite some time.
Micromeritics offers the following suggestions to assist you in maintaining high purity gases
(particularly helium) for the TriStar.
• Use metal gas lines only

• Remove trapped air from the regulator and gas lines
Using Metal Gas Lines

You should always use metal gas lines which have been carefully cleaned of any oils and
greases used in the manufacturing process. Do not use plastic or rubber gas lines. When these
types of permeable, nonmetallic gas lines are used with helium, contaminants accumulate at a
much faster rate. This causes errors in analysis results and can also contaminate a clean sam-
ple.
Removing Trapped Air
When connecting the regulator to the gas bottle, air is unavoidably trapped on the high- and
low-pressure sides of the regulator, as well as in the gas lines. You should remove as much of
this air as is possible before opening the gas bottle valve. If this air is allowed to remain in the
regulator, it will mix with the helium and cause inaccurate results in subsequent analyses. Or if
the valve is open for any length of time, the air trapped on the high pressure side may diffuse
back into the gas bottle and contaminate its entire contents.
There are two methods for removing trapped air from the regulator lines: the Purge Method
and the Evacuation Method.
Mar 08 G-1
Appendix G TriStar II 3020
Purge Method
This is the preferred method for removing trapped air.
1. Select Unit > Enable manual control (if the instrument schematic is not displayed, select Show
instrument schematic).
If you have multiple TriStars installed, make sure you choose the correct Unit menu.
2. Close all valves.
3. Open the regulator Shut-off valve.

4. Open the gas bottle valve briefly and allow the regulator to be charged with gas until the high-
pressure gauge reads just over half the tank pressure; then quickly close the valve.
High-Pressure gauge
Regulator
Shut-off valve
Gas Bottle valve
Pressure Control knob
5. Using the Pressure Control knob, set the output pressure (gas bottle pressure gauge) to 15
psig.
6. Loosen the fitting at the helium inlet (on the rear panel of the TriStar) until the low
pressure side drops to approximately 3 psig (0.02 MPa), then tighten the fitting.
G-2 Mar 08
TriStar II 3020 Appendix G
7. Repeat steps 4, 5, and 6 three times.
8. Briefly open the gas bottle valve; then, using the Pressure Control knob, reset the regulator
output pressure to 15 psig.
9. After the pressure has stabilized (indicating there are no leaks), open the gas bottle valve.
Evacuation Method
To use this method, your gas tank must be within 10 feet of the instrument.
1. Do one of the following:
If... Then...
The regulator has not Close the gas bottle valve.
been filled with gas and Open the regulator Shut-off valve.
the gas line is attached to
the instrument:
The regulator is filled Close the gas bottle valve.
with gas: Open the regulator Shut-off valve.
Loosen the helium inlet fitting (or nut) on the rear panel of
the instrument.
Allow all of the gas in the regulator to expel from the line
(pressure reading will be zero).
Retighten the helium inlet fitting (or nut).
2. Select Unit > Enable manual control (if the instrument schematic is not displayed, select Show
instrument schematic).
If you have multiple TriStars installed, make sure you choose the correct Unit menu.
Mar 08 G-3
Appendix G TriStar II 3020
3. Close all valves; then open valves 6, 7, and 10.
Open valves 6,
7, and 10
4. Allow evacuation to continue for 20 minutes. This pulls a vacuum on the helium line to
the gas bottle. The manifold pressure transducer should fall close to zero.
Be sure to allow evacuation for a full 20 minutes. If evacuation time is too short,
trapped air may remain in the lines.
5. Close valves 6, 7, and 10.
G-4 Mar 08
TriStar II 3020l Index
INDEX
$ symbol, 8-11 moving from one computer to another, 4-11

physical dimensions, 1-9
removing from computer, 4-16
A schematic, 6-14
Absolute pressure dosing, 5-22, 5-28 turning on/off, 2-5
Absolute pressure tolerance, 5-20 weight and dimensions, 1-9
Accessories, ordering, 10-1 Analyzing file status, 2-12
Add log entry, 8-9 AR Cylindrical Pores - Oxide Surface model, F-8
Add Log Entry push button, 5-7 AR DFT model, F-7
Adding an analyzer, 4-9 AR Modified Density Functional Model, F-9
Adsorbate property factor, 5-59 Astakhov report, 5-75
Adsorption isotherm, F-1 Autoscale, 5-63
Adsorptive properties file, 5-28 Autoscale x- and y-axis, 5-43
creating, 3-10 Avogadro's number, C-22
listing statistics, 3-33 Axis
printing contents, 3-31, 5-94 coordinates, viewing, 7-28
Adsorptive push button properties, editing, 7-27
BJH report, 5-58 Axis Properties dialog, 7-27
Dubinin report, 5-76
Advanced format, 5-5, 8-2
sample defaults, 8-6 B
sample information file, 3-14, 8-3 Backfill
All file status, 2-12 gas, 5-27
Alpha-S curve, 5-92 options, 5-27
Alpha-S report, 5-52 Basic format, 8-4
Alumina, replacing in oil vapor traps, 9-11 sample file defaults, 8-10
Analysis sample information file, 3-16, 5-8
Dewar, 3-25 BET surface area report, 5-39
Dewar, checking, 9-4 calculations, C-7
performing, 3-27, 6-3 example of, 7-31
QuickStart method, 3-29, 6-8 BJH Adsorption/Desorption report, 5-57
Analysis conditions file, 5-15 calculations, C-12
creating, 3-9 examples of, 7-34
listing statistics, 3-33 plot options, 5-62
printing contents, 3-31, 5-94 tabular options, 5-60
Analysis Preparation dialog, 5-22 BJH Adsorptive Options dialog, 5-58
Analysis program, 1-5 Blank analysis, 5-11, 6-12
exiting, 5-99 Boltzmann’s constant, F-8
installing upgrade, 4-8 Bookmarks tab, 2-17
installling, 4-1 Broekhoff-de Boer thickness curve, 5-49
uninstalling, 4-20 Browse push button, 2-10
using, 2-6
Analyzer
adding another, 4-9 C
changing ethernet connection, 4-17 Calibrate Pressure Offset dialog, 6-27
cleaning, 9-4 Calibration, 6-27, 9-29
configurations, 6-23 information, 6-23
electrical, 1-9 match transducers, 6-28, 9-30
maintaining, 9-3
Jul 09 Index-1
Index TriStar II 3020
servo valve, 6-28, 9-30 entered, 5-87

zero pressure, 6-27, 9-29 exported, 5-96
Calibration command, 6-27 selecting display options, 8-12
Calibration file Date Range push button, 2-12
loading, 6-30 Defaults
reinstalling, 4-19 for sample information files, 8-6
saving, 6-29 parameter files, 8-6
Cancel push button, 6-7 Restricted sample information file, 8-6
Carbon Black STSA thickness curve, 5-49 Degas Conditions dialog, 5-13
Catalysts, 5-19 Degas conditions file, 5-13
Cautions, defined, 1-3 defining, 3-8
Check box, 2-10 listing statistics, 3-33
Chemical potential, F-3 printing contents, 3-31, 5-94
Cheng/Yang Degassing units, 1-6
calculations, C-25 ordering, 10-1
correction, 5-65 Density conversion factor, 5-29
Pore Geometry, C-24 Density Functional theory, F-3
Cleaning Destination, 5-94
analyzer, 9-4 Dewar
Dewars, 9-4 checking, 9-4
Close All command, 5-93 cleaning, 9-4
Close command, 5-93 installing, 3-25
Close push button, 2-11 precautions, 3-25
Close Reports command, 7-5 DFT models, F-1
CO2 DFT Model, F-9 See Models
Cold free space, 5-11, 5-24 DFT Pore Size Report Options dialog, 5-71
Collected data, 5-87 DFT report
Columns, editing on onscreen reports, 7-24 Pore size, 5-71
Comments window, 8-9 surface energy, 5-74
Complete file status, 2-12 DFT Surface Energy Report Options dialog, 5-74
Components and Connectors, 2-1 Diagnostics
front panel, 2-1 gas line test, 9-24
rear panel, 2-4 leak test, 9-16
sample compartment, 2-2 Diagnostics command, 6-24
side panel, 2-3 Dialog boxes, using, 2-8
Computer requirements, 1-9 Directory
Control Chart command, 7-11 navigating to a different, 2-13
Control Chart dialog, 7-11 parameter files, 8-15
Control Chart Graph Options dialog, 7-12 Dollimore-Heal Adsorption/Desorption report, 5-64
Control Chart report, 7-11 example of, 7-36
defining the Y-axis, 7-12 Dose increment, 5-20, 5-21
recalculating archived results, 7-13 Dose Increment Edit dialog, 5-21
Control Chart Sample Selection dialog, 7-13 Dose Increments dialog, 5-21
Conventions, used in operator’s manual, 1-3 Drop-down list, 2-10
Convert command, 5-98 Dubinin Adsorptive Options dialog, 5-76
Convert StarDriver Sample Files dialog, 5-98 Dubinin report, 5-75
Cross hair, axis, 7-28 calculations, C-30
Cross-references, 2-20 pore volume options, 5-79
Curve Properties dialog, 7-26 tabular options, 5-77
Transformed isotherm plot, 5-78
types available, 5-76
D Dubinin Report Options dialog, 5-79
Data Dubinin Tabular Report Column Options dialog, 5-77
collected, 5-87 Dubinin Transformed Isotherm Plot Options dialog, 5-78
Index-2 Jul 09
Dubinin-Astakhov calculations, C-32 File menu, 5-1

