ATOMIC SPECTROMETRY
MHS 15
Mercury Hydride System
Users Guide
abcdr
ATOMIC SPECTROMETRY
MHS 15
Mercury Hydride System
Users Guide
Release history
Part Number
Release
Publication Date
0993-5288
July 2000
Any comments about the documetation for this product should be addressed to:
User Assistance
PerkinElmer, Inc.
710 Bridgeport Avenue
Shelton, Connecticut 06484-4794
U.S.A.
Or emailed to:
info@perkinelmer.com
Notices
The information contained in this document is subject to change without notice. Except as specifically set forth in its
terms and conditions of sale, PerkinElmer makes no warranty of any kind with regaed to this document, including,
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.
Copyright information
This document contains proprietary information that is protected by copyright.
All rights are reserved. No part of this document may be reproduced in any form whatsoever
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
Trademarks
PerkinElmer is a trademark of PerkinElmer, Inc.
AA WinLab, AAnalyst, Lumina, and THGA are trademarks of affiliates of PerkinElmer, Inc.
Windows is a trademark and Microsoft is a registered trademark of Microsoft Corporation.
Registered names, trademarks, etc. used in this document, even when not specifically marked as such, are not to be considered unprotected by law.
Contents
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Contents
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Contents
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Contents
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Contents
Safety practices and conventions . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
Correct use of the instrument . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
Operating conditions . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
Laboratory hygiene . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
Laboratory ventilation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
Safe handling of chemicals . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
Waste disposal . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
Handling compressed gases . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
Safety practices for flame operation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
Safety practices for mercury/hydride systems . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
References for laboratory safety practice . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
Regulatory information . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
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1-1
Safety/Regulatory Information
1-2
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Safety/Regulatory Information
This symbol alerts you to the risk of hot surfaces that could cause personal
injury to yourself or other persons.
Details about these circumstances are in a box like this one.
Caution
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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.
1-3
Safety/Regulatory Information
1-4
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Safety/Regulatory Information
Operating conditions
W1.3
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:
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.
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1-5
Safety/Regulatory Information
Depending on the types of chemicals you are handling, wear safety glasses
with side shields, or goggles, or a full-face shield.
1-6
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Safety/Regulatory Information
Sodium tetrahydroborate
Make sure that the work area has an adequate ventilation system to prevent
the build-up of explosive air-hydrogen mixtures.
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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1-7
Safety/Regulatory Information
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 NaBH4 or SnCl2 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 NaBH4 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.
1-8
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Safety/Regulatory Information
Gas
Argon
Nitrogen
Suffocation
x
x
Explosion
Spontaneous
Decomposition
or Combustion
Contact the gas supplier for a safety data sheet containing detailed information on
the potential hazards associated with the gas.
Warning: Compressed Gases
Legibly mark cylinders to clearly identify the contents and status (full, empty,
etc.). Use the chemical name or commercially accepted name for the gas.
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Safety/Regulatory Information
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.
Use and store cylinders away from exits and exit routes.
Locate gas cylinders away from heat sources, including heat lamps.
Do not allow ignition sources in the storage area and keep cylinders away
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).
1-10
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Safety/Regulatory Information
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.
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/Regulatory Information
Do not attempt to defeat these interlocks; you may compromise your own, or
someone elses, safety.
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 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.
1-12
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Safety/Regulatory Information
Safe operation of the flame
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.
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
Keep the atomizer compartment door closed when the flame is burning and
never directly view the flame unless you are wearing UV-absorbing glasses.
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1-13
Safety/Regulatory Information
Safety checks
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.
Toxic metal vapors, hydrogen, etc., can be generated by the system, depending on
the type of analyses being performed.
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.
1-14
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Safety/Regulatory Information
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
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 NaBH4 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.
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Safety/Regulatory Information
9th edition, Sax, N.I. and Lewis, R.J., eds.,Wiley, New York, USA, 1998.
1-16
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Safety/Regulatory Information
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.
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Safety/Regulatory Information
1-18
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MHS 15:
Analyzing Samples
Contents
Setting up the system . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
Positioning the MHS 15 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
Preparing the system for analyses . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
Aligning the QTA . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
Selecting operating mode . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
Performing a measurement . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
Methods development . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
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2-1
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Transfer tube
from reactor assembly
QTA
Burner head
Burner spray
chamber
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.
