Application

Note:
The analysis of environmental materials by
AN40689_E
Atomic Absorption Spectrometry

Introduction environment and to measure their impact upon it. This, in

Key Words In the field of laboratory analysis, environmental turn, has meant that there has been a major requirement
applications have long been a number one priority for for instrumentation and methodology capable of
• AAS
many laboratories. implementing the new regulations.
• Environmental The present concerns about global warming, and the One of the main instrumental techniques that has had
desire to clean up the environment for the benefit of a leading role in the analysis of environmental samples is
• Atomic
everyone, have produced many new pieces of legislation Atomic Absorption Spectrometry (AAS). As a technique, it
Absorption
governing the permitted discharges into waters, the air possesses the right combination of performance and ease
Spectrometry
and on to the land. This increased level of legislation is of use to carry out the analytical tasks and is priced at a
• Overview being enacted by various authorities with a number of key level within the range of many laboratories. This paper
agencies, such as the Environmental Protection Agency in will discuss the application of a new environmental
America and the EEC Committees in Europe, leading the version of the Thermo M Series AA systems to a selection
way. Such legislation places a responsibility on every of typical environmental analyses.
organisation to monitor the condition of the local
1) Introduction: From these lists it can be seen that Atomic Absorption
Major sources of pollution come from many of our can measure the legal limits for toxic metals such as As,
day-today activities, such as Farming, Industry, Cd, Pb and Hg in most sample types. The use of Hydride
Transportation and Urban sites. The effects of these techniques can improve the performance for hydride
activities impact on the three main areas of our forming elements such as As and Se.
environment; the land, the water and the air. For example,
consider the mining and metal processing industry. The
mining activity can add pollution to the air (in the form of
dust), to the water (in the form of washings from ore
processing) and the land (in the form of mining waste
heaps). Metals production introduces fumes and
particulate to the air and land and produces waste water
which flows into the surface water layers.
Environmental pollution is monitored in a number of
ways and this has resulted in a wide variety of sample ELEMENT CLP D.L. GFAAS D.L.
types being supplied for analysis. This list shows the Aluminium 200 0.21
main types: Antimony 60 0.4
Biological - serum, urine, tissue. Arsenic 10 0.53
Waters - sea, fresh, waste. Beryllium 5 0.003
Plant materials Cadmium 5 0.02
Soils, sludges and sediments Chromium 10 0.025
Airborne particulates Cobalt 50 0.17
As a result of this variety of sample types, a number Copper 25 0.29
of different sampling and preparation techniques have to Iron 100 0.18
be used. Lead 3 0.07
Pollution legislation generally specifies certain element Manganese 15 0.06
concentration levels which it considers to be representative Nickel 40 0.16
of pollution in the different sample types. Selenium 5 0.8
This means that any analytical technique must possess Silver 10 0.04
a sensitivity at least equal to, but preferably better than, Thallium 10 0.5
these levels before it is suitable for use in environmental
Table 2: Comparison of the EPA Method 200.9 required detection limits
analysis. As legislation changes it is more often the case
(µg/L) and the Zeeman GFAAS detection limits (3 σ µg/L) for water analysis.
that these limits are further reduced. Tables 1 and 2
shown here indicate the applicability of AAS for the The Cold Vapour Mercury technique still has a major
different chemical elements and the main sample types role to play in environmental analysis as this permits the
characteristic of environmental applications. lowest possible detection limit, especially when linked to
the Gold Amalgam Concentration unit.
ELEMENT EEC MAC TECHNIQUE

Magnesium 50,000 FAAS (2.2)

2) Features of the AA Series MQZe System:
Sodium 150,000 FAAS (3.7)
The Thermo M Series of AA spectrometers includes a
Potassium 12,000 FAAS (0.9)
special version for environmental use, the MQZe. This is
Aluminium 200 GFAAS (0.21)
a system tailored specifically to handle the toxic element
Iron 200 FAAS (4.3)
analyses required by the various regulatory authorities.
Manganese 50 GFAAS (0.06)
(1) Dual atomiser system, consisting of a combination
Copper 3,000 FAAS (4.5)
of the VP90 Continuous Flow Vapour system and EC90
Zinc 5,000 FAAS (3.3)
Electrically Heated Vapour cell, together with a GF95
Silver 10 GFAAS (0.04)
Zeeman Furnace System.
Arsenic 50 HGAAS (0.05)
(2) When equipped with the FS95 Furnace
Cadmium 5 GFAAS (0.02)
Autosampler and the appropriate vapour autosampler, the
Chromium 50 GFAAS (0.025)
system is capable of fully automated analysis for both
Mercury 1 HGAAS (0.15)
vapour and furnace elements. This includes overnight,
Nickel 50 GFAAS (0.16)
unattended analyses.
Lead 50 GFAAS (0.07)
(3) Auto change-over between vapour and furnace
Antimony 10 HGAAS (0.27)
analysis carried out by software means only, no manual
Selenium 10 HGAAS (0.27)
intervention required.
Barium 1,000 FAAS (3.0)

Table 1: List of Maximum Allowable Concentrations for drinking water in

µg/L, (Council for European Communities Journal), showing the technique
(and its detection limit in µg/L in parentheses). FAAS = Flame AAS, GFAAS =
Graphite Furnace AAS, HGAAS = Hydride Generation AAS.
 (4) Easy to use, Wizard-driven software to simplify
operation and including comprehensive QC facilities and
printout options.
(5) Optional high sensitivity mercury accessories
permit mercury perfomance down to µg/L levels.
(6) Validator and Validatorplus accessories enable
systems to be validated as part of a regulatory compliance
programme.

Figure 1: Complete Thermo MQZe System.

3) Environmental Analysis in practice:

