Ba Dumatherm GB

Dumatherm
DT
02. Aug. 2007_GB
Instruction Manual
Please read this instruction manual with care before you start operating
the system!
Please observe the safety instructions of this manual marked with in
order to avoid any dangerous handling!
2 Dumatherm
Content
Important notes ........................................................... 5
How to use this instruction manual .................................................................... 5
Explanation of symbols...................................................................................... 5
1 Safety ......................................................................... 6
1.1 Operation as directed .................................................................................. 6
1.2 Safety instructions ....................................................................................... 6
1.3 Work bench / Authorized user ..................................................................... 7
1.4. Danger spots at the instrument .................................................................. 7
2 Technical description ............................................... 8
2.1. Warranty conditions .................................................................................... 8
2.2. Technical data ............................................................................................. 8
3 Delivery...................................................................... 9
3.1. Check for transport damage ....................................................................... 9
3.2. Parts list ..................................................................................................... 9
4 Operating principle................................................. 10
4.1. General ..................................................................................................... 10
4.2. Dumas method ......................................................................................... 10
5 Description of the Dumatherm .............................. 12
5.1 Front view Dumatherm .............................................................................. 12
5.2 Rear view Dumatherm ............................................................................... 13
5.3 Open front view, right side ......................................................................... 14
5.4 Front view, upper part open furnace section ............................................. 15
5.5 Rear view, open furnace section ............................................................... 16
5.6 Rear view, open carousel and electronics section..................................... 17
5.7 Side view, open, pneumatic section .......................................................... 18
5.8 Open top view, carousel section ................................................................ 19
6 Assembly and installation ..................................... 20
6.1. General informations ................................................................................ 20
6.2. Working environment ................................................................................ 20
6.3. Placement area and weight Requirements:.............................................. 20
6.4. Gas connections ....................................................................................... 20
6.5. Communication......................................................................................... 20
6.6. Connection of pneumatic autosampler ..................................................... 21
6.6.1. Installation of the pneumatic autosampler ............................................. 22
6.7. Mains connection:..................................................................................... 22
7 Prepare for operation ............................................. 23
7.1. Gas connections ....................................................................................... 23
7.1.1. Purge the He and O
2
lines ..................................................................... 23
7.2.Tube packing ............................................................................................. 23
7.2.1. Preparation of tubes .............................................................................. 23
7.2.2. Combustion Reactor Packing ................................................................ 24
7.2.3. Reduction Reactor Packing ................................................................... 24
7.2.4. Insert Packing ............................................................................................
7.2.4. Befllen des Ascheeinsatzes ................................................................. 24
7.3. Installing the tubes into the furnaces ........................................................ 25
7.3.1. How to insert the tubes .......................................................................... 25
7.4. Installing the Co
2
adsorbers into the carousel .......................................... 26
7.5. Water trap packing ................................................................................... 27
3
Dumatherm
Content
7.6. Starting the "Dumatherm Manager" software ........................................... 27
7.7. Heating up reactor tubes .......................................................................... 28
7.8. Catalyst oxydation .................................................................................... 28
7.9. Dichtigkeitsprfung ................................................................................... 28
7.9.1. Dichtigkeitsprfung allgemein................................................................ 28
7.9.2. Dichtigkeitsprfung im Bereich der CO
2
Adsorber. ................................ 28
8 Dumatherm Manager - Software description ....... 30
8.1. SOFTWARE INSTALLATION ................................................................... 30
8.1.1. System requirements............................................................................. 30
8.1.2. Installation of the 'Dumatherm Manager' Software ............................... 30
8.1.3. Removing the Dumatherm Manager Software .................................... 30
8.2. GENERAL ................................................................................................ 30
8.2.1. Choose language .................................................................................. 30
8.3. MENUS..................................................................................................... 31
8.3.1. Category menu ...................................................................................... 31
8.3.2. Standard menu ...................................................................................... 32
8.3.3. Maintenance menu ................................................................................ 32
8.3.4. Tools menu ............................................................................................ 33
8.3.4.1. Lock Analyzer submenu ..................................................................... 33
8.3.4.2. Change Password submenu .............................................................. 33
8.3.4.3. Change Master Password submenu ................................................ 33
8.3.4.4. Enable Grid Controls submenu .......................................................... 33
8.3.4.5. Test dbase submenu .......................................................................... 33
8.3.4.6. Default Constants submenu ............................................................... 33
8.3.4.7. View Current Logbook submenu ........................................................ 35
8.3.4.8. Balance Type submenu ...................................................................... 36
8.3.4.9. Change Communication Port submenu.............................................. 36
8.3.4.10. Excel Documents Protected ............................................................. 36
8.3.4.11. Balance Type .................................................................................... 36
8.3.4.12. Choose language ............................................................................. 36
8.3.5. Help menu ............................................................................................. 36
8.3.5.1. About submenu................................................................................... 36
8.4. Sheets ...................................................................................................... 37
8.4.1. Analysis conditions.............................................................................. 37
8.4.1.1. "Operator" ........................................................................................... 37
8.4.1.2. "Method" ............................................................................................. 37
8.4.1.3. "Send to instrument" ........................................................................... 38
8.4.1.4.WORK ................................................................................................ 40
8.4.1.5. STANDBY .......................................................................................... 40
8.4.1.6. "Wake up .......................................................................................... 40
8.4.2. "Sample Table" ...................................................................................... 41
8.4.2.1. Sample analysis ................................................................................. 42
8.4.2.2. Description of the table ....................................................................... 43
8.4.3. Calibration ............................................................................................. 45
8.4.3.1. Right Table. ........................................................................................ 46
8.4.3.2. Left table ............................................................................................. 47
8.4.3.3. Polynominal ........................................................................................ 48
8.4.4. History ................................................................................................... 49
8.4.4.1. Description of the history table ........................................................... 49
8.4.4.2. Create Document ............................................................................... 51
8.4.4.3. Create Document for each Row ........................................................ 52
8.4.4.4. Filter ................................................................................................... 53
8.4.4.5. Copy to Archive ................................................................................. 53
8.4.4.6. Move to Archive ................................................................................. 53
4 Dumatherm
Content
8.4.4.7. View Archive ...................................................................................... 53
8.4.5. Plots....................................................................................................... 54
8.4.6. Service .................................................................................................. 55
8.4.6.1. Carousel ............................................................................................. 55
8.4.6.2. Indications of current operational parameters .................................... 55
8.4.6.3. Valve State ......................................................................................... 56
8.4.6.4. Communication boxes ........................................................................ 57
8.4.6.5. Manual Control ................................................................................... 57
8.4.6.6. User access level ............................................................................... 57
9 Operation................................................................. 58
9.1. General ..................................................................................................... 58
9.1.1. Checkliste vor dem Start einer Analyse ................................................. 58
9.2. Analyse von unbekannten Proben ............................................................ 58
9.2.1. Leitfaden fr die Bestimmung des richtigen Verbrennungsfaktors fr eine
unbekannte Probe .................................................................................... 58
9.2.2. Bestimmung des Verbrennungsfaktors bei einer unbekannten Probe .. 59
9.3. Homogenization of samples ..................................................................... 59
9.4. Weighing of samples ................................................................................ 60
9.5. Inserting the sample weights into the sample table .................................. 61
9.5.1. Data transfer via balance....................................................................... 61
9.6. Weighing of liquid samples ....................................................................... 61
9.7. Sample analysis ....................................................................................... 61
10 Trouble Shooting .................................................. 62
10.1. Error actions catalogue........................................................................... 62
11 Maintenance .......................................................... 65
11.1. Service and cleaning .............................................................................. 65
11.2. Spare parts and consumables ................................................................ 65
11.3. Accessories ............................................................................................. 66
11.4. Service and contact ................................................................................ 66
11.5. Disposal .................................................................................................. 67
11.5.1. Information for the Disposal of Electric and Electronic Instruments within
the European Union ................................................................................... 67
11.5.2. Ban on Materials according to ROHS Regulation 2002/95/EG ........... 67
11.5.3. Transfer ................................................................................................ 67
5
Dumatherm
Important notes
How to use this instruction manual
Please make sure that the persons working with the Dumatherm must have read,
understood this manual in order to observe the instructions.
This instruction manual must be accessible to all users at any time and is a part
of the Dumatherm system!
The instrument will be called 'Dumatherm' in the entire document.
This instruction manual only explains the technical details necessary for the ope-
ration of the instrument but is NOT a complete technical description.
The security advises given in this manual have to be observed under all circum-
stances! The symbols at the border of the text emphasize the dangers cited in
the text.
Symbols at the instrument warn of possible dangers and will refer you to this
manual!
The copy right of this manual remains with C.Gerhardt GmbH & Co. KG
Reproduction and copying are only allowed with the permission of C.Gerhardt
GmbH & Co. KG
Explanation of symbols
Warnung vor gefhrlicher,
elektrischer Spannung
Warnung vor
einer Gefahrenstelle
Attention!
Hot surface!
Attention!
Mains voltage!
Attention! Advance notice of substances
which might be a health risk or cause
irritation!
Attention!
Read instruction manual!
Attention!
Use eye protection!
Attention!
Use protective gloves!
Attention! Advance notice of danger spots,
carefully read instruction manual!
Dumatherm
1 Safety
1.1 Operation as directed
The DUMATHERM Nitrogen/Protein Analyzer is intended for the quantitative de-
termination of Nitrogen/Protein content in foods, feeds, meals, oilseeds, plants pet
foods, milling products, soils, fertilizers etc.
Make sure to use the instrument according to our instructions, especially:
- all instructions of this manual
- the regulations in place in the country the instrument is used
All other usage is not recommended!
C. Gerhardt GmbH & Co. KG is not liable for any damages caused due to non
recommended usage
- anymodifcationsarenotallowedforsafetyreasons
- repairs of electric, electronic or mechanical components may only be done by
authorized personnel!
1.2 Safety instructions
The DUMATHERM corresponds to the technical standard used at this date and
observes the safety rules and regulations in place.
It is understood that the user has to observe
- the accident prevention regulations in place
- the general accident prevention regulations
- EU-regulationsorothercountryspecifcinstructions
Explosives or substances, which might release explosive gas mixtures, must not
be analyzed. If in doubt, contact the manufacturer.
Gas lines must have the pressures listed on this manual. Check gas supply system
for leaks at regular intervals (about every 2 months).
Please check the nominal voltage on the product information plate before con-
necting to the mains. Should the nominal voltage deviate for more than +/- 10%,
then you must contact your service engineer.
Further protective measures must be taken to prevent an accidental start-up.
- Prior to restarting the instrument, please check whether all panels have been
replaced correctly. Dont use power cords with frayed insulation. Check the
actual line voltage to make sure that it is what the instrument needs.
- Be sure the power cords are plugged into correct voltage sources.
- Replace blown fuses with size and rating stipulated on the fuse panel or holder
and in the manual where listed.
When replacing any of the heated tubes or the ash insert, always wear protective
gloves and safety goggles. Beware of burns.
Always wear the protective leather gloves when handling quartz and glass com-
ponents. Beware of broken glass.
When handling chemicals please observe the manufactures safety instructions
(see label).
Make sure that the analyser is in stand-by mode before you start replacing of any
tubes.
Warnung vor
Warnung vor
Warnung vor
Warnung vor
Warnung vor
Warnung vor
Warnung vor
Warnung vor
7
Dumatherm
Make sure that no liquid gets into contact with cable connections or the interior of
the electrical parts of the unit!
- Danger of electric shock!
In case of an emergency disconnect from mains immediately!
Always pull the mains plug before opening!
- Danger of electric shock!
1.3 Work bench / Authorized user
The DUMATHERM must not be run in damp or hazardous location. The maximum
humidity allowed is 80 %, the maximum room temperature must not exceed 35
C!
The DUMATHERM has to be placed on a horizontal and stable footprint.
The DUMATHERM may only be operated by trained staff or especially trained
persons.
The user has to:
- read, comprehend, and observe the operation manual
- wear suitable clothes for laboratory work
- deny access to any unauthorized personnel
1.4. Danger spots at the instrument
1 Safety
Warnung vor
Warnung vor
Warnung vor
Warnung vor
Warnung vor
- Be careful! The surface of the upper reactor screw
connections is hot. In order to avoid burns, you
always have to make sure to put the insulation cap
over the upper reactor screw connection. Always
use special Dumatherm tools for opening the re-
actor screw.
- Be careful! The surface of the bottom of the reactor
is hot. Make sure to wear gloves every time you
change the reactors!
8 Dumatherm
2.1. Warranty conditions
The DUMATHERM is manufactured following the high quality guidelines of EN ISO
9001:2000. On the basis of the C. Gerhardt conditions of warranty our products
are guaranteed for 1 year, as long as the apparatus is used in accordance with
the instructions mentioned in this manual.
Please note that the working parts are excluded from warranty.
2.2. Technical data
Order No.: 7700
Type: DT
Nominal voltage: 230 V, 50/ 60 Hz
Relative standard deviation: < 0.5 % abs. with 200 mg test substance (EDTA)
Detection limit: N minimum < 0.01 mg, maximum 50 mg
Sample weight: 0.5 mg to 1 g
Duration of analysis: 2 - 4 minutes depending on sample substance and
weight
Dimensions (WxDxH ): 500 x 370 x 500 mm (675 with autosampler)
Weight: 65 kg
Power consumption: maximum 6 Ampere
Admissible ambient temp.: 15C < t < 35C

Temperature of furnaces:
- Combustion: 400 - 1100C
- Reduction: 400 - 1100C
- Desorption: 50 - 350C
Supplied gases and their minimum demands on quality:
- Helium (He) 99.999 % purity (quality grade 5.0)
- Oxygen (O
2
) 99.999 % purity (quality grade 5.0)
- Compressed air or industrial nitrogen (N
2
)
99.996 % purity (quality grade 4.6), without dust, oil
and water vapours
Gas inlet pressures:
- He 3-6 bar
- O2 3-6 bar
- Clean compressed air or N
2
3-6 bar
PC:
- CPU speed 2 GHz
- RAM 512 MB
- Free hard disk space 80 MB
- Operation system Windows XP
- Additional needed software Microsoft Excel
- Free ports 1 x RS 232, 1 x USB
- Monitor 17
- Printer A4 printer
2 Technical description
Dumatherm
3 Delivery
3.1. Check for transport damage
Before assembling the apparatus please check if the content of the box is com-
plete and intact!
In case of any damage, please notify your carrier (post, rail, road) as well as your
supplier!
The exact contents of the delivery can be checked by the packing list.
Depending on the means of transport used, the DUMATHERM Protein Analyzer
is delivered upright in a transport casing.
Unpack the DUMATHERM Protein Analyzer carefull!
3.2. Parts list
Please see enclosed packing list!
The basic unit is delivered in the following condition:
1. The two empty reactor tubes are not assembled. They are packed in the in-
stallation kit.
2. The autosampler PN120 is not assembled. The Sampler is packed in a separate
container.
3. Thestandardoutftsarepackedinaseparatebox.
10 Dumatherm
4.1. General
DUMATHERM is a fully digital instrument: all main functions are controlled by a
built-in microprocessor. Analysis parameters, instrument control, measurements
of samples and processing of measured data are set and controlled by Windows
NT based Dumatherm Manager software. The real-time measuring process
and the nitrogen/protein content calculations with all necessary informations are
directly displayed and stored in the memory. Sample results can be printed out as
a complete report. The software warns the operator when the instrument mainte-
nance is required.
The combustion conditions are optimized to reduce the cost per analysis of samples
andmaximizethelongevityofthereactor.Theuniquetwo-stagewaterfltering
system increases the lifetime of the water trap-packing considerably.
Six tubes, packed with CO
2
adsorbent, are mounted on the carousel. While one
tube is always in line with the analytical circuit and adsorbs all the CO
2
from the
current sample analysis, three other tubes are in the furnace desorbing their trap-
ped CO
2
to the atmosphere. This simultaneously done absorption and disorption
process drastically reduces the analysis time.
4.2. Dumas method
The operation of DUMATHERM is based on the Dumas method, i.e. quick
combustion of liquid or solid samples in a pure oxygen atmosphere, followed by
analysing the resulting gases. The measurement of the thermal conductivity with
a TCD-detector gives a signal which corresponds to the amount of nitrogen in the
combustedsample.ThesimplifedfowdiagramisshowninFigure4.2.
Figure4.2:SimplifedfowchartoftheDumatherm:
AS=autosampler, He=Helium gas inlet, O
2
=Oxygen gas inlet, LF=left furnace,
combustion reactor, RF=right furnace, reduction reactor, F1 Perma pure gas dryer,
F2=flters for water separation, F3=CO
2
absorber/desorber tube, TCD=thermal
conductivity detector, PC=personal computer.
Helium circulates as a carrier gas through the entire analytical circuit, which consists
of autosampler (AS), combustion reactor (LF), reduction reactor (RF), traps for
4 Operating principle
Fig. 4.2.:
Flow diagram
11
Dumatherm
water (F1, F2) and carbon dioxide (F3) and a thermal conductivity detector (TCD).
Before the sample drops from the autosampler into the combustion reactor, the
carrierfowisswitchedfromheliumtooxygen.Theexothermicreactionwhenthe
oxygen gets in touch with the tin capsule including the sample at a temperature of
about 1000 C raises the temperature in the reactor from 1000 up to 1700 1800
C within seconds. At this temperature - and in the presence of specially designed
heterogeneous oxidation catalysts - the sample is completely converted into its
elementaloxides.Aftercombustion,theoxygenfowisswitchedbacktohelium
which serves as the transport gas for the combustion products through the rest
of the analytical circuit.
The byproduct water (H
2
O)isseparatedfromthisgasmixturebytwoflters-F1and
F2. F1 is the Perma Pure gas dryer, which separates the majority of water from the
gasmixture(comparefgure5.5).ThesecondflterF2ispackedwithmagnesium
perchlorate to remove the residual amount of water from the gas stream. Carbon
dioxide (CO
2
) is separated from the gas mixture in the CO
2
absorber/desorber
system(F3infgure1).TheCO
2
absorber tubes are regenerated in the degassing
furnace. The remaining gas mixture passes the TC detector leading to an output
signal which is proportional to the N
2
concentration in the combusted sample.
Standard samples with a known concentration of nitrogen (e.g. EDTA, Glycin, ...)
are used for calibration of the TCD.
4 Operating principle
12 Dumatherm
5 Description of the Dumatherm
5.1 Front view Dumatherm
1 High temperature section (oxidation and reduction furnaces)
2 Pneumatic autosampler
3 Carousel, power supply, electronics and pneumatics
On the upper part of section 3 are the following LED indicators:
4 Left furnace LED (green/red)
5 Right furnace LED (green/red)
6 Desorption furnace LED (green/red)
7 Alarm LED (red)
8 Standby LED (red)
Fig. 5.1.:
Front view Dumatherm
with autosampler
4 5 6 7 8
1
3
2
Infgure4.1.youcanseeashortdescriptionofthemainpartsoftheC.Gerhardt
nitrogen/protein analyser Dumatherm. The DUMATHERM can be divided into
three main sections:
13
Dumatherm
1 Degassing gas output - DEGAS
2 Measuring system output - OUTPUT
3 Purge gas connection for autosampler - PURGE
4 Carrier gas helium or gas oxygen combustion connection for AS - He or O2
5 Piston forward - AIR1
6 Piston back/ tray turn - AIR2
7 Ground terminal
8 Mains power cord
9 ON/OFF switch
10 Fuses 10 Ampere
11 Helium inlet - He
12 Oxygen inlet - O2
13 Compressed air/ industrial nitrogen inlet - AIR
14 USB port
15 RS-232 port
16 Cooling fan for adsorbers
5.2 Rear view Dumatherm
Fig. 5.2.:
Rear view Dumatherm
with autosampler
Infgure5.2youcanseethebacksideoftheinstrumentwiththefollowingspeci-
fcations.
1 2 3 4 5 6
7 8
9
10
11
12
13
14
15
16
14 Dumatherm
5.3 Open front view, right side
Fig. 5.3.:
The power/electronics
section (lower part),
carousel section (up-
per part), gauges and
pressure regulators of
the pneumatic sections
(right side).
1 Damper volume
2 Power supply
3 Degassing furnace
4 H
2
O trap
5 CO
2
Adsorbent tubes TRAP1-TRAP6
6 Adsorbent tube ports
7 Carousel with the 6 adsorption tubes
8 6-way switching valve
9 LED block
10 He gauge P1
11 He pressure regulator PRV1
12 O
2
gauge P2
13 O
2
pressure regulator PRV2
14 Compressed air (or industrial N2) gauge P3
15 Compressed air (or industrial N2 ) pressure regulator PRV3
In fgure 5.3 you can see a short description of the power/electronic section, a
detailed view on the absorber/desorber carousel and the pneumatic section of
the Dumatherm
1
2
3
4
5
6
7
8
9
10
11
12
13
15
Dumatherm
5.4 Front view, upper part open furnace section
Fig. 5.4.:
Furnace section front
view
1 Quick-tension lever (LF and RF)
2 Thermocouple of LF
3 Combustion reactor LF
4 Combustion/Reduction reactors joint, Order-No.: 77009
5 Thermocouple of RF
6 Reduction reactor (RF)
7 Heating resistance leads terminal block
8 Protective lid RR (please put it over the opening of the reactor connection when
replacing the reactor to prevent that dirt gets in there)
9 Reactor accommodation complete with connection, fast clamping devises
and protective lid RR and LR, order no.:77128
10 Protective lid LR (please put it over the opening of the reactor connection when
replacing the reactor to prevent that dirt gets in there)
Infgure5.4youcanseeashortdescriptionofthefrontviewofthefurnacesection.
You can see the stainless steel tubing (No. 7) going from the oxidation furnace to
the reduction furnace.
2
1
10
4 5
8 7
3 6
9
1 Dumatherm
5.5 Rear view, open furnace section
Fig. 5.5.:
Rear view of the furnace
section
1 Gas dryer Perma Pure (Dr)
2 Output of dry gas
3 Input of purge gas
4 Solenoid valve EV9 (Purge air)
5 Solenoid valve EV2 (Vent for combustion products)
6 Needle valve NV3 (Purge air)
7 Fan-Furnace cooling
8 Solenoid valve EV8 (Piston forward)
9 Solenoid valve EV7 (Piston back/tray turn)
10 Output of purge gas
11 Inlet of wet gas
12 Thermocouples terminal block
Infgure5.5youcanseeashortdescriptionoftherearviewofthefurnacesec-
tion.
1
2
3
4
5 6 7 8 9
10
11
12
17
Dumatherm
5.6 Rear view, open carousel and electronics section
Fig. 5.6.:
Rear view of carousel
and power/electronics
sections:
1 Pneumatic cylinder (PS) for turning the carousel
2 Fan - adsorbers cooling
3 6-way switching valve
4 Degassing furnace
5 Controller printed circuit board (PCB)
Infgure5.6youcanseeashortdescriptionoftherearviewofthecarouselsec-
tion.
1
2
3
4
5
18 Dumatherm
5.7 Side view, open, pneumatic section
Fig. 5.7.:
Pneumatic section
1 Needle valve NV4 (Carousel cylinder)
2 Solenoid valve EV6 (Carousel cylinder)
3 Compressed air or industrial nitrogen pressure regulator PRV3
4 Compressed air or industrial nitrogen gauge P2
5 Solenoid valve EV3 (Combustion oxygen)
6 O
2
pressure regulator PRV2
7 O
2
gauge P1
8 Solenoid valve EV1 (Purge helium)
9 Solenoid valve EV5 (Degas helium)
10 He pressure regulator PRV1
11 He gauge P3
12 Solenoid valve EV4 (He or O2)
13 Mass Flow Controller (MFC 1) (He/O2)
14 Thermo Conductivity Detector (TCD)
15 Mass Flow Controller (MFC 2)

16 Mains Filter
Infgure5.7.youcanseeadetaileddescriptionofthepneumaticsection.
1 2
3
4
5
6
7
8
9
10
11
12
13
14
15
16
1
Dumatherm
5.8 Open top view, carousel section
Fig. 5.8.:
carousel
1 Carousel
2 Carousel position reader
3 Damper volume V
4 H
2
O trap TRAP1
Infgure5.8youcanseeashortdescriptionofthetopviewofthecarouselsec-
tion.
1
2
3
4
20 Dumatherm
6.1. General information
Depending on the means of transport used, the DUMATHERM Nitrogen Analyzer
is delivered upright in a transport casing.
The basic unit is delivered in the following condition:
1 The two empty reactor tubes are not assembled. They are packed in the in-
stallation kit.
2 The autosampler PN120 is not assembled. Sampler is packed in a separate
container.
3 The degassing furnace is secured by transport guards. Open the front cover
of the carousel (for this lift the panel up and remove it) section and remove the
guards.
6.2. Working environment
The entire installation, consisting of the DUMATHERM and all peripheral equip-
ment must be operated in a dry, well ventilated and hazard free environment (i.e.
laboratory) at predominantly constant temperature between 15C min and 35C
max.
It is not allowed that the instrument be installed near the heat source or in direct
sunlight.
6.3. Placement area and weight requirements:
Put the instrument on a solid base.
- Length (width) min. 2 m
- Depth min. 0.75 m
- Minimum clearance between the sides and back of the instrument should be
0,20 m
6.4. Gas connections
Gasinputfttingsarelocatedintherearoftheinstrument(seefgure5.2.)
Required gases and their minimum purity:
- Helium (He) - 99.999 % (quality grade 5.0)
- Oxygen (O
2
) - 99.999 % (quality grade 5.0)
- Compressed air (oilo and fat free) or industrial Nitrogen (N
2
) - 99.6 %
Inlet pressures:
- Helium (He), Oxygen (O
2
) - 3-5 bar
2
) - 4 bar

Gas lines:
- He, O
2
- 2 0.5 mm (stainless steel tubes)
2
) - 4 0.75 (PU or PE)
6.5. Communication
For the communication between DUMATHERM and PC, you can either use a
serial I/0 COM-port RS 232 C or USB-port. Connectors of these ports are located
onleftsideoftheinstrument(seefgure5.2.).
- For RS 232, use a modem cable DB9F - DB9F 5 m (DEL -25B)
- For USB, use a cable type A-B Plug-Plug, 3 m.
6 Assembly and installation
21
Dumatherm
Figure 6.6.1:
Detailed view on the pneu-
matic autosampler with one
sample tray on the top
1 Plastic lid, transparaent, order-no.: 77046
2 Viewing port (window)
3 Tube connecting AS with combustion reactor
4 Autosampler support, silicone rubber disc, order-no.: 77041
5 Carrier inlet tube for (He or O
2
), order-no.: 77012
6 Purge inlet tube, order-no.: 77059
7 Compressed air or industrial N2 inlet - piston forward (sample drops)
8 Compressed air or industrial N2 inlet - piston back (tray turns)
9 Leveling legs
10 Slider movable
11 Tray for 40 samples, order-no.: 77029
Figure 6.6.2
Operating principle of the
pneumatic autosampler
6.6. Connection of pneumatic autosampler
To reach a higher sample throughput you can mount up to three sample trays with
40sampleseachontopofthepneumaticautosampler.Infgure6.1.the40-position
autosampler is shown. The trays of the autosampler are open to atmosphere, so
samples can be added continuously while running. The sample holes in the trays
are 15 mm in diameter. A viewing port (2) allows the operator to view the sample
combustion during sample analysis.
1
2
3
5 6 7 8
9
4
11
10
22 Dumatherm
Infgure6.6.2.theautosamplerisintheactivatedpositioni.e.thepistonhasmo-
ved forward and the sample drops into the combustion reactor (air is switched to
input 1). The operator can observe the combustion process through the viewing
port. When air is switched to input 2, the piston moves back and the sample tray
turns to the next position. The sample drops into the centre hole of the piston and
the cycle is repeated.
6.6.1. Installation of the pneumatic autosampler
The carrier gas line for the analytical circuit is connected to the port on the side of
the tube, which connects to the combustion reactor. The purge line is connected
to the port in the bottom of the sampler.
Forpurgeandcarriergaslinesusestainlesssteeltubingcode77012andtefon
tubing code 77039 to ensure there are no leaks.(they are packed in the installation
kit).Thetefontubinghastobeconnectedtotheportinthebottomofsampler.
The helium carrier gas line has to be connected to the port in the side of the tube
to the combustion reactor.
Compressed air or industrial N2 is used to operate the pneumatic autosampler.
For pneumatics i.e. compressed air use the PU tubing 40.75 mm code 77003.
Cut 2 pieces appr. 25 cm and connect them to ports AIR N1 and AIR N2 of
autosampler (use ferrules code 77004 ).
- Connect the pneumatic tubing from the outlet marked AIR1 (pos. 5 on the Fig.
5.2.) on the top of the DUMATHERM to the port labeled AIR N1 (pos. 7 on
the Fig. 6.6.1.) in the back of the Autosampler.
- ConnectthepneumatictubingfromtheoutletmarkedAIR2(pos.6onthefg.
5.2.) on the top of the Dumatherm in the side of the autosampler (pos. 8 on
the Fig.6.6.1.).
Something to keep in mind when working with this type of autosampler:
1 Compressed air or industrial N2 inlet pressure must be 2.5 - 3 bars.
2 The plastic lid must always be placed on top of the sample tray, to minimize
the nitrogen blank.
6.7. Mains connection:
Please check the nominal voltage on the type plate before connecting to the
mains. Should the nominal voltage deviate for more than +/- 10%, then you have
to contact your service engineer.
TheNitrogenAnalyzerDUMATHERMisequippedwithfexiblepowercableand
250 V / 16 A plugs. The placement of mains switch and fuses 10 A is shown in
Fig 3.
23
Dumatherm
7 Prepare for operation
7.1. Gas connections
For connecting He and O
2
usethestainlesssteeltubings(20.5mm).Gasfttings
areonrearpanel(seefg5.2.pos.11and12).
- For connection use nuts code 77005 and ferrules code 77006.
- For compressed air or industrial N
2
use a PU tubing (4 0.75, code 77003).
Cuttheendperpendicularlyandpushitintothefttingontherearoftheinstru-
ment.
Open the cylinder valves. Adjust input pressures:
He, O
2
- 3 bar
compr.air - 4 bar
Remove the front panels. For this lift the panel up and remove it. Check the pres-
sure indications of gauges:
He, O
2
- 2 bar
compressed - 3 bar
If the indications differ from the above mentioned values, regulate them to correct
values using pressure regulators below each gauge.
7.1.1. Purge the He and O
2
lines
Newly installed He and O
2
gas lines must be purged to eliminate moisture and
air. For this:
1 Open on the rear panel He and O
2
inletfttingsoneturn
2 Purge He lines 2 seconds and O
2
lines 5 seconds
3 Closebothfttings
7.2.Tube packing
7.2.1. Preparation of tubes
For the packing of the tubes we recommend the following procedures.
In general, all tubes have to be cleaned before use. Clean tubes with a solvent
suchasacetonebeforeinsertingthemintothefurnaceandremoveanyfnger-
prints. Otherwise the forming of crystallisation zones can cause the premature
aging of quartz.
The manufacturer supplies in the consumables start-up kit the proper quality of
chemicals for the tube packing. They may also be purchased separately as ac-
cessories.
Handle the quarts and glass tubes very carefully!
Always use the special tool, order no. 77022, for the transport of the glass
tubes,
The manufacturer is not responsible for incorrect analysis results if the customer
uses the chemicals from other suppliers.
Alltubefllingsmustbepackeddownastightlyaspossibletoavoidairpockets.
For this tap the tube to the rubber plate.
When you pack the tubes, dont touch them with bare hands and always use gloves
to protect your hands.
Warnung vor
Warnung vor
Warnung vor
Warnung vor
Warnung vor
24 Dumatherm
7.2.2. Combustion Re-
actor Packing
The packing begins from
the bottom i.e. the end
with smaller diameter.
Tighten the quartz wool
withthereactorfllingrod
code 77023. Tighten the
fllingasmentionedabo-
ve. Fill in the packing with
the distances described.
7.2.3. Reduction Reac-
tor Packing
The technique for packing
the reduction reactor is
the same as the proce-
dure for the combustion
reactor.
Fig. 7.2.2. Combustion
Reactor Packing
Fig. 7.2.3. Reduction Re-
actor Packing
Fig 7.2.4. Ash insert pa-
cking
40
50
10
120
10
High temperature
catalyst (HT)
Quarz wool
Quarz wool
Low temperature
catalyst (LT)
Quarz wool
All dimensions in mm
7.2.4. Filling of the ash
insert
The ash insert is inserted
using the tongs (code
77014) included in the
shipment into the com-
bustion reactor. It is used
as a catchment tank for
the ash which is produced
during combustion. To
avoid overheating of the
ash insert it has to be re-
moved after an analysis
break of more than 1 h.
It has to be renewed after
the analysis of about 100
to 120 analyses.
This can also be done
while it is still hot. In order
to do so, loosen the box
nut between the sample
feeder and the combusti-
on reactor using tool order
no.:77031, carefully lift
the sample feeder from
the reactor tube (dont
touch hot glass or metal
parts! Make sure to wear
protective gloves!) Push
the sample feeder to the
side and take out the ash
insert using tongs order
no.: 77014.
25
Dumatherm
Cover-angle,
closed
Quick tension lever closed Quick tension lever opened
7.3. Installing the tubes into the furnaces
Please always use the special tool, code 77022, to insert the tubes into the fur-
naces.
Attention: please make sure to wear protective gloves when replacing the tubes!
Beware of burns!
7.3.1. How to insert the tubes
Step 1
- Please take off the left cover of the high temperature range on the left (slightly
lift the cover and pull to the front)
- Now,insertthecompletelyflledandentirelycleaned(fngerprints)reactorinto
the corresponding furnace (LF respectively RF).
Step 2
- Press the reactors as far as possible into the reactor connection, so that both
reactors stick out an max. amount of 0.5 cm from the upper side of the instru-
ment housing.
- Close the quick tension lever
- Put the auto sampler on the combustion reactor and screw it on by turning the
cap nut (can be turned easily).
- The reaction reactor is closed with the cap nut
- Close the instrument by putting on the front cover.
Tool,
code 77022
Reactor tube
Quick tension
lever
Seal for top of
reactor tubes,
code 7721
1. Step 2. Step
Fig. 7.3.
Connection of the reactor
tubes
Warnung vor
Warnung vor
Cap nut
Cover-angle,
open
2 Dumatherm
5 Place the front panel back to it place.
6 Connect the purge He tubing of sampler to the PURGE port of instrument
and He carrier tubing to the He or O2 port of instrument.
AIR N1 of the sampler connects to the AIR1 port near by the He or O
2
port
and AIR N2 to the second AIR2.
7.4. Installing the Co
2
adsorbers into the carousel
(If they are not installed)
Open the right section of instrument. To do so, lift the right front panel and remove
the panel.
New CO
2
adsorber tubes are closed airtight with gaps. Open the adsorber tubes
only immediately before installing into the carousel port, otherwise the flling of
tubes contaminated.
Fig. 7.4 The adsorber tube sealing elements layout
AtfrstinstalltheCO
2
adsorberintotheportrightfromthedegassingfurnace(fg.
5.3, pos. 3).
Portnumbersonthecarouselfttingsmustbesame.
Gently, put the sealing elements onto the tube in order shown at Fig. 7.4.
Putthetubeintothecarouselfttingswithutmostcare.Thetubemustsupportthe
fttings.Then,tightenthenutsfrmlytopreventanyleaks.
Turn carousel counter-clockwise 60 so that installed tube is parallel to partition
of instrument cabinet. Install the next tube as described above. Repeat it until all
adsorber tubes are installed.
Then turn carefully the carousel by steps of 60 one full round to check that all
tubes are installed correctly i.e. they dont touch the degassing furnace.
Incorrect installing of adsorber tubes can cause the cracking of tubes.
Place the right part of front panel back to its place.
O-Ring 7,94 x 1,78 mm
Distance spacer
O-Ring 7,94 x 1,78 mm
Back spacer
Nut M16
Quartz wool
Warnung vor
27
Dumatherm
7.5. Water trap packing
Dumatherm is shipped with packed water trap. After meaning several analysis
thistrappackingneedstobeexchanged.Infg.7.6.thepackingofthewatertrap
is described.
7.6. Starting the "Dumatherm Manager" software
1 Connect the mains cord plug of PC to mains socket 230 V AC 50/60 Hz.
2 Turn on the PC.
3 Install the software Dumatherm Manager as described in chapter "8.1. Soft-
ware installation" (if the software is not installed).
4 Switch one free COM-port or USB-port on window Select Serial Port on.
5 Connect the connector RS-232 on the rear panel of Dumatherm to chosen
for communication COM or USB ports of PC. Use the cables from Standard
OutftsKit.
6 Connect the mains cord plug of Dumatherm to mains socket 230 V AC 50/60
Hz.
7 Switch the DUMATHERM on.
8 Start the Dumatherm Manager software with double- click on the Dumatherm
Manager icon.
9 The PC displayed sheet ANALYSIS CONDITIONS" (see chapter 8.4.1.).
10 Check that on this sheet right from Method is Standby.
There must be following settings of operational parameters:
- Left Furnace - is switched off, set temperature 850 C
- Right Furnace - is switched off, set temperature 450 C
- Deg.Furnace - is switched off, set temperature 300 C
Flow rates:
- He I - set 40 sccm
- He II - set 0 sccm
- O
2
- set 0 sccm
11 Click on tab service and sheet SERVICE will open. In the box of right upper
corner of this sheet must run numbers and characters - this indicates that the
data communications between DUMATHERM and PC is working.
Quarz wool
Magnesium Perchlorate
Mg(CIO )
4 2
Quarz wool
Gas flow
Screw cap GL
Silicone seal GL
Fig. 7.5 packing of H
2
O
trap
28 Dumatherm
7.7. Heating up reactor tubes
Beforeheatingupthereactortubesafternewfllingtheventvalveafterreduction
reactor tube must be opened to avoid moistures to go in the measuring system.
For this open the menu Maintenance. Click with mouse left button to the button
VENT Closed changes to Open. Refresh on the Maintenance window Left
Reactor, Right Reactor, CO
2
Traps and Insert Runs data. If their packing is
changed to the new, packing formula must be inserted.
Now close the Maintenance window and open the sheet ANALYSIS CONDI-
TIONS. Check the boxes Left Furnace and Right Furnace. Heating of furnaces
is switched on. Click on the button WORK and Deg.Furnace switches on. HeI
Flow Rate changes to 190 and HeII Flow Rate changes to 200 sccm.
After 50 min, the instrument is ready - all values of current parameters are changed
from red to green.
7.8. Catalyst oxydation
After replacing the combustion reactor, the catalyst in the reactor tube
must be oxidised/ regenerated. In order to avoid the oxidation of the copper
in the second reactor, please make sure to open the quick tension lever on
the right front side (also see ill. 7.3. Installing the reactor tubes. This
way, the combustion gases are diverted into the ambient air. Please insert 3
new lines into the the sample table and insert 200 mg initial sample weight,
sample type "unknown" and category "user". In the software, you have to
switch over to the worksheet "analysis conditions" (see chapter 8.4.1.) and
amendtheoxygen-stoppingtimeto50s.Confrmthechangebypressing
"Send to Dumatherm". Start this series of 3 samples. Upon termination of the
series, the message "Analysis terminated".