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2-4
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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.
Fitting for
reductant bottle
Inert gas
Reductant bottle
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2-6
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2. Fine alignment
Perform fine alignment before the start of every analysis series.
Warning: UV Radiation Risk of Eye Damage
W3.1
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.
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
spectrometers guide.
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.
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2-7
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.
2-8
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Wing nut
Valve cover
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 SnCl2 and NaBH4, we strongly recommend that
you purchase a second MHS 15 and reserve it solely for use with SnCl2. Likewise
you should reserve a set of reaction flasks, an immersion tube, and a reductant
bottle solely for use with SnCl2.
A set of adhesive labels is provided with the MHS 15 so that you can mark the
reductant being used.
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2-9
Performing a measurement
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.
2-10
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Plunger
Lugs
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.
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2-11
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 NaBH4 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 prereaction purge time experimentally for your system, since radiation absorption by
air in the QTA can interfere in the determination of these elements.
1. Set up the system as described under Preparing the system for analyses on
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.
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Determine the reaction time and post-reaction purge time by measuring a suitable
calibration solution of the analyte element, as described below:
1. Set up the system as described under Preparing the system for analyses on
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.
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MHS 15:
Recommended Analytical Conditions
Contents
page
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 mercury . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
3-9
Recommended conditions for mercury . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-11
Recommended conditions for antimony . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-13
Recommended conditions for selenium . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-15
Recommended conditions for tin . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-17
Recommended conditions for tellurium . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-19
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Depending on the types of chemicals you are handling, wear safety glasses
with side shields, or goggles, or a full-face shield.
Sodium tetrahydroborate
Make sure that the work area has an adequate ventilation system to prevent
the build-up of explosive air-hydrogen mixtures.
3-3
3-4
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As
Calibration solution
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
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:
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3-5
Analytical wavelength
193.7 nm
0.7 nm
Radiation source
QTA heating
Prepared measurement
volume
10 mL minimum to 50 mL maximum.
approx. 50 s
approx. 40 s
Characteristic mass
Characteristic
concentration
Characteristic
concentration check
Alternate analytical
wavelengths
Notes
3-6
Low
Wavelength
nm
Slit width
nm
189.0
197.2
0.7
0.7
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Bi
Calibration solution
Reductant solution
Oxidation state
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3-7
223.0 nm
0.2 nm
Radiation source
QTA heating
Prepared measurement
volume
10 mL minimum to 50 mL maximum.
approx. 30 s
approx. 40 s
Characteristic mass
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.
Alternate analytical
wavelengths
3-8
Low
Wavelength
nm
Slit width
nm
222.8
306.8
206.2
227.7
0.2
0.7
0.2
0.2
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Hg
Calibration solution
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3-9
253.6 nm
0.7 nm
Radiation source
QTA heating
No flame required.
If condensation in the QTA is a problem, heat the QTA gently by
mounting an infrared lamp above it.
Prepared measurement
volume
10 mL minimum to 50 mL maximum.
approx. 5 s
approx. 50 s
Characteristic mass
Characteristic
concentration
Characteristic
concentration check
Notes
3-10
Low
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Hg
Stock solution
Calibration solution
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3-11
253.6 nm
0.7 nm
Radiation source
QTA heating
No flame required.
If condensation in the QTA is a problem, heat the QTA gently by
mounting an infrared lamp above it.
Prepared measurement
volume
10 mL minimum to 50 mL maximum.
approx. 5 s
approx. 50 s
Characteristic mass
Characteristic
concentration
Characteristic
concentration check
Notes
3-12
Low
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Sb
Calibration solution
Reductant solution
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:
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3-13
Analytical wavelength
217.6 nm
0.2 nm
Radiation source
QTA heating
Prepared measurement
volume
10 mL minimum to 50 mL maximum.
approx. 30 s
approx. 50 s
Characteristic mass
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.
Alternate analytical
wavelengths
3-14
Low
Wavelength
nm
Slit width
nm
206.8
231.2
0.2
0.2
0993-5288
Se
Calibration solution
Reductant solution
Oxidation state
0993-5288
3-15
196.0 nm
2.0 nm
Radiation source
QTA heating
Prepared measurement
volume
10 mL minimum to 50 mL maximum.
approx. 50 s
approx. 30 s
Characteristic mass
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.
Alternate analytical
wavelengths
Notes
3-16
Low
Wavelength
nm
Slit width
nm
204.0
206.3
0.7
0.7
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
Sn
Calibration solution
0993-5288
3-17
286.3 nm
0.7 nm
Radiation source
QTA heating
Prepared measurement
volume
10 mL minimum to 50 mL maximum.
approx. 30 s
approx. 50 s
Characteristic mass
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.
Alternate analytical
wavelengths
Notes
Low
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
3-18
0993-5288
Te
Calibration solution
Reductant solution
Oxidation state
0993-5288
3-19
214.3 nm
0.2 nm
Radiation source
QTA heating
Prepared measurement
volume
10 mL minimum to 50 mL maximum.
approx. 30 s
approx. 50 s
Characteristic mass
Characteristic
concentration
Characteristic
concentration check
Notes
3-20
Low
0993-5288
Contents
PerkinElmer Service . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
Routine maintenance . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
Maintaining the flashback arrestor . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
QTA maintenance . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
Replacing worn parts . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
0993-5288
page
4-3
4-4
4-6
4-7
4-10
4-1
4-2
0993-5288
PerkinElmer Service
W1.2
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.
0993-5288
4-3
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.
4-4
Reaction flask
Immersion tube
Reductant bottle
Reductant
transport system
Flashback
arrestor
Transfer tube
0993-5288
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 NaBH4.
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 NaBH4 or SnCl2 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 NaBH4 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.
0993-5288
4-5
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
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.
Baffle
Transfer tube
to reactor assembly
4-6
0993-5288
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
Warning: High Temperatures Risk of Burns
W4.5
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.
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.
0993-5288
4-7
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
W8.1
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.
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.
QTA
Plastic container
Hydrofluoric acid
4-8
0993-5288
0993-5288
4-9
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:
Warning: High Temperatures Risk of Burns
W4.5
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.
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.
4-10
0993-5288
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.
0993-5288
4-11
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.
Graphite ring
Sleeve
QTA
W4.5
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.
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 it is not possible to pull the sleeves off, carefully cut them off using a sharp
scalpel.
4-12
0993-5288
0993-5288
4-13
4-14
0993-5288
MHS 15:
Parts and Supplies
Contents
Parts provided . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
Obtaining supplies, replacement parts, and accessories . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
Replacement parts . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
0993-5288
page
5-3
5-4
5-5
5-1
5-2
0993-5288
Parts provided
PerkinElmer reserves the right to alter the schedule of parts provided without prior notice.
Qty. Item
1
1
2
0993-5288
Part No.
2
3
2
1
1
2
5
1
B314-0763
B300-0350
B009-4414
B009-4139
B009-4152
B009-4032
B314-0735
B007-9873
B050-5881
B010-4049
B010-4053
B010-4052
1
1
Users Guide . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
Quick Reference . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
0993-5288
0993-5289
5-3
5-4
0993-5288
Replacement parts
0993-5288
Item
Part No.
Reaction flask . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
Immersion tube . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
Gasket for reaction flask socket . . . . . . . . . . . . . . . . . . . . . . . . .
Transfer tube. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
Flashback arrestor . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
Quartz tube atomizer,
complete with graphite rings and sleeves. . . . . . . . . . . . . . . . . . .
Quartz tube atomizer,
without graphite rings or sleeves . . . . . . . . . . . . . . . . . . . . . . . . .
QTA sleeves (pack of 4) . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
Graphite cooling ring . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
Reductant bottle . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
Drip tray . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
B009-4139
B009-4138
B010-4049
B009-4140
B009-8640
B009-4415
B009-4414
B050-5881
B009-4413
B009-4032
B314-0735
5-5
5-6
0993-5288
MHS 15:
Installation
6MHS 15: Installation
Marker for header
Contents
Unpacking and inspection . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
Installing the QTA burner mount . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
Installing the reactor assembly . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
Connecting the inert gas supply . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
Preparing the reactor assembly . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
0993-5288
page
6-3
6-4
6-6
6-6
6-8
6-1
6-2
0993-5288
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.
0993-5288
6-3
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
0993-5288
QTA bracket
in up position
Adjusting screw
(2 each clamp)
Securing clamp
(1 of 2)
Burner head
seen from the
rear
Burner head
Figure 6-1. Attaching the QTA burner mount to the burner head
Burner slot
QTA bracket
in down position
V in QTA
bracket
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.
0993-5288
6-5
A suitable supply of argon or nitrogen. The gas must conform with the
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
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.
6-6
0993-5288
Inert Gas
Gaz inerte
Inertgas
N2 or Ar only
N2 ou Ar seulement
Nur N2 oder Ar
Pmin
250
2.5
36
Pmax
350
3.5
51
kPa
bar
psig
Connector for
gas supply tube
Inert gas supply
nitrogen or argon
0993-5288
6-7
QTA
Flashback
arrestor
Transfer tube
Reaction flask socket
Connector
Immersion tube
Drip tray
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.
6-8
0993-5288
MHS 15:
Laboratory Requirements
Contents
Operating conditions . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
Gas supply requirements . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
Inert gas . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
0993-5288
page
7-3
7-5
7-6
7-1
7-2
0993-5288
Operating conditions
W1.3
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 you choose for the spectrometer and mercury/hydride system must
fulfil the criteria listed below:
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.
0993-5288
7-3
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
7-4
0993-5288
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.
0993-5288
7-5
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.
Table 7-1. Specifications and Requirements for the Inert Gas
Gas
Purity
bar
Max. Flowrate
psig
mL/min
(nominal) at
250 kPa
Pmin
Pmax
Pmin
Pmax
Pmin
Pmax
NaBH4
SnCl2
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
Argon
Set the outlet gauge pressure for the gas supply exactly to 250 kPa (Pmin ).
Never set the outlet pressure to a value exceeding the maximum pressure
(Pmax ).
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.
7-6
0993-5288
MHS 15:
System Description
Contents
Introduction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
Chemical vapor generation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
The cold vapor technique . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
The hydride-generation technique . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
Literature on chemical vapor generation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
Principle of operation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
Technical data . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
0993-5288
page
8-3
8-6
8-6
8-6
8-7
8-8
8-11
8-1
8-2
0993-5288
Introduction
Plunger
Reductant
bottle
Transfer tube
Reaction flask
Flashback arrestor
to QTA
0993-5288
8-3
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.
8-4
0993-5288
Sample inlet
Transfer tube
from reactor assembly
QTA
Burner head
Burner spray
chamber
0993-5288
8-5
(2)
and
8-6
0993-5288
0993-5288
8-7
Principle of operation
Changeover
valve
(in SnCl2 position)
Changeover
valve
(in NaBH 4 position)
Multipath
valve
SnCl2
d
Pressure
reducer
1
Inert gas
F1
2
g
F3
NaBH4
F2
b
e
a
g
Flashback
arrestor
d
h
QTA
Immersion
tube
Reductant
reservoir
Burner
Reaction
flask
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
8-8
0993-5288
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 (prereaction 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 (NaBH4):
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 (SnCl2):
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.
0993-5288
8-9
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.
8-10
0993-5288
Technical data
QTA heating
Reaction flask
Measurement
solution volume
Reductants
Inert gas
Argon or nitrogen.
Required inlet
pressure
Reactor assembly
dimensions
Mass (weight) of
reactor assembly
Approx. 4.3 kg
0993-5288
8-11
8-12
0993-5288
MHS 15:
Analytical Notes
Contents
Features of the MHS 15 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
Sample volume and dilution . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
Purge gas function . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
Calibration techniques . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
Chemical factors . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
0993-5288
page
9-3
9-3
9-4
9-6
9-7
9-1
9-2
0993-5288
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
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.
0993-5288
9-3
To purge air from the system prior to the determination (pre-reaction purge).
To purge the analyte element from the system after the determination (postreaction 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.