We will now break down a typical analysis into its
separate parts and consider the main factors which must
be borne in mind at each stage of the procedure. Another example is from the biological field. When
(a) The sampling phase using human hair as an indicator of exposure to toxic
This is the most important phase of an analysis, and often materials, it must be remembered that the concentration
the one most poorly carried out. It must be remembered levels in normal hair increase the closer one moves to the
that any mistakes made at this stage can ruin the excellence root of the hair. Similar differences occur in plant
of all the stages that follow. There must be a sampling materials, where element concentration levels in old wood
strategy in place which is carefully thought out and takes can be totally different to those in the growing tip.
into account all the known possible sources of error. Now moving on to point 2. Sample containers can
There are two main considerations which are produce negative, or positive, errors in trace metal
absolutely vital to the success of any analysis: analysis by either of two actions.
(1) The sample taken must be representative of the Firstly, they can add contaminants by leaching or
whole sample. surface desorption of material already present on the
(2) The sample containers must be clean. container walls. This may be residues of a previous sample
or from detergents used to clean the container. In
As an example of point 1, consider the sampling of
addition, materials used in manufacturing the sample
waters where the following factors must all be considered:
container itself may be a problem. For example, zinc
• the influence of tides in seawater sampling. compounds used as mould release agents in manufacturing
• the proximity of tributaries or sewage outfalls when are a notorious source of contamination in new
sampling river water. containers.
• the possibility of noncontinuous discharge of effluents Secondly, loss by surface adsorption can reduce the
into a river. apparent concentration of elements in a sample. This is
• the presence of cold and warm layers in lakes. particularly true of certain plastic materials, such as low
• the fact that still tapwater can contain erroneously high density polyethylene, and glass.
metal concentrations which are not seen in a flowing
sample.
• the disturbance of sediments in a river or lake bottom
caused by the action of taking the sample.
• that rainwater composition varies with the type of
weather, the season and even the time of day.
 Laboratory containers, whether glass or plastic (this required elements. The columns are sealed and taken back
includes polyethylene, polypropylene or fluorocarbon) to the laboratory where the trapped metals are eluted
should always be washed first with a detergent solution using a small volume of eluent. Concentration factors of
that does not contain high levels of metal compounds. It is 10 – 20 times can be achieved, an added benefit which
important to remember that certain detergents can contain improves the ultimate detection limits attainable. Columns
high levels of metals, such as zinc and sodium, which can be stored for several weeks before carrying out the
remain bound to container walls even after flushing with analysis.
clean distilled or deionised water. Glassware is often
(c) Water analysis : Treatment and analysis
cleaned with a chromic acid wash because it is a powerful
For soluble metals analysis, the filtered and acid-preserved
cleaning agent for removing organic material. However,
samples can often be analysed as received. If a precipitate
the chromium persists in glassware for a long time, even
forms during storage, it must be re-dissolved by adding
after thorough washing with water, and is a major source
acid and/or heating. It is normal practice to analyse
of contamination.
samples against matrix matched standards.
After the detergent wash, the containers should then
The suspended solids held on the filter paper must be
be rinsed thoroughly in distilled or deionised water,
solubilised before analysis. This is carried out in the
followed by rinsing with a (1 + 1) solution of nitric acid.
following manner. Place the filter membrane in a suitable
The acid is used to strip any metals adhering to the walls
clean beaker and add 4 mL concentrated nitric acid.
of the container. Another distilled water wash should be
A cover is placed over the beaker and it is heated gently to
followed by a (1 + 1) solution of hydrochloric acid.
dissolve the membrane. The temperature is raised to digest
A final distilled wash is made before the container is hot-
the material, continuing until the contents are reduced to
air dried.
low volume. After cooling, another 3 mL of concentrated
We will now consider some of the more important
nitric acid is added and the beaker covered again. Heating
analyses. The single most important analysis concerns
is continued until digestion is completed and the contents
water - there are currently more water samples analysed
are then reduced to about 2 mL. The contents are cooled
than any other single type.This is a very convenient
and 10 mL of (1 + 1) hydrochloric acid plus 15 mL
sample for AAS because it is already liquid. Solid samples
of distilled water are added for every 100 mL in the final
cannot, in general, be analysed directly by AAS.
sample volume. The metals are re-solubilised by heating
(b) Water analysis : The pre-treatment phase for 15 minutes, then the contents are cooled and washed
Before a sample is collected, the kind of data required at into a volumetric flask. Any remaining insoluble material
the end of the analysis must be defined. For instance, in is filtered off, if necessary, and the contents of the flask are
water analysis, is it the soluble metals or the suspended made up to volume.
solids or a total analysis that is required? When analyzing In the case of the total analysis, the preserved sample
soil samples, is it the available metals that are to be is heated with an additional 3 mL. of concentrated nitric
analysed or the total. acid and evaporated to near dryness. It is important that
Taking water analysis as an example and with soluble the sample is not boiled or heated to dryness. After
metals to be measured, the following procedure is used. cooling, a further 5 mL of concentrated nitric acid is
The water must be filtered through a 0.45µm added and the sample re-heated to reflux the acid. The
membrane filter as soon as possible after collection. It is sample is heated, with the addition of more acid as
normal to use the first 50 - 100 mL of sample to rinse the necessary, until the digestion is complete. From this point
apparatus and discard the filtrate. The required sample onwards the finish is the same as for the suspended solids.
volume is then collected. Acidification with (1 + 1) nitric
(d) Water analysis : Results
acid to pH 2 or less is used to stabilise the metal content.
Water analysis is carried out and measured against a
Normally 3 mL of (1 + 1) nitric acid per litre of sample
number of criteria, which tend to be different in different
should be sufficient.
parts of the world. There is presently no universally
If the suspended solids content is required, basically
accepted list of limits but the most commonly used values
the same initial procedure is used. The difference is that
for natural waters are those published by the USEPA in
the filter containing the suspended solids is retained and
America. Table 3 shows the guide figures for the different
stored in a suitable container. No preservation is needed.
types of natural waters and the typical detection limits
For a total analysis, the whole sample is acidified with
which can be obtained when using the appropriate AA
(1+ 1) nitric acid to pH 2 or less, preferably at the time of
technique.
collection. The sample is not filtered.
A relatively new technique that shows great promise
for water analysis is on-line pre-concentration. The basis
of the method involves the preparation of small mini-
columns containing an ion-exchange material. These are
taken to the sampling site where known volumes of the
sample are drawn through the column, trapping the
ELEMENT RIVER SEA RAIN AA D.L. Where samples are mainly metals, as in welding fume,
As 2 3 < 0.3 0.05 * and collected using personal samplers, the usual
Ba 20 30 70 0.5 dissolution procedure is to use simple acid digestion. The
Cd 0.1 0.1 0.5 0.02 metals involved define the procedure used. For Cr, Cu, Fe,
Cr 1 0.05 7 0.025 Mn, Ni, Zn, Ag, Cd, Pb, Au, B, Ba, Bi, Ca, Mg, Sr and V
Cu 3 3 30 0.3 the filters are simply digested in 10 mL of concentrated
Fe 100 10 1000 0.18 nitric acid. For Al, Be, Co, Mo and Ti the filters are
Hg 0.07 0.03 0.01 0.15 * digested in 10 mL of a 50:50 mixture of nitric and
Mn 15 2 60 0.06 hydrochloric acids. After digestion the samples are heated
Ni 10 2 10 0.16 at 140 ºC to near dryness and then re-solubilised to a final
Pb 3 0.03 50 0.07 volume of 10 mL with 0.1% nitric acid.
Sb 1 0.5 2 0.26 *
METAL EXPOSURE LIMIT AIR VOLUME
Se 0.2 0.4 <1 0.27 * (8 HOURS) MG.M3 SAMPLED (LITRES)