Dubinin-Radushkevich calculations, C-30 Close All command, 5-93
Close command, 5-93
Convert command, 5-98
E Exit command, 5-99
Edit push button, 5-46 Export command, 5-96
Edit Quantities Adsorbed dialog, 7-16 List command, 5-95
Elevator Open command, 5-3
manual control options, 6-16 Print command, 5-94
screw, 9-2 Save All command, 5-93
Enable Manual Control command, 6-14 Save command, 5-91
Entered data, 5-87 File name
Entered file status, 2-12 default extensions, 2-14
Entered Pressures dialog, 5-16 included as part of ID, 8-7
Environment conditions, 1-9 sequence, 8-10
Equation Filler rod, 5-12, 5-33
Broekhoff-de Boer, 5-49 cleaning, 3-18
Carbon Black STSA, 5-49 Find command, 2-21
Halsey, 5-48 Firewall
Harkins and Jura, 5-49 disabling for Windows Vista, E-8
Kruk-Jaroniec-Sayari, 5-48 disabling for Windows XP, E-7
Equation push button, 5-81 Fixed dose, 5-19
Equilibration Format of exported data, 5-97
calculations, C-5 Forms, A-1
interval, 5-27 f-Ratio report, 5-55
push button, 5-26 Free space, D-1
Error messages, B-1 calculated method, 5-24, D-2
2400 series, B-1 calculations, C-3
2500 series, B-12 cold, 5-24
4000 series, B-18 entered method, 5-24, D-3
6000 series, B-34 measured method, D-2
Ethernet warm, 5-24
configuring port for Vista, E-4 Free Space dialog, 5-23
configuring port for XP, E-1 Freundlich report, 5-42
disabling a firewall, E-7 calculations, C-38
switch, connecting, 4-9 Freundlich Report Options dialog, 5-42
Evacuation options, 5-22 Front Panel, 2-1
Exit command, 5-99 Function keys
Exiting the analysis program, 5-99 See Shortcut keys
Export
format, 5-97
Export command, 5-96 G
Export Sample File dialog, 5-96 Gas, 1-8
Export Settings dialog, 6-5 connecting, 9-19
Exporting sample files, 3-34, 5-96 disconnecting depleted bottle, 9-19
guidelines for connecting to analyzer, 9-19
hazardous, 9-19
F line, clean and verify, 9-24
File maintaining high purity, G-1
printing to, 7-4 selecting, 6-23
selecting, 2-11 specifying port location, 9-28
statistics, 3-33 toxic, 9-21
status, 2-12
Jul 09 Index-3
Graph data, exporting, 5-96