NaBH4 mode
If the system is not purged free of air before the reaction with NaBH4 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 NaBH4 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 prereaction 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.
SnCl2 mode
This mode can be used for the determination of mercury, but not for the hydrideforming elements. A pre-reaction purge time is not required and you can add
SnCl2 solution immediately after connecting the reaction flask to the reactor
assembly.
9-4
0993-5288
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.
NaBH4 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.
SnCl2 mode
A longer post-reaction purge time of typically 60 s is required to drive mercury
from the system.
0993-5288
9-5
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
9-6
0993-5288
Chemical factors
Interferences
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 109 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.
0993-5288
9-7
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.
Stock solutions with a concentration of 1000 mg/L or more are usually stable
for one year.
used for dilution and any acids or other added reagent for contamination with
the analyte element.
9-8
0993-5288
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.
0993-5288
9-9
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.
Antifoam Emulsion
110A
Dow Corning
Midland, MI 48601
U.S.A.
9-10
0993-5288
MHS 15:
Translations of Warnings
10
0993-5288
10-1
10-2
0993-5288
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
espaol
italiano
Nederlands
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.
0993-5288
10-3
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.
10-4
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
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
0993-5288
This symbol alerts you to the risk of hot surfaces that could cause personal injury to
yourself or other persons.
Details about these circumstances are in a box like this one.
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.
En los recuadros como ste se proporciona informacin sobre este tipo de
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.
Troverete informazioni su tali circostanze in un riquadro come questo.
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.
Detalhes referentes a estas circunstncias encontram-se referidos numa caixa como
esta.
suomea
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.
0993-5288
10-5
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.
En los recuadros como ste se proporciona informacin sobre este tipo de
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.
10-6
0993-5288
=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.
Troverete informazioni su tali circostanze in un riquadro come questo.
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.
Detalhes referentes a estas circunstncias encontram-se referidos numa caixa como
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.
0993-5288
10-7
W1.2
dansk
Deutsch
espaol
franais
10-8
0993-5288
=Warning (continued)
W1.2
italiano
Nederlands
portugus
suomea
svenska
0993-5288
10-9
10-10
0993-5288
dansk
Deutsch
espaol
franais
italiano
Nederlands
portugus
suomea
svenska
0993-5288
W1.3
10-11
W3.1
dansk
Deutsch
espaol
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.
10-12
0993-5288
=Warning (continued)
W3.1
italiano
Nederlands
portugus
suomea
svenska
0993-5288
10-13
10-14
0993-5288
W4.2
dansk
Deutsch
Warnung: Verbrennungsgefahr
Den heien Brennerkopf nur mit hitzebestndigen Schutzhandschuhen anfassen oder
vor dem Anfassen auf Krpertemperatur abkhlen lassen.
espaol
franais
italiano
Nederlands
portugus
suomea
svenska
0993-5288
10-15
W4.5
dansk
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
franais
10-16
0993-5288
=Warning (continued)
W4.5
italiano
Nederlands
portugus
suomea
svenska
0993-5288
10-17
W8.1
dansk
Deutsch
espaol
franais
10-18
0993-5288
=Warning (continued)
W8.1
italiano
Nederlands
portugus
suomea
svenska
0993-5288
10-19
10-20
0993-5288
Index
0993-5288
In-1
Index
In-2
0993-5288
Index
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
0993-5288
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
gasket in reaction flask socket
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
In-3
Index
mercury
calibration solutions 9-8
recommended conditions
(NaBH4) 3-9
recommended conditions
(SnCl2) 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
establishing pre-reaction purge
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
In-4
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
recommended conditions
antimony 3-13
arsenic 3-5
bismuth 3-7
mercury (NaBH4) 3-9
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
0993-5288
Index
selenium
establishing pre-reaction purge
time 2-12
recommended conditions
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
0993-5288
T
technical data 8-11
tellurium
recommended conditions
3-19
test solution 9-3
tin
contamination 2-9, 9-7
recommended conditions
3-17
transfer tube
replacing 4-10
V
ventilation, laboratory 1-5
W
waste disposal
contents of waste containers
1-8, 4-5
reaction residues 1-8, 4-5
U
unpacking 6-3
In-5
Index
In-6
0993-5288