ASTM D7441-08
(Practice)Standard Practice for Separation of Beryllium from Other Metals in Digestion and Extraction Solutions from Workplace Dust Samples
Standard Practice for Separation of Beryllium from Other Metals in Digestion and Extraction Solutions from Workplace Dust Samples
SIGNIFICANCE AND USE
Beryllium is an important analyte in industrial hygiene because of the risk of exposed workers developing Chronic Beryllium Disease (CBD). CBD is a granulomatous lung disease that is caused by the body’s immune system response to inhaled dust or fumes containing beryllium, a human carcinogen (2). Surface wipe samples and air filter samples are collected to monitor the workplace. This practice addresses the problem of spurious results caused by the presence of interfering elements in the solution analyzed. The practice has been evaluated for all elements having emission spectra near the 313.042 and 313.107 nm beryllium lines, as well as elements of general concern including aluminum, calcium, iron and lead. Below is a table listing each possible spectrally interfering element:
CeriumChromiumHafnium Molybdenum NiobiumThoriumTitaniumThulium UraniumVanadiumUranium
Measurement of beryllium on the order of 1 ppb (0.003 µg Be/100 cm2 wipe sample) has been successfully accomplished in the presence of spectrally interfering elements on the order of hundreds of ppm. This method has been validated on matrices containing 10 mg of each of the above elements. In some cases including interferents such as chromium and calcium, the single 2 mL beryllium extraction chromatography resin can handle >100 mg of total dissolved solids and still deliver >90 % beryllium yield. Should the matrix contain greater amounts of contaminants, additional resin may be used or, more likely, a combination of different resins may be used. (3,4).
SCOPE
1.1 This practice covers the separation of beryllium from other metals and metalloids in acid solutions, by extraction chromatography, for subsequent determination of beryllium by atomic spectroscopy techniques such as inductively coupled plasma atomic emission spectroscopy (ICP-AES).
1.2 This practice is applicable to samples of settled dust that have been collected in accordance with Practices D 6966 or D 7296.
1.3 This practice is compatible with a wide variety of acid digestion techniques used in digesting settled dust samples, such as those described in Test Method D 7035.
1.4 This practice is appropriate for the preparation of settled dust samples where an unacceptable bias is suspected or known because of spectral interferences caused by other metals or metalloids present in the sample. This practice may also be appropriate for the analysis of other types of samples.
1.5 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: D7441 − 08
StandardPractice for
Separation of Beryllium from Other Metals in Digestion and
Extraction Solutions from Workplace Dust Samples
This standard is issued under the fixed designation D7441; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
1. Scope Coupled Plasma Atomic Emission Spectrometry (ICP-
AES)
1.1 This practice covers the separation of beryllium from
D7296 Practice for Collection of Settled Dust Samples
other metals and metalloids in acid solutions, by extraction
Using Dry Wipe Sampling Methods for Subsequent De-
chromatography, for subsequent determination of beryllium by
termination of Beryllium and Compounds
atomic spectroscopy techniques such as inductively coupled
E882 Guide for Accountability and Quality Control in the
plasma atomic emission spectroscopy (ICP-AES).
Chemical Analysis Laboratory
1.2 This practice is applicable to samples of settled dust that
have been collected in accordance with Practices D6966 or
3. Terminology
D7296.
3.1 For discussion of pertinent terms not discussed here, see
1.3 This practice is compatible with a wide variety of acid
Terminology D1356.
digestion techniques used in digesting settled dust samples,
3.2 Definitions:
such as those described in Test Method D7035.
3.2.1 digestion—dissolution using a combination of acids
1.4 This practice is appropriate for the preparation of settled and other reagents of solid materials into solution for subse-
dustsampleswhereanunacceptablebiasissuspectedorknown quent instrumental analysis.
because of spectral interferences caused by other metals or
3.2.2 eluate—the effluent from a chromatography or resin
metalloids present in the sample. This practice may also be
column.
appropriate for the analysis of other types of samples.
3.2.3 extraction chromatography—liquid chromatography
1.5 This standard does not purport to address all of the
applied to the separation of metal ions utilizing selective
safety concerns, if any, associated with its use. It is the
organic extractants as the stationary phase and the aqueous
responsibility of the user of this standard to establish appro-
solution as the mobile phase (1) .
priate safety and health practices and determine the applica-
3.2.3.1 Discussion—Extraction chromