Manual Usuario Fias Mhs15 PDF

ATOMIC SPECTROMETRY
Users Guide
MHS 15
Mercury Hydride System
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ATOMIC SPECTROMETRY
MHS 15
Mercury Hydride System
Users Guide
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User Assistance
PerkinElmer, Inc.
710 Bridgeport Avenue
Shelton, Connecticut 06484-4794
U.S.A.
Or emailed to: info@perkinelmer.com
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but not limited to, the implied warranties of merchantability and fitness for a particular purpose. PerkinElmer shall
not be liable for errors contained herein for incidental consequential damages in connection with furnishing, performance
or use of this material.
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or translated into any language without the prior written permission of PerkinElmer, Inc.
or one of its affiliates.
Copyright 19982000 by affiliates of PerkinElmer, Inc.
Produced in Singapore
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AA WinLab, AAnalyst, Lumina, and THGA are trademarks of affiliates of PerkinElmer, Inc.
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Part Number Release Publication Date
0993-5288 A J uly 2000 Valid for Software Version 6.5
0993-5288
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Chapter 1 Safety and Regulatory Information
Safety practices and conventions . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1-3
Correct use of the instrument . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1-4
Operating conditions . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1-5
Laboratory hygiene . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1-5
Laboratory ventilation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1-5
Safe handling of chemicals . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1-6
Waste disposal . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1-8
Handling compressed gases . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1-9
Safety practices for flame operation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1-12
Safety practices for mercury/hydride systems . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1-14
References for laboratory safety practice . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1-16
Regulatory information . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1-17
Chapter 2 MHS 15: Analyzing Samples
Setting up the system . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-3
Positioning the MHS 15 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-3
Preparing the system for analyses . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-4
Aligning the QTA . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-6
Selecting operating mode . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-8
Performing a measurement . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-10
Methods development . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-12
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Chapter 3 MHS 15: Recommended Analytical Conditions
Safe handling of chemicals . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-3
Recommended conditions for arsenic . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-5
Recommended conditions for bismuth . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-7
Recommended conditions for mercury . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-9
Recommended conditions for antimony . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-13
Recommended conditions for selenium . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-15
Recommended conditions for tin . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-17
Recommended conditions for tellurium . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-19
Chapter 4 MHS 15: Maintenance
PerkinElmer Service . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-3
Routine maintenance . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-4
Maintaining the flashback arrestor . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-6
QTA maintenance . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-7
Replacing worn parts . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-10
Chapter 5 MHS 15: Parts and Supplies
Parts provided . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-3
Obtaining supplies, replacement parts, and accessories . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-4
Replacement parts . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-5
Chapter 6 MHS 15: Installation
Unpacking and inspection . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6-3
Installing the QTA burner mount . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6-4
Installing the reactor assembly . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6-6
Connecting the inert gas supply . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6-6
Preparing the reactor assembly . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6-8
Chapter 7 MHS 15: Laboratory Requirements
Operating conditions . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-3
Gas supply requirements . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-5
Inert gas . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-6
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Chapter 8 MHS 15: System Description
Introduction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8-3
Chemical vapor generation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8-6
The cold vapor technique . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8-6
The hydride-generation technique . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8-6
Literature on chemical vapor generation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8-7
Principle of operation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8-8
Technical data . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8-11
Chapter 9 MHS 15: Analytical Notes
Features of the MHS 15 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 9-3
Sample volume and dilution . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 9-3
Purge gas function . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 9-4
Calibration techniques . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 9-6
Chemical factors . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 9-7
Chapter 10 MHS 15: Translations of Warnings
Index
Customer Service
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Safety practices and conventions . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1-3
Correct use of the instrument . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1-4
Operating conditions . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1-5
Laboratory hygiene . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1-5
Laboratory ventilation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1-5
Safe handling of chemicals . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1-6
Waste disposal . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1-8
Handling compressed gases . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1-9
Safety practices for flame operation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1-12
Safety practices for mercury/hydride systems . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1-14
References for laboratory safety practice . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1-16
Regulatory information . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1-17
Safety and Regulatory Information 1
1Safety and Regulatory Information
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Safety practices and conventions
The guide provided with the instrument contains information and warnings that
must be followed by the user to ensure safe operation and to maintain the
instrument in a safe condition. This advice is intended to supplement, not
supersede, the normal safety code of behavior prevailing in the country of
operation.
The information provided does not cover every safety procedure that should be
practiced. Ultimately, maintenance of a safe laboratory environment is the
responsibility of the user and the users organization.
Possible hazards that could harm the user or result in damage to the instrument
are clearly stated at appropriate places throughout this guide.
Any of the following safety conventions can be used throughout this guide:
This symbol alerts you to situations that could result in personal injury to yourself
or other persons.
Details about these circumstances are in a box like this one.
This symbol alerts you to the risk of hot surfaces that could cause personal
injury to yourself or other persons.
Caution The term CAUTION alerts you to situations that could result in serious damage
to the instrument or other equipment.
Details about these circumstances are described in a message similar to this
one.
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Correct use of the instrument
Before you install or use your instrument, and in order to get the best results, you
should be familiar with all of the instruments in the system and know how to
operate them. You should also be aware of the safety procedures in force in your
laboratory, especially those concerning atomic spectrometry instruments. Read
the guides supplied with the instruments before you start.
If you use the instrument in a manner not specified in the guide, or if you use it
for a purpose other than that intended, you may damage the instrument, or
compromise your own, or someone elses, safety.
This instrument should only be operated by persons who are suitably qualified
and have received adequate training.
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Operating conditions
The instrument will operate correctly under the following conditions:
Indoors.
Ambient temperature +15 C to +35 C (+59 F to +95 F), with a maximum
change not exceeding 2.8 C (5 F) per hour.
Ambient relative humidity 20% to 80%, without condensation.
Altitude in the range 0 m to 2000 m.
You can store the instrument safely under the following conditions:
Ambient temperature 20 C to +60 C (4 F to +140 F).
When you remove the instrument from storage and before you put it into
operation, allow it to stand for at least a day under the approved operating
conditions.
Laboratory hygiene
Keep the work area scrupulously clean to avoid contaminating your samples
and to maintain a safe working environment. Clean up spilled chemicals
immediately and dispose of them properly.
Do not allow smoking in the work area. Smoking is a source of significant
contamination and also a potential route for ingesting harmful chemicals.
Do not store, handle, or consume food in the work area.
Laboratory ventilation
Toxic combustion products, metal vapor, ozone, etc., can be generated by the
system, depending on the type of analyses being performed.
You must provide an efficient laboratory ventilation system to remove toxic
products generated during instrument operation.
W1.3
Warning: Explosive Atmosphere
This instrument is not designed for operation in an explosive atmosphere.
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Safe handling of chemicals
Some chemicals used with the instrument may be hazardous or may become
hazardous after completion of an analysis.
The responsible body
1
must take the necessary precautions to ensure that the
surrounding workplace is safe and that instrument operators are not exposed to
hazardous levels of toxic substances (chemical or biological) as defined in the
applicable national, state, and local health and safety regulations and laws.
Venting for fumes and disposal of wastes must be in accordance with all national,
state, and local health and safety regulations and laws.
Use, store, and dispose of chemicals in accordance with the manufacturers
recommendations and the applicable national, state, and/or local regulations.
Wear appropriate eye protection at all times while handling chemicals.
Depending on the types of chemicals you are handling, wear safety glasses
with side shields, or goggles, or a full-face shield.
Wear suitable protective clothing, including gloves if necessary, resistant to
the chemicals you are handling.
When preparing chemical solutions, always work in a fume hood that is
suitable for the chemicals you are using.
Perform sample preparation away from the instrument to minimize corrosion
and contamination.
Clean up spills immediately using the appropriate equipment and supplies,
such as spill cleanup kits.
Do not put open containers of solvent near the instrument.
Store solvents in an approved cabinet (with the appropriate ventilation) away
from the instrument.
1. Definitions from IEC 1010-1:
Responsible body: individual or group responsible for the use and maintenance of
equipment, and for ensuring that operators are adequately trained.
Operator: person operating equipment for its intended purpose.
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Sodium tetrahydroborate
Sodium tetrahydroborate is used as a reductant in the mercury cold vapor
technique and the hydride-generation technique. Sodium tetrahydroborate
solutions are unstable and decompose, releasing hydrogen. Sodium
tetrahydroborate also releases hydrogen when it comes into contact with acids.
Make sure that the work area has an adequate ventilation system to prevent
the build-up of explosive air-hydrogen mixtures.
Use and store sodium tetrahydroborate according to the manufacturers
recommendations.
Keep sodium tetrahydroborate solutions:
Out of direct sunlight.
Away from open flames.
In an area with an efficient ventilation system.
Protect sodium tetrahydroborate solutions from temperature variations.
Handle sodium tetrahydroborate solutions with care since they are corrosive.
Do not allow smoking in areas where sodium tetrahydroborate is used.
When you are using sodium tetrahydroborate as the reductant, hydrogen is
formed when it comes into contact with the acidified measurement solution.
Do not loosen or remove any connections when the system is operating.
The maximum concentration of sodium tetrahydroborate that you should
use with the PerkinElmer MHS 15 system is 3% W/V (30 g/L).
At the end of the work session, purge the system with deionized water to
remove all traces of the reductant.
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Waste disposal
Disposing of reaction residues
Do not empty the reaction flask directly into the laboratorys waste water system;
there may be an excess of NaBH
4
or SnCl
2
in the flask.
Collect the reaction residues in a suitable waste container. Store the waste
container in a fume hood and make sure that the contents are sufficiently acidic
so that NaBH
4
residues react completely. Do not put a cap on the waste container.
Contents of waste containers
The materials that you collect in waste containers may include small amounts of
the substances that were analyzed and other chemicals used in the analyses.
If these materials are toxic, corrosive, or contain organics you may have to treat
the collected effluent as hazardous waste. Refer to your local safety regulations
for proper disposal procedures.
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Handling compressed gases
Note: The permanent installation of gas supplies is the responsibility of the user
and should conform to local safety and building regulations.
Summary of gas hazards
Hazards associated with the different gases used in atomic absorption
spectrometry are presented in the table below:
Contact the gas supplier for a safety data sheet containing detailed information on
the potential hazards associated with the gas.
Identifying cylinders
Legibly mark cylinders to clearly identify the contents and status (full, empty,
etc.). Use the chemical name or commercially accepted name for the gas.
Gas Suffocation Explosion
Spontaneous
Decomposition
or Combustion
Argon x
Nitrogen x
Warning: Compressed Gases
High pressure gas cylinders can be dangerous if mishandled or misused.
Always handle gas cylinders with caution and observe your local regulations
for the safe handling of gas cylinders.
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Storing cylinders
Store cylinders in accordance with the applicable national, state, and/or local
regulations and standards.
When gas cylinders are stored in confined areas, such as a storage room, make
sure that ventilation is adequate to prevent toxic or explosive accumulations
of gas.
The storage room should be well ventilated and dry. This is particularly
important in confined areas.
Do not store cylinders near elevators, gangways, or in locations where heavy
moving objects may strike or fall against them.
Use and store cylinders away from exits and exit routes.
Locate gas cylinders away from heat sources, including heat lamps.
Compressed gas cylinders should not be subjected to temperatures above
52 C (125 F).
Do not allow ignition sources in the storage area and keep cylinders away
from readily ignitable substances such as gasoline or waste, or combustibles
in bulk, including oil.
Store all gas cylinders only in a vertical position, with the valve cap in place,
and fastened securely to an immovable bulkhead or a permanent wall.
If you are storing cylinders outdoors, store them above ground on a suitable
floor where they are protected against temperature extremes (including the
direct rays of the sun).
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Handling cylinders
Move cylinders with a suitable hand truck after making sure that the valve cap
is securely in place and that the cylinder is properly fastened to the hand truck.
Use only approved regulators, tubing, and hose connectors. When you
connect fittings, keep in mind that left-hand thread fittings are used for fuel
gas connections (e.g., acetylene), whereas right-hand thread fittings are used
for oxidant and support gas connections (e.g., nitrous oxide, air).
Arrange gas hoses where they will not be damaged or stepped on and where
things will not be dropped on them.
Do not attempt to refill gas cylinders.
Check the condition of pipes, hoses, and connectors regularly, and replace any
damaged parts.
Perform periodic gas leak tests at all joints and seals of the gas system by
applying an approved gas leak detection solution.
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Safety practices for flame operation
Safety interlocks
PerkinElmer provides a number of safety interlocks on the burner system to
monitor gas pressure and check for the proper setup of the burner head, nebulizer,
and drain system. In addition a flame sensor checks that the flame is burning.
Do not attempt to defeat these interlocks; you may compromise your own, or
someone elses, safety.
Safe use of burner gases
The seepage of fuel gas or fuel gas mixture from the burner system, the drain
system, the gas control system, or the gas connections constitutes a serious fire
hazard.
Make sure that there are no breaks or leaks in any of these systems and that
all the seals are correctly installed and in good condition.
Regularly check for leaks at joints and seals using an approved leak test
solution.
When you perform any maintenance or installation procedures, follow the
instructions in the guide exactly.
Do not attempt to service the gas control system yourself.
A PerkinElmer service engineer, or similarly authorized and trained person,
must perform the work.
When you shut down the instrument, for example at the end of the working
day, shut all the gas lines at the cylinder or regulator valves. Bleed the lines
between the regulator and instrument to atmosphere before switching off the
ventilation system.
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Safe operation of the flame
Before you ignite the flame make sure that:
The laboratory fume ventilation system is operating;
The burner head is installed correctly;
The burner end cap is secured firmly;
The fuel and oxidant tubing fittings are properly connected;
The atomizer compartment door is closed.
Do not leave the flame unattended. Always make sure that there is a fire
extinguisher near the instrument.
Never change the gas pressure or shut a gas valve while the flame is burning.
Do not allow the burner head slot to become blocked. This can cause a
flashback of the flame.
Do not place open containers of flammable liquids and solvents near to the
flame. Be especially careful with samples that contain highly volatile
solvents.
Hazards with flame operation
High temperatures
The flame can generate temperatures of up to 2800 C.
To avoid serious burns, never touch the quartz tube atomizer (QTA), QTA
mount, or burner head until they have cooled to room temperature.
UV radiation
The flame emits ultraviolet radiation.
Keep the atomizer compartment door closed when the flame is burning and
never directly view the flame unless you are wearing UV-absorbing glasses.
1-14
0993-5288
Safety practices for mercury/hydride systems
FIAS-Cells To all users who have an MHS 15 in addition to FIAS
Never use the FIAS-cell for the MHS 15.
The smaller diameter of the FIAS-cell can cause an increase in back pressure.
This could force the acidic reaction mixture back into the sodium
tetrahydroborate bottle where large quantities of hydrogen would be
produced.
Safety checks
Before you start an analysis, make sure that:
The laboratory fume ventilation system is operating;
The tubing in the system is not constricted since this could lead to a
pressure build-up in the system;
If you are using a flame to heat the QTA, refer to the information under
Safety practices for flame operation on page 1-12 before you ignite the
flame.
Hazards with mercury/hydride systems
Toxic products
Toxic metal vapors, hydrogen, etc., can be generated by the system, depending on
the type of analyses being performed.
You must provide an efficient laboratory ventilation system to remove toxic
products generated during instrument operation.
High temperatures
The QTA used for the hydride-generation technique can reach temperatures of up
to 1000 C.
Do not touch any part of the QTA mount or the QTA until they have cooled
to room temperature.
0993-5288
1-15
Hazardous chemicals
Some of the chemicals required for analyses are corrosive and/or toxic.
Refer to the information under Safe handling of chemicals on page 1-6 and
to the specific warnings in the documentation provided with the system before
you start an analysis.
Operational precautions
The MHS 15 mercury/hydride system is characterized by simplicity of operation.
Nevertheless you should realize that during the determination a chemical reaction
takes place with the liberation of hydrogen when you are using NaBH
4
as the
reductant. Since hydrogen can form flammable mixtures with air, you must take
the following precautions to prevent the buildup of air-hydrogen mixtures.
Carefully observe the precautions listed under Sodium tetrahydroborate on
page 1-7.
Do not fill the reductant bottle more than three-quarters full.
Do not position the reactor assembly such that the reductant bottle can be
subjected to heat radiation from the flame.
Do not overfill the reaction flask. The maximum prepared measurement
solution volume is 50 mL.
Once the reaction has been started, do not remove the reaction flask from the
reactor assembly and then reconnect it. Air entrained in the flask may lead to
the formation of a potentially flammable air-hydrogen mixture.
If you have to remove the reaction flask before the reaction is complete (e.g.
due to excessive foam development), place the flask in a fume hood until the
liberation of hydrogen has ceased. Repeat the determination on a fresh
sample.
Do not empty the reaction flask directly into the laboratorys waste water
system; there may be an excess of NaBH
4
in the flask.
Make sure that the sample transfer tube is not restricted in any way and that
the flashback arrestor is not blocked.
Never depress the plunger when a reaction flask or other vessel is not placed
underneath the immersion tube.
Do not operate the system with the graphite cooling rings removed from the
ends of the QTA.
At the end of the working day, purge the reductant transfer system with
deionized water to remove any reductant residues.
1-16
0993-5288
References for laboratory safety practice
Bretherik, L., Bretheriks Handbook of Reactive Chemical Hazards, 4th ed.,
Butterworth & Co. Ltd., London, UK, 1990.
Safe Practices in Chemical Laboratories,
Royal Society of Chemistry, London, UK, 1989.
Hazards in the Chemical Laboratory, 5th edition, Luxon, S.G., ed.,
Royal Society of Chemistry, London, UK, 1992.
CRC Handbook of Laboratory Safety, 3rd edition, Furr, K., ed.,
The Chemical Rubber Co. Press, Florida, USA, 1990.
Prudent Practices for Handling Hazardous Chemicals in Laboratories,
National Research Council, National Academic Press, Washington D.C.,
USA, 1981.
Saxs Dangerous Properties of Industrial Materials,
9th edition, Sax, N.I. and Lewis, R.J., eds.,Wiley, New York, USA, 1998.
Pohanish, R.P. and Greene, S.A., Hazardous Materials Handbook,
Wiley, New York, USA, 1996.
Compressed Gas Association, Inc., Arlington, VA 22202, USA, various
publications.
Data Sheets provided by chemical manufacturers, e.g.:
USA, Material Safety Data Sheets (MSDS),
FRG, DIN-Sicherheitsbltter,
UK, Hazard Data Sheets.
0993-5288
1-17
Regulatory information
This instrument has been designed to comply with a wide variety of international
standards governing the safety of laboratory equipment. In routine use, the
instrument poses virtually no risk to you. If you take some simple, common-sense
precautions, you can maintain the continued safe operation of the instrument.
1-18
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2-1
Setting up the system . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-3
Positioning the MHS 15 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-3
Preparing the system for analyses . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-4
Aligning the QTA . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-6
Selecting operating mode . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-8
Performing a measurement . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-10
Methods development . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-12
MHS 15:
Analyzing Samples 2
2MHS 15: Analyzing Samples
Marker for header
Contents
page
MHS 15: Analyzing Samples
2-2
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2-3
Setting up the system
Positioning the MHS 15
1. Place the MHS 15 reactor assembly adjacent to the spectrometers atomizer
compartment. A small table in front of the spectrometer is ideal.
2. Remove the QTA from the holder at the rear of the reactor assembly and place
it in the QTA bracket on the burner.
Position the QTA so that the side arm rests in the locating notch in the QTA
bracket.
Note: Make sure that the transfer tube runs in a smooth loop from the
reactor assembly and that it cannot be pinched or kinked. A restriction in the
transfer tube can lead to a pressure buildup in the system.
Figure 2-1. QTA mounted on the burner
Note: When you position the MHS 15 in front of the spectrometer, make sure
that the reductant bottle is not exposed to heat radiation from the flame.
Hinged QTA bracket
(shown in down position)
Burner head
Burner spray
chamber
QTA
Transfer tube
from reactor assembly
(nebulizer not shown)
2-4
0993-5288
Preparing the system for analyses
1. Read the safety information at the front of this guide and in the spectrometers
guide before you operate the system.
2. Switch on the fume ventilation system for the work area.
3. Install the proper radiation source for the element to be determined.
4. Switch on the spectrometer, following the routine described in the
spectrometers guide.
5. Select the atomization technique (refer to the spectrometers guide).
For the MHS 15, select the Flame technique.
6. Set up a method on the spectrometer (refer to the spectrometers guide or the
Online Help in AA WinLab).
1. Select Peak Height for Signal Measurement.
2. Select a Read Time of sufficient length (more information: page 2-13).
3. Do not select a Read Delay.
7. Align the radiation source for maximum energy.
8. Perform fine alignment of the QTA, if required (procedure: page 2-7).
9. If you require a flame to heat the QTA, turn on the burner gases and adjust the
outlet gauge pressures to the recommended values (refer to the spectrometers
guide).
You do not require a flame to heat the QTA for mercury determinations.
10. With the QTA tilted out of the radiation beam, ignite the air-acetylene flame.
To prevent soot formation on the QTA, use a lean, oxidizing flame.
11. Tilt the QTA into the radiation beam and allow 10 to 15 minutes for
stabilization in the flame before you start measurements.
12. Prepare the required reductant solution (refer to the Recommended
Conditions for the analyte element).
13. Fill the reductant bottle three-quarters full with the reductant solution.
Do not overfill the bottle.
Screw the reductant bottle finger-tight into the fitting on the reactor
assembly.
14. Select the operating mode for the reductant you are using, if required
(procedure: page 2-8).
0993-5288
2-5
15. Turn on the inert gas supply to the reactor assembly and set the outlet gauge
pressure to 250 kPa (see Table 7-1 on page 7-6).
Note: Inert gas flows continuously when the supply is turned on. To conserve
gas, turn off the supply during longer pauses in operation.
Since the pressure of the inert gas to the MHS 15 has a slight influence on the flow
rate of the gas through the system, always set the pressure consistently to
250 kPa.
Figure 2-2. Reactor assembly with reductant bottle
Inert gas
Reductant bottle
Fitting for
reductant bottle
2-6
0993-5288
Aligning the QTA
Before you perform analyses, you must align the QTA in the spectrometers
sample beam to make sure that the radiation passes through the QTA and does not
impinge on the walls.
1. Coarse alignment
You should perform coarse alignment at the first installation of the QTA burner
mount and every time that you have removed the burner head from the burner.
1. Tilt the QTA bracket to the up position, out of the radiation beam.
2. Install a suitable radiation source in the spectrometer that emits a beam of
visible light, such as a copper hollow cathode lamp.
3. Switch on the spectrometer, following the routine described in the
Do not ignite the flame.
4. Align the radiation source for maximum energy.
5. Tilt the QTA bracket to the down position so that the QTA is in the radiation
beam.
6. Hold a piece of white paper at the radiation exit end of the QTA and visually
inspect the light spot.
7. If necessary, make incremental adjustments to the burners adjustment
controls so that the radiation beam passes through the QTA without
impinging on the walls.
0993-5288
2-7
2. Fine alignment
Perform fine alignment before the start of every analysis series.
1. Tilt the QTA bracket to the up position, out of the radiation beam.
2. Install the proper radiation source for the element to be determined.
3. Set up the spectrometer for the determination as described in the
Do not ignite the flame.
4. Tilt the QTA bracket to the down position so that the QTA is in the radiation
beam.
5. Select the correct mode on the spectrometer for performing optimization
procedures (normally Continuous mode on most instruments).
Do not select background correction.
6. If necessary, make incremental adjustments to the burners adjustment
controls to obtain the lowest possible absorbance reading.
This completes the fine alignment procedure.
W3.1
Warning: UV Radiation Risk of Eye Damage
The lamps may emit UV radiation which can damage your eyes.
Do not gaze into a lighted lamp.
Always wear UV-absorbing safety glasses when looking at the radiation from
the lamps.
2-8
0993-5288
Selecting operating mode
Figure 2-3. Reductant changeover valve
If the reductant changeover valve is not set to the reductant you intend to use,
change the position of the valve as follows:
1. Slacken, but do not remove, the wing nut.
2. Lift up the valve cover to release the locking pin (on the underside).
3. Turn the valve cover until the black arrow is opposite the required reductant.
4. Lower the valve cover, making sure that the locking pin locates in the hole.
5. Tighten the wing nut finger-tight.
Reductant changeover valve
0993-5288
2-9
Figure 2-4. Reductant changeover valve set to NaBH
4
Note: If you determine mercury using tin(II) chloride as the reductant, the
apparatus will be contaminated with tin. If you subsequently determine tin in the
same apparatus using sodium tetrahydroborate as the reductant, the tin
contamination will interfere in the determination. Since tin is a hydride-forming
element, the tin contamination may also interfere in the determination of other
hydride-forming elements.
If you change regularly between SnCl
2
and NaBH
4
, we strongly recommend that
you purchase a second MHS 15 and reserve it solely for use with SnCl
2
. Likewise
you should reserve a set of reaction flasks, an immersion tube, and a reductant
bottle solely for use with SnCl
2
.
A set of adhesive labels is provided with the MHS 15 so that you can mark the
reductant being used.
Valve cover
Wing nut
2-10
0993-5288
Performing a measurement

Note: If you are going to analyze a sample of unknown composition, perform a
preliminary trial first to check whether there is excessive foaming or precipitation
(more information: page 9-9).
1. Read and make note of the operational precautions at the front of this guide
before you operate the system (see page 1-15).
2. Set up the system as described under Preparing the system for analyses on
page 2-4.
3. Prepare calibration and test sample solutions as required.
4. Dispense 10 mL (or the required volume) of dilute acid into the reaction flask
using a measuring cylinder.
5. Dispense an accurately measured volume of a test solution (a blank solution,
a calibration solution, or a test sample solution) into the reaction flask using
a suitable pipet.
6. Attach the reaction flask to the reactor assembly:
1. Insert the reaction flask into the socket.
2. Turn the reaction flask so that the lugs are gripped in the bayonet lock.
7. Wait for the pre-reaction purge time (more information: page 2-12).
Note: You do not need to wait if you are using SnCl
2
as reductant.
8. Start the Read function on the spectrometer (refer to the spectrometers guide
or the Online Help in AA WinLab).
9. Wait for approximately 5 seconds for the spectrometer to perform BOC.
Warning: Corrosive Chemicals Risk of Burns
Some of the chemicals used with the instrument are hazardous (acids, reductant
solutions, etc.).
When using hazardous chemicals, always wear suitable protective clothing
including eye protection, and observe the manufacturers instructions and
your local safety regulations.
0993-5288
2-11
Figure 2-5. Attaching the reaction flask
10. Depress and hold the plunger for the predetermined reaction time (more
information: page 2-13).
Note: Release the plunger immediately if foam is transported into the
flashback arrestor or the QTA.
11. Then release the plunger and wait for the post-reaction purge time (more
information: page 2-13).
12. Remove the reaction flask from the reactor assembly and empty the contents
into a waste container.
13. Holding the reaction flask under the immersion tube, use a wash bottle to rinse
the immersion tube with dilute acid.
14. Rinse the inside of the reaction flask with dilute acid and empty the contents
into a waste container.
15. Follow the above procedure to measure all other test solutions.
Reaction flask socket
Lugs
Reaction flask
with bayonet lock
Plunger
2-12
0993-5288
Methods development
To establish the optimum periods for the pre- and post-reaction purge times, the
reaction time, and also the Read Time on the spectrometer, you must perform
preliminary measurements.
Pre-reaction purge time
As explained on page 9-4, you must purge the system free of air before starting a
measurement when you are using NaBH
4
as reductant. The pre-reaction purge
time for each element quoted in the Recommended Conditions is generally
adequate. However, for arsenic and selenium you should determine the pre-
reaction purge time experimentally for your system, since radiation absorption by
air in the QTA can interfere in the determination of these elements.
page 2-4.
2. Set up a method on the spectrometer for the element you wish to determine
(refer to the spectrometers guide or the Online Help in AA WinLab).
3. Display the Continuous Graphics window.
You will obtain a continuous absorbance reading since air in the QTA absorbs
radiation.
4. Connect an empty reaction flask to the reactor assembly.
5. Watch the continuous graphics display.
As air is purged from the system by the inert gas, the absorbance plot falls
toward the baseline.
6. Wait until the plot levels out on the baseline and then note the time taken.
This is the pre-reaction purge time.
0993-5288
2-13
Reaction time, post-reaction purge time, and read time
Determine the reaction time and post-reaction purge time by measuring a suitable
calibration solution of the analyte element, as described below:
page 2-4.
2. Set up a method on the spectrometer for the element you wish to determine
(refer to the spectrometers guide or the Online Help in AA WinLab).
3. Display the Continuous Graphics window.
4. Dispense 10 mL dilute acid into the reaction flask using a measuring cylinder.
5. Dispense an accurately measured volume of a calibration solution into the
reaction flask using a suitable pipet.
6. Attach the reaction flask to the reactor assembly.
7. Wait for the pre-reaction purge time.
8. Depress and hold the plunger.
9. Watch the continuous graphics display.
1. An analyte absorbance signal will be generated.
2. Keep the plunger depressed until peak maximum has clearly been
exceeded and the peak starts to fall.
3. Then release the plunger.
4. Note the time taken until you released the plunger.
This is the reaction time.
10. Continue to watch the continuous graphics display.
1. As the analyte element is purged from the system, the absorbance plot
falls toward the baseline.
2. Wait until the plot levels out on the baseline and then note the time taken
from when you released the plunger.
This is the post-reaction purge time.
11. The Read Time you select in the spectrometer method should be 510 s longer
than the reaction time.
2-14
0993-5288
0993-5288
3-1
The recommended analytical conditions for the determination of individual elements are listed alphabetically by element
symbol in this section.
Safe handling of chemicals . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-3
Recommended conditions for arsenic . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-5
Recommended conditions for bismuth . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-7
Recommended conditions for antimony . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-13
Recommended conditions for selenium . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-15
Recommended conditions for tin . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-17
Recommended conditions for tellurium . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-19
MHS 15:
Recommended Analytical Conditions 3
3MHS 15: Recommended Analytical Conditions
Marker for header
Contents
page
MHS 15: Recommended Analytical Conditions
3-2
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3-3
Safe handling of chemicals
Some chemicals used with the instrument may be hazardous or may become
hazardous after completion of an analysis.
Use, store, and dispose of chemicals in accordance with the manufacturers
recommendations and the applicable national, state, and/or local regulations.
Wear appropriate eye protection at all times while handling chemicals.
Depending on the types of chemicals you are handling, wear safety glasses
with side shields, or goggles, or a full-face shield.
Wear suitable protective clothing, including gloves if necessary, resistant to
the chemicals you are handling.
When preparing chemical solutions, always work in a fume hood that is
suitable for the chemicals you are using.
Perform sample preparation away from the instrument to minimize corrosion
and contamination.
Clean up spills immediately using the appropriate equipment and supplies,
such as spill cleanup kits.
Sodium tetrahydroborate
Sodium tetrahydroborate is used as a reductant in the mercury cold vapor
technique and the hydride-generation technique. Sodium tetrahydroborate
solutions are unstable and decompose, releasing hydrogen. Sodium
tetrahydroborate also releases hydrogen when it comes into contact with acids.
Make sure that the work area has an adequate ventilation system to prevent
the build-up of explosive air-hydrogen mixtures.
Use and store sodium tetrahydroborate according to the manufacturers
recommendations.
Keep sodium tetrahydroborate solutions:
Out of direct sunlight.
Away from open flames.
In an area with an efficient ventilation system.
Protect sodium tetrahydroborate solutions from temperature variations.
Handle sodium tetrahydroborate solutions with care since they are corrosive.
Do not allow smoking in areas where sodium tetrahydroborate is used.
3-4
0993-5288
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3-5

Recommended conditions for arsenic
Reagents 0.15 mol/L (] 1.5% V/V)
hydrochloric acid:
0.25 mol/L (] 1% W/V)
NaOH solution:
0.8 mol/L (] 3% W/V)
NaBH
4
solution:
Carefully add 15 mL conc. HCl to
deionized water and make up to 1 L.
Carefully dissolve 10 g sodium
hydroxide flakes in deionized water
and make up to 1 L.
Dissolve 3 g sodium tetrahydroborate
in 1% NaOH solution and make up to
100 mL with 1% NaOH solution.
Stock solution The stock solution contains 1000 mg/L As.
The use of commercially-available concentrated calibration solutions
for AAS is recommended.
Warning: Arsenic solutions are toxic.
Calibration solution
Aliquots for calibration:
Corresponding to:
Diluent:
Calibration volume:
1 mg As/L (in 1.5% HCl)
10, 25, 50 L
10, 25, 50 ng As
1.5% (V/V) hydrochloric acid
10 mL
(Refer to Calibration techniques on page 9-6 for more information)
Reductant solution 3% NaBH
4
in 1% NaOH solution.
Oxidation state The hydride is generated much more slowly from As(V) than from
As(III). To prevent interferences, As(V) must be prereduced to As(III)
prior to the determination.
Prereduction can be performed with KI in semiconcentrated (5 mol/L)
HCl solution or, preferably, with L-cysteine
1, 2
.
References: 1. Welz, B.; M. ucmanov, Analyst (London) 118/11, 14171423 (1993)
2. Welz, B.; M. ucmanov, Analyst (London) 118/11, 14251432 (1993)
As
3-6
0993-5288
Recommended conditions for arsenic (cont.)
Prereduction 1. KI solution: Dissolve 3 g KI and 5 g L(+)-ascorbic acid in 100 mL
water. Prepare fresh daily. Add 1 mL of the KI solution per 10 mL of
the sample solution in 5 mol/L HCl and stand for 30 min.
or
2. L-cysteine solution: Dissolve 5 g L-cysteine in 100 mL 0.5 mol/L
HCl. This solution is stable for at least a month. Add 2 mL of the
L-cysteine solution per 10 mL of the sample solution and stand for
30 min.
Analytical wavelength 193.7 nm
Slit width and height 0.7 nm Low
Radiation source Electrodeless discharge lamp for As.
QTA heating Heat the QTA in a lean, blue air-acetylene flame.
Prepared measurement
volume
10 mL minimum to 50 mL maximum.
Pre-reaction purge time approx. 50 s
Post-reaction purge time approx. 40 s
Characteristic mass 0.95 ng As for 1% absorption (A=0.0044).
Characteristic
concentration
0.095 g/L / 1% absorption for 10 mL calibration volume.
Characteristic
concentration check
50 L of the 1000 mg/L As stock solution (50 ng) give an absorbance
of approx. A=0.2.
Alternate analytical
wavelengths
Wavelength
nm
Slit width
nm
Sensitivity relative to main
analytical wavelength
189.0
197.2
0.7
0.7
0.8
2.0
Notes Condition the QTA in cold hydrofluoric acid if there is a decrease in
sensitivity (and other causes are excluded) (procedure: page 4-8).
0993-5288
3-7
Recommended conditions for bismuth
hydrochloric acid:
0.25 mol/L (] 1% W/V)
NaOH solution:
0.8 mol/L (] 3% W/V)
NaBH
4
solution:
and make up to 1 L.
Stock solution The stock solution contains 1000 mg/L Bi.
Corresponding to:
Diluent:
Calibration volume:
1 mg Bi/L (in 1.5% HCl)
25, 50, 100 L
25, 50, 100 ng Bi
10 mL
4
Oxidation state The rate of hydride-generation is different for Bi(V) and Bi(III). To
prevent interferences, Bi(V) must be prereduced to Bi(III) prior to the
determination.
Bi(V) is reduced immediately to Bi(III) by the addition of conc. HCl.
Bi
3-8
0993-5288
Recommended conditions for bismuth (cont.)
Radiation source Electrodeless discharge lamp for Bi.
volume
Characteristic mass 1.46 ng Bi for 1% absorption (A=0.0044).
Characteristic
concentration
Characteristic
concentration check
100 L of the 1000 mg/L Bi stock solution (100 ng) give an absorbance
of approx. A=0.3.
wavelengths
Wavelength
nm
Slit width
nm
222.8
306.8
206.2
227.7
0.2
0.7
0.2
0.2
2.4
3.7
8.6
14.0
0993-5288
3-9
Recommended conditions for mercury
Using sodium tetrahydroborate (NaBH
4
) as reductant
hydrochloric acid:
0.22 mol/L (] 1.5% V/V)
nitric acid:
5% (W/V) KMnO
4
solution:
0.25 mol/L (] 1% W/V)
NaOH solution:
0.8 mol/L (] 3% W/V) NaBH
4

solution:
Carefully add 15 mL conc. HNO
3
to
Dissolve 5 g potassium permanganate
in deionized water and make up to
100 mL.
and make up to 1 L.
Stock solution The stock solution contains 1000 mg/L Hg.
Warning: Mercury solutions are toxic.
Corresponding to:
Diluent:
Calibration volume:
1 mg Hg/L (in 1.5% HNO
3
, stabilized by the addition of a few drops of
5% KMnO
4
solution)
100, 200, 500 L
100, 200, 500 ng Hg
1.5% (V/V) nitric acid or 1.5% (V/V) hydrochloric acid
10 mL
4
Hg
3-10
0993-5288
Recommended conditions for mercury using NaBH
4
(cont.)
Radiation source Electrodeless discharge lamp or hollow cathode lamp for Hg.
QTA heating No flame required.
If condensation in the QTA is a problem, heat the QTA gently by
mounting an infrared lamp above it.
volume
Characteristic mass 4.68 ng Hg for 1% absorption (A=0.0044).
Characteristic
concentration
Characteristic
concentration check
250 L of the 1000 mg/L Hg stock solution (250 ng) give an
absorbance of approx. A=0.2.
Notes Stabilize stock and calibration solutions by adding KMnO
4
or KI
solution. (Refer to Reagents and calibration solutions on page 9-8 for
more information.)
Stabilize all solutions in the reaction flask by adding 1 drop of 5%
(W/V) KMnO
4
solution before starting the determination.
0993-5288
3-11
Recommended conditions for mercury
Using tin(II) chloride (SnCl
2
) as reductant
Reagents
0.15 mol/L (] 1.5% V/V)
hydrochloric acid:
1 mol/L (] 10% V/V)
hydrochloric acid:
0.22 mol/L (] 1.5% V/V)
nitric acid:
5% (W/V) KMnO
4
solution:
5% (W/V) SnCl
2
solution:
3
to
Dissolve 5 g potassium permanganate
in deionized water and make up to
100 mL.
Dissolve 50 g tin(II) chloride dihydrate
(SnCl
2
2H
2
O) in 10% HCl solution
and make up to 1 L with 10% HCl
solution.
Stock solution The stock solution contains 1000 mg/L Hg.
Warning: Mercury solutions are toxic.
Corresponding to:
Diluent:
Calibration volume:
1 mg Hg/L (in 1.5% HNO
3
, stabilized by the addition of a few drops of
5% KMnO
4
solution)
100, 200, 500 L
100, 200, 500 ng Hg
1.5% (V/V) nitric acid or 1.5% (V/V) hydrochloric acid
10 mL
Reductant solution 5% SnCl
2
2H
2
O in 10% HCl solution.
Hg
3-12
0993-5288
Recommended conditions for mercury using SnCl
2
(cont.)
Radiation source Electrodeless discharge lamp or hollow cathode lamp for Hg.
QTA heating No flame required.
If condensation in the QTA is a problem, heat the QTA gently by
mounting an infrared lamp above it.
volume
Characteristic mass 4.68 ng Hg for 1% absorption (A=0.0044).
Characteristic
concentration
Characteristic
concentration check
250 L of the 1000 mg/L Hg stock solution (250 ng) give an
absorbance of approx. A=0.2.
Notes Stabilize stock and calibration solutions by adding KMnO
4
solution.
Do not use KI solution since iodide interferes in the release of mercury.
(Refer to Reagents and calibration solutions on page 9-8 for more
information.)
Stabilize all solutions in the reaction flask by adding 1 drop of 5%
(W/V) KMnO
4
solution before starting the determination.
0993-5288
3-13
Recommended conditions for antimony
Reagents 0.3 mol/L (] 3% V/V)
hydrochloric acid:
0.15 mol/L (] 1.5% V/V)
hydrochloric acid:
0.25 mol/L (] 1% W/V)
NaOH solution:
0.8 mol/L (] 3% W/V)
NaBH
4
solution:
and make up to 1 L.
Stock solution The stock solution contains 1000 mg/L Sb.
Warning: Antimony solutions are toxic.
Corresponding to:
Diluent:
Calibration volume:
1 mg Sb/L (in 1.5% HCl)
50, 100, 200 L
50, 100, 200 ng Sb
3% (V/V) hydrochloric acid
10 mL
4
Oxidation state The hydride is generated much more slowly from Sb(V) than from
Sb(III). To prevent interferences, Sb(V) must be prereduced to Sb(III)
prior to the determination.
Prereduction can be performed with KI in semiconcentrated (5 mol/L)
HCl solution or, preferably, with L-cysteine
1, 2
.
References: 1. Welz, B.; M. ucmanov, Analyst (London) 118/11, 14171423 (1993)
2. Welz, B.; M. ucmanov, Analyst (London) 118/11, 14251432 (1993)
Sb
3-14
0993-5288
Recommended conditions for antimony (cont.)
Prereduction 1. KI solution: Dissolve 3 g KI and 5 g L(+)-ascorbic acid in 100 mL
water. Prepare fresh daily. Add 1 mL of the KI solution per 10 mL of
the sample solution in 5 mol/L HCl.
or
2. L-cysteine solution: Dissolve 5 g L-cysteine in 100 mL 0.5 mol/L
HCl. This solution is stable for at least a month. Add 2 mL of the
L-cysteine solution per 10 mL of the sample solution. Reduction is
spontaneous.
Radiation source Electrodeless discharge lamp for Sb.
volume
Characteristic mass 2.05 ng Sb for 1% absorption (A=0.0044).
Characteristic
concentration
Characteristic
concentration check
100 L of the 1000 mg/L Sb stock solution (100 ng) give an absorbance
of approx. A=0.2.
wavelengths
Wavelength
nm
Slit width
nm
206.8
231.2
0.2
0.2
1.5
2.1
0993-5288
3-15
Recommended conditions for selenium
hydrochloric acid:
0.25 mol/L (] 1% W/V)
NaOH solution:
0.8 mol/L (] 3% W/V)
NaBH
4
solution:
and make up to 1 L.
Stock solution The stock solution contains 1000 mg/L Se.
Warning: Selenium solutions are toxic.
Corresponding to:
Diluent:
Calibration volume:
1 mg Se/L (in 1.5% HCl)
20, 50, 100 L
20, 50, 100 ng Se
10 mL
4
Oxidation state Se(VI) does not generate a measurable signal. To prevent interferences,
Se(VI) must be prereduced to Se(IV) prior to the determination.
Prereduction can be performed by heating with 56 mol/L HCl for 15
30 minutes under reflux
3, 4
.
References: 3. Bye, R.; W. Lund, Fresenius Z. Anal. Chem.332/3, 242244 (1988)
4. Pettersson, J.; . Olin, Talanta 38/4, 413417 (1991)
Se
3-16
0993-5288
Recommended conditions for selenium (cont.)
Radiation source Electrodeless discharge lamp for Se.
volume
Characteristic mass 2.2 ng Se for 1% absorption (A=0.0044).
Characteristic
concentration
Characteristic
concentration check
100 L of the 1000 mg/L Se stock solution (100 ng) give an absorbance
of approx. A=0.2.
wavelengths
Wavelength
nm
Slit width
nm
204.0
206.3
0.7
0.7
3.0
11.0
Notes Potassium iodide (KI) reduces selenium to the element, which does not
react to form the hydride. Systems that have been contaminated with
high concentrations of KI must be thoroughly cleaned before they can
be used for the determination of selenium.
0993-5288
3-17
Recommended conditions for tin
Reagents saturated boric acid solution:
0.05 mol/L (] 0.5% V/V)
hydrochloric acid:
0.15 mol/L (] 1.5% V/V)
hydrochloric acid:
0.25 mol/L (] 1% W/V)
NaOH solution:
0.8 mol/L (] 3% W/V)
NaBH
4
solution:
approx. 50 g/L H
3
BO
4
in 0.5%
hydrochloric acid.
and make up to 1 L.
Stock solution The stock solution contains 1000 mg/L Sn.
Corresponding to:
Diluent:
Calibration volume:
1 mg Sn/L (in 1.5% HCl)
20, 50, 100 L
20, 50, 100 ng Sn
saturated boric acid solution
25 mL
4
Sn
3-18
0993-5288
Recommended conditions for tin (cont.)
Radiation source Electrodeless discharge lamp for Sn.
volume
Characteristic mass 2.2 ng Sn for 1% absorption (A=0.0044).
Characteristic
concentration
Characteristic
concentration check
100 L of the 1000 mg/L Sn stock solution (100 ng) give an absorbance
of approx. A=0.2.
wavelengths
Wavelength
nm
Slit width
nm
224.6
235.5
270.7
303.4
254.7
219.9
300.9
233.5
0.2
0.7
0.7
0.2
0.7
0.2
0.7
0.7
1.8
1.6
2.9
3.8
5.4
5.7
6.9
6.9
Notes Memory signals are occasionally encountered during the determination
of tin.
Condition the QTA in cold hydrofluoric acid if there is a decrease in
0993-5288
3-19
Recommended conditions for tellurium
hydrochloric acid:
0.3 mol/L (] 3% V/V)
hydrochloric acid:
0.44 mol/L (] 3% V/V)
nitric acid:
0.25 mol/L (] 1% W/V)
NaOH solution:
0.8 mol/L (] 3% W/V)
NaBH
4
solution:
3
to
and make up to 1 L.
Stock solution The stock solution contains 1000 mg/L Te.
Warning: Tellurium solutions are very toxic.
Corresponding to:
Diluent:
Calibration volume:
1 mg Te/L (in 1.5% HCl)
20, 50, 100 L
20, 50, 100 ng Te
3% (V/V) hydrochloric acid + 3% (V/V) nitric acid
10 mL
4
Oxidation state Te(VI) does not generate a measurable signal. To prevent interferences,
Te(VI) must be prereduced to Te(IV) prior to the determination.
Prereduction can be performed by heating briefly with 56 mol/L HCl.
Te
3-20
0993-5288
Recommended conditions for tellurium (cont.)
Radiation source Electrodeless discharge lamp for Te.
volume
Characteristic mass 1.1 ng Te for 1% absorption (A=0.0044).
Characteristic
concentration
Characteristic
concentration check
40 L of the 1000 mg/L Te stock solution (40 ng) give an absorbance
of approx. A=0.15.
Notes Condition the QTA in cold hydrofluoric acid if there is a decrease in
0993-5288
4-1
PerkinElmer Service . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-3
Routine maintenance . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-4
Maintaining the flashback arrestor . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-6
QTA maintenance . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-7
Replacing worn parts . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-10
MHS 15: Maintenance 4
4MHS 15: Maintenance
Marker for header
Contents
page
MHS 15: Maintenance
4-2
0993-5288
MHS 15: Maintenance
0993-5288
4-3
PerkinElmer Service
If the instrument does not function correctly
Contact your local PerkinElmer office.
You should only perform the maintenance procedures described in this guide.
For any other maintenance or service contact your local PerkinElmer office to
arrange for a service engineer to visit.
In particular you must only allow a PerkinElmer service engineer or PerkinElmer
trained person to perform any work on the pneumatic components inside the
instrument.
Before the service engineer arrives:
1. Make sure that the instrument and the work area are clean.
2. Make certain that there are no corrosive solutions present in any of the tubes.
W1.2
Warning: Unauthorized Adjustments and Servicing
Only a PerkinElmer service engineer or similarly trained and authorized person
should be permitted to service the instrument.
Do not attempt to make adjustments, replacements, repairs, or modifications
to this instrument except as described in the documentation supplied with the
instrument.
MHS 15: Maintenance
4-4
0993-5288
Routine maintenance
The MHS 15 is a precision instrument constructed from high quality components.
To maintain the high level of performance, you must treat the instrument with due
care.
Maintenance checklist
External surfaces Regularly wipe over the surfaces with a lint-free cloth
moistened with a dilute solution of laboratory detergent.
The surfaces are resistant to dilute acids and alkalis, and to a
lesser extent to strong acids and alkalis and organic solvents.
Immediately clean all spilled materials from the affected
area. Wear protective gloves if the materials are toxic or
corrosive.
Remove the drip tray and wash it in detergent solution as
required.
Reaction flask During routine operation, rinse the reaction flask with dilute
acid at regular intervals.
For mercury use 1.5% to 3% (V/V) nitric acid.
For hydride-forming elements use 1.5% to 3% (V/V)
hydrochloric acid.
Immersion tube During routine operation, rinse the outside of the immersion
tube with dilute acid after every measurement, and
periodically remove it and rinse it with dilute acid.
Reductant bottle At the end of the working day, unscrew the reductant bottle
from the reactor assembly and place it in a fume hood.
Do not stopper a bottle containing NaBH
4
.
Reductant
transport system
At the end of every working day, purge the reductant
transport system well with deionized water (procedure:
page 4-5).
Flashback
arrestor
Check the baffle in the flashback arrestor regularly to make
sure that it has not become blocked (procedure: page 4-6).
Transfer tube Check the condition of the transfer tube regularly. If it shows
signs of deterioration, or has become seriously
contaminated, replace it (more information: page 4-10).
MHS 15: Maintenance
0993-5288
4-5
Reductant transport system
At the end of every working day, purge (flush) the reductant transport system well
with deionized water.
1. Unscrew the reductant bottle from the reactor assembly and place it in a fume
hood. Do not stopper the bottle if it contains NaBH
4
.
2. Screw a plastic bottle containing deionized water into the fitting in the reactor
assembly.
3. Place a beaker under the immersion tube.
4. Press and hold down the plunger for some time so that the reductant transport
tubes are well purged with deionized water.
5. Empty the beaker and unscrew the plastic bottle.
6. Shut down the inert gas supply at source.
Disposing of reaction residues
Do not empty the reaction flask directly into the laboratorys waste water system;
there may be an excess of NaBH
4
or SnCl
2
in the flask.
Collect the reaction residues in a suitable waste container. Store the waste
container in a fume hood and make sure that the contents are sufficiently acidic
so that NaBH
4
residues react completely. Do not put a cap on the waste container.
Contents of waste containers
The materials that you collect in waste containers include small amounts of the
substances that were analyzed and other chemicals used in the analyses.
If these materials are toxic, corrosive, or contain organics you may have to treat
the collected effluent as hazardous waste. Refer to your local safety regulations
for proper disposal procedures.
MHS 15: Maintenance
4-6
0993-5288
Maintaining the flashback arrestor
Check the flashback arrestor regularly to see that the internal baffle has not
become blocked. Always clean the baffle if any solution is transported into it.

Check and clean the flashback arrestor as follows:
1. Shut down the inert gas supply at source.
2. Disconnect the transfer tube from the QTA.
3. Screw the flashback arrestor apart and take out the perforated baffle.
4. Check the holes in the baffle for blockage.
Soak the baffle in dilute hydrochloric acid, if required.
Rinse the baffle with deionized water and dry before reassembly.
5. Place the baffle back into the arrestor, screw the arrestor back together, and
reconnect the transfer tube to the QTA.
Warning: Pressure buildup in the system
Blockage of any of the holes in the baffle reduces the flow rate of gas to the QTA.
Severe blockage can cause a pressure buildup in the reaction flask.
Check the baffle regularly to make sure that none of the holes are blocked.
W4.5
Warning: High Temperatures Risk of Burns
The burner head, QTA burner mount, and QTA can reach high temperatures.
When you handle the mount or the QTA, wear flame- and heat-resistant
gloves or wait until the mount and QTA have cooled to room temperature.
Transfer tube
to reactor assembly
Baffle
MHS 15: Maintenance
0993-5288
4-7
QTA maintenance
The sensitivity that can be attained with the hydride-generation technique is
critically dependent on the condition of the inner surface of the QTA. This is
especially the case for the determination of arsenic, tellurium, and tin. The
condition of the quartz inner surface can, under given circumstances, be
responsible for a deterioration in the sensitivity.
Under normal working conditions the inner surface of the QTA only requires
cleaning if the sensitivity is significantly reduced, or if the QTA has become
seriously contaminated (e.g. by solution from the reaction flask foaming over into
it). If there is a marked decrease in the sensitivity, make sure that this is not due
to other factors, such as unsuitable analytical parameters or instrument settings,
or aged solutions, before you clean the inner surface of the QTA.
Note: After prolonged use the inner surface of the QTA may become opaque.
This is normal and does not affect the sensitivity.
Cleaning the inner surface of the QTA
1. Where applicable, tilt the QTA out of the flame and allow it to cool before
removing it from the mount.
2. Carefully pull the transfer tube off the side inlet tube of the QTA.
3. Remove the graphite cooling rings from the ends of the QTA by very
carefully pulling them out of the sleeves.
Note: The graphite cooling rings are fragile. Handle them with care.
4. Remove the sleeves from the ends of the QTA.
If the sleeves are difficult to remove, refer to page 4-12.
5. Wash the QTA out well in running water.
Do not use sharp or pointed tools to scrape the inside of the QTA.
6. Rinse the QTA thoroughly with deionized water and then dry in a drying
cabinet.
W4.5
MHS 15: Maintenance
4-8
0993-5288
7. Refit the sleeves on the ends of the QTA and carefully insert the graphite
cooling rings into the sleeves (more information: page 4-12).
8. Reconnect the transfer tube to the QTA and place the QTA back in the mount.
9. Perform a characteristic mass measurement. If cleaning has not improved the
sensitivity, condition the QTA as described in the next section.
Conditioning the QTA
Note: The QTA is conditioned at the factory before shipment. Before you
condition the QTA, make certain that there are no other causes for the loss in
sensitivity, such as aged or contaminated calibration solutions or reductant
solutions, or improper spectrometer settings.
Use a suitable plastic container for the hydrofluoric acid bath. The container
should be suitably large so that you can place the QTA in the container and the
acid level comes up to the side inlet tube. A plastic storage box from a
PerkinElmer hollow cathode lamp is ideal for this purpose.
W8.1
Warning: Hydrofluoric Acid Risk of Burns
Hydrofluoric acid (HF) is toxic, corrosive, and can cause severe burns.
When using hydrofluoric acid, always wear suitable protective clothing
including a face mask, work in a fume hood, and observe the manufacturers
instructions and your local safety regulations.
QTA
Hydrofluoric acid
Plastic container
MHS 15: Maintenance
0993-5288
4-9
1. Prepare the QTA as described in steps 1 through 5, above.
2. Carefully place the QTA in a bath of cold concentrated hydrofluoric acid and
allow it to stand for 1015 minutes.
3. Very carefully remove the QTA and thoroughly rinse it under running water.
4. Rinse the QTA thoroughly with deionized water and then dry in a drying
cabinet.
5. Refit the sleeves on the ends of the QTA and carefully insert the graphite
cooling rings into the sleeves ( more information: page 4-12).
7. Check the characteristic mass.
MHS 15: Maintenance
4-10
0993-5288
Replacing worn parts
Gasket in the reaction flask socket
After prolonged operation, the gasket in the reaction flask socket may lose its
resilience and cease to be gastight. You should replace the gasket when a good
seal with the reaction flask is no longer provided.
Five replacement gaskets are provided with the instrument.
Transfer tube
Check the condition of the transfer tube between the reactor assembly and the
QTA regularly. If it shows signs of deterioration, such as brittleness or cracks, or
if it has become seriously contaminated, you should replace it.
Replace the transfer tube as follows:
W4.5
Gasket in reaction flask socket
MHS 15: Maintenance
0993-5288
4-11
3. Carefully pull the transfer tube off the nozzle at the side of the reaction flask
socket.
4. Pull the long and the short sections of transfer tube off the flashback arrestor.
Discard the old transfer tube.
5. Take the replacement transfer tube and cut off a piece 5 cm long.
Push this piece onto the body of the flashback arrestor.
6. Push the longer piece of transfer tube onto the screw-in cap of the flashback
arrestor.
7. Carefully push the replacement transfer tube onto the nozzle at the side of the
reaction flask socket.
8. Carefully push the end piece of the transfer tube onto the side inlet tube of the
QTA.
Note: Use only original replacement transfer tubes. Do not use any other type
of tube.
MHS 15: Maintenance
4-12
0993-5288
Sleeves on the QTA
After a long period of use, particularly at the temperatures involved, the sleeves
retaining the graphite cooling rings tend to seal onto the quartz surface of the
QTA. If this problem arises, do not apply force to remove the sleeves since you
may break the QTA. Carefully cut off the old sleeves using a sharp scalpel.
Figure 4-1. QTA, sleeves and graphite rings
Replace sleeves as follows:
3. Remove the graphite cooling rings from the ends of the QTA by very
carefully pulling them out of the sleeves.
Note: The graphite cooling rings are fragile. Handle them with care.
4. Remove the sleeves from the ends of the QTA.
If it is not possible to pull the sleeves off, carefully cut them off using a sharp
scalpel.
W4.5
Graphite ring
Sleeve
QTA
MHS 15: Maintenance
0993-5288
4-13
5. Fit new sleeves on the ends of the QTA.
The sleeves are dusted on the inside with talcum powder; this aids fitting and reduces
the tendency to sticking.
6. Carefully insert the graphite cooling rings into the sleeves.
MHS 15: Maintenance
4-14
0993-5288
0993-5288
5-1
Parts provided . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-3
Obtaining supplies, replacement parts, and accessories . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-4
Replacement parts . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-5
MHS 15:
Parts and Supplies 5
5MHS 15: Parts and Supplies
Marker for header
Contents
page
MHS 15: Parts and Supplies
5-2
0993-5288
0993-5288
5-3
Parts provided
PerkinElmer reserves the right to alter the schedule of parts provided without prior notice.
Qty. Item Part No.
1 MHS 15 reactor assembly . . . . . . . . . . . . . . . . . . . . . . . . B314-0763
1 QTA burner mount . . . . . . . . . . . . . . . . . . . . . . . . . . . . . B300-0350
2 Quartz tube atomizers,
complete with graphite rings and sleeves . . . . . . . . . . . . B009-4414
2 Reaction flasks . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . B009-4139
3 Covers for reaction flasks . . . . . . . . . . . . . . . . . . . . . . . . B009-4152
2 Plastic bottles, 500 mL . . . . . . . . . . . . . . . . . . . . . . . . . . B009-4032
1 Drip tray . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . B314-0735
1 Gas supply tube . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . B007-9873
2 Replacement QTA sleeves (pack of 4) . . . . . . . . . . . . . . B050-5881
5 Gaskets for reaction flask socket . . . . . . . . . . . . . . . . . . B010-4049
1 Adhesive label NaBH
4
. . . . . . . . . . . . . . . . . . . . . . . . . B010-4053
1 Adhesive label SnCl
2
. . . . . . . . . . . . . . . . . . . . . . . . . . B010-4052
1 Users Guide . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 0993-5288
1 Quick Reference . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 0993-5289
5-4
0993-5288
Obtaining supplies, replacement parts, and accessories
Supplies, replacement parts, and accessories can be ordered directly from
PerkinElmer, using the part numbers quoted in this guide. PerkinElmers catalog
service offers a full selection of high-quality atomic spectroscopy supplies
through the Atomic Spectroscopy Supplies Catalog.
To place an order for supplies and many replacement parts, request a free catalog,
or ask for information:
If you are located within the U.S., call toll free 1-800-762-4002, 8 a.m. to
8 p.m. EST. Your order will be shipped promptly, usually within 24 hours.
If you are located outside of the U.S., call your local PerkinElmer sales or
service office.
What is listed in this chapter
This chapter lists the most important replacement parts for MHS 15 system.
Information about other parts and accessories is given in the current PerkinElmer
brochures and price lists.
0993-5288
5-5
Replacement parts
Item Part No.
Reaction flask . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. . . . . . . B009-4139
Immersion tube . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. . . . . . . B009-4138
Gasket for reaction flask socket . . . . . . . . . . . . . . . . . . .. . . . . . . B010-4049
Transfer tube. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. . . . . . . B009-4140
Flashback arrestor . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . B009-8640
Quartz tube atomizer,
complete with graphite rings and sleeves. . . . . . . . . . . . .. . . . . . . B009-4415
Quartz tube atomizer,
without graphite rings or sleeves . . . . . . . . . . . . . . . . . . . . . . . . . . B009-4414
QTA sleeves (pack of 4) . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . B050-5881
Graphite cooling ring . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . B009-4413
Reductant bottle . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . B009-4032
Drip tray . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. . . . . . . B314-0735
5-6
0993-5288
0993-5288
6-1
Unpacking and inspection . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6-3
Installing the QTA burner mount . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6-4
Installing the reactor assembly . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6-6
Connecting the inert gas supply . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6-6
Preparing the reactor assembly . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6-8
MHS 15:
Installation 6
6MHS 15: Installation
Marker for header
Contents
page
MHS 15: Installation
6-2
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0993-5288
6-3
Unpacking and inspection
The MHS 15 is shipped in a single packing carton.
After you receive the instrument, unpack the components carefully:
1. Open the carton and remove packing materials.
2. Lift out the QTA Burner mount and the cartons containing small parts.
3. Carefully lift out the MHS 15 and place it on the bench.
4. Examine the components for any signs of damage during shipment.
In the event of damage, file an immediate claim with the authorized carrier,
and inform your local PerkinElmer office or representative.
A list of parts provided is given under MHS 15: Parts and Supplies on page 5-3.
Carton recycling instructions
The carton can be folded down for easy storage. You can store the carton for
future use (to transport the instrument), recycle it by returning it to PerkinElmer,
or break it down completely and give it to your local recycling center.
6-4
0993-5288
Installing the QTA burner mount
To install the QTA burner mount (QTA=quartz tube atomizer) you must remove
the burner head, attach the mount to the burner head, and then reinstall the burner
head.
Remove the burner head
1. Where applicable, extinguish the flame, allow the burner head to cool, shut
down the gases at source, and bleed the gas supply lines (the correct procedure
is described in the Users Guide for your AA spectrometer).
2. Remove the burner head as described in the Users Guide for your AA
spectrometer.
Attach the QTA burner mount
Note: A heat shield is provided with the QTA burner mount. You only require
the heat shield if your spectrometer is a Model 3100, 3110, or 3300.
1. Tilt the QTA bracket on the mount into the up position.
2. Slacken (but do not remove) the two adjusting screws in each securing clamp.
3. Slide the QTA burner mount onto the burner head and position the two
securing clamps over the ends of the burner head. The QTA bracket must be
at the front of the burner head.
4. Tighten the adjusting screws, but leave them slack enough so that you can
move the mount.
Align the QTA burner mount
1. Tilt the QTA bracket into the down position.
2. Visually sight along the burner slot and move the QTA burner mount with
respect to the burner head until the two Vs in the QTA bracket line up with
the burner slot.
3. Tighten the adjusting screws in the securing brackets.
W4.2
The burner head can reach very high temperatures.
Do not touch the burner head until it has cooled to room temperature.
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6-5
Figure 6-1. Attaching the QTA burner mount to the burner head
Figure 6-2. Aligning the QTA burner mount on the burner head
Reinstall the burner head
1. Reinstall the burner head as described in the Users Guide for your AA
spectrometer.
Note: The QTA burner mount can remain permanently installed on the burner
head.
If you wish to change over to normal flame analyses, tilt the QTA bracket to the
up position and park the QTA in the holder at the back of the reactor assembly.
Move the reactor assembly away from the immediate vicinity of the atomizer
compartment.
QTA bracket
in up position
Securing clamp
(1 of 2)
Adjusting screw
(2 each clamp)
Burner head
Burner head
seen from the
rear
Burner slot
V in QTA
bracket
QTA bracket
in down position
6-6
0993-5288
Installing the reactor assembly
Connecting the inert gas supply
What you need to provide
A suitable supply of argon or nitrogen. The gas must conform with the
requirements listed in MHS 15: Laboratory Requirements on page 7-6.
A suitable pressure regulator and on/off valve near to the system for the inert
gas supply.
The gas supply system must comply with your local safety regulations.
Refer also to the information given under Handling compressed gases on page
1-9.
What is provided with the MHS 15
Gas supply tube, B007-9873
To connect the inert gas
The connector for the inert gas is located underneath at the rear of the reactor
assembly.
Refer to Figure 6-3 on the following page.
1. Make sure that the gas supply is turned off.
2. Connect the gas supply tube to the argon (or nitrogen) pressure regulator. Use
the R '' screw connector provided or use a connector or adapter suitable for
the gas regulator. Make sure that all the connections are secure.
3. Pass the gas supply tube to the rear of the reactor assembly. Make sure that
the tube cannot be damaged or strained.
4. Connect the gas supply tube to the reactor assembly:
1. Unscrew the nut from the connector and slide the nut onto the gas supply
tube.
2. Push the gas supply tube onto the fitting on the connector.
3. Screw the nut finger-tight back onto the connector.
0993-5288
6-7
Figure 6-3. Connecting the inert gas
Inert Gas
Gaz inerte
Inertgas
Pmin
250
2.5
36
Pmax
350
3.5
51
kPa
bar
psig
N or Ar only
Nur
2
N ou Ar seulement
N oder Ar
2
2
Inert gas supply
nitrogen or argon
Gas supply tube
Connector for
gas supply tube
6-8
0993-5288
Preparing the reactor assembly
Figure 6-4. MHS 15 reactor assembly and QTA
1. If not already done, place the drip tray onto the base of the reactor assembly.
2. Slip an immersion tube carefully over the capillary tube and onto the
connector of the reaction flask socket.
Note: Do not kink or damage the capillary tube.
3. Take the transfer tube (fitted with flashback arrestor) that emerges from the
side of the reaction flask socket and carefully push the end piece of the tube
onto the side arm of the QTA.
4. Place the QTA in the holder at the back of the reactor assembly.
Drip tray
Immersion tube
Connector
Reaction flask socket
Transfer tube
Flashback
arrestor
QTA
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7-1
Operating conditions . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-3
Gas supply requirements . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-5
Inert gas . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-6
MHS 15:
Laboratory Requirements 7
7MHS 15: Laboratory Requirements
Marker for header
Contents
page
MHS 15: Laboratory Requirements
7-2
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7-3
Operating conditions
Operating requirements
The spectrometer and mercury/hydride system will operate correctly under the
following conditions:
Indoors.
Ambient temperature +15 C to +35 C (+59 F to +95 F), with a maximum
change not exceeding 2.8 C (5 F) per hour.
The location must be free of dust, smoke, and corrosive fumes.
Bench and location requirements
The location you choose for the spectrometer and mercury/hydride system must
fulfil the criteria listed below:
Place the spectrometer on a sturdy bench or trolley (cart) capable of sustaining
the weight. The work surface must be level, flat, clean, dry, and free from
vibration. It should be strong and stiff enough to bear the weight of the
spectrometer system over a long period without warping or bending. A
movable table is very convenient, but make sure that the wheels can be
securely locked.
Position the bench or trolley out of direct sunlight and away from radiators
and heaters.
Position the system near to the electricity and gas supply points.
Position the system so that the atomizer compartment is located beneath a
suitable fume ventilation system.
Make sure that there is space at the rear and sides of the system for air to
circulate freely.
W1.3
7-4
0993-5288
Make sure that there is sufficient room for you to work comfortably with the
instruments, and that you can reach the connections at the rear of the
instruments and the electricity and gas supply points.
Fume ventilation
You must provide an efficient fume ventilation system to remove the fumes
generated by the atomizer.
The specification for a suitable system is described in brochure no. L-301
Preparing Your Laboratory for PerkinElmer Atomic Spectroscopy Instruments.
This brochure is available from PerkinElmer.
Warning: Toxic Gases Fume Ventilation System
Without adequate ventilation, potentially toxic vapors can build up in the
laboratory.
Your laboratory must have a reliable fume ventilation system before you use
this instrument.
0993-5288
7-5
Gas supply requirements
The permanent installation of gas supplies is the responsibility of the user and
should conform to local safety and building regulations.
PerkinElmer recommends that cylinders be stored outside the laboratory and that
gases be piped to the spectrometer system in approved gas lines.
The user must provide the gas supplies, regulators, connectors, and valves.
Either the gas supplier or PerkinElmer can supply the correct regulators and
valves.
You must be able to reach the on/off valves easily and see the pressure
indicators.
Consult the chapter entitled Safety and Regulatory Information for
recommended safety procedures.
Warning: Compressed Gases
High pressure gas cylinders can be dangerous if mishandled or misused.
Always handle gas cylinders with caution and observe your local regulations
for the safe handling of gas cylinders.
7-6
0993-5288
Inert gas
The MHS 15 requires a supply of argon or nitrogen to operate the pneumatic
system and to provide purging facilities. The specifications and requirements for
the inert gas are listed in Table 7-1.