Don't forget to close the quick tension lever at the bottom of the reaction
reaction. Open the menu 'Maintainance' and with the left key of you mouse
click on "Ventilation", the display "OFF" will switch to "ON".
7.9. Checking leak tightness
Dumathermhas2measuringdevisesforthegasfow.Oneinfrontoftheanalysis
area and one in front of the detector. The idea of the leakage test is to turn off the
secondfowcontrollerandthen,tomeasurethegasfowregulatedbythatone.
7.9.1. Leakage check in general
1. OnthesheetConditionsofanalysisyousetthefowspeedFC2to0.
2. ConfrmtheinputbypushingtheblinkingbuttonsendtoDumatherm.
3. Afterabout2minutescomparethecurrentvalueofthefowspeedatFC1
andFC2.Shouldthevaluesdiffermorethan5sccmthenyoumustfndthe
leaking spot with a leakage detector. Have you found the leakage, then, repair
the leakage.
7.9.2. Check the leakage tightness in the area of the CO
2
Adsorber.
1. Switch to the work sheet Service and click on turning of the carousel. This
way, the carousel is turned one position further. Wait about 3 minutes after
each turn and repeat the procedure 5 times altogether.
2. Switch to the work sheet Curve image and compare the level of the detector-
base line after each turn.
2
Dumatherm
3. ThesignalatthefowmeterFC2mustnotdeviatemorethan2ml/minafter
eachturnofthecarouselfromthepreviousvalue.Shouldthefowspeeddrop
to a value less than 190ml/min at this test, there might be a leaking spot at the
adsorberwhichwasjustchecked.IfthefowspeedatFC2shownatthistest
is higher than 190ml/min and if at the same time the signal of the detector is
also higher, then the adsorber needs degassing again
In the work sheet Conditions of the analysis you reset the FC2 fow speed
to 20 sccm again and click on the button Send to Dumatherm to confrm the
changes.
30 Dumatherm
8 Dumatherm Manager - Software description
8.1. SOFTWARE INSTALLATION
8.1.1. System requirements
The DUMATHERM Protein Analyzer has the following system requirements:
- CPU speed 2 GHz
- RAM 512 MB
- Free hard disk space 80 MB
- Operation system Windows XP
- Additional needed software Microsoft Excel
- Free ports 1 x RS 232, 1 x USB
- Monitor 17
- Printer A4 printer
8.1.2. Installation of the 'Dumatherm Manager' Software
1 Please make sure to close down all other programs prior to the installation in
order to avoid malfunctions.
2 The connection between the PC and the Dumatherm can either be established
with the RS 232 cable or the USB cable (it is of utmost importance that the
connection is established prior to the software installation!). When using
the connection with the USB cable you must install additional drivers in the PC.
OntheinstallationCDyouwillfndthedriverswhichareappropriateforthe
operating system as well as detailed information for the installation process.
3 The installation CD starts automatically when it is inserted into the CD-ROM
drive - if you have the function auto start activated on your PC. Alternatively,
youcanstartthefle'setup.exe'inthedirectory'DumathermManager'.
4 The dialogue will guide you through the installation. Just follow the directions
on your screen.
8.1.3. Removing the Dumatherm Manager Software
1 Click START, SETTINGS, CONTROL PANEL and ADD/ REMOVE PRO-
GRAMS.
2 Select Dumatherm Manager Software and click ADD/REMOVE
3 Confrmremoval.
8.2. GENERAL
The software Dumatherm Manager works in dialog mode windows. There you can
fndthepull-downmenusontheupperpartofmainwindow.Onthemainwindow,
you can select six sheets: ANALYSIS CONDITIONS, SAMPLE TABLE, PLOTS,
CALIBRATION, HISTORY and SERVICE. These sheets make it possible to
run all main operations needed for the analysis of samples.
On the lower part of the main window there is the status bar, where the current
phase of analysis and its duration are shown. The window title bar shows the
instrument name, model number and serial number.
8.2.1. Choose language
See chapter 8.3.4.12. "choose language"
31
Dumatherm
8.3. MENUS
To open a menu, click on it with the left mouse button or press the ALT-key and
underlined character simultaneously.
8.3.1. Category menu
Opens the samples Category table
Figure 8.3.1
The Category menu
In this table, samples (test substances) are grouped by an oxygen factor (i.e. the
oxygen amount in milliliters needed for a complete combustion of one milligram
of sample).
The oxygen factor is determined:
1 By calculation if the formula of the substance is known.
2 Experimentally if formula of substance is not known
Table description:
Category Name - designation of the samples category with similar combustion
conditions.
Description - short-list of characteristics and examples of samples in this ca-
tegory.
C Content - the range of carbon content in samples belonging to this catego-
ry.
O2 Factor [ml/mg] - oxygen amount in ml needed for full combustion of 1
mg sample. This is the most important characteristic of samples in a materials
group. The Dumatherm Manager determines the Oxy Stop Time according to
this amount.
max. sample weight [mg] - It follows from the maximum amount of O
2
from
400 ml/min and the category.
O2 Flow Rate [ml/ min] - recommended O2 fow rate for this category of
samples.
User can add or delete categories in this table using the buttons ADD CATEGORY
and DELETE CATEGORY. The user can also change the O2 Factor.
32 Dumatherm
8.3.2. Standard menu
Opens the Standard Table
In this table, the operator can see the standard materials used for calibration of the
instrument and their elemental composition. Using this data, the analyzer creates
the calibration curves used to determine the nitrogen concentration of unknown
samples.
The operator can add to or delete standard materials from this table using NEW
STANDARD and DELETE buttons.
8.3.3. Maintenance menu
Opens the maintainance table
The maintenance menu gives information when lifetime of reactor packing or
tube packing is over and has to be exchanged. After exchanging a packing click
refresh. Dumatherm Manager will count backwards from up to this date. The soft-
ware keeps track of the number of analyses performed on the Left (Combustion)
Reactor, Right (Reduction) Reactor, H
2
O Trap, CO
2
Adsorption Traps and
the Insert.
Packing - packing materials, amounts, order of packing etc.
Lifetime - maximum number of analyses each component can perform.
Runs Since Last Maintenance - number of analyses performed after the last
maintenance.
Runs to Warning Message - sets the number of analyses for a warning prior
to reaching the Lifetime of each analytical section.
The analyzer will display the message Left Reactor Packing has X Runs Left.
If the message is ignored and the analysis is continued, the message Packing
Lifetime Over is displayed. These messages do not stop the analytical cycle when
the set number of analysis is done.
Figure 8.3.2
Table with standard samples
and their nitrogen content
Figure 8.3.3
The maintenance menu
33
Dumatherm
REFRESH - the button refreshes data in column Runs Since Last Maintenance
and changes the old date to the current date. Press refresh when you've exchanged
reactor packings or also plain tubes.
The date when you've exchanged the reactor packing is shown right to the refresh
button. You can edit these settings according to the packing or other analysis
parameters.
Click on the "Restore factory settings" button to restore all factory set data.
Button "VENT" (On) - controls the valve to switch the output of RF (Reduction
Reactor) to measuring system or vent all gases out to atmosphere.
Closed Gases are sent to the measuring system (the valve EV2 is ener-
gized)
Open - Gases from RF are vented out (the valve EV2 is de-energized)
8.3.4. Tools menu
8.3.4.1. Lock Analyzer submenu
Opens the Password Dialog window
Choose this function to lock the program from unauthorized access.
Enter your password to unlock this function..
8.3.4.2. Change Password submenu
To change the password you will have to enter the master password and then
enter the new password twice.
8.3.4.3. Change Master Password submenu
Opens the Password Dialog Window
To change the master password you will have to enter the old master password
and then enter the new master password twice
8.3.4.4. Enable Grid Controls submenu
Enable Grid Controls is used to refresh the Grid Controls
8.3.4.5. Test dbase submenu
Operator can correct the collected databases.
8.3.4.6. Default Constants submenu
Opens Defaults Constants dialog where the basic constants and limits of the
instrument are defned. Also the user can select Documents Folders (Fig.
8.3.4.6).
Figure 8.3.4.1
The lock analyser submenu
34 Dumatherm
Figure 8.3.4.6
The default constants sub-
menu
The basic constants and limits are divided into three groups: Peak and Baseline,
Run and Varia.
1 "Peak and Baseline"- here the peak detection and measurement parame-
ters are set:
"Drift Limits" - if the drift of the TCD output voltage is less than this value the
instrument begins the analysis cycle.
"Begin Derivative" - if the derivative of the TCD output voltage exceeds this
value, the instrument begins the measurement of peak area. This value must
be positive.
"End Derivative" - if the derivative of TCD output voltage is negative and
lower than this value, the instrument ends the peak area measurement. The
instrument begins to check this value if the TCD output voltage differs from the
baselinevaluefxedatbeginningoftheanalysiscycleandiftheTCDoutput
voltage is less than the value determined by "Peak End Cap" setting.
"Blank Peak Min Area" - the minimum detected peak area if no weight is
entered for a sample on the SAMPLE TABLE sheet.
"Sample Peak Min Area" - the minimum detected sample peak area for
samples where weight is entered on the SAMPLE TABLE sheet.
"Peak Waiting Time" - time from the end of Oxy Stop Time to the beginning
of the integration. The integration must begin before the real peak begins.
2 "Run"- this group determines the general limits and special working
modes of the instrument:
35
Dumatherm
"Delay Between Samples" - the minimum time between the two analyses
cycles. If the TCD output voltage drift exceeds the Drift Limits then this du-
ration is longer.
"Leakage Test" - if this box is checked, the instrument checks for leaks after
the START button is pressed on SAMPLE TABLE sheet. The instrument
comparesthefowratesofHeIandHeII(thesettingofHeIIduringleakage
testiszeroandHeIIMFCworksasmassfowmeter).Ifthesetwofowrates
differ more than the Leakage Cap, then the message Leakage Error is
displayed.Thenanalysisstopsandtheoperatormustfndandeliminatethe
leak.
You can of course set the HeII on sheet "ANALYSIS CONDITIONS" to zero
andcomparethenHIandHeII.Ifthedifferenceofthesefowratesexceeds
"Leakage Cap" then there is a leak in the instrument.
3 "Varia"-group determines the limits and constants of measurement in
the analysis cycle:
"Min Oxy Time" - the minimum O
2
dosing time. O
2
volume is the minimum
needed for combustion of a tin capsule. The instrument sets this time auto-
matically when no sample weight is entered (Blank and Empty).
"Increased He"-HefowratebywhichtheHefowisincreasedafterchanging
thegasfowfromO
2
to He through the combustion reactor.
"Pressure Offset" - The pressure difference in the analysis system from the
pressure that was set at the beginning of analysis cycle, and determines the
end of the increased He time. This pressure is measured before the combustion
reactor.
"TCD Raw Data Saving Interval" - there are two radio buttons ("0,2 s" and
"1s"). Using these radio buttons operator can save all measured values of TCD
outputvoltage(0,2s)oronlyeachffth(1s).
8.3.4.7. View Current Logbook submenu
Opens the Logbook, where user can observe the sequence of the main measu-
rement process commands. This logbook describes the analysis or analyses cycle.
This logbook is displayed until the next START command (Fig. 21).
Figure 8.3.4.7
View current Loogbook sub-
menu
3 Dumatherm
8.3.4.8. Balance Type submenu
Opens the list of choices to select the weighing mode and type of balances, if they
areconnectedtothePC(seefg.8.3.4.8)
8.3.4.9. Change Communication Port submenu
To change communication port, restart program and switch on communication port
on window Select Instruments Serial Port.
8.3.4.10. Excel Documents Protected
Excel Documents Protected can switch on/off only Master. For this he must enter
Master Password and click on list of tools submenus on Excel Documents Protected
and protection switches on/off. At access level Operator the name of Submenu is
grey and the operator cant switch Protection on/off.
Figure 8.3.4.8
View current Loogbook sub-
menu
8.3.4.11. Balance Type
None - operator enters the sample weights manually using the keyboard.
Gibertini Crystal 100 the sample weights are transferred using RS 232 I/O com-
munication between the Balance and PC.
Sartorius the sample weights are transferred using RS-232 I/O communication
between Sartorius M2P Balance and PC.
8.3.4.12. Choose language
Choose between german and english language
8.3.5. Help menu
8.3.5.1. About submenu
Opens the window Dumatherm.
This window gives to user the information about the Software Version, Hardware
Version, Hardware Serial Number etc.
Use this information for checking right version of hardware and software!
Figure 8.3.5
The Help menu
37
Dumatherm
8.4. Sheets
8.4.1. Analysis conditions
This sheet appears on the screen after the Dumatherm Manager software has
been started.
On this sheet, the operator can set general data and main operational parameters
of the instrument and choose the working modes:
8.4.1.1. "Operator"
Enter the operator name.
8.4.1.2. "Method"
List of methods, which differ by operational parameters of instrument.
Click on the desired method and the window "Information" will open. To look the
chosen method, click on "Yes". The button "Send to Instrument" starts to blink and
under the button appears "Instrument Worked With Method: xxxxx".
This way, the operator can look at several methods. To change the method, the
operator must click "Yes" and then click on button "Send to Instrument" and in-
strument works with selected method.
Figure 8.4.1.
