ASTM D7202-05
(Test Method)Standard Test Method for Determination of Beryllium in the Workplace Using Field-Based Extraction and Fluorescence Detection
Standard Test Method for Determination of Beryllium in the Workplace Using Field-Based Extraction and Fluorescence Detection
SCOPE
1.1 This test method is intended for use in the determination of beryllium by sampling workplace air and surface dust.
1.2 This test method assumes that air and surface samples are collected using appropriate and applicable ASTM International standard practices for sampling of workplace air and surface dust. These samples are typically collected using air filter sampling, vacuum sampling or wiping techniques.
1.3 This test method includes a procedure for on-site extraction (dissolution) of beryllium in weakly acidic medium (pH of 1 % aqueous ammonium bifluoride is 4.8), followed by field analysis of aliquots of the extract solution using a beryllium-specific fluorescent dye.
1.4 The procedure is targeted for on-site use in the field for occupational and environmental hygiene monitoring purposes.
1.5 No detailed operating instructions are provided because of differences among various makes and models of suitable fluorometric instruments. Instead, the analyst shall follow the instructions provided by the manufacturer of the particular instrument. This test method does not address comparative accuracy of different devices or the precision between instruments of the same make and model.
1.6 The values stated in SI units are to be regarded as standard.
1.7 This test method contains notes which are explanatory and not part of mandatory requirements of the standard.
1.8 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use.
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Designation:D7202–05
Standard Test Method for
Determination of Beryllium in the Workplace Using Field-
Based Extraction and Fluorescence Detection
This standard is issued under the fixed designation D7202; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision.Anumber in parentheses indicates the year of last reapproval.A
superscript epsilon (e) indicates an editorial change since the last revision or reapproval.
1. Scope D1356 Terminology Related to Sampling and Analysis of
Atmospheres
1.1 Thistestmethodisintendedforuseinthedetermination
D4840 Guide for Sampling Chain-of-Custody Procedures
of beryllium by sampling workplace air and surface dust.
D5337 Practice for Flow Rate Calibration of Personal
1.2 This test method assumes that air and surface samples
Sampling Pumps
are collected using appropriate and applicableASTM Interna-
D6966 Practice for Collection of Settled Dust Samples
tional standard practices for sampling of workplace air and
Using Wipe Sampling Methods for Subsequent Metals
surface dust. These samples are typically collected using air
Determination
filter sampling, vacuum sampling or wiping techniques.
D7035 Test Method for Determination of Metals and Met-
1.3 This test method includes a procedure for on-site ex-
alloids in Airborne Particulate Matter by Inductively
traction (dissolution) of beryllium in weakly acidic medium
Coupled Plasma Atomic Emission Spectrometry (ICP-
(pH of 1% aqueous ammonium bifluoride is 4.8), followed by
AES)
field analysis of aliquots of the extract solution using a
D7144 Practice for Collection of Surface Dust by Micro-
beryllium-specific fluorescent dye.
vacuum Technique for Subsequent Determination of Met-
1.4 The procedure is targeted for on-site use in the field for
als
occupational and environmental hygiene monitoring purposes.
E691 Practice for Conducting an Interlaboratory Study to
1.5 No detailed operating instructions are provided because
Determine the Precision of a Test Method
of differences among various makes and models of suitable
E882 Guide for Control Charts
fluorometric instruments. Instead, the analyst shall follow the
E1792 SpecificationforWipeSamplingMaterialsforLead
instructions provided by the manufacturer of the particular
in Surface Dust
instrument. This test method does not address comparative
accuracy of different devices or the precision between instru-
3. Terminology
ments of the same make and model.
3.1 Definitions—For definitions of terms not appearing
1.6 The values stated in SI units are to be regarded as
here, see Terminology D1356.
standard.
3.2 Definition of Terms Specific to This Test Method:
1.7 This test method contains notes which are explanatory
3.2.1 wipe, n—adisposabletowelettethatismoistenedwith
and not part of mandatory requirements of the standard.
a wetting agent such as water (E1792; D6966).
1.8 This standard does not purport to address all of the
3.2.1.1 Discussion—These towelettes are used for collect-
safety concerns, if any, associated with its use. It is the
ing samples of dust, potentially containing beryllium, from
responsibility of the user of this standard to establish appro-
surfaces.
priate safety and health practices and determine the applica-
bility of regulatory limitations prior to use.
4. Summary of Test Method
4.1 Particles comprising beryllium from workplace air or
2. Referenced Documents
surfaces, or both, are collected in the field using procedures
2.1 ASTM Standards:
described in ASTM International standards. To extract (or
D1193 Specifications for Reagent Water
dissolve)berylliuminthecollectedsamples,themediainoron
which the samples are collected (that is, air sample, vacuum
sample or wipe) are treated on-site using an acidic extraction
This test method is under the jurisdiction of ASTM Committee D22 on Air
solution. The presence of active fluoride ions (HF by dissocia-
Quality and is the direct responsibility of Subcommittee D22.04 on Workplace
tion of ammonium bifluoride in acidic medium) enables
Atmospheres.
Current edition approved Nov. 1, 2005. Published December 2005. dissolutionofrefractorymaterialssuchasberylliumoxide.The
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
D7202–05
extraction solution produced from each sample is then filtered 7.3.5 Pipet tips, plastic, disposable, of assorted sizes as
and an aliquot of this extract is added to a pH-adjusted needed
detection solution which contains a beryllium-specific fluores-
7.3.6 Fluorescence cuvettes, disposable, 10-mm diameter,
cence reagent. The fluorescence of this final solution is then
transparent to UV/Vis radiation
measuredonacalibratedfield-portablefluorometertoquantify
7.3.7 Labware, plastic (for example, beakers, flasks, gradu-
the amount of beryllium in the sample.
ated cylinders, etc.), of assorted sizes as needed
7.3.8 Forceps, plastic or plastic-coated
5. Significance and Use
7.3.9 Personal protective wear, for example, respirators,
5.1 Exposure to beryllium can cause a potentially fatal
masks, gloves, lab coats, safety eyewear, etc. as needed
disease, and occupational exposure limits for beryllium in air
7.3.10 Other general laboratory supplies as needed.
andonsurfaceshavebeenestablishedtoreduceexposurerisks
to potentially affected workers (1, 2). Sampling and analytical
7.4 Reagents
methods for beryllium are needed in order to meet the
7.4.1 Water—Unless otherwise indicated, references to wa-
challenges relating to exposure assessment and risk reduction.
tershallbeunderstoodtomeanreagentasdefinedbyTypeIof
Field-portable sampling and analysis methods, such as the
Specification D1193 (ASTM Type I Water: minimum resis-
procedure described in this test method, are desired in order to
tance of 18 MV-cm or equivalent)
facilitate on-site measurement of beryllium. On-site beryllium
7.4.2 Calibration Stock Solution—1000-ppm beryllium in
analysis results can then be used as a basis for management of
dilute nitric acid or equivalent.
protection of human health.
7.4.3 Ethylenediamine tetraacetic acid disodium salt dihy-
6. Interferences drate (EDTA)
6.1 This test method is highly specific for beryllium. Other 7.4.4 L-lysine monohydrochloride
solvated metal ions are either bound by ethylene diamine
7.4.5 10-hydroxybenzo[h]quinoline-7-sulfonate
tetraacetic acid (EDTA) in the detection solution, or they
(10-HBQS).
precipitate out due to the high alkalinity of the detection
7.4.6 Sodium hydroxide
solution.
7.4.7 Extraction (or Dissolution) Solution—1%ammonium
6.2 If iron is present in high excess in the sample (typically
bifluoride (NH HF ) solution (aqueous) for dissolution of
4 2
more than 20 µM), the resulting measurement solution may
beryllium in collected particulate matter. (Warning—
appear golden-yellow. In this case the solution should be left
Ammonium bifluoride will etch glass, so it is essential that all
for an hour or more for the iron to precipitate. The solution
NH HF solutions are contained in plastic labware.)
should then be re-filtered using the same procedure as for 4 2
filtering the dissolution solution (after the dissolution step), 7.4.8 Detection Solution—63.4 µM 10-
prior to fluorescence measurement.