Set the outlet gauge pressure for the gas supply exactly to 250 kPa (P
min
).
Never set the outlet pressure to a value exceeding the maximum pressure
(P
max
).
Note: Since the pressure of the inert gas to the MHS 15 has a slight influence on
the flow rate of the gas through the system, always set the pressure consistently
to 250 kPa.
Table 7-1. Specifications and Requirements for the Inert Gas
Gas Purity Outlet Gauge Pressure Max. Flowrate
kPa bar psig
mL/min
(nominal) at
250 kPa
P
min
P
max
P
min
P
max
P
min
P
max
NaBH
4
SnCl
2
Argon 99.996% 250 350 2.5 3.5 36 51 700 1100
Nitrogen 99.996% 250 350 2.5 3.5 36 51 700 1100
0993-5288
8-1
Introduction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8-3
Chemical vapor generation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8-6
The cold vapor technique . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8-6
The hydride-generation technique . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8-6
Literature on chemical vapor generation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8-7
Principle of operation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8-8
Technical data . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8-11
MHS 15:
System Description 8
8MHS 15: System Description
Marker for header
Contents
page
MHS 15: System Description
8-2
0993-5288
0993-5288
8-3
Introduction
Figure 8-1. MHS 15 Mercury Hydride System reactor assembly
The MHS 15 Mercury Hydride System is a manually-operated accessory for
chemical vapor generation that allows the high-sensitivity determinations of
mercury and the metallic hydride-forming elements by atomic absorption
spectrometry. The MHS 15 comprises a reactor assembly and a quartz tube
atomizer (QTA) assembly.
Reactor assembly
The reactor assembly is free-standing and is placed adjacent to the AA
spectrometer. This assembly includes a reaction flask, a reservoir bottle for the
reductant solution, and all pneumatic components for control of the carrier gas
and transport of the analyte vapors to the QTA. A holder at the back of the reactor
assembly allows you to park the QTA when you are not using the system.
The socket on the reactor assembly for the reaction flask includes a bayonet lock.
The reaction flasks are provided with bayonet lugs so that you can easily attach
and remove the reaction flasks from the reactor assembly.
Transfer tube
Reductant
bottle
Reaction flask
Flashback arrestor
to QTA
Plunger
Reductant changeover valve
8-4
0993-5288
Quartz tube atomizer (QTA)
The QTA assembly consists of the quartz tube atomizer and a burner mount.
The burner mount installs on any PerkinElmer standard 10 cm burner head, thus
permitting the QTA to be heated in the flame of the AA spectrometer. The QTA
is located in the spectrometers sample radiation beam and can be aligned in the
beam by means of the burners alignment controls. A hinged bracket on the burner
mount allows you to tilt the QTA out of the flame.
The QTA resembles a cylindrical quartz cell. It has a central side tube inlet and is
open at both ends. It is connected to the reactor assembly by a sample transfer
tube. The QTA can be heated to about 1000 C in the air-acetylene flame.
Graphite cooling rings at the QTA ends prevent ignition of the hydrogen liberated
during the determination when sodium tetrahydroborate is used as the reductant.
In the unlikely event that the hydrogen should ignite, a flashback arrestor in the
sample transfer tube prevents a flashback into the reaction flask.
If you wish to use the spectrometer for normal flame analyses, you can remove
the QTA from the mount and park it in the holder at the back of the reactor
assembly. The burner mount can remain permanently installed on the burner
head.
Note: The QTA is referred to as the quartz cell or quartz tube in some
publications.
0993-5288
8-5
Figure 8-2. QTA mounted on the burner
Sample inlet
Hinged QTA bracket
(shown in down position)
Burner head
Burner spray
chamber
QTA
Transfer tube
from reactor assembly
(nebulizer not shown)
8-6
0993-5288
Chemical vapor generation
The cold vapor technique
The cold vapor technique (CV AAS) is used for the determination of mercury.
Depending on the form in which mercury is present in the test sample, the test
sample is treated chemically (digested) to bring mercury into the ionic state in
acidic solution. A reductant is dispensed into the test sample solution and mercury
is reduced to the metallic state. Since mercury has an appreciable volatility even
at ambient temperature, metallic mercury vapor can be driven from solution by a
stream of inert gas and transported to the QTA, where its atomic absorption is
measured.
The reductants used most commonly in the cold vapor technique are sodium
tetrahydroborate (NaBH
4
) and tin(II) chloride (SnCl
2
).
The hydride-generation technique
The hydride-generation technique (HG AAS) is used for the determination of the
hydride-forming elements (As, Bi, Ge, Pb, Sb, Se, Sn, Te).
The test sample is first treated chemically so that the analyte is present in ionic
form in acidic solution. Sodium tetrahydroborate solution is dispensed into the
acidic test sample solution. The reaction of sodium tetrahydroborate in acidic
solution and the simultaneous reduction of the hydride-forming element can be
described simply as follows:
BH
4