The Start-window
38 Dumatherm
To add new method to the list of methods, click with your right mouse button on
Method window. A list of choices will open.
"New Method" - you can enter the new method with new operational parame-
ters. Click on it with the left mouse button and open the window Enter Method
Name.
Print the name of new method, and click OK. Open the window "Enter Sample
Table Name". Print new sample table name and then click OK. Button "Send to
Instrument" begins to blink and under the button you see "Instrument Worked with
method: xxx". Enter the new operational parameters on the sheet "ANALYSIS
CONDITIONS" and click on button "SEND TO INSTRUMENT". The new method
is entered. The SAMPLE TABLE sheet of the entered method is empty i.e. begins
from the row no 1. If the operator does not enter the new parameters, but clicks on
button "Send to Instrument" the new method has the factory default parameters,
but the new name and an empty Sample Table with a new name.
"Copy Method" - you can enter the Method with the same operational parameters,
but with a new name and an empty "SAMPLE TABLE" with a new name. Click
on it, print the new method name and click OK. Then print the new sample table
name and click on button Send to Instrument.
"Delete Method" - you can delete the method from list of choice and the "SAMPLE
TABLE" of this method. Measurement results from "SAMPLE TABLE" are stored
in "HISTORY". Click on Delete Method in list of choice, click "Yes" and click on
button "Send to Instrument".
Attention: Calibration and sample measurement must be done under the same
measurement conditions i.e. the method for calibration and for measurement must
be the same.
8.4.1.3. "Send to instrument"
Click this button to send data to instrument.
This can be operational parameters, selected method, a new method, a copied or
deletedmethodasdescribedabove.Operationalparametersaregroupedintofve
panels - some of them are only informative (Pressure and Detector).
Panel 1 - Temperatures - there are three columns of temperature values:
"Range" - the ranges of working temperatures;
"Set" - textboxes where operator can see or write the desired working tempe-
rature;
Current - the real temperatures of furnaces.
If the numbers of the current temperature are red, the temperature is out of
operational range. If temperature is within the operational range the numbers
are green. The colour change is synchronous with the colour change of LEDs
on the front panel. To switch the furnace on/off, the operator can click on the
corresponding checkbox.

"Left Furnace" (LF) - temperature of combustion furnace.
3
Dumatherm
"Right Furnace" (RF) - temperature of reduction furnace.
"Deg.Furnace" - temperature of degassing furnace. In this furnace the adsor-
bedCO2isdesorbedfromadsorbentatanelevatedtemperatureinHefow.
Three adsorber tubes are degassed simultaneously.
"Detector" - temperature of measuring TCD. This temperature is factory
set.
Panel 2 - Pressure
"System" pressure measured at the carrier gas input port of autosampler. If
the current pressure is in the allowed range of 900-1300 mbar the numbers of
current pressure are written in green. If the current pressure is higher than 1300
mbar the numbers become red and the instrument will not start. If the pressure
exceeds 1500 mbar, He II and He Degas are switched off automatically.
Panel 3 - Flow Rates-theoperatorcansetthreefowrates:
"He I"-carriergasfowrate;
"He II"(HeII>HeI)-carriergasfowratetostabilizefowthroughTCD(HeI
+additional He);
"O2"-oxygenfowrateforcombustion(recommendedO
2
fowratesareshown
in table category);
"Purge Air"-AftercheckingthisapurgeairfowthroughthePermaPureGas
Dryerwillstartwiththesetfowrate.Thefowrateofpurgeair(additionalto
He purge) is factory set to 200 ml/min. Purge air has to be checked when big
sample or samples with high water content are measured.
Panel 4 - Times - the meaning of columns is the same as at Temperatures.
"Sample Delay" - this delay is the time needed by the oxygen gas to arrive
into the combustion reactor (LF) before the autosampler is activated and the
sample drops into the reactor. This time depends on the O
2
fowrate.Theope-
rator can set the delay time in a range of 1 99 s e.g. for O
2
~ 400 sccm the
sample delay time is recommended 6-7 s.
"Sample Stop" - it is the time needed to terminate the activation of the au-
tosampler. It must be longer than the sample delay time for up to 3-4 s and less
than 100 s (3 - 4 s is most recommended difference between sample delay
and sample stop times). This time has no analytical effect, but determines the
time during which the combustion is seen through the window of pneumatic
autosampler. At the end of this time the piston of the autosampler goes back
andthesampletrayturnstothenextposition.Theremustbethesuffcient
time from the sample stop to the beginning of a new analysis cycle to purge
the new sample with He.
"Oxy stop" - this is the entire time during which the solenoid valves are swit-
ched to oxygen for the combustion of samples in the left furnance. This time
must be enough to achieve a complete combustion of samples.
InstrumentcalculatesOxyStoptimebyformula:
[s]
40 Dumatherm
"Oxy Stop" time also can be set by the operator. For this open the list of choices
"Category" on the sheet "SAMPLE TABLE" and choose the category Customer
(See the chapter "SAMPLE TABLE" column "Category").
"Run" - this is time from the beginning of one cycle to the end of this cycle.
Usually it must be app. 30 sec longer, than the expected end of peak integra-
tion.
"Auto" - is used for shortening "Run" time. If Auto is checked the analysis cycle
of one sample ends when the integration of peak ends, but not lasts longer
than set Run time if peak was not detected.
"Current" - shows the length of last cycle.
Panel 5 - Detector - there, the operator can see the current parameters of peaks
measurement and integration during the cycle:
"Voltage [V]" - output signal of TCD;
"Baseline [V]"-TCDoutputvoltagefxedatthecyclebeginning.
"Peak [V]" - peak running value (Peak = Voltage - Baseline).
"Drift [mV/min]" - characteristics of peaks used for peak integration,
"Derivative [mV/s]" - characteristics of peaks used for peak integration.
"Peak Area [mV/s]" - peak area integrated for last measured sample. Changes
to zero at the beginning of next cycle;
"Peak Height [V]" - last measured peak height.
8.4.1.4. WORK
Click on this button switches instrument from Standby to Work mode and LED
STANDBY turns off.
8.4.1.5. STANDBY
Click on this button instrument switches to standby condition i.e. the LF and RF
temperaturesdecrease,degassingfurnaceswitchesoffandtheHecarrierfowrate
decreases. Also switch off He Purge, Purge Air and He Degas. In Standby
mode the list of Methods changes to Standby.
8.4.1.6. "Wake up
On this panel operator can set the date and time when instrument automatically
goes from Standby to Work mode. For this, click with the left button of your
mouse in checkbox.
Figure 8.4.1.6
Set Wake Up Date and Time
41
Dumatherm
8.4.2. "Sample Table"
The "Sample Table" of analytical method contains all information concerning the
seriesofsamplestobeacquiredandprocessed(seefg.8.4.2.).
On this sheet the operator enters the data of samples which must be analysed,
starts analysis, stops analysis, gets the analyses results etc.
Each row correspond to one sample. Date and Time gives you the information
when the sample was analysed.
"Working Method" - is entered on sheet ANALYSIS CONDITIONS.
"Sample Table" using this combo box operator can:
Clicking with left button of mouse on the combo box Sample Table the list of Samp-
le Tables opens and the operator can choose needed for him Sample Table
Clicking with the right mouse button on the combo box "Sample Table", a list of
options will be shown.
Figure 8.4.2.
Sample table
42 Dumatherm
To "Add New Sample Table" or "Rename Current Sample Table" click on the
needed option. The following window will open:
Type the new name and click "OK" or click "Cancel" to go back.
To Remove Current Sample Table click on this option the and "Sample Table
will be removed.
"Working Calibration" - is entered on the sheet CALIBRATION by clicking with
right mouse button on the calibration table row, where the most suited calibration
for this sample is located.
8.4.2.1. Sample analysis
The start and end numbers of samples in analyses series operator enters into
textboxes:
- Start Row:
- End Row:
The same operation can be done by clicking the right button of the mouse or click
ontherowwhereisthefrstnotanalysedsample.Opensthelistofchoices
Click on Set Start Sample # using the left mouse button. Then click with the right
button of the mouse on the end row and click on Set End Sample #.
By clicking on Balance the operator can enter the sample weight into the SAMPLE
TABLE using the communication between balance and PC.
With the item Adjust Calibration the operator can correct analysis results via cor-
rection factor. For this operator chooses row or rows where are measured standard
material samples (shift key +mouse left button). Clicking on item Adjust Calibration
opens the window Select Standard to Adjust Calibration, where operator chooses
marked standard material name. Click OK and nitrogen [%] is corrected by the
correction factor. If the operator marked several rows for correction, the correction
factor value is calculated as the average value. The calculated value of correction
factor is written in the column Correction Factor of the calibration curves table.
With item Add Current Point to Calibration, the operator can add to calibration
curve suitable for him standard material measurement result from the Sample Ta-
ble. If the standard material is measured as unknown, operator must change the
type unknown to standard. Then, the operator marks the row (shift key +mouse
left button) and clicks on item Add Current Point to Calibration.Afterconfrming
by clicking OK, the window Select Standard for Calibration Point Adding opens
where the operator chooses the marked row of Sample Table Calibration material
43
Dumatherm
name. Then click OK and the marked point will be added to the calibration curve.
With items Copy Field and Paste Fieldtheoperatorcancopymarkedfelds
from one row to other rows.
"Current Row" - gives the number of sample that is analysed at this moment. If
the cycle is ended, the last analysed sample number will be displayed.
If the checkbox Standby After Last Sample is checked, then the instrument turns
to the Standby mode after the analysis of the last sample.
If the checkbox He Saving Mode after Last Sample is checked, then the instru-
mentaftertheanalysisoflastsampledecreasestheHefowratei.e.goestoHe
Saving Mode. On He Saving Mode After Last Sample unlike from Standby mode,
the temperatures of the furnaces are not decreased.
"Start" a click on this button starts the analysis of samples.
"Stop" a click on this button stops the analysis of samples but the analysis of
the current sample completed.
"Add Sample" - by click on this button, the operator can add row i.e. sample into
the SAMPLE TABLE.
"Remove Sample" - to remove row mark it and then click on this button.
8.4.2.2. Description of the table
Each row in the SAMPLE TABLE contains both the information entered by ope-
rator and the analysis results of one sample.
Columns: Weight [mg], Sample Name, Submitter, Type, Standard Name,
Protein Factor Category and Moisture contain sample initial data entered by
operator.
Weight [mg] - is entered manually or using the balances data interface. The
weighing technology is described in the chapter 9.5.
Submitter - operator enters the origin of sample.
Type click with left mouse button on a row to open list of choice.
- Unknown - choose when unknown sample is analysed.
- Blank - choose when the Weight [mg] is not entered. The result of the measu-
rementofthelastblankisfxedonthecalibrationtableontherow#0.
- Bypass - this type of samples is used to condition the analysis system.
- New Calibration from this point (row ) without sample starts a new calibra-
tioncurvemeasurement.Theresultofthismeasurementisintherow#1of
calibration curve table.
- Standard - adds a new point to the existing calibration.
44 Dumatherm
If category Customer is chosen, then operator can enter on sheet ANALYSIS CON-
DITIONS Oxy Stop time manually. At other choices, the instrument determines
the Oxy Stop time by O
2
factor in submenu Category and by sample weight. For
Empty and Blank samples (sample weight is 0) - the Oxy Stop time is 6 s i.e.
the factory set as default.
"Protein Factor" - operator can edit if it is needed according to the properties of
the sample.
"Calibr.Number"-isthesameasWorkingCalibration.Thiscolumnisflledin
via software.
"Standard Name" - if on the column Type is chosen Standard or New Cali-
bration, a click on the column Standard Name opens the list of choices and
operator can select the standard needed.
"Moisture %" - the real % of moisture in sample. With this value the software
calculates the % nitrogen with regard to the given % of moisture.
"Commentary" - to open the "MEMO" window the operator must double click on
the row selected. Here, the operator can type a most detailed description of the
sample or other important information about the sample. Commentaries must
be entered before sample analysis is done.
"Operator" - is entered on sheet ANALYSIS CONDITIONS
"Date", "Time", "N Area [mVs]", "N [%]", "Prot [%]" and "N Weight [mg]"
areflledinviasoftwarewhenanalysisisdone.
Below the table are navigators. From left to right they are:
-movetofrstrecord
- move backward 10 records
- move to previous record
- move to next record
- move forward 10 records
- move to last record
Category - the click with mouse right button opens the list of choices:
45
Dumatherm
8.4.3. Calibration
The DUMATHERM Protein Analyzer does not perform absolute measurements
i.e. the relationship between the N contents and the measured N values (detec-
tor response) must be calculated by means of calibration curves. To obtain the
calibration curve, the substances with known N content (standard materials) are
analysed with different sample weights. To perform these analysis, use the sheet
SAMPLETABLE.Togettheanalysisresultasnewcalibrationchoosethefrst
point in column Type of SAMPLE TABLE the New Calibration. If the operator
wants to add calibration points to existing calibration curve the operator chooses in
column Type of sheet SAMPLE TABLE the Standard or chooses add Current
Point to Calibration. The software Dumatherm Manager computes calibration
functions (polynomial up to third degree) or linear calibration.
A faultless calibration of the analyzer covering the whole working range is of crucial
importance for the accuracy of all later analysis results. Therefore the calibration
procedures must be carried out with the utmost care. Therefore, the operator must
run some bypass and blank analyses until the results stabilized.