hydroxybenzo[h]quinoline-7-sulfonate (10-HBQS) (3) / 2.5
mMethylenediaminetetraaceticacid(EDTA)/50.8mMlysine
7. Apparatus
monohydrochloride (pH adjusted to 12.8 with NaOH): The
aqueous detection reagent is prepared by the addition of 12.5
7.1 Sampling Equipment
mL of 10.7 mM ethylenediamine tetraacetic acid (EDTA)
7.1.1 Air Sampling—Useairsamplersandfiltersforcollect-
ing personal air samples as described in Test Method D7035. disodium salt dihydrate and 25 mL of 107 mM L-lysine
7.1.2 Wipe Sampling—Use wipe sampling apparatus for monohydrochloride to 3 mL of 1.1 mM 10-
collecting surface dust samples as described in Practice
hydroxybenzo[h]quinoline-7-sulfonate (10-HBQS). The pH is
D6966.
adjustedto12.85withadditionofsodiumhydroxideandwater
7.1.3 Vacuum Sampling—Ifwipesamplingisnotadvisable,
added to a total of 50 mL.
use vacuum sampling apparatus collecting surface dust
NOTE 2—It is recommended to prepare the extraction and detection
samples as described in Practice D7144.
solutions in a fixed-site laboratory prior to transport to the field.
7.2 Instrumentation
7.2.1 Ultraviolet/Visible (UV/Vis) Fluorometer, with irradi-
8. Procedure
ance excitation lamp (excitation l=380 nm) and time-
integrating visible detector (400-700 nm, lmax ' 475 nm)
8.1 Sampling
7.2.2 Mechanical Agitator, shaker or rotator.
8.1.1 Air Samples—Collect workplace air samples for be-
ryllium in accordance with Test Method D7035, using per-
NOTE 1—An ultrasonic bath is an acceptable alternative.
sonal sampling pumps calibrated in accordance with Practice
7.3 Laboratory Supplies
D5337.
7.3.1 Centrifuge tubes, plastic, 15-mL (plus 50-mL, if
8.1.2 Wipe Samples—Collect surface wipe samples for
necessary)
beryllium in accordance with Practice D6966.
7.3.2 Syringe filters, 0.45-µm nylon, 13- or 25-mm diam-
8.1.3 Vacuum Samples—If wipe sampling is inadvisable for
eter, in plastic housings
surface dust sampling, collect surface vacuum samples for
7.3.3 Syringes, plastic, 5-mL
7.3.4 Pipetters, mechanical, of assorted sizes as needed beryllium in accordance with Practice D7144.
D7202–05
NOTE 7—Extraction is an example of a dissolution and solvating
8.1.4 Sample Transport—If applicable (that is, if samples
process.Methodevaluationmightindicatethatforcompletedissolutionof
are transported to a different location prior to sample prepara-
beryllium,itmaybenecessaryforthedissolutionprocesstobeassistedby
tion and analysis), follow sampling chain-of-custody proce-
ultrasonic energy, heat or longer treatment periods to obtain acceptable
dures to document sample traceability. Ensure that the docu-
recoveries. This will be dependent upon the sample media, particle
mentation that accompanies the samples is suitable for a chain
physical characteristics (such as shape and size) and the inertness of
of custody to be established in accordance with Guide D4840.
beryllium-containing compounds. Heating can aid in the dissolution of
8.2 Sample Preparation—Wear appropriate personal pro- refractory compounds such as beryllium oxide.
tection during sample preparation and analysis activities.
8.2.2.5 If the samples are heated during the extraction step,
Perform sample preparation and analysis in a clean area that is
theyshallbecooledtoambienttemperaturebeforealiquotsare
well removed from any possible beryllium contamination.
removed prior to addition of the detection solution.
8.2.1 Extraction of Air Filter Samples
8.2.3 Filtration—Filter aliquots (for example, 5 mL) of
8.2.1.1 Don clean gloves and open the samplers. Using
extract solution through inert microfilters.
forceps, remove the filters from the cassette and place them
NOTE 8—0.45-micrometre filters are acceptable. Preferred filters are
into 15-mL centrifuge tubes.
made out of nylon.
NOTE 3—Iftheentirecontentsofthesamplerareregardedaspartofthe
NOTE 9—Thefiltrationprocesscanbecarriedoutbyattachinga25-mm
sample, the interior of the cassette should be rinsed with extraction
diameter syringe filter to a 5- or 10-mLluer lock syringe and pouring the
solution, or wiped with another clean filter, and included in the centrifuge
liquid contents into the syringe. The liquid is forced out through the filter
tube. Alternatively, the extraction can be carried out within the sampling
into a separate 15-mL centrifuge tube.
cassette (see Test Method D7035).
8.2.4 Measurement solution preparation: Pipet 100 µL of
8.2.1.2 Pipet 5 mL of 1% ammonium bifluoride extraction
filteredsolutionextractsintofluorescencecuvettes.Tothisadd
solution (see 7.4.7) into the centrifuge tubes containing the air
1.9 mLof detection (dye) solution and ensure these are mixed
filter samples.
well.
8.2.1.3 Cap the centrifuge tubes and place them in a
mechanical shaker or agitator.
NOTE 10—Ifironispresentinhighexcess(typicallymorethan20µM)
in the sample, the resulting measurement solution may be golden-yellow.
8.2.1.4 Activate the mechanical shaker or agitator and
In this case the solution should be left for an hour for iron to precipitate.
agitate for a minimum of 30 minutes.
The solution should then be re-filtered using the same procedure as for
NOTE 4—Extraction is an example of a dissolution and solvating
filtering the dissolution solution and then used for fluorescence measure-
process.Methodevaluationmightindicatethatforcompletedissolutionof
ment.
beryllium,itmaybenecessaryforthedissolutionprocesstobeassistedby
8.3 Fluorometer Set-Up—Set up the fluorometer for excita-
ultrasonic energy, heat or longer treatment periods to obtain acceptable
recoveries. This will be dependent upon the sample media, particle tion radiation from 360 to 390 nm and measurement of
physical characteristics (such as shape and size) and the inertness of
emission in a spectral window selected from a range of (at
beryllium-containing compounds. Heating can aid in the dissolution of
least)440to490nm.Allowappropriatewarm-upofthesystem
refractory compounds such as beryllium oxide.
prior to analysis (follow manufacturer’s instructions).
8.2.1.5 If the samples are heated during the extraction step,
NOTE 11—For fluorescence measurement, a band pass filter with peak
theyshallbecooledtoambienttemperaturebeforealiquotsare
transmission wavelength at ~475 nm and with a full width at half
removed prior to addition of the detection solution.
maximum(FWHM)oflessthan 610nmhavebeenshowntobeeffective
8.2.2 Extraction of Wipe Samples
(4).
8.2.2.1 Doncleanglovesand,usingforceps,placethewipes
8.4 Preparation of Calibration Standards—Using calibra-
into 15- or 50-mL centrifuge tubes.
tion stock solution and 1% aqueous ammonium bifluoride
NOTE 5—Thesizeofthewipesusedforsampling(8.1.2)willdetermine solution, prepare at least four standards covering the concen-
thesizeofthecentrifugetubestouseforextraction.Smallwipematerials,
tration range of interest.
suchas47-mmdiameterfilters,canbeplacedinto15-mLcentrifugetubes.
NOTE 12—Example:To measure the range of 0.02 to 4 µg of beryllium
Larger wipes, however, will require the use of larger tubes such as 50-mL
inthesamples,arecommendedrangeofcalibrationstandardsis0,10,40,
volume.
200 and 800 parts per billion (ppb).
8.2.2.2 Pipet 5 mL or 10 mL of 1% ammonium bifluoride
8.5 Calibration and Specifications
extraction solution (see 7.4.7) into the centrifuge tubes con-
8.5.1 Calibration Blank and Calibration Standard Solutions
taining the wipe samples.
Preparation—Calibration blank is prepared by adding in a
NOTE 6—The size of the wipes used for sampling (8.1.2) and the size
proportion of 1:19 (by volu
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