copying as metafile, 7-27 report options, 5-37
editing onscreen, 7-25 Isotherm collection
grid lines, 8-13 dose increments, 5-20
legend, editing, 7-27 target pressures, 5-16
Graph Grid Lines command, 8-13 Isotherm report, 5-37
Graph Grid Lines dialog, 8-13 example of, 7-30
Graph overlay, 3-35 Isothermal jacket, 5-12
for multiple graphs, 3-38
for multiple samples, 3-35
Graph Overlay Samples dialog, 5-33 K
Graphic, appearing in report title, 5-32 Kernel function, F-11, F-12
Grid lines, 8-13 Kruk-Jaroniec-Sayari Thickness Equation, 5-48
H L
Halsey thickness curve, 5-48 Langmuir surface area report, 5-39
Harkins and Jura thickness curve, 5-49 calculations, C-9
Heat of Adsorption dialog, 7-15 Leak test, 5-23
Heat of Adsorption report, 7-15 performing, 9-16
Help menu, 2-24 Legend Properties dialog, 7-27
How-To videos, 2-15 Lennard-Jones, F-2, F-8
Horvath-Kawazoe calculations Links, 2-19
Cylinder pore geometry (Saito/Foley), C-23 List command, 5-95
Slit pore geometry (original HK), C-22 List, generating, 5-95
Sphere pore geometry (Cheng/Yang), C-24 Live Graph command, 8-14
Horvath-Kawazoe Physical Properties dialog, 5-66 Local area connection, E-2
Horvath-Kawazoe Plot Options dialog, 5-69 Log entry, 5-7
Horvath-Kawazoe report, 5-65 Log Report settings, 6-22
calculations, C-22 Low surface area sample, analyzing, G-1
plot options, 5-69
tabular options, 5-69
Horvath-Kawazoe Report Options dialog, 5-65 M
How-To videos, 2-15 Maintenance, system, 9-1
Manual control, 6-14
accessing shortcut menu, 6-14
I enabling, 6-14
Increment, maximum volume, 5-19 Maximum BJH diameter (or radius), 5-58
Index, online, 2-20 Maximum volume increment, 5-19
Insert Predefined Pressures dialog, 5-18 MCM-41 materials, F-8
Insert Pressure Range dialog, 5-17 Menu bar, 2-23
Insert Quantity Range dialog, 7-16 Menu structure, 2-23
Installation videos, 2-15 Mesoporous materials, 5-19
Instrument log, 6-2, 6-21 Metafile, copying graphs as, 7-27
Instrument schematic Minimum BJH diameter (or radius), 5-58
manual control, 6-14 Models, F-1
showing, 6-17 AR Cylindrical Pores - Oxide Surface, F-8
Interaction parameter, C-26 AR DFT model, F-7
IP address AR Modified Density Functional, F-9
entering, Windows Vista, E-5 based on classical theories, F-11
entering, Windows XP, E-3 based on statistical thermodynamics, F-1
Isosteric heat of adsorption, 7-15 CO2 DFT Model, F-9
Isotherm, F-1 N2 Broekhoff-de Boer Model, F-13
collecting, 5-15
Index-4 Jul 09
N2 Cylindrical Pores - Oxide Surface, F-8 Options menu, 8-1

N2 Cylindrical Pores - Pillared Clay Surface, F-8 Graph Grid Lines command, 8-13
N2 DFT model, F-7 Live Graph command, 8-14
N2 Halsey Thickness Curve, F-12 Option presentation command, 8-2
N2 Harkins and Jura Thickness Curve, F-12, F-13 Parameter Files Directory command, 8-15
N2 Harkins and Jura Thickness Curve model, F-12 Sample Defaults command, 8-6
N2 Modified Density Functional, F-7 Service Test Mode command, 8-15
N2 Tarazona NLDFT, Esf = 30.0K, F-10 Units command, 8-12
Molecular dynamics, F-2 Options report, 5-85
Molecular simulation methods, F-2 Ordering information, 10-1
Monolayer capacity, 5-42 O-ring, replacing port, 9-6
Monte Carlo, F-2 Outgas test, 5-24
Montmorillionite, F-8 Overlay samples, 5-39
Moving an analyzer to another computer, 4-11 Overlays push button, 5-33
MP-Method report, 5-80
calculations, C-36
plot options, 5-83 P
tabular options, 5-82 Parameter File Directory Selection dialog, 8-15
types available, 5-81 Parameter files, 5-4
MP-Method Tabular Report Column Option dialog, 5-82 default values, 3-1
defining, 3-6
listing statistics, 3-33
N printing contents, 3-31, 5-94
N2 Broekhoff-de Boer model, F-13 specifying location, 8-15
N2 Broekhoff-de Boer Model model, F-13 Parameter Files Directory command, 8-15
N2 Cylindrical Pores - Oxide Surface model, F-8 Parameters, user, 8-8
N2 Cylindrical Pores - Pillared Clay Surface model, F-8 Parts, ordering, 10-1
N2 DFT model, F-7 Pass/Fail Options dialog, 5-36
N2 Halsey Thickness Curve model, F-12 Password, restricted format, 8-5
N2 Harkins and Jura Thickness Curve model, F-13 Po and T dialog, 5-25
N2 Modified Density Functional model, F-7 collected data, 5-89
N2 Tarazona NLDFT, Esf = 30.0K model, F-10 Po and T push button, 5-25
Next push button, 6-7 Po and Temperature Options dialog, 5-25
nk, 5-11 Po tube, on schematic, 6-16
No analysis file status, 2-12 Po value, 6-4
Non-ideality factor, 5-12, 5-29 Pore filling pressure, F-4
Notes, defined, 1-3 Pore Geometry
cylinder (Saito-Foley), C-23
slit (original Horvath-Kawazoe), C-22
O sphere (Cheng/Yang), C-24
Oil vapor trap, replacing alumina, 9-11 Pore size, F-11
Online manual Preparation push button, 5-22
cross references, 2-20 Prepared file status, 2-12
index, 2-20 Preparing file status, 2-12
printing options, 2-22 Presentation options, 8-2
using, 2-17 Pressure
See also Operator’s manual offset, 6-27
Open command, 5-3 relative, calculations, C-2
Open Report command, 7-5 table, 5-16
Operator, specifying, 8-7 target, 5-16
Operator’s manual tolerance, 5-20
conventions, 1-3 Preventive maintenance schedule, 9-3
online, 2-17 Print command, 5-94
Option Presentation command, 8-2 Printing file contents, 3-31
Jul 09 Index-5
Psat vs t push button, 5-29 Isotherm, 5-37, 7-30