The software Dumatherm Manager calculates the concentration of nitrogen, on
the appropriate sample basis, as follows:
[%]
where:
A = the percent of the nitrogen in the sample, mass %
B = the detector response for nitrogen in the sample minus response from blank
(row#0)
C = the detector response for nitrogen in the standard minus response from blank
(row#1)
D = the mass of the sample, m
E = the mass of the standard, mg
F = the percent of nitrogen in the standard, mass %
4 Dumatherm
All measured points of calibration curve are automatically saved on the sheet
CALIBRATION(seefg.8.4.3.).Operatorcantheredooperationswithcalibration
curves:changecurvefttypes,addorremovepointsetc.
On this sheet there are two tables:
In the right table are all calibration curves that are saved in the analyzer and the
operator can use them for the analyses of samples;
In the left table are the calibration curve measurement results by points selected
by the operator.
8.4.3.1. Right Table.
In each row of this table are main characteristics of one calibration curve saved
in analyzer:

Cal # - calibration number;
Method - method, which is used for measuring of this calibration curve.
Date, Time - date and time when this calibration was performed.
Fit Type-calibrationcurvefttypechosenfromlistCurveFitType:Linear,"
Quadratic and Cubic.
Compute Curve - indicates the calibration curve calculation mode.
A0, A1, A2, A3-polynomialcoeffcientscomputedfromthecalibration
curve.
Correction Factor - the factor by which the analyses results is corrected.
Instrument Number - indicates the instrument where this calibration curve was
measured.
Figure 8.4.3.
Calibration
47
Dumatherm
Figure 8.4.3.1
Right table
For working with calibration curves in this table you can click with the right button
of the mouse to row needed.
- Remove Selected Calibration - you can remove the calibration curve from
the table.
- Copy Current Calibration - you can copy the calibration curve. This is needed
when you want to change something in this calibration curve, but want to store
the initial calibration curve in this table.
- Set Current Calibration As Working - you want to perform analysis of samples
with this calibration curve.
- Undo Adjustment Calibration - cancels corrections made with this calibration
curve and restore the primary calibration curve.
To measure the new calibration curve you must choose in column Type (on the
SAMPLE TABLE) the submenu New Calibration.
If you choose in this column Standard then you can add the point or points to this
calibration curve (what is as working).
On the right side of this table are navigators of table. The meaning of these navi-
gators is same as on sheet SAMPLE TABLE.
8.4.3.2. Left table
On the sheet CALIBRATION, the measurement points parameters of chosen
calibration curve are shown. This table contains max. 20 rows i.e. measurement
points:
# - Measurement point number: First point (row) is always reserved for the last
measured blank. Second point (row) is always the blank measured before new
Figure 8.4.3,2.
Left table
48 Dumatherm
calibration. For this you choose on sheet SAMPLE TABLE type New Calibration
and a empty capsule must be measured as a sample. If on the sheet SAMPLE
TABLEischosenTypeUnknown,theinstrumentusestheblankvaluefromfrst
row of the Left Table from the sheet CALIBRATION as the sample measurements.
If after calibration curve measurements are not blank measurements, instrument
uses calibration blank from second row i.e. calibration measurement blank.
Sample Weight [mg] - sample weight in mg to get this calibration curve point
and is entered on the sheet SAMPLE TABLE.
Nitrogen Weight [mg] - nitrogen weight in mg of this sample, calculated from
given nitrogen content in this standard material.
Area [mVs] - integrated nitrogen peak area in mVs for this sample weight.
By click with mouse right button on this table you can use Add Point or Remove
Point to add or remove rows in this table.
8.4.3.3. Polynominal
Below right table are parameters of polynomial Polynomial
Curve Fit Type - opens the list of choices (Fig 44) for correcting the calibration
curve:
Compute Curve - opens the list of choices (Fig. 45 ) to choose calibration curve
calculation modes.
Belowthiscomboboxthepolynomialcoeffcientsforcomputingcalibrationcurve
are given.
On the right lower corner of panel Polynomial is given the calibration curve cor-
relationcoeffcient-R2.
Calibration curve
At the lower right part of the "Calibration" window is the calibration curve in gra-
phical form.
4
Dumatherm
8.4.4. History
On this sheet the results of all performed analyses are stored. Here you can create
reports as documents.
8.4.4.1. Description of the history table
All results are presented, as table where in each row are the results of one sample
analysis sample. In columns are samples data, analysis results, and operational
parameters during analysis etc
For Example:
Category - the oxygen factor what is used for calculating the Oxy Stop time.
Nitrogen Area [mVs] - integrated area of nitrogen peak in mVs for this
sample.
Nitrogen Weight [mg] - nitrogen content in mg in this sample calculated from
Nitrogen Area and Calibration.
Nitrogen [%] - nitrogen content in percents in this sample.
Standard Name - standard material name for this calibration.
Calibration Number - calibration number on sheet CALIBRATION used for
calculating Nitrogen Weight [mg], i.e. working calibration.
Curve Fit Type - used for measurement of this sample calibration curve ft
type.
Compute Curve - used for measurement of this sample calibration curve cal-
culation mode.
Correction Factor - factor is used to correct measurement results.
Figure 8.4.4.
History
50 Dumatherm
Method - the method used for the analysis of this sample.
HeI Flow [sccm]-carriergas(He)fowrateinsccm.
O2 Flow [sccm]-oxygenfowrateforfullcombustionofthissampleinsccm.
HeII Flow [sccm] - He fow rate in sccm to stabilize the fow rate through
TCD.
Oxy Stop [s], Sample Delay [s], Sample Stop [s] - analysis cycle timing
parameters. More detailed see chapter 9.4.1. ANALYSIS CONDITIONS.
Autorun - if on sheet ANALYSIS CONDITIONS is checked checkbox Auto
there is Yes, if unchecked No.
Analysis Time [s] - duration of this sample analysis cycle in s.
Adsorber Number carousel port number used for measurement of this
sample.
Instrument Number instrument number where was measured this sample.
Commentary ( Memo) mouse left button double click opens window Com-
ment where are the commentaries entered on sheet Sample Table. Operator
can there complement commentaries.
Logbook (Memo) - mouse left button double click on the marked row opens
window Logbook where are the sequence of the main measurement commands
of this sample.
The mouse right button click on the table of sheet History opens the list of con-
text menus.
"Select all" - click on this context menu selects all rows that are in the table on
sheet History at this moment. Use this to copy or move to archive or delete the
tableorflteredpartoftable.
"Unselect All" - unselects all marked parts of table.
"Delete" - deletes all marked parts of table.
"Recalculate"-opensthewindowRecalculatedResults(seefg.8.4.4.2.).
Figure 8.4.4.1
List of context menus
51
Dumatherm
For recalculating results, click on the sample row to mark the samples to recalcu-
late in table "History".
Open the window "Recalculated Results", type the new calibration number and
click on button "Recalculate". If the results are satisfactory click "Save" and the
newly calculated results are transferred to the table History. Recalculated results
of analyses of types Blank, New Calibration and Standard are transferred
to the table Calibration Curve on the left side of the sheet Calibration.
For reintegrating, mark the row on the table History, mark the new beginning
and end points of integration on the plot, click the button Reintegrate and you
will see the newly reintegrated Nitrogen Area. Click Recalculate and you obtain
new results. If it is necessary, the operator can repeat these operations until he
fndstheresultsatisfactory.
Export Raw Data opens window Save Raw Data. The operator can give
thenametotheflewithrawdataofthisanalysis.Theoperatorcanselectraw
data saving interval on the window Defaults Constants.
8.4.4.2. Create Document
If the samples names are same, instrument creates the report of repeatability test
for this substance.
if the samples names are different, instrument creates report of this sample
group.
Figure 8.4.4.2.
Recalculated results
52 Dumatherm
8.4.4.3. Create Document for each Row
You can create the report of one analysis cycle (one sample) results.
Figure 8.4.4.4
Create Document for each
Row
Figure 8.4.4.3.
Create Document
Version 19.08.2005
o
C s
o
C s
o
C
sccm
sccm
sccm
Average
Standard Deviation
Dumatherm Nitrogen / Protein Analyser
B 1,3 6,25 8,236E+00
Date Time Protein
factor
Sample name
0,43
31,16
0,022 0,13
0,434
4,985
Protein
[%]
Category
4,989 3,492E+04 31,18
Peak Area
[mV*s]
Nitrogen
[%]
N Weight
[mg]
Standard name Weight
[mg]
14 (Cubic, Without Zero )
Sample Table :
650 Reduction Reactor
5
Factory
28.03.2007 17:57:43 1546
Degassing Oven
28.03.2007
Analysis Conditions for Method :
1030
Temperatures:
17:52:53 1546
Calibration # :
Combustion Reactor
299
O
2
294
He II 200
He I 195
Flow Rates:
Auto
9
Proben Maerz 2007
Times:
Sample Delay
Sample Stop
Run Time
RSD [%]
Serial Number :
Software Version:
19
DUMATHERM MANAGER V2.04d
CGe France
Kueppers
Submitter:
Operator:
165,100
151,800 B 1,3 6,25 3,184E+04 7,529E+00 4,960 31,00
28.03.2007 18:03:06 1546 159,300 B 1,3 6,25 3,358E+04 7,929E+00 4,977 31,11
28.03.2007 18:08:06 1546 154,700 B 1,3 6,25 3,286E+04 7,764E+00 5,019 31,37
28.03.2007 18:12:59 1546 160,400 7,990E+00 4,981 31,13 B 1,3 6,25 3,384E+04
Version 19.08.2005
019
99,000 mg
9,590 %
0,000
0,000 %
0 0,003
9 -0,069
19 -0,016
29 0,007
38 0,007
48 0,007
58 0,007
67 0,007
77 0,006
87 0,010
96 1,597
106 2,039
116 0,374
125 0,049
135 0,018
145 0,013
154 0,011
164 0,010
174 0,009
183 0,009
193 0,009
203 0,008
1030
o
C 5 s
650
o
C 9 s
299
o
C 20 s
218 s
195
200
400
Dumatherm Nitrogen / Protein Analyser
Analysis Time :
Sample Delay
Sample Stop
Sample Table: Proben Maerz 2007
Combustion Reactor
Temperatures:
Standard:
Category:
O
2
He I
He II
Flow Rates:
Reduction Reactor
Degassing Oven
A 1,0
Times:
sccm
Analysis Conditions for Method: Factory
Calibration # :
Protein Factor :
Protein :
14 (Cubic, Without Zero )
Kueppers
Nitrogen :
Date : 29.03.2007
Serial Number :
Sample Weight :
Sample ID : EDTA
Software Version : DUMATHERM MANAGER V2.04d
14:38:06
Submitter :
Operator :
sccm
sccm
Oxy Stop
Run Time
-0,5
0,0
0,5
1,0
1,5
2,0
2,5
0 50 100 150 200 250
Time [s]
S
i
g
n
a
l

o
u
t
p
u
t

[
V
]
53
Dumatherm
For creating reports, the operator must mark the row or rows where are the data
of sample or samples to be in report using button Shift of keyboard and click
with the left button of the mouse on the corresponding button. Reports are created
in excel format.
8.4.4.4. Filter
The button Filter opens the window "History Database Filter", to group the
analysisresultsbyfeldscharacterizingthedifferentofsamplesoranalysespa-
rameters.TheflteringfeldsarethecolumnsoftableonsheetHISTORY.The
flteringresultisthetablewheretheanalysisresultswithcharacteristicschosen
byoperatorfeld(s)arelocated.Theoperatorcanflternottheallfeld,butonly
thepartofthefeldheisinterestedin.Thismustbedonestep-by-stepfrstflter
thelargerfeldandthenspecifythefeldbysteps.
8.4.4.5. Copy to Archive
Mark the desired part on the table. Click on the button and the marked part of the
table is copied to archive. This part remains in the table on sheet HISTORY.
8.4.4.6. Move to Archive
Mark the desired part in the table. Click on the button and the marked part is sanded
to archive. This part doesnt remain in the table on sheet HISTORY.
8.4.4.7. View Archive
Usingthisbuttonyoucanobservethearchivefles.Clickonthisbuttonopensthe
ArchiveFilesCatalogue.Openthenecessaryforyourfle.Whenthefleopens
thetabHISTORYchangestotabwhereischosenbyyouarchiveflename.Simul-
taneously the button changes to CLOSE button. Other archive buttons changed
from black to grey. Click on button CLOSE closed the Archive File and the sheet
HISTORY is again in usual form.
In the lower right corner of the sheet is the marked sample nitrogen peak graphical
image. Left from the plot are pointer x and y coordinates on the plots area. Operator
can zoom this plot. For this use keyboard Shift button and mark the area to zoom
with pointer and mouse left button. To zoom out, use keyboard button r .
Figure 8.4.4.5
History Database Filter
54 Dumatherm
8.4.5. Plots
The sheet PLOTS opens by click on tab PLOTS.
The analysis run and the current values of parameters are displayed there in graphi-
cal form. At the same time, plots of two parameters selected from list Check Charts
Channel that opens by clicking on the right button of mouse can be displayed.
SCALE button - centres the graph on graph area.
UNDO button - reverses the last action (scale).