+ H
3
O
+
+ 2H
2
O H
3
BO
3
+ 4H
2

and
3BH
4

+ 3H
+
+ 4H
3
AsO
3
4AsH
3
+ 3H
2
O + 3H
3
BO
3
(2)
Equation 2 is representative for all of the hydride-forming elements. These two
equations are coarse simplifications of the actual processes taking place.
The volatile metal hydride (AsH
3
) is driven from solution by a stream of gas and
transported to the heated QTA. The hydride decomposes in the QTA, the analyte
is atomized, and its atomic absorption is measured.
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8-7
Literature on chemical vapor generation
The following monograph provides detailed information on chemical vapor
generation and other aspects of atomic absorption analyses:
B. Welz and M. Sperling, Atomic Absorption Spectrometry,
third, completely revised edition,
Wiley-VCH, New York and Weinheim, 1999,
ISBN 3-527-28571-7
8-8
0993-5288
Principle of operation
Figure 8-3. Schematic of pneumatic system
The MHS 15 is operated pneumatically. The system requires a supply of inert gas
(argon or nitrogen) at an inlet pressure of 250 kPa (2.5 bar; 3637 psig).
The system incorporates a pressure reducer that regulates the pressure of the
incoming inert gas to the system to an overpressure of 10 kPa. From the pressure
reducer the inert gas is split into three streams. One stream flows through flow
restrictor F3 and through line a to the reaction flask. The second stream flows
through flow restrictor F2 and through line b to the changeover valve. The third
stream flows through inlet port 1 to outlet port 2 of the multipath valve and thence
through flow restrictor F1 and line c to the changeover valve. Depending on the
NaBH
4
SnCl
2
F3 F2
F1
a
h
b
c
d
d
e
e
e
Inert gas
QTA
Pressure
reducer
Multipath
valve
Changeover
valve
(in NaBH position)
4
Changeover
valve
(in SnCl position)
2
Burner Reductant
reservoir
Reaction
flask
Immersion
tube
Flashback
arrestor
f
g
g
1
2
4
0993-5288
8-9
setting of the changeover valve, the inert gas flows either through line d or line e
to the reaction flask. If a reaction flask is not attached to the reactor assembly the
inert gas escapes to atmosphere. When a reaction flask is attached, the inert gas
flows through line f and escapes through the QTA. This gas flow purges the
system free of air. Inert gas flows continuously as long as the gas supply is turned
on.
To perform a determination, you attach the reaction flask containing the prepared
measurement solution (blank solution, calibration solution, or test sample
solution) to the reactor assembly, wait for air to be purged from the system (pre-
reaction purge), and then depress and hold the plunger.
While the plunger is depressed the gas stream from port 2 is shut off. Gas pressure
is applied via port 1 to port 4 and then via line g to the reductant bottle. Reductant
solution is forced through line h into the immersion tube and thence into the
measurement solution. The stream of inert gas via F3 and line a through the
immersion tube, together with the conical shape of the reaction flask, promotes
good mixing of the reductant and measurement solutions. At the end of reductant
addition this gas stream also purges the immersion tube free of reductant solution.
Depending on the reductant you are using, one of the following processes takes
place:
Sodium tetrahydroborate (NaBH
4
):
The changeover valve must be set to NaBH4 for this mode of operation.
The violent reaction of the sodium tetrahydroborate solution with the acidic
measurement solution and the liberation of hydrogen further aids in mixing the
solutions. The reaction takes place and the metal hydride or the metallic mercury
vapor is liberated and transported through the transfer tube f to the QTA by the
stream of inert gas through F3 and line a, and also by the hydrogen liberated.
Tin(II) chloride (SnCl
2
):
The changeover valve must be set to SnCl2 for this mode of operation.
Since hydrogen is not liberated during the reaction, an additional stream of inert
gas is required through the immersion tube to promote mixing of the solutions and
to drive out the metallic mercury vapor; this stream of gas comes via F2 and lines
b and e to the immersion tube. The metallic mercury vapor is transported by the
combined gas streams through the transfer tube f to the QTA.
8-10
0993-5288
You hold the plunger depressed for the reaction time determined during methods
development (typically 2030 s). You release the plunger at the end of this time.
The flow of reductant solution to the reaction flask stops immediately and the
purge gas stream via F1 resumes. The reaction proceeds rapidly to completion.
You wait for the post-reaction purge time, after which you can remove the
reaction flask and prepare the next sample.
0993-5288
8-11
Technical data
Quartz tube atomizer
(QTA)
165 mm long, 12 mm diameter.
QTA heating Up to approx. 1200 C in the spectrometers air-acetylene flame.
Reaction flask Polypropylene, with special internal conical form. Connection to the
reactor assembly via bayonet lugs.
Measurement
solution volume
Max 50 mL prepared measurement solution.
Reductants Sodium tetrahydroborate (NaBH
4
) or tin(II) chloride (SnCl
2
).
Inert gas Argon or nitrogen.
Required inlet
pressure
250350 kPa (2.53.5 bar; 3651 psig).
Max gas consumption Approx. 1100 mL/min in SnCl
2
mode;
approx. 700 mL/min in NaBH
4
mode
Reactor assembly
dimensions
170 mm wide x 160 mm deep x 375 mm high
Mass (weight) of
reactor assembly
Approx. 4.3 kg
8-12
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9-1
Features of the MHS 15 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 9-3
Sample volume and dilution . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 9-3
Purge gas function . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 9-4
Calibration techniques . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 9-6
Chemical factors . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 9-7
MHS 15:
Analytical Notes 9
9MHS 15: Analytical Notes
Marker for header
Contents
page
MHS 15: Analytical Notes
9-2
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0993-5288
9-3
Features of the MHS 15
Sample volume and dilution
With the MHS 15, the measured analyte signal is proportional to the mass of the
analyte in the test solution and not to its concentration. The test solution can thus
undergo substantial dilution without the risk of dilution errors occurring since the
dilution is performed in the reaction flask. (In this guide the term test solution is
used generically for a blank solution, a calibration solution, or a test sample
solution. The term measurement solution refers to the solution being measured,
i.e. the test solution that has been diluted.)
We make a clear distinction between the volume of test solution taken and the
final total prepared measurement volume.
For satisfactory operation of the MHS 15 the minimum prepared measurement
volume is 10 mL, while the maximum permitted measurement volume is 50 mL.
The volume of test solution can be from a few microliters up to the maximum
permitted measurement volume of 50 mL.
Examples:
A 100 L aliquot of a digestion solution is pipetted into the reaction flask and
diluted with 10 mL dilute acid solution.
Test solution volume = 100 L
Prepared measurement volume = 10 mL + 100 L
In a water analysis a 10 mL test sample aliquot is taken for the determination
without further dilution. In this case the test solution volume is the same as
the prepared measurement volume.
It is essential that you measure the test solution volume accurately, using a
suitable pipet. You can measure the diluent using a suitable measuring cylinder,
since variations of 1 mL in the prepared measurement volume are insignificant.
Nevertheless you should avoid large variations in the prepared measurement
volume since for every analyte element there is a given dependence of the
sensitivity on the measurement volume.
9-4
0993-5288
Purge gas function
The inert purge gas has two functions in the MHS 15:
To purge air from the system prior to the determination (pre-reaction purge).
To purge the analyte element from the system after the determination (post-
reaction purge).
Pre-reaction purge
Since the function of the pre-reaction purge is different for the two operating
modes, different principles apply to the selection of the pre-reaction purge time
for each mode.
NaBH
4
mode
If the system is not purged free of air before the reaction with NaBH
4
is started, a
potentially flammable air-hydrogen mixture may be formed. This mixture could
ignite in the QTA when the temperature exceeds 500 C. This is not dangerous,
but interferes with the determination. The flashback arrestor reliably prevents a
flame in the QTA from flashing back into the reaction flask. Thus after connecting
the reaction flask to the reactor assembly, wait for the recommended pre-reaction
time to allow the system to be purged free of air before adding NaBH
4
solution.
As a rule of thumb, the minimum pre-reaction purge time is 2030 s.
The analytical lines of arsenic (193.7 nm) and selenium (196.0 nm) are at
wavelengths at which hot air exhibits an appreciable radiation absorption. For
these two elements a relatively long pre-reaction purge time is required to remove
all air from the system so that the absorption of air does not interfere in the
determination. A loss in sensitivity has however been observed if the pre-reaction
purge time is too long.
For the determination of mercury, a loss in sensitivity may occur if the pre-
reaction purge time is too long. The maximum pre-reaction purge time is 10 s.
Since the QTA is not heated, it is unlikely that the air-hydrogen mixture will
ignite.
Recommended pre-reaction purge times are quoted in the recommended
conditions for each element.
SnCl
2
mode
This mode can be used for the determination of mercury, but not for the hydride-
forming elements. A pre-reaction purge time is not required and you can add
SnCl
2
solution immediately after connecting the reaction flask to the reactor
assembly.
0993-5288
9-5
Post-reaction purge
Without gas purging at the end of the determination, some of the analyte element
would remain in the system, leading to carryover problems. Thus at the end of the
determination, do not remove the reaction flask from the reactor assembly until
the system has been thoroughly purged with inert gas.
Also, if the reaction flask is removed before the system has been purged, the
hydrogen still present in the system may ignite.
NaBH
4
mode
As a rule of thumb, the minimum post-reaction purge time is 4050 s.
For heavy elements such as mercury, tellurium, and tin, longer times of typically
5060 s are required to prevent carryover.
Recommended post-reaction purge times are quoted in the recommended
conditions for each element.
SnCl
2
mode
A longer post-reaction purge time of typically 60 s is required to drive mercury
from the system.
9-6
0993-5288
Calibration techniques
Calibration can be performed in terms of mass of the analyte or in terms of
concentration of the analyte. There are thus two techniques of calibration.
Technique 1 mass calibration
Prepare a single calibration solution containing 1 mg/L of the analyte.
Pipet various volumes of the single calibration solution with a micropipet into
10 mL dilute acid in the reaction flask. The acid diluent can be measured with a
measuring cylinder. Run the determination each time and establish a calibration
plot of absorbance versus mass.
10 L of 1 mg/L calibration solution 10 ng
100 L of 1 mg/L calibration solution 100 ng
Technique 2 concentration calibration
Prepare suitably large volumes of a set of calibration solutions, each containing
an appropriate concentration of the analyte.
Pipet a 10 mL aliquot of each solution into the reaction flask and run the
determination each time to establish a calibration plot of absorbance versus
concentration.
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9-7
Chemical factors
Interferences
Analyses using the mercury cold-vapor or hydride-generation techniques are
largely free of chemical and matrix effects during the measurement stage since the
analyte is separated from the sample matrix. Those interferences which may
potentially occur are generally associated with sample preparation, or to
interferences on the release of the metal hydride.
Note: If you determine mercury using tin(II) chloride as the reductant, the
apparatus will be contaminated with tin. If you subsequently determine tin in the
same apparatus using sodium tetrahydroborate as the reductant, the tin
contamination will interfere in the determination. Since tin is a hydride-forming
element, the tin contamination may also interfere in the determination of other
hydride-forming elements.
If you change regularly between SnCl
2
and NaBH
4
, we strongly recommend that
you purchase a second MHS 15 and reserve it solely for use with SnCl
2
. Likewise
you should reserve a set of reaction flasks, an immersion tube, and a reductant
bottle solely for use with SnCl
2
.
Contamination
The limits of detection attainable with the MHS 15 are often a function of the
level of contamination present rather than the instrumental capabilities. When
working in the 10
9
g range typical for the MHS 15, contamination can be a major
source of error.
Cautious handling of apparatus and careful technique will minimize this problem.
Observe the following precautions to reduce the risk of contaminating the sample:
Use only high-quality deionized water.
Take care that all materials in contact with the water are made of an inert
plastic. Pure water, even when stored in PTFE, can leach impurities from the
container in very short periods of time.
Chemicals used for sample preparation can be a major source of
contamination. As far as possible, use only chemicals of analytical reagent
grade.
Determine the reagent blank values of the reductant and other chemicals
before using them.
Beakers, pipets, volumetric flasks, etc., are all major sources of metal
contamination. As far as possible, use only inert plastics for sample handling.
9-8
0993-5288
Reagents and calibration solutions
The factors which can affect the generation of the hydride and the sensitivity can
be as simple as not using freshly prepared reductant. The purity of all reagents
used is critical when determining low levels of the hydride-forming elements.
You must make sure that all reductants, acids and reagents are free from the
analyte elements and any other elements which may react with the generated
hydride.
Prepare NaBH
4
reductant daily and preserve it by making it up in sodium
hydroxide solution. Filter the reductant solution before use.
You can prepare calibration solutions by appropriate dilution of stock
solutions.
Stock solutions with a concentration of 1000 mg/L or more are usually stable
for one year.
Store stock and calibration solutions in inert plastic containers.
Prepare solutions with a concentration of 1 mg/L or less daily.
For all solutions with concentrations of less than 10 mg/L, check the water
used for dilution and any acids or other added reagent for contamination with
the analyte element.
Determine the blank concentration of the analyte element in the reducing
agents and all other chemicals required for the analysis before use.
The stability of Hg calibration solutions can be severely affected by
adsorption onto the walls of the storage container. Stabilize mercury
calibration solutions by adding either potassium permanganate solution
(KMnO
4
; concentration: 5 g/100 mL add 5 drops per 50 mL) or potassium
iodide solution (KI; concentration: 0.1 g/100 mL).
Note: Do not stabilize mercury calibration solutions with KI if you are using
SnCl
2
as reductant since iodide interferes in the release of mercury when this
reductant is used.
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9-9
The importance of testing the samples
Some samples exhibit behavior such as foaming or precipitation that can
adversely affect the analytical results. A common problem is excessive foaming
or precipitation when samples are mixed with NaBH
4
. To identify such problems,
you should test unknown sample types before you use them in the system to
determine if they produce foams or precipitates when you add the reagents you
propose to use. You can perform these preliminary tests by working in a
laboratory hood using a tall, open beaker.
Acidity of sample solutions
In the hydride-generation technique, the test sample solutions must be acidified.
The Recommended Conditions contain details about the acids you should use.
Oxidation state of the analyte
The oxidation state of the analyte can affect the sensitivity. In solution, arsenic,
selenium, antimony, bismuth and tellurium can all exist in one of two oxidation
states. The oxidation state affects the rate at which the metal hydride is formed
and thus the sensitivity. To ensure that all of the analyte exists in the same
oxidation state, you should prereduce the calibration and test sample solutions
when you determine the elements listed above. The Recommended Conditions
contain details about the correct prereduction procedure for each element.
9-10
0993-5288
Foaming
Excessive foam production in the reaction flask can result in liquid entering the
transfer tube and being transported into the QTA. If foam enters the transfer tube
it can interfere with the transport of the hydride to the QTA. If this happens, you
must clean and dry the transfer tube. If foam enters the QTA you must clean the
inner surface of the QTA.
You can usually prevent excessive foaming by placing 1% of an antifoaming
agent into the reductant solution. The following antifoaming agents have been
successfully used in PerkinElmer applications laboratories.
Precipitation
Precipitates may be formed, for example, when protein-containing samples come
into contact with acids or when samples with a high metal content come into
contact with sodium tetrahydroborate. Precipitates can interfere with the
determination.
If precipitation causes problems, you must perform appropriate digestions or
separations to remove the offending constituent from such samples.
If heavy precipitation occurs, you should check to see that the addition of
reductant solution or the inert gas stream has not been interrupted.
Antifoam Emulsion
110A
Dow Corning
Midland, MI 48601
U.S.A.
This is available from PerkinElmer as
part number B050-7226
Silicone antifoaming agent
Type 7743
Fa. E. Merck AG
6100 Darmstadt
Germany
0993-5288
10-1
MHS 15:
Translations of Warnings 10
10MHS 15: Translations of Warnings
Marker for header
MHS 15: Translations
10-2
0993-5288
0993-5288
10-3
Translations of Warnings
This section contains translations of the safety conventions and warnings used in this guide.
dansk Oversttelser af advarsler
Denne del indeholder oversttelserne af de advarsler, som er indeholdt i denne hndbog.
Deutsch bersetzungen der Warnungen
Dieser Abschnitt enthlt die bersetzungen der in diesem Handbuch verwendeten
Warnungen.
espaol Traducciones de las advertencias
Esta seccin contiene traducciones de las advertencias utilizadas en el presente manual.
italiano Traduzione dei simboli di avvertenza
La presente sezione contiene la traduzione dei simboli di avvertenza utilizzati nel presente
manuale.
Nederlands Vertalingen van de Waarschuwingen
Dit gedeelte bevat vertalingen van de waarschuwingen gebruikt in dit handboek.
portugus Tradues de avisos
Esta seco contm tradues dos avisos usados no manual.
suomea Varoitusten knnkset
Tm osa sislt tss ksikirjassa kytettyjen varoitusten knnkset.
svenska versttning av varningstexter
Detta avsnitt innehller versttningar av de varningstexter som anvnds i handboken.
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0993-5288
This symbol alerts you to situations that could result in personal injury to yourself or other
persons.
dansk Dette symbol gr Dem opmrksom p situationer, som kan medfre kvstelser af Dem
selv eller andre personer.
Detaljer vedrrende disse omstndigheder er indrammet p tilsvarende mde som
denne henvisning.
Deutsch Dieses Symbol warnt vor Situationen, in denen Sie oder andere Personen verletzt
werden knnen.
Einzelheiten darber sind in einem Rahmen wie diesem angegeben.
espaol Este smbolo le advierte de situaciones que pueden provocar lesiones corporales a
usted o a otras personas.
En los recuadros como ste se proporciona informacin sobre este tipo de
circunstancias.
franais Ce symbole vous signale des situations pouvant occasionner des dommages corporels
l'utilisateur ou d'autres personnes.
Les dtails sur ces circonstances sont donnes dans un encadr semblable celui-ci.
italiano Questo simbolo segnala situazioni che possono generare incidenti a voi stessi o ad
altre persone.
Troverete informazioni su tali circostanze in un riquadro come questo.
Nederlands Dit symbool maakt U attent op situaties die tot verwondingen voor Uzelf of anderen
kunnen leiden.
Bijzonderheden over deze omstandigheden staan in een kader zoals dit.
portugus Este smbolo alerta para situaes que podero causar um ferimento ao usurio.
Detalhes referentes a estas circunstncias encontram-se referidos numa caixa como
esta.
suomea Tm symboli haluaa kiinnitt huomiotasi tilanteisiin, joiden seurauksena voi olla itsesi
tai muiden henkiliden loukkaantuminen.
Yksityiskohtaisia tietoja tllaisista tapauksista on tmntapaisessa ruudussa.
svenska Denna symbol anvnds fr situationer dr det finns risk fr personskador om
anvndaren inte fljer anvisningarna.
Detaljerad information ges i en ruta som denna.
0993-5288
10-5
This symbol alerts you to the risk of hot surfaces that could cause personal injury to
yourself or other persons.
dansk Dette symbol gr Dem opmrksom p risikoen for varme overflader, som kan medfre
kvstelser af Dem selv eller andre personer.
Detaljer vedrrende disse omstndigheder er indrammet p tilsvarende mde som
denne henvisning.
Deutsch Dieses Symbol warnt vor Gefahr durch heie Oberflchen, durch die Sie oder andere
Personen verletzt werden knnen.
Einzelheiten darber sind in einem Rahmen wie diesem angegeben.
espaol Este smbolo le advierte del peligro de que las superficies candentes provoquen
quemaduras a usted o a otras personas.
circunstancias.
franais Ce symbole vous avertit d'un risque de surfaces chaudes pouvant occasionner des
dommages corporels l'utilisateur ou d'autres personnes.
Les dtails sur ces circonstances sont donnes dans un encadr semblable celui-ci.
italiano Questo simbolo vi mette in guardia da superfici molto calde che possono causare
incidenti a voi stessi o ad altre persone.
Nederlands Dit symbool maakt U attent op het risico van hete oppervlaktes dat tot verwondingen
voor Uzelf of anderen kunnen leiden.
Bijzonderheden over deze omstandigheden staan in een kader zoals dit.
portugus Este smbolo alerta para um risco de superfcies quentes que podero causar um
ferimento ao usurio.
esta.
suomea Tm symboli haluaa kiinnitt huomiotasi kuumiin pintoihin, joiden seurauksena voi
olla itsesi tai muiden henkiliden loukkaantuminen.
Yksityiskohtaisia tietoja tllaisista tapauksista on tmntapaisessa ruudussa.
svenska Denna symbol anvnds fr situationer dr det finns risk fr varma ytor som kan ge
personskador om anvndaren inte fljer anvisningarna.
Detaljerad information ges i en ruta som denna.
10-6
0993-5288
Caution:
The term CAUTION alerts you to situations that could result in serious damage to the
instrument or other equipment.
Details about these circumstances are described in a message similar to this one.
dansk Bemrk:
Angivelsen CAUTION (BEMRK) gr Dem opmrksom p situationer, som kan
medfre alvorlig delggelse af apparatet eller andet udstyr.
Detaljer vedrrende disse omstndigheder er beskrevet i henvisninger svarende til
denne.
Deutsch Achtung:
Der Ausdruck CAUTION (ACHTUNG) warnt vor Situationen, die eine ernste
Beschdigung des Gerts oder anderer Systemteile zur Folge haben knnen.
Einzelheiten darber sind auf die gleiche Weise wie dieser Text hervorgehoben.
espaol Advertencia:
El trmino CAUTION (ADVERTENCIA) le previene de situacones que pueden provocar
averas graves en ste u otros equipos.
circunstancias.
franais Attention:
Le terme CAUTION (ATTENTION) vous signale des situations susceptibles de provoquer
de graves dtriorations de l'instrument ou d'autre matriel.
Les dtails sur ces circonstances figurent dans un message semblable celui-ci.

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10-7
Caution (continued)
italiano Attenzione:
Con il termine CAUTION (ATTENZIONE) vi si mette in guardia da situazioni che possono
comportare il serio danneggiamento della strumentazione o di altre apparecchiature.
Nederlands Let op:
De term CAUTION (LET OP) maakt U attent op situaties die tot ernstige
beschadigingen aan het instrument of andere apparaten kunnen leiden.
Bijzonderheden over deze omstandigheden worden beschreven in een mededeling gelijk
aan.
portugus Ateno:
O termo CAUTION (ATENO) alerta para situaes que podero causar danificao
do aparelho.
esta.
suomea Huomio:
CAUTION (HUOMIO) haluaa kiinnitt huomiotasi tilanteisiin, joiden seurauksena voi olla
laitteen tai muiden varusteiden vakava vaurioituminen.
Tllaiset tapaukset selostetaan yksityiskohtaisesti tmntapaisessa huomautuksessa.
svenska Observera:
Termen CAUTION (OBSERVERA) skall gra anvndaren uppmrksam p att apparaten
eller annan utrustning kan ta allvarlig skada om anvisningarna inte fljs. Detaljerad
information ges i en ruta som denna.
10-8
0993-5288
W1.2
Warning: Unauthorized Adjustments and Servicing
Only a PerkinElmer service engineer or similarly trained and authorized person should be
permitted to service the instrument.
Do not attempt to make adjustments, replacements, repairs, or modifications to this
instrument except as described in the documentation supplied with the instrument.
dansk Advarsel: Ikke-tilladte indstillinger og arbejder p apparatet
Vedligeholdelse af apparatet er kun tilladt for PerkinElmer kundeservice-ingeniren eller
tilsvarende uddannede og autoriserede personer.
Prv ikke p at foretage indstillinger, udskiftninger, reparationer eller ndringer af
apparatet, som ikke er beskrevet i den dokumentation, der er vedlagt apparatet.
Deutsch Warnung: Unzulssige Arbeiten am Gert
Wartungs- oder Reparaturarbeiten oder Justierungen, die in der Benutzerdokumentation
zum Gert nicht beschrieben sind, drfen nur vom PerkinElmer Kundendienst oder von
entsprechend ausgebildeten und autorisierten Fachkrften ausgefhrt werden.
espaol Advertencia: Ajustes y servicios sin autorizacin
Tan slo un ingeniero de Servicio Tcnico de PerkinElmer o una persona de formacin y
autorizacin similares podrn realizar trabajos de revisin y mantenimiento del
instrumento.
No intente realizar ningn tipo de ajuste, sustitucin o reparacin en este aparato, a
excepcin de lo descrito en la Documentacin del Usuario que se adjunta.
franais Danger: Rglages et entretien non autoriss
Seul un ingnieur du service aprs vente PerkinElmer ou une personne autorise et de
mme formation sont autorises intervenir sur l'instrument.
Ne pas essayer d'effectuer des rglages, des remplacements, des rparations ou des
modifications sur cet instrument d'une manire autre que celle dcrite dans la
documentation fournie avec l'instrument.

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10-9
Warning (continued) W1.2
italiano Pericolo: Regolazioni e manutenzione non autorizzati
L'asservimento dello strumento permesso esclusivamente ad un tecnico di assistenza
della PerkinElmer oppure da simile persona addestrata e autorizzata.
Non provare ad eseguire regolazioni, sostituzioni, riparazioni o modifiche a questo
strumento se non come descritto nella documentazione allegata allo strumento.
Nederlands Waarschuwing: Ongeautoriseerde aanpassingen en service
Alleen een PerkinElmer service-monteur of een gelijksoortig opgeleid en geautoriseerd
persoon mag service verlenen aan het instrument.
Probeer niet zelf aanpassingen aan dit instrument aan te brengen, het te repareren of
te veranderen behalve zoals beschreven in de documentatie die bij het instrument
geleverd is.
portugus Aviso: Trabalhos no permitidos no aparelho
Trabalhos de manuteno apenas podem ser executados pelo Servio Tcnico da
PerkinElmer ou por pessoal especializado devidamente formado e autorizado.
No tente realizar ajustamentos, substituies, reparaes ou modificaes neste
aparelho que no estejam descritos na documentao fornecida com o aparelho.
suomea Varo: Luvattomat st - ja huoltotyt
Laitteen huoltotyt saa antaa vain PerkinElmer -huoltoteknikoiden tai vastaavasti
koulutettujen ja valtuutettujen henkiliden tehtvksi.
l tee muita st-, vaihto-, korjaus- tai muutostit tss laitteessa kuin sellaisia,
jotka on selostettu laitteen mukana toimitetussa dokumentaatiossa.
svenska Varning: Icke tilltna arbeten p apparaten
Endast servicepersonal frn PerkinElmer eller personal med liknande utbildning och
behrighet fr utfra servicearbeten p apparaten.
Underhlls- eller reparationsarbeten, justeringar eller ndringar som inte finns
beskrivna i anvndarmanualen till apparaten fr inte utfras.
10-10
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10-11
W1.3
dansk Advarsel: Eksplosive omgivelser
Dette apparat er ikke konstrueret til brug i eksplosive omgivelser.
Deutsch Warnung: Explosionsfhige Atmosphren
Das Gert darf nicht in explosionsfhigen Atmosphren betrieben werden.
espaol Advertencia: Atmsfera explosiva
Este aparato no est diseado para utilizarlo en atmsferas explosivas.
franais Danger: Atmosphre explosive
Cet instrument n'est pas conu pour fonctionner dans une atmosphre explosive.
italiano Pericolo: Atmosfera esplosiva
Questo strumento non concepito per operare in atmosfera esplosiva.
Nederlands Waarschuwing: Explosiegevaarlijke omgevingen
Dit instrument mag niet in een explosiegevaarlijke omgeving gebruikt worden.
portugus Aviso: Atmosferas explodveis
O aparelho no pode ser utilizado em atmosferas explodveis.
suomea Varo: Rjhdysvaarallinen ymprist
Tt laitetta ei saa kytt rjhdysvaarallisessa ympristss.
svenska Varning: Explosiv atmosfr
Apparaten r inte avsedd att anvndas i explosionsfarliga miljer.
10-12
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W3.1
Warning: UV Radiation Risk of Eye Damage
The lamps may emit UV radiation which can damage your eyes.
Do not gaze into a lighted lamp.
Always wear UV-absorbing safety glasses when looking at the radiation from the
lamps.
dansk Advarsel: Ultraviolet strling farligt for jnene
Lamperne kan emittere ultraviolet strling, som kan forrsage jenskader.
Se ikke direkte ind i en tndt lampe.
Br altid beskyttelsesbriller, som absorberer ultraviolet strling, nr De ser ind i den
den lysende strlingskilde.
Deutsch Warnung: UV-Strahlung Gefhrdung der Augen
Die Lampen emittieren UV-Strahlung in unterschiedlicher Strke und knnen dadurch
Augenschden verursachen.
Nicht mit ungeschtzten Augen direkt in die leuchtenden Lampen schauen.
Tragen Sie eine Schutzbrille, die die emittierte UV-Strahlung ausreichend absorbiert,
wenn Sie in die leuchtende Lampe schauen.
espaol Advertencia: Radiacin ultravioleta Peligro de daos a los ojos
Las lmparas pueden emitir una intensa radiacin ultravioleta que puede ser perjudicial
para los ojos.
No dirija la vista a una lmpara encendida.
Use siempre gafas de seguridad que absorban este tipo de rayos.
franais Danger: Rayonnement UV
Les lampes peuvent mettre des UV susceptibles de provoquer des lsions oculaires.
Ne pas regarder fixement une lampe allume.
Toujours porter des lunettes de protection absorbant les UV pour regarder le
rayonnement des lampes.