Push button, 2-9 Langmuir surface area, 5-39
Browse, 2-10 legend, editing, 7-27
Close, 2-11 onscreen, 7-19
Date Range, 2-12 onscreen, shortcut menus for, 7-24
Equilibration, 5-26 opening, 7-5
Free Space, 5-23 Options, 5-85
Overlays, 5-33 Regression, 7-7
Po and T, 5-25 Sample log, 5-85
Preparation, 5-22 saving in other formats, 7-22
Psat vs t, 5-29 selecting, 2-13
Replace, 2-10 Statistical Process Control (SPC), 7-6
Save, 2-10 Summary, 5-35
Skip, 6-6 Tabular options, 5-60
Suspend, 6-6 Tabular, editing onscreen, 7-24
Tool bar, 7-20
t-Plot, 5-46
Q types available, 5-34
QuickStart command, 6-8 Validation, 5-86
zoom feature, 7-28
Report button, 7-10
R Report options file, 5-31
Radio button, 2-10 creating, 3-12
Radushkevich report, 5-75 listing statistics, 3-33
Ramp rate, 5-14 printing contents, 3-31, 5-94
Ranges, valid, 2-9 Report Relative Pressure Table dialog, 5-40
Rear panel, 2-4 Reports menu, 7-1
Reference thickness curve, 5-47 Close Reports command, 7-5
Regression report, 7-7 Control Chart command, 7-11
recalculaing SPC values, 7-8 Open report command, 7-5
selecting X- and Y-Axes variables, 7-8 Regression Report command, 7-7
Regression Report command, 7-7 SPC Report Options command, 7-6
Regression Report dialog, 7-7 Start Report command, 7-3
Regression Report Sample Selection dialog, 7-8 Restricted format, 8-5
Regularization, 5-72 Sample information file, 3-16, 5-10
Relative pressure tolerance, 5-20 Resume push button, 6-7
Removing an analyzer, 4-16
Replace All pushbutton, 5-7
Replace push button, 2-10 S
Report Saito-Foley
Alpha-S method, 5-52 calculations, C-23
BET Surface Area, 5-39 Pore Geometry, C-23
BJH Adsorption/Desorption, 5-57 Sample
closing, 7-5 degassing, 3-23
Control Chart, 7-11 entering density, 8-11
displaying company logo in title, 5-32 low surface area, G-1
Dollimore-Heal, 5-64 weighing, 3-21
Dubinin, 5-75 Sample Analysis command, 6-3
examples, 7-29 Sample Backfill Options dialog, 5-27
f-Ratio method, 5-55 Sample compartment, 2-2
generating, 7-3 Sample defaults, 8-6
graphs, editing onscreen, 7-25 Advanced format, 3-1, 8-6
header, 7-19 Basic format, 3-4, 8-10
Heat of Adsorption, 7-15 Sample Defaults command, 8-6
Index-6 Jul 09
Sample Defaults dialog reinstalling analysis program, 4-8