ZOOM buttons - on both sides of graphs feld zooms out or in the graphs va-
lues.
Numbers at the top corners indicates the current value of corresponding graph.
Under the graph area are navigator and ZOOM buttons.
Functions of these buttons are from left to right are:
- move to the beginning of graph
- move to prior page
- move to next page
- move to the end of graph
Numbers at the top corners indicates the current value of corresponding graph.
Under the graph area are navigator and ZOOM buttons.
Right from navigators are ZOOM OUT and ZOOM IN buttons for Time scale.
PRINT button - the operator can print out the plots. After clicking on the button
PRINT the standard Windows Print dialog opens. After that, the background of
print out area changes from yellow to white.
At right lower corner of graphs area are the current value of Detector Drift in
mV/min and the area of last nitrogen peak - Peak Area in mVs.
Enable Chart Control Property - if this checkbox is checked, operator can
open window Chart Control Properties. If this checkbox is unchecked opens
only list Check Chart Channel.
Figure 8.4.5.
Sheet Plots
Figure:
Check Charts Channel
55
Dumatherm
8.4.6. Service
Attention! This sheet is used for analyzer manual control functions! MAKE SURE
TO USE IT ONLY FOR SERVICE OR TROUBLESHOOTING!
Never change any settings on this sheet during analysis cycles as it will interrupt
the analysis cycle or can even damage the instrument!
This sheet opens with click on tab "SERVICE"
8.4.6.1. Carousel
Carousel - used for loading CO
2
adsorber tubes into the carousel and checking
thecarouselstepscorrectfxing.
Position - indicates the carousel port in measuring position.
ROTATE button - click on this button turns carousel one-step counter- counter
clockwise by 60. If you rotate carousel manually (rotate only counter clockwise)
take care that you stop the moving carousel ports with same numbers are in
measuring position i.e. Position has indication. For indicating position on manual
turning the checkbox Send Position must be checked.
If you put carousel between two positions gas lines in the switching valve of ca-
rousel are closed, pressure increases and reactor tubes can break.
8.4.6.2. Indications of current operational parameters
These are the indications of current operational parameters of analyzer.
Checkboxes left from indications switch on/off the data sending from analyzer
controller board to PC.
Det.Temp. - TCD drum temperature in C.
N-Det.Data - output voltage of measuring TCD in V.
Figure 8.4.6.
Sheet Service
5 Dumatherm
LF Temp. - combustion reactor temperature in C.
RF Temp. - reduction reactor temperature in C.
DGF Temp. - CO2 adsorbent degassing furnace temperature in C.
Pressure - working pressure in mbars in measuring system. This pressure
measured at the inlet of combustion reactor.
CJ Temp. - LF and RF thermocouples cold junctions temperature in C.
Transf.Temp. - outer surface temperature of power supply mains transformer
in C.
Checkbox Sending - switches on/off all temperature and pressure data sending
toPC.Alsoswitchedon/offdatasendingoftwofowrates.
FC1 (He or O2) Flow-massfowcontroller(MFC)forcontrollinggasfowrates
through the reactors. (Reference designators for MFC-s and Valves are the desi-
gnators from Fluidic Part Schematic Diagram 4040.00.000FD version N).
FC2 (He) Flow-MFCforcontrollingadditionalHefow.
Flow rates you can set in corresponding textboxes. Flow rates switched on/off by
checkboxesrightfromtextboxes.Indicationsofsetfowratesareleftfromtextbox
and can switch on/off by adjacent checkboxes.
8.4.6.3. Valve State
Operator can use these buttons switch on/off all solenoid valves and some other
electric components. Right from Buttons is Valves state, left valve, controlling
this function.
He Purge -valveEV1,switcheson/offHefowforpurgingsamplesinautosamp-
ler.Factorysetfowrateis60-70ml/min.
O
2
- valve EV3, switches on/off oxygen for combustion the sample.
He or O
2
-valveEV4,turnsovertheHeliumandOxygenfowintothecombustion
reactor.WhenvalveisdeactivatedthenHefowisopened.
He Degas Gas-valveEV5,switcheson/offtheHeliumfowfordegassingthe
CO
2
adsorbentindegassingfurnace.Factorysetfowrateis50-60ml/min.
Carousel - valve EV6, switches on/off the compr.air/industrial N2 for turning
carousel.
AS Backward - valve EV7, switches on/off the compr.air/industrial N2 to move
the Autosampler main piston backward and turn the tray.
AS Forward - valve EV8, switches on/off the compr.air/industrial N2 to move the
Autosampler main piston forward (sample drops into combustion reactor).
Purge Air - valve EV9, switches on/off the compr.air/industrial N2 to purge the
GasDryer.Factorysetfowrateis200ml/min.
Vent - valve EV2; turn over the reduction reactor outlet from Vent to Gas Dryer,
wheninstrumentisswitchedon.Alsousedtoventreductionreactorafterflling
with new packing.
57
Dumatherm
Relay1,3, Relay2 - relays switched the power on LF and RF on/off.
Ads.Fan - switches the CO2 adsorption tubes cooling fan on/off.
Peep - switches the sound signal (PEEP) on/off.
8.4.6.4. Communication boxes
On the right edge of sheet there are two boxes.
On the upper side, you see the data communication from analyzer controller
board to PC. This data communication switched on/off by checkbox Sending. By
choice you can switch on/off the data sending using adjacent to every indication
checkbox.
In the lower box, you see the sending of commands from PC to analyzer control-
ler board. You can switch on/off this communication using the checkbox Send
Commands.
8.4.6.5. Manual Control
Click with right button of mouse opens the choice (Fig 8.4.6.5)
TheoperatorcanrecalibratePressureSensorandsetzerofowcontrollersFC1
andFC2.Inordertostarttheseprocedures-theremustbenogasfowinthe
system. Also, the operator can start Leakage Test or stop it.
8.4.6.6. User access level
Below the Valve State panel, there are user access levels. User: OPERATOR
or user: MASTER.
Access level OPERATOR enables all operations needed for samples measu-
rement and treating measurement results, excepted changing following working
parameters of instrument: LF, RF and degassing furnace temperatures; HeI, HeII
andO2fowratesandSample Delay, Sample Stop, Oxy Stop, Run
times. As these are the parameters of Method at level OPERATOR it is im-
possible to make up new methods.
To do above-mentioned operations is possible in access level MASTER
ATTENTION! NEVER USE THE MANUAL CONTROL DURING THE ANALYSIS
CYCLE!
Figure 8.4.6.5.
Sheet Service
58 Dumatherm
9.1. General
To start the real samples analysis, run some blank tests and tests with standard
materials. Blank test means to analyse empty capsules and the sample weight
is not entered into the SAMPLE TABLE. During a blank test, the oxygen dosing
time is default 6s. Blank tests must be run until the test results- peak areas are
decreased and stabilized. It means that the peak areas are less than 100 mVs.
and that the difference between peak areas at two adjacent tests is less than 40
mVs.Theresultofthelastblanktest,iswrittenonthefrstrowofthecalibration
table.
To check the calibration curve, some tests with standard material must be run. It
is recommended to run samples with weights 50 mg, 100 mg, 150 mg and 200
mg for example of EDTA. The results must be (9.57 0.05) % of nitrogen. If the
results are not within this value, the calibration curve must be corrected or the new
calibration must be measured.
9.1.1. Check list prior to the start of an analysis
1. Checkwhethergasisavailableinsuffcientamount
2. Open the inlets of the gas
3. Check the pressure and purity of the gases (see demands on page 8).
Should there be a deviation, set the gas pressure with utmost care. Please
note that the pressure reducer may only be changed when in a state of non-
pressure.
4. Turn on the instrument
5. Turn on the PC
6. Start software Dumatherm Manager
Only start the analysis of real samples after the blank value test and the check of
a standard have been successful. Make sure to use the worksheet Quality control
by the user which is found on the CD-ROM enclosed.
9.2. Analysis of unknown samples
9.2.1. Guideline for the determination of the correct combustion factor for
an unknown sample
Thegeneralruleisthatthemorediffcultitistocombustasubstance(i.e.the
carbon content is high), the higher the O
2
fowrateandO
2
factor must be.
Recommended ranges are:
- for O
2
fowrates-200to400ml/min;
- for O
2
factor 0.4 to 2.0 ml/mg.
Examples:
1 Low carbon content (e.g. soils) the O
2
fowrateis200ml/minandO
2
factor is
0.4 ml/mg.
2 Great carbon content (e.g. acetanilide) the O
2
fowrateis400ml/minandO
2

factor is 1.8 ml/mg.
For substances with known chemical composition the O
2
amount for combustion
can be calculated. To this theoretical amount must be added 10 % of oxygen. For
thechosenoxygenfowrateandknownoxygenamountforfullcombustiontheO2
factor can be calculated.
Thegreateroxygenamountsarenopoorinfuencetomeasurementresults,but
are important to lifetime of copper packing in reduction reactor: excess oxygen
decreasesgreatlythereductionreactorpackinglifetime.Insuffcientforfullcom-
9 Operation
5
Dumatherm
bustion oxygen amount causes the formation of CO in combustion gases. CO
increased the measured nitrogen peak area i.e. the higher measurement results
of nitrogen. CO also reduces the catalyst in combustion reactor. Therefore is
recommendable sometimes to check the condition of catalyst. To do so, analyse
some nitrogen-free substance e.g. benzoic acid or sugar - these substances dont
give the nitrogen peak.
If it is needed to analyse different unknown samples it is better to work with larger
oxygen amounts. For analysing unknown samples with similar composition it is
recommended to determine the O2 factor experimentally.
9.2.2. Determination of the combustion factor for an unknown sample
When the sample is unknown, you can proceed the following way:
1. Measure the sample twice with a standard initial weight of 100 mg and a com-
bustion factor of A 1.0.
2. Is the blank value okay after this series?
a) If NO, then start as described in point 1, however this time with a higher
combustion factor of A 1.2.
b) If YES, then start as described in point 1, however this time with a lower
combustion factor of A 0.8.
3. Carry on this procedure till the blank value after the measurement is okay and
the factor has reached the smallest value possible.
Try to put your samples in the various categories and then to measure them with
the appropriate factor. This way, you will obtain a library of the categories after a
short time which serves as a reference for your unknown samples.
IntheworksheetCategoriesyoucaninserttheappropriatetextinfointhefeld
Description.
9.3. Homogenization of samples
Before weighing samples must be properly homogenized.
Soil and plant samples must be oven-dried (appr. 80 C, 24 hours). Should the
samples contain forms of N such as ammonia that would lost in oven drying use
freeze-drying. Dried samples of soils are ground to talcum powder consistency
(250 m or less) using ball mills. The granules of vegetables may be little bigger.
Samples must be free of test material great pieces!
The amounts of prepared substances must be enough for good homogenization.
The amount of homogenized material must be enough for several samples.
Dont use for low-cost improvisations such as home coffee mills for grinding.
Remember that poorly prepared samples will obtain poor analysis results.
9 Operation
0 Dumatherm
9 Operation
3. 3. Weighing in of
samples
Solid samples are flled
in using a spatula then
wei gh agai n. Put the
weight into the sample
table (see chapter 8.4.2.
Sample Table).
Please use Celite as a
carrier material for liquid
samples (see chapter
9.6.).
1. 1. Shaping of the tin
foils.
Using the tweezers put
the tin foil on the shaping
tool. With the help of the
shaping stamp the foil
has to be put into the
opening.
Be careful: Make sure to
only touch the tin foil with
clean tweezers in order to
avoidfngerprints.
9.4. Weighing of samples
In order to run an analysis, the sample has to be weighted in tin foil. Thus, we
recommend using the tools included in the delivery, which help to handle the tin
foil and help you to close the tin foil capsules. This way, the process of weighing in
the samples will become very easy. The goal of the procedure is to obtain airtight
tin capsules.
2. 2. Tare the balance
Put the shaped tin foil on
the balance and press
tare.
left - tin foil cups,
Order-No.: 7718
right - pressed tin capsules
Order-No.: 7717
1
Dumatherm
9 Operation
4. 4. Closing of the
sample capsules
Afterfllinginthesamples,
close the tin foil using the
shaping tool.
Put the tin foil into the
shaping tool and close the
tin foil by pressing and si-
multaneously turning the
closing cap clockwise.
5. 5. Collect Samples
The thus prepared tin
capsules, are now stored
in the sample tray
9.5. Inserting the sample weights into the sample table
You can insert the sample weights in the sample table manually or using the au-
tomated data transfer of the weights from the balance to the PC.
9.5.1. Data transfer via balance
In general, the DUMATHERM- MANAGER is capable to work with the Sartorius
balance type CP64 (can be obtained as an option). You only need a free COM_Port
atyourPC.ConnectthebalancetothePCanddefnethecommunicationport
with the balance in the software.
9.6. Weighing of liquid samples
For analysing liquid samples use the support Celite.
Put the proper amount of support material to into the capsule. Put the capsule with
support on the weighing pan and push the TARE-key.
Take it from the pan and using a syringe drop the substance to analyse into the
capsule with support. Dont wet the walls of capsule during sample introduction.
Weight the sample, seal the capsule and enter the weight as described at solid
samples.
After weighing the samples of one material, clean the syringe!
9.7. Sample analysis
Pleases read chapter "8.4.2.1. Sample analysis".