Table 3. Natural levels of elements in natural waters. All figures are in µg/L. Al 5.0 180
AA detection limits are for the graphite furnace, apart from those shown B 10.0 60
with a * which are hydride performance figures. Be 0.002 500
Cd 0.025 280
The same situation largely applies for drinking water
Cu 0.2 90
but Tables 1 and 2 (shown earlier) represent the figures
Cr 0.5 90
currently used within Europe and the USA.
Fe 5.0 150
Moving on to other types of environmental samples,
Mn 1.0 22
we will consider their main characteristics.
Ni 1.0 90
Pb 0.15 180
4) Airborne particulate analysis:
Ti 5.0 100
There are many sources of airborne particulate, such as
Zn 5.0 100
waste incineration and welding activities to name but a
few. Waste incineration has caused a much higher Table 4: List of airborne particulate exposure limits (according to 91/332/EEC
awareness of the problems caused to the environment, on and 96/94/EC.
the one hand solid wastes are reduced by up to 90% but
Table 4 shows the current limits for exposure
on the other hand new waste products like dust are
measured over an 8-hour working day, together with the
created.
approximate volume of air which needs to be sampled in
Samples are commonly collected by sucking known
order to get a measureable signal.
volumes of air through a glass fibre or membrane filter.
For samples containing a high ash content, dissolution
The volume of air used depends on the level of
schemes developed for the analysis of siliceous materials
contamination and the elements being measured. A high
are generally used. Increasingly the use of microwave
volume set-up with a 20 - 25 cm wide filter typically has
digestion is becoming the preferred technique. By using a
collection times (for a flow rate of 75 m3h-1) of 1 hour for
sealed vessel and heating it in a microwave oven, it is
contaminated urban air and up to 12 hours for clean rural
possible to considerably shorten the dissolution time.
atmospheres. A number of portable, battery-powered
There are a number of commercially available laboratory
samplers are available for personal monitoring at the
microwave systems which are specifically designed for use
workplace. Using 25 mm glass fibre filters, a flow rate of
with the corrosive chemicals used in dissolution
about 2 litres/min is used. This type of sampler is also
procedures. Typically a sample treated by the traditional
used for sampling at sites where no mains electricity is
pressure digestion method requires about 50 minutes of
available. An alternative for use at large installations, such
heating whereas the microwave takes about 6 minutes.
as power stations or incinerator chimneys, is the cascade
The USEPA has certified some of its methods (often these
impactor or electrostatic filter. Two types of sample are,
become the standard methods elsewhere in the world)
therefore, generally available - particles held on a
with microwave dissolution.
membrane filter or loose powder taken from a cascade
The results shown below in Table 5 are for an Urban
impactor or the like.
particulate, NBS SRM1648, prepared using microwave
dissolution.
METAL CERTIFIED VALUE FOUND ELEMENT LANDFILL MATERIAL UNDERLYING SOIL

Al 3.4 +/- 0.11 3.60 Al 12,000 8,800

Fe 3.91 +/- 0.10 3.32 As 0.1 18
Pb 0.655 +/- 0.008 0.579 Cd 0.8 0.3
Zn 0.476 +/- 0.014 0.434 Co 8.4 3.8
All results in % weight Cr 37 18
Cu 430 79
Cd 75 +/- 7 77.3 Fe 36,000 14,000
Cu 609 +/- 27 603 Mn 340 200
Mn 860 666 Ni 27 24
Ni 82 +/- 3 84 Pb 140 110
V 140 +/- 3 112 V 5.5 4.9
All results in mg/g Zn 420 95