0993-5288
10-13
italiano Pericolo: Radiazioni UV Rischio di lesioni agli occhi
Le lampade possono emettere radiazioni UV che possono lesionare gli occhi.
Non guardare direttamente in una lampada accesa.
Se guardate una lampada accesa indossate sempre occhiali di sicurezza in grado di
assorbire le radiazioni UV.
Nederlands Waarschuwing: Ultraviolette straling Risicos voor de ogen
De lampen kunnen UV-straling uitzenden die Uw ogen kan beschadigen.
Staar niet in een brandende lamp.
Draag altijd een veiligheidsbril die ultraviolette straling absorbeert wanneer U in de
brandende stralingsbron moet kijken.
portugus Aviso: Radiao UV perigo para os olhos
As lmpadas emitem uma radiao UV com intensidades diferentes podendo assim
provocar ferimentos aos olhos.
No olhar directamente para uma lmpada acesa.
Use sempre culos de proteco que absorvam suficientemente a radiao UV
emitida ao olhar directamente para a fonte de radiao luminosa.
suomea Varo: UV-steily silmvammojen vaara
Lamput saattavat lhett UV-steily, joka voi vahingoittaa silmi.
l tuijota valaistuun lamppuun.
Kyt aina UV-steilylt suojaavia suojasilmlaseja, kun katsot lampuista lhtev
steily kohti.
svenska Varning: UV-strlning risk fr gonskador
Strlningskllorna/lamporna alstrar UV-strlning som kan ge gonskador.
Titta inte in i en tnd strlningsklla/lampa.
Anvnd alltid skyddsglasgon som absorberar UV-strlar nr du tittar in i en tnd
strlningsklla/lampa.
10-14
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10-15
W4.2
The burner head can reach very high temperatures.
Do not touch the burner head until it has cooled to room temperature.
dansk Advarsel: Hje temperaturer Fare for forbrndinger
Brnderhovedet kan opn meget hje temperaturer.
Berr aldrig brnderhovedet, fr det er klet ned til stuetemperatur.
Deutsch Warnung: Verbrennungsgefahr
Den heien Brennerkopf nur mit hitzebestndigen Schutzhandschuhen anfassen oder
vor dem Anfassen auf Krpertemperatur abkhlen lassen.
espaol Advertencia: Altas temperaturas Riesgo de quemaduras
La cabeza del mechero puede alcanzar temperaturas muy altas.
Asegrese, antes de tocar el mechero, que ste se haya enfriado hasta alcanzar la
temperatura ambiente.
franais Danger: Tempratures leves Risque de brlures
La tte de brleur peut atteindre de trs hautes tempratures.
Ne pas toucher la tte de brleur avant qu'elle ait refroidi la temprature ambiante.
italiano Pericolo: Alte temperature Rischio di ustioni
La testa del bruciatore pu raggiungere temperature estremamente elevate.
Non toccare la testa del bruciatore sino a che non si raffreddato sino a raggiungere
temperatura ambiente.
Nederlands Waarschuwing: Hoge temperaturen Verbrandingsgevaar
De branderkop kan zeer hoge temperaturen bereiken.
Raak de branderkop pas aan als hij tot kamertemperatuur is afgekoeld.
portugus Aviso: Altas temperaturas perigo de queimaduras
A cabea do queimador pode alcanar temperaturas muito altas.
No toque na cabea do queimador at ter alcanado a temperatura.
suomea Varo: Korkeat lmptilat palovammavaara
Polttimen p voi saavuttaa korkeita lmptiloja.
l kosketa polttimen pt, ennen kuin se on jhtynyt
huoneenlmptilaan.
svenska Varning: Hga temperaturer risk fr brnnskador
Brnnaren kan n mycket hga temperaturer.
Vidrr inte brnnarmunstycket frrn det har svalnat till rumstemperatur.
10-16
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W4.5
The burner head, cell holder, and QTA-cell can reach high temperatures.
When you handle the cell holder or the QTA-cell, wear flame- and heat-resistant gloves
or wait until the cell and holder have cooled to room temperature.
dansk Advarsel: Hje temperaturer Fare for forbrndinger
Brnderhovedet, kuvetteholderen og QTA-kuvetten kan opn hje temperaturer.
Ved hndteringen af kuvetteholderen eller QTA-kuvetten skal man bre ikke-
brndbare, varmebestandige handsker eller vente, til kuvetten og holderen er klet
ned til stuetemperatur.
Deutsch Warnung: Verbrennungsgefahr
Beim Hantieren mit der auf dem Brenner montierten Kvettenhalterung nichtbrennbare
hitzebestndige Schutzhandschuhe tragen oder vor dem Anfassen abwarten, bis
Kvettenhalterung, Kvette und Brennerkopf auf Krpertemperatur abgekhlt sind.
espaol Advertencia: Altas temperaturas Riesgo de quemaduras
La cabeza del mechero, el soporte de la clula y la clula QTA pueden alcanzar
temperaturas elevadas.
Al manejar el soporte de la cabeza del mechero de la clula QTA, utilice guantes
resistentes al calor y al fuego, o bien, espere hasta que clula y soporte se hayan
enfriado hasta alcanzar la temperatura ambiente.
franais Danger: Tempratures leves Risque de brlures
La tte de brleur, le porte-cellule, et la cellule QTA peuvent atteindre de hautes
tempratures.
Quand vous manipulez le porte-cellule ou la cellule QTA, portez des gants rsistants
aux flammes et la chaleur ou patientez jusqu' ce que la cellule et son support aient
refroidi la temprature ambiante.

0993-5288
10-17
italiano Pericolo: Alte temperature Rischio di ustioni
La testa del bruciatore, il supporto della cella e la cella QTA possono raggiungere
temperature etremamente elevate.
Se manipolate il supporto della cella o la cella QTA indossate guanti antitermici ed
ignifughi oppure attendete sino a che la cella e il suo supporto si siano raffreddati sino
a raggiungere temperatura ambiente.
Nederlands Waarschuwing: Hoge temperaturen Verbrandingsgevaar
De branderkop, cuvettehouder en cuvette kunnen zeer hoge temperaturen bereiken.
Bij het vastpakken van de cuvettehouder of de cuvette hittebestendige handschoenen
dragen of wachten tot de cuvette en de cuvettehouder tot kamertemperatuur afgekoeld
zijn.
portugus Aviso: Altas temperaturas - perigo de queimaduras
A cabea do queimador, o porta-cubetas, e a cubeta QTA podem alcanar temperaturas
elevadas.
Ao manejar com o porta-cubetas ou a cubeta QTA, use luvas de proteco no
inflamveis e resistentes ao calor, ou espere at que o porta-cubetas e a cubeta
tenham alcanado a temperatura ambiente normal.
suomea Varo: Korkeat lmptilat palovammavaara
Polttimen p, kyvetinpidike ja QTA-kyvetti voivat saavuttaa korkeita lmptiloja.
Kun ksittelet kyvetinpidikett tai QTA-kyvetti, kyt liekin- ja kuumuudenkestvi
ksineit tai odota, kunnes kyvetti ja pidike ovat jhtyneet huoneenlmptilaan.
svenska Varning: Hga temperaturer risk fr brnnskador
Brnnarmunstycket, sklhllaren och QTA-sklen kan n mycket hga temperaturer.
Anvnd icke-brnnbara, vrmebestndiga skyddshandskar vid hanteringen av
sklhllaren och QTA-sklen eller vnta tills sklen och hllaren svalnat till
rumstemperatur.
10-18
0993-5288
W8.1
Warning: Hydrofluoric Acid Risk of Burns
Hydrofluoric acid (HF) is toxic, corrosive and can cause severe burns.
When using hydrofluoric acid, always wear suitable protective clothing including a face
mask, work in a fume hood, and observe the manufacturers instructions and your local
safety regulations.
dansk Advarsel: Flussyre Fare for tsninger
Flussyre (HF) er giftig, korrosiv og strkt tsende.
Under brugen af flussyre skal man altid bre tilsvarende beskyttelsestj, inklusive
ansigtsbeskyttelse, arbejde i et aftrk samt overholde producentens henvisninger og
de stedlige sikkerhedsforskrifter.
Deutsch Warnung: Fluorwasserstoffsure Vertzungsgefahr
Fluorwasserstoffsure (HF) ist giftig, stark tzend und korrosiv.
Tragen Sie beim Umgang mit Fluorwasserstoffsure eine Schutzbrille oder
Gesichtsschutz, Schutzhandschuhe und surebestndige Schutzkleidung und
arbeiten Sie in einem Abzug. Beachten Sie die Gefahrenhinweise und
Sicherheitsratschlge des Herstellers.
espaol Advertencia: cido fluorhdrico peligro de quemaduras
El cido fluorhdrico (HF) es txico, corrosivo y puede causar quemaduras graves.
Al usar este cido, utilice siempre ropa de proteccin incluyendo una mscara facial;
trabaje en la campana de humos y siga las instrucciones del fabricante y las reglas de
seguridad nacionales.
franais Danger: Acide fluorhydrique Risque de brlure
L'acide fluorhydrique (HF) est toxique, corrosif et susceptible de provoquer de graves
brlures.
Lors de l'utilisation d'acide fluorhydrique, toujours porter une tenue protectrice
approprie comportant un masque, travailler dans une hotte ferme et respecter les
instructions du fabricant et les rglements de scurit de l'entreprise.

0993-5288
10-19
italiano Pericolo: Acido fluoridrico Rischio di ustioni
L'acido fluoridrico (HF) tossico e corrosivo e pu causare severe ustioni.
Se utilizzate acido fluoridrico indossate sempre indumenti protettivi comprendenti una
maschera, lavorate in una cappa per fumi e osservate le istruzioni del produttore
cosccome le norme di sicurezza vigenti localmente.
Nederlands Waarschuwing: Fluorwaterstofzuur Etsingsgevaar
Fluorwaterstofzuur (HF) is giftig, bijtend en sterk etsend.
Draag tijdens het gebruik van fluorwaterstofzuur een veiligheidsbril of gezichtsmasker,
veiligheidshandschoenen en zuurbestendige veiligheidskleding en werk in een ruimte
waarin wordt afgezogen! Neem de risicorichtlijnen en de veiligheidsvoorschriften van
de fabrikant en die ter plaatse in acht.
portugus Aviso: cido fluordico perigo de queimaduras
cido fluordico (HF) txico, corrosivo e pode causar queimaduras graves.
Ao lidar com cido fluordico, use sempre vesturio de proteco, incluindo culos ou
mscara de proteco, trabalhe dentro de um exaustor e respeite as instrues do
fabricante bem como as regulamentaes locais em matria de segurana.
suomea Varo: Fluorivetyhappo vaarana sypymisvammat
Fluorivetyhappo (HF) on myrkyllist ja syvyttv ja se voi aiheuttaa vakavia
sypymisvammoja.
Kun ksittelet fluorivetyhappoa, kyt aina sopivaa suojavaatetusta, johon kuuluu
mys naamari, tyskentele vetokaapissa ja ota huomioon valmistajan antamat ohjeet
ja paikalliset turvamrykset.
svenska Varning: Fluorvtesyra risk fr brnnskador
Fluorvtesyra (HF) r giftig, frtande och kan ge svra brnnskador.
Anvnd alltid skyddsklder och skyddsmask vid hantering av fluorvtesyra och arbeta
under en utsugningshuv. Flj tillverkarens instruktioner och de lokala
skerhetsfreskrifterna.
10-20
0993-5288
0993-5288
In-1
Index
Index
In-2
0993-5288
Index
0993-5288
In-3
A
acidity of test samples 9-9
aligning QTA burner mount on
burner head 6-4
aligning the QTA 2-6
analyte
oxidation state 9-9
antimony
recommended conditions
3-13
arsenic
establishing pre-reaction purge
time 2-12
recommended conditions 3-5
atomizer see quartz tube atomizer
(QTA)
attaching reaction flask 2-10
B
bismuth
recommended conditions 3-7
burner mount for QTA 8-4
burner system
safe operation 1-13
C
calibration solutions
preparing 9-6
stability 9-8
calibration techniques 9-6
carton recycling 6-3
changeover valve 2-8, 8-9
checklist
maintenance 4-4
chemical vapor generation 8-6
chemicals
safe handling 1-6, 3-3
cleaning 4-4
cleaning the QTA 4-7
cold vapor technique 8-6
concentration calibration 9-6
conditioning the QTA 4-8
connecting inert gas supply 6-6
contamination 9-7
contamination with tin(II)
chloride 2-9, 9-7
correct use of the instrument 1-4
CV AAS 8-6
D
disposing of
contents of waste containers
1-8, 4-5
reaction residues 1-8, 4-5
E
environment
operating conditions 1-5
storage conditions 1-5
F
flame
safe operation 1-13
flame operation
safe use of burner gases 1-12
foaming 9-10
fume ventilation 7-4
G
gas supply requirements 7-5
gasket in reaction flask socket
replacing 4-10
H
hazards with flame operation
high temperatures 1-13
UV radiation 1-13
hazards with mercury/hydride
systems
hazardous chemicals 1-14
high temperatures 1-14
toxic products 1-14
HG AAS 8-6
hydride-forming elements 8-6
hydride-generation technique
8-6
hygiene 1-5
I
inert gas
connecting supply 6-6
pressure 7-6
requirements 7-6
installing QTA burner mount
6-4
installing the reactor assembly
6-6
internal servicing 4-3
L
laboratory hygiene 1-5
laboratory requirements
fume ventilation 7-4
gas supplies 7-5
operating conditions 7-3
laboratory ventilation 1-5
literature on chemical vapor
generation 8-7
M
maintenance 4-4
cleaning the QTA 4-7
conditioning the QTA 4-8
external surfaces 4-4
4-10
replacing sleeves on QTA
4-12
transfer tube 4-10
mass calibration 9-6
measurement solution 8-9, 9-3
measurement volume 9-3
measurements 2-10
Index
In-4
0993-5288
mercury
calibration solutions 9-8
(NaBH
4
) 3-9
(SnCl
2
) 3-11
mercury determination 8-6
mercury/hydride systems
hazards 1-14
safety practices 1-14
method for spectrometer 2-4
methods development 2-12
establishing post-reaction
purge time 2-13
time 2-12
establishing reaction time
2-13
establishing read time 2-13
MHS 15
description 8-3
technical data 8-11
O
operating conditions 1-5, 7-3
operating mode 2-8, 8-9, 9-4
operating principle 8-8
oxidation state 9-9
P
parts provided 5-3
performing measurements 2-10
PerkinElmer service 4-3
placing QTA in QTA bracket
2-3
positioning the MHS 15 2-3
post-reaction purge 8-10, 9-5
post-reaction purge time
establishing 2-13
precipitates 9-10
prepared measurement volume
9-3
preparing for analyses 2-4
pre-reaction purge 8-9, 9-4
establishing time 2-12
principle of operation 8-8
purge gas
function 9-4
see also inert gas
purging (flushing) the reductant
transport system 4-5
Q
QTA
aligning 2-6
cleaning the inner surface 4-7
conditioning 4-8
description 8-4
placing in bracket 2-3
QTA burner mount 8-4
aligning on burner head 6-4
installing 6-4
quartz tube atomizer see QTA
R
reaction flask
attaching 2-10
reaction time
establishing 2-13
reactor assembly
description 8-3
installing 6-6
read time
establishing 2-13
reagents
purity 9-8
antimony 3-13
arsenic 3-5
bismuth 3-7
mercury (NaBH
4
) 3-9
mercury (SnCl
2
) 3-11
selenium 3-15
tellurium 3-19
tin 3-17
reductant changeover valve 2-8,
8-9
reductant transport system
purging (flushing) 4-5
references for laboratory safety
practice 1-16
replacement parts 5-5
obtaining 5-4
replacements
4-10
sleeves on QTA 4-12
transfer tube 4-10
routine maintenance 4-4
S
safe handling of chemicals 1-6,
3-3
sodium tetrahydroborate 1-7,
3-3
safe operation of the flame 1-13
safety
correct use of the instrument
1-4
handling chemicals 1-6, 3-3
operation of the flame 1-13
safety conventions 1-3
safety practices
mercury/hydride systems
1-14
references 1-16
samples
acidity 9-9
analyte oxidation state 9-9
testing 9-9
Index
0993-5288
In-5
selenium
time 2-12
3-15
service 4-3
setting up the system 2-3
sleeves on QTA
replacing 4-12
sodium tetrahydroborate 1-7,
3-3
spectrometer method 2-4
storage conditions 1-5
symbols used in the guide 1-3
T
technical data 8-11
tellurium
3-19
test solution 9-3
tin
contamination 2-9, 9-7
3-17
transfer tube
replacing 4-10
U
unpacking 6-3
V
ventilation, laboratory 1-5
W
waste disposal
contents of waste containers
1-8, 4-5
reaction residues 1-8, 4-5
Index
In-6
0993-5288

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MHS 15: Translations

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