Advanced format, 8-6 reinstalling calibration files, 4-19
Basic format, 8-10 removing an analyzer from the computer, 4-16
Sample file name, specifying default sequence, 8-6 uninstalling software, 4-20
Sample information dialog Shortcut keys, 2-6
Advanced format, 5-5 for Select Dates dialog, 2-12
Basic format, 5-8 list of, 2-7
Restricted format, 5-10 Shortcut menu, 2-6
Sample information file, 5-4 for graphs, 7-25
Advanced format, 5-5 for instrument schematic, 6-14
Basic format, 5-8 for tabular reports, 7-24
creating in Advanced format, 3-14 Show Instrument Log command, 6-21
creating in Basic format, 3-16 Show Instrument Schematic command, 6-17
defaults, restricted format, 8-10 Show Status command, 6-19
exporting, 3-34, 5-96 Side panel, 2-3
listing statistics, 3-33, 5-95 Skip push button, 6-6
printing contents, 3-31, 5-94 SmartPrep, 3-23
Restricted format, 5-10 SmartPrep Degasser, 1-6
Sample log report, 5-85 Soak
example of, 7-38 temperature, 5-14
Sample ports time, 5-14
location, 2-2 Software
replacing O-rings, 9-6 installing, 4-1
Sample tube installing upgrade, 4-8
cleaning and labeling, 3-18 uninstalling, 4-20
file, 5-11 using, 2-6
installing, 3-24 using for other functions, 4-6
on schematic, 6-16 SPC report, 7-6
replacing O-ring, 9-7 Control chart, 7-11
Sample Tube dialog, 5-11 Regression, 7-7
Sample tube file, 5-11 user parameters, 5-6, 8-8
creating, 3-6 SPC Report Options command, 7-6
listing statistics, 3-33 SPC Report Options dialog, 7-6
printing contents, 3-31, 5-94 Specifications, 1-8
Save All command, 5-93 Spreadsheet format
Save As command, 5-91 exporting isotherm data, 5-96
Save as Default push button, 7-14 saving reports, 7-22
Save command, 5-91 StarDriver files, converting, 5-98
Save push button, 2-10 Start push button, 6-7
Schematic, 6-14 Start Report command, 7-3
Select Calibration File dialog, 6-29 Start Report dialog, 7-3
Select Dates dialog, 2-12 Status list, 7-4
Selecting Status window, 6-19
files, 2-11 STSA thickness curve, 5-49
reports, 2-13 Submitter, specifying, 8-7
Service Test command, 6-30 Subnet mask
Service Test mode, 8-15 entering, Windows Vista, E-5
Servo valve entering, Windows XP, E-3
calibrating, 6-28 Summary report, 5-35
settings, 6-15 calculations, C-45
Servo Valve dialog, 6-28 example of, 7-37
Setup program, 4-6 Surface area correction factor, 5-50
adding an analyzer, 4-9 Surface Energy, F-11
moving an analyzer to another computer, 4-11 Surface Energy report, 5-74
Jul 09 Index-7
Suspend push button, 6-6 Unit Configuration command, 6-23

System installation videos, 2-15 Units command, 8-12
System valves, 6-15 Units Selections dialog, 8-12
Units, selecting, 8-12
Use calculation assignments, 5-88
T User parameters, 5-6
Table of Contents, online, 2-19 specifying, 8-8
Tarazona, F-7
Target pressure, 5-16
Temkim Report Options dialog, 5-44 V
Temkin report, 5-44 Vacuum
calculations, C-39 seal type, 5-12
Temperature Vacuum pump, 1-5
soak, 5-14 changing or adding oil, 9-8
specifications, 1-9 inspecting oil level, 9-8
Text, copy graph data as, 7-27 replacing alumina in oil vapor trap, 9-11
Thermal transpiration correction, 5-33 replacing exhaust filter, 9-15
calculations, C-6 Validation report, 5-86
Thermodynamic law, F-2 Valves
Thickness curve, 5-46, 5-57 failure, 9-1
Broekhoff-de Boer, 5-49 system, 6-15
Carbon Black STSA, 5-49 Van der Waal force, F-1
Halsey, 5-48 Videos, 2-15
Harkins and Jura, 5-49
Reference, 5-47
user-defined, 5-47 W
Thumbnails tab, 2-22 Wall potential, F-10
Title Properties dialog, 7-27 Warm free space, 5-11, 5-24
Tool bar, reports window, 7-20 Warnings, defined, 1-3
t-Plot report, 5-46 Weighing sample, 3-21
calculations, C-10 Windows
example of, 7-33 tile and cascade, 2-24
Transducer Windows menu, 2-24
match, 6-28
offset, 6-27
TriStar X
description, 1-4 X-axis order by, 7-12
specifications, 1-8
See also Analyzer
Troubleshooting, 9-1 Z
Zero pressure calibration, 6-27
Zoom feature, 7-28
U
Unit configuration, 6-23
Unit menu, 6-1
Calibration command, 6-27
Diagnostics, 6-24
Enable Manual Control command, 6-14
QuickStart command, 6-8
Sample Analysis command, 6-3
Service Test command, 6-30
Show Instrument Log command, 6-21
Show Instrument Schematic command, 6-17
Show Status command, 6-19
Index-8 Jul 09