2 Dumatherm
10 Trouble Shooting
Cause of error
1.1. Some of CO2 adsor-
bers (Traps 27 on Fluidic
Diagram) are not fully
degassed
2.1. The H
2
O is not com-
pletely separated.
2.2. From CO
2
adsorber
desorbed CO
2
.
3.1. CO2 adsorber cant
adsorb all CO
2
.
4.1. Through the TCD
goes mixture of N2 and
O2. The reduction re-
actor-packing (reduced
copper) lifetime is over.
4.2. To the N2 peak is
added the CO.
4.2.1. The amount of O2
isinsuffcientforfullcom-
bustion of sample.
4.2.2. Oxidation capacity
of catalyst in combustion
reactor is decreased.
4.2.3. The sample weight
is too great
5.1. The O
2
is not suff-
ciently pure.
5.2.The fow rate ofAu-
tosampler purge He is
too low
5.3. In O
2
line is air
5.4. On the Autosampler
is not the plastic lid
Measures
1.1.1. Turn CO
2
adsorbers with higher baseline level
into the degassing furnace and degas each of them
1 hour.
1.2.1. Check the TCD output signal (baseline) level.
For this turn carousel 6 times counter clockwise and
hold each adsorber 2 min in measuring position. Ba-
seline level difference must be less than 3-4 mV.
2.1.1. Change the H
2
O traps packing (Trap 1 on Fluidic
Diagram).
2.1.2. Check that valve (EV9 on Fluidic Diagram) is
open and Gas Dryer (Dr on Fluidic Diagram) purged
with additional air.
2.1.3.Checkthefowrateofpurgeair-itmustbeappr.
200 ml/min. Adjust it to the correct value (with NV3 on
Fluidic Diagram).
2.2.1. Turn to the measuring position next CO2 ad-
sorber.
3.1. Decrease the sample weight.
4.1.1. Change the reduction reactor tube for tube with
new packing.
4.2.1. Increase the O2 factor
4.2.2. Oxidise the catalyst in combustion reactor:- re-
lease the lower compression nut of reduction reactor-
choose Category Customer in the SAMPLE TABLE-
set Oxy Stop time 50 s in the sheet ANALYSIS
CONDITIONS- run 3 analyses without samples.- tight
the lower compression nut of reduction reactor.- check
the completeness of combustion inserting 150 mg ben-
zoic acid. Peak area must be less than 300 mVs.- if
the area is more than 300 mVs, change catalysts in
combustion reactor.
4.2.3. Decrease the sample weight.
5.1. Change the O
2
to the O
2
with purity 5.0.
5.2.1. Disconnect the Autosampler purge He line from
fttingonrearofinstrument(Purge)
5.2.2.Connecttothisfttingthegasfowmeter.
5.2.3. Adjust by needle valve (NV2 on Fluidic Diagram)
thefowratetoappr.70ml/min.
5.2.4. Connect the He purge with Autosampler.
5.3.1. Release the O
2
inletfttingonrearofinstrument
and purge it during 15 s.
5.3.2. Tight the ftting.5.4. Place the plastic lid to it
place.
Failure
1. Baseline level changes
from sample to sample
i.e. at carousel different
positions
2. Baseline level is too
high more than 10 mV
3. After N2 peak followed
another great peak
4. Measurement results
of the same substance
i ncreased af t er each
measurement
5. The blank analysis
peak is too great and at
repeating of analyses
dont decrease or decre-
ases very slowly
10.1. Error actions catalogue
3
Dumatherm
Cause of error
6.1. Leaks in gas lines
6.2. Insert is filled with
ash.
6.3. Uncompleted com-
bustion
6.3.1. Oxidation capacity
of catalyst in combustion
reactor is poor
6.3.2. The O2 amount is
insuffcient
6.4. Autosampler purge
withHeisinsuffcient
7.1. No compressed air
7.2. The pressure of com-
pressed air is low.
7.3. Hindered carousel
turning - CO2 adsorber
tubes are fall down.
7.4. Carousel turns too
quickly (or slowly)
8. 1. Def aul t set t i ng
Sample Peak Min. Area
is too great.
9.1. Default setting Blank
Peak Min. Area is too
great.
10.1. Leaks in gas lines
11. Carrier gas fow rate
is very high. Mass Flow
Controllers have zero
offset
Measures
6.1. Perform the leak test (chapter 10.11.) and elimi-
nate leaks.
6.2. Change the insert.
6.3.1. Check the oxidation capacity of catalyst with
150 mg Benzoic acid samples (see p. 4.2.2 of Trou-
bleshooting).
6.3.2. Increase the O2 factor.
6.4.CheckandadjustthepurgeHefowrate(p.5.2.1
of Troubleshooting).
7.1. Open the compressed air or change the com-
pressed air cylinder.
7.2. Adjust with pressure regulator on front of instru-
ment (PRV4 on Fluidic Diagram) the pressure to 3
bars.
7.3. Turn the carousel manually counter clockwise
and if it is needed fx the CO
2
adsorber tubes in its
correct position.
7.4.Adjustthecompressedairfowratewithneedle
valve (NV4 on Fluidic Diagram) so that carousel turns
correctly.
7.4.1. Regulate position reader to its right place.
8.1. Decrease in window Default constants the setting
of Sample Peak Min. Area.
9.1. Decrease in window Default Constants the set-
ting of Blank Peak Min. Area.
10.1. Perform the leak test (chapter 10.11.) and elimi-
nate the leaks.
11.1. Open the Service sheet
11.2.SetFC1andFC2fowratetozero
11.3 If they differ from zero, click right button of
mouse.
11.4 Open list of choices. Select Gas Flow Controller
FC1 Zero or FC2 Zero. Zerothe FC1 and FC2
11.5Checkthatfowratesarereallyzero
Failure
6. At repeatability tests of
homogeneous substance
(e.g. EDTA) RSD > 1%
7. Error message Carou-
sel illegal position
8. At sample measure-
ment in SAMPLE TA-
BLE is No Detected
but on sheet PLOTS the
peak is normal.
9. At blank measurement
in SAMPLE TABLE is
No Detected but on
sheet PLOTS the peak
is normal.
10. N
2
peak is very de-
layed
11. System pressure is
out of range
10 Trouble Shooting
4 Dumatherm
Cause of error
12. Temperatures com-
bustion furnace (LF) or
reduction furnace (RF)
or degassi ng furnace
(OVEN) out of caps.*
12.1. Heating resistance
or LF, RF on OVEN is bro-
ken or short circuited.
12.2. Thermocouple of LF
or RF is broken or short
-circuited.*
12.3. RTD (Pt-100) of
OVEN is broken or short-
.circuited.*
13.1. Real flow rate is
zerofowcontrollerzero
has zero off set.
13.2 Leak in the controller
valve.
Measures
12.1. Contact with technician
13.1.Setfowcontrollertozero
13.2.1. Open the Service sheet
13.2.2.Setfor20secfowrate400ml/min.
13.2.3.Setfowratezero,checkrealfowrate.Ifthe
realfowratediffersfromzerorepeatprocedure.
Failure
12. Front panel lights LED
ALARM
13. Carrier gas fowrate
is set zero, but measured
fowrateisnotzero
* Instrument displayed corresponding to each failure the error message.
10 Trouble Shooting
5
Dumatherm
11 Maintenance
Please make sure that only original C. Gerhardt spare parts are used.
To minimize malfunctions of the DUMATHERM, we recommend having it checked
by authorized service personnel annually.
11.1. Service and cleaning
Always wear gloves before cleaning any parts of the instrument.
Never use abrasive cleaners! In most cases it will be suffcient after each use
to clean the plates using a moist cloth and some household washing-up liquid.
Subsequently rub dry.
11.2. Spare parts and consumables
Order-No. Quantity Description
7710 250 g Copper reduced wires, 0,5 dia.
7711 100 g HT Oxydation catalyst
7712 20 g Quartz wool
7713 10 g Magnesium perchlorate
7714 50 g LT Oxydation catalyst
7715 1pc. Ashfngerinsertceramic
7717 100 pc . Pressed TIN capsules (9 x 10 mm)
7718 100 pc. Tin Foil cups
7719 4 pc. Transparent quartz tube 26 x 450 mm
7720 4 pc. Seals for bottom connector, green
7721 4 pc. Seals for top of quartz tubes (diam. 26 mm)
7723 1 pc. gas tight closed CO2 adsorber tube with adsorbent
7724 10 g Chromosorb
7725 1pc. Ashfnger(insert),glass
7726 1pc. PrepackedCombustionReactor(flledwithHT,LTCatalyst)
7730 50 g Copper oxide wires
7731 25 g HT oxydation catalyst
77001 1 pc. Trap for water complet with glastrap, seals and Endcaps
77002 2 x 1,5 m SS-tubing 2 x 1 mm
77003 4 m Polyurethan tubing 4 x 0.75 mm
77004 6 pc. Ferrule for 4 x 0.75 mm tubing
77005 10 pc. Nuts M 6
77006 10 pc. Ferrules for 2 mm tubing
77009 1 pc. Combustion/reduction reactors joint
77012 1 pc. SS tubing 2 x 0.5 with nuts and ferrule for autosamplergas
connections
77015 1 pc. CO
2
adsorber tube connecting set (dist. Ferrule, back fer-
rules, O-rings)
77017 1 pc. Autosampler PN120 complete
77018 1 pc. Fuse 10 A
77030 3 pc. Spare O-rings.
77032 2 pc. Threated end caps for water traps
77033 2 pc. Siliconseals for Watertrap
77034 1 pc. Permapure tube
77035 2 pc. Bottom Isolation collars
77058 1pc. Tefonisolatingring21x6mm
77059 1pc. Purgelinetefondia.2mm,400mmlongwithferrules,nuts
7706 1pc. TefonlineRRdia.2mm,450mmlongwithferrules,nuts
Dumatherm
11.3. Accessories
Order No. Quantity Description
4267 1 pc. USB-Converter
7727 1 pc. Capsule forming and closing device
7728 1 pc. Balance for Dumatherm with Datatransfer Software
77007 1 pc. Pinzette
77008 1 pc. Spatula for solid samples
77011 1pc. AufagegestellfrReaktoren
77014 1pc. Ashfngerextractor
77016 1 pc. Syringe 1ml
77020 1 pc. Dumatherm Manager Software CD
77021 1 pc. Sample preparation plate
77022 1 pc. Tool for taking out reactor tubes
77023 1pc. Rodforreactortubeflling
77025 1 pc. Sample tablet for 40 capsulated samples
77029 1 pc. Sample disc for 40 samples
77031 1 pc. Wrench for top reactor nut
77041 1 pc. Autosampler support, silicone rubber disc
77042 1 pc. Piston removal tool
77044 1 pc. Tray for samples, position 40 - 79
77045 1 pc. Tray for samples, position 80 - 119
77046 1 pc. Plastic lid transparent for PN 120 carousel
77057 m. Capillary tube (stainless steel) 2 x 0,5 mm
77061 1 pc. Isolation cup, diam. 90 mm
77063 1 pc. Foamed plastic block 450 x 120 x 60 mm
Further accessories and information about the shaker program can be found in
the product catalogue or at your local dealer!
11.4. Service and contact
Make sure to handle error messages as described in chapter 10. Trouble shoo-
ting.
In case of breakdown or failure of your DUMATHERM, please contact your local
dealer or:
C. Gerhardt GmbH & Co. KG
Csariusstr. 97
D-53639 Knigswinter
Tel.: +49 (0)22 23 - 29 99 0
Fax: +49 (0)22 23 - 29 99 99
info@Gerhardt.de
www.gerhardt.de
11 Maintenance
7
Dumatherm
11 Maintenance
11.5. Disposal
The disposal of the packaging and the parts used has to be done according to the
rules and regulations which are valid in the country of installation. Should the pro-
duct itself be disposed of, make sure to observe the local rules and regulations..
11.5.1. Information for the Disposal of Electric and Electronic Instruments
within the European Union
The disposal of electrically operated instruments is settled within the European Uni-
on by national regulations, which are based on the EU-directive 2002/96EC about
electric and electronic used-instruments (WEEE). Thus, all instruments delivered
after August 13th 2005 must not disposed into the communal domestic waste.
Since the regulations about disposal of waste might vary from one country to the
other within the European Community, we kindly ask you to contact your supplier
or dealer.
InGermany,thisobligationforidentifcationwillbevalidasofMarch,23rd2006.
As of this date, C. Gerhardt will take back all instruments delivered after August,
13th, 2005 without charges and will dispose of them according to the regulations,
or Gerhardt will come to an agreement with the last user of the unit. For all instru-
ments delivered prior to August 13th, 2005 the last user will be held responsible
for the proper disposal. The only crucial factor accepted, for the chronological
placement, it the serial number at the back of the instrument.
11.5.2. Ban on Materials according to ROHS Regulation 2002/95/EG
Ban on materials from the ROHS regulation 2002/95/EG is not valid for the electro-
and electronic instruments of category 8 and 9 and thus not for those instruments
described in this instruction manual. However, we want to draw your attention to the
fact that we feel obliged to observe the regulations for the RoHs for all our products.
Please be kind enough to contact us if you have any further questions.
11.5.3. Transfer
We kindly ask you to always make sure to add this instruction manual to the product
in case of transferring it to another party.

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