Table 5: Analysis results obtained for NIST SRM1648. All results in µg/g
Table 6: Analysis of leachate from a landfill site compared to the underlying
5) Analysis of soils and sediments: base soil.
A serious source of long-term pollution results from the ELEMENT MEASURED CERTIFIED
common practice of disposing of urban solid wastes by
Al 49.4 +/- 0.2% 47.0
burying them in landfill sites. Similarly, the use of some
Ba 2.92 +/- 0.5% 2.50
sewage sludges for agricultural purposes can cause
Cd 0.879 +/- 0.3% 0.90
problems, both by contamination of the crops and also of
Cr 57.3 +/- 0.9% 55.4
surface and groundwater. Toxic elements in these
Cu 3.98 +/- 0.3% 3.91
materials are leached out slowly with time by the action of
Fe 444 +/- 0.3% 441
rainwater percolating down through the layers. The result
Mn 1.84 +/- 0.1% 1.87
can be severe contamination of underlying soil and
Ni 0.56 +/- 2.4% 0.53
groundwater, with the consequent risk to extracted water
Pb 6.38 +/- 0.6% 6.42
supplies. The metals found in the groundwater depends on
Ti 3.42 +/- 2.3% 3.50
a number of factors but the ultimate aim of the analysis is
V 1.10 +/- 0.7% 0.97
to simulate the natural leaching action of rain in order to
Zn 10.8 +/- 0.7% 10.6
estimate the available metals content. This is normally
done by taking a known weight of waste and leaching it All results in µg/g
with a dilute acid, typically 0.5M acetic acid. Table 7: Analysis of a wet digested river sediment.
Soil samples are dried to constant weight at about
The second set of results shown in Table 7 are for a
110 ºC. It may take as long as 2 days to achieve this.
river sediment using the aqua regia treatment.
Stones and other debris must be removed before the dried
sample is ground in a metal-free mortar and pestle to pass
a 100 mesh sieve. Each sample powder is then shaken
6) Plant material analysis:
Plant materials are often used as indicators of both
thoroughly to ensure homogeneity before a known weight
airborne and sub-soil contamination. Samples may be root
of sample is taken for the analysis.
crops, like turnip or beetroot, or leaves of plants, such as
Soil and sediment analyses are good examples of the
lettuce or cabbage.
problems of taking truly representative samples. Sufficient
Roadside vegetation has commonly been used to
material must be taken to be indicative of the whole site
monitor Pb contamination from vehicle exhausts.
being sampled and then the bulk material must be
Table 8 shows some typical values for a range of
subdivided to provide the final representative sample. For
elements in different crops.
a total analysis, conventional pressure dissolution or
microwave attack are used. Leaching can also be carried
out using aqua regia attack. Typically 1 gram of sample is
digested with 30 mL aqua regia by boiling to low volume.
After cooling, 25 mL concentrated nitric acid is added
and boiled to dryness. The residue is dissolved in distilled
water and analysed against standards which have had
similar treatment.
The results in Table 6 are for the analysis of a landfill
sample and the underlying soil levels measured after an
acetic acid leach.
PLANT PART Cd Cu Ni Pb Zn 7) Biological Samples:
Tomato Fruit 1 6.8 7.1 2.3 18.5 The range of biological sample can be quite wide, with
Leaf 8.5 10.9 11.1 10.3 24.6 some available in liquid form (serum and urine) but others
Lettuce Fruit 5.5 9.4 6.3 2.7 111 are taken as solids (tissue and hair) requiring
Leaf 5.5 9.4 6.3 2.7 111 solubilisation. Biological samples are often taken from
Carrot Fruit 0.92 2.85 2.0 0.92 53.9 workers as part of an Industrial Health programme;
Leaf 1.8 8.8 3.7 8.2 166 typical examples are monitoring workers in plating bath
Cabbage Fruit 1.1 5.7 9.7 3.0 58.5 works or people handling toxic materials such as
Leaf 1.1 5.7 9.7 3.0 58.5 beryllium in the semiconductor industry. Urine is not a
Oats Fruit 0.3 6.0 3.7 0.77 43.1 good indicator of long-term exposure; blood and blood
Leaf 0.92 15.4 7.7 0.77 93.9 serum are better.
Pea Fruit 0.15 7.6 6.0 1.5 50.8 Tissue and bone are the best indicators but the most
Leaf 0.15 11.1 2.0 6.9 93.9 difficult samples to obtain.
Total soil 7.4 113.0 81.3 164 318 In the environmental field, tissue from a variety of
Extractable 5.9 17.4 25.6 8.87 73.7 species is used but a particularly useful indicator of
(acetic acid) pollution in natural waters, like the sea, and sediments are
All results as mg/kg dry matter shellfish.
Table 8: Results for various crops and the soil on which they were grown.

We will consider the determination of arsenic and

selenium in plant materials using the Hydride technique.
The actual sampling procedures for plant materials
will vary considerably, depending whether it is a root or
foliage sample. Again, taking a representative sample is
These filter feeders convert inorganic metals, such as
important. Foliage should be cut, not plucked or torn, at
Hg, Pb and Cd, into their organo-metallic forms and these
least 3 cm. above the soil level to avoid contamination
are stored, generally in the fatty tissues. They can amplify
from the soil itself. A composite sample of at least 25
natural surrounding levels of pollution many-fold, as
plants should be taken and this should weigh not less than
shown in Table 11 below. Care must be taken, therefore,
1 kg in weight. Materials like roots should be washed free
when sampling shellfish because the toxic metals are
of soil and about 200 g of sample taken.
preferentially stored in certain tissues, as shown below in
These samples are then air-dried and ground to pass a
Table 12.
1 mm sieve. A representative sample is then digested in a
Fluid samples are normally treated by simple dilution
nitric acid/perchloric acid mixture (with care - there can
but tissue samples require solubilisation by an appropriate
be a risk of explosion if too much organic material is
wet-digestion procedure.
involved). The digest is then heated in concentrated
hydrochloric acid to convert the As and Se to their lower METAL AMPLIFICATION FACTOR
oxidation state (due to the lower sensitivity of the higher Cd 2,260,000 times
states). Cr 200,000
Results are shown for As in certified plant foliage Fe 290,000
materials in Table 9 and for Se in flour in Table 10. Pb 290,000
Mn 56,000
SAMPLE MEASURED CERTIFIED
Mo 90
Pine Needles 0.19 0.21
Ni 12,000
(NIST 1575)
Spinach 0.13 0.15 Table 11: Examples of the metal enrichment that can occur in shellfish tissue
(NIST 1570) relative to surrounding waters.

All results in µg/g SAMPLE TYPE % OF BODY Pb CONC Cd CONC

MASS (mg/kg) (mg/kg)
Table 9: Analysis of plant materials for As.
Scallop: Gills 10 52 < 20
SAMPLE MEASURED CERTIFIED Muscle 24 <5 < 20
Wheat Flour 0.19 0.21 Fatty tissue 17 8 2000
(NIST 1567) Intestine 1 28 < 20
Kidney 1 137 < 20
All results in µg/g
Gonads 20 78 < 20
Table 10: Analysis of wheat flour for Se.
Sediment <5 < 20
Seawater * 3 0.11

* Seawater results are in µg/L

Table 12: Comparison of trace metal concentrations in shellfish tissue to
local seawater and sediments.
9) Conclusions: In addition to these
At the present time, AAS has a leading role in offices, Thermo Electron
environmental analysis because of its sensitivity for a large Corporation maintains
selection of elements typically determined by a network of represen-
environmentalists. Graphite furnace-AAS continues to be tative organizations
the preferred technique for ppb level determinations of the throughout the world.
heavy, toxic metals like Pb and Cd. In addition, hydride
techniques provide excellent performance for the
semimetals like As, Se and Sb. Finally, a range of specific
accessories provide detection limits for Hg down to the
ppt level.
Australia
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combination of Zeeman correction graphite furnace and Belgium
+32 2 482 30 30
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AN40689_E 05/04