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TriStar II 3020

© Micromeritics Instrument Corporation 2008-2009. All rights reserved.

4356 Communications Drive Norcross, GA 30093-1877 Fax (770) 662-3696

Domestic Sales - (770) 662-3633 Domestic Repair Service - (770) 662-3666

4. SOFTWARE AND SETUP MODIFICATIONS

9. TROUBLESHOOTING AND MAINTENANCE

10. ORDERING INFORMATION

G. MAINTAINING HIGH PURITY GASES

To help you operate the TriStar more efficiently:

• use the step-by-step instructions in Chapter 3 when performing common operations

Organization of the Manual

Chapter 1 GENERAL DESCRIPTION

Chapter 2 USER INTERFACE

Chapter 3 OPERATIONAL PROCEDURES

Chapter 4 SOFTWARE AND SETUP MODIFICATIONS

Chapter 5 FILE MENU

Chapter 6 UNIT MENU

Chapter 7 REPORTS MENU

Chapter 8 OPTIONS MENU

Chapter 9 TROUBLESHOOTING AND MAINTENANCE

Chapter 10 ORDERING INFORMATION

Appendix B ERROR MESSAGES

Appendix D FREE-SPACE CORRECTION

Appendix E ETHERNET CONFIGURATION

Appendix F DFT MODELS

Appendix G MAINTAINING HIGH PURITY GASES

Notes contain important information pertinent to the subject matter.

• be able to achieve vacuums better than 20 µmHg at the instrument inlet

• contain an NW16 inlet port for connection to the TriStar

Refer to Chapter 10, page 10-1 for ordering information.

About Micromeritics A brief history of Micromeritics, office locations, awards/cer-

Products Product information and printable brochures

Applications Application Notes, Product Bulletins, Tech Tips, Technical

Online Catalog Catalog of instruments and accessories, allowing you to place

Customer Support Customer support contacts, product registration, instrument

Contact Us Contact information, office locations, maps and driving direc-

Specific Surface Area: From 0.01 m2/g, nitrogen unit

Nitrogen unit: Nitrogen; argon, carbon dioxide, or other non-corrosive gases;

Temperature: 10 and 35 ºC (50 to 95 ºF), operating;

Height: 74 cm (29 in.)

Voltage: 100/120, 220/240 VAC

Minimum Pentium 333 MHz computer (or equivalent)

Instrument Components and Connectors

Power indicator Blinks when power is applied to the analyzer; illuminates

Sample Compartment Sliding door which encloses the sample compartment.

Sample ports (three)

Saturation pressure (Po) tube Diagram of port locations

Po tube For measuring the saturation pressure.

Diagram Provides a pictorial representation of port numbers and their

Elevator Allows placement of the Dewar around the sample and Po

Ethernet connector For connecting the ethernet cable, allowing communication

RS-232 connector Used by service personnel to perform calibration procedures.

Analysis inlet valves Vacuum Pump connector

Maximum inlet Helium inlet valve

Power cord connector

Vacuum Pump connector For attaching the vacuum pump hose.

On/Off switch For turning the analyzer on and off.

Power connector For connecting the analyzer to the power supply.

Turning the Analyzer On and Off

Turning the Analyzer On

Turning the Analyzer Off

If an analysis is in progress, the following message is displayed:

2459- An Instrument is busy. A delay in restarting this

TriStar II 3020 Operator's Manual

TriStar II 3020 Operator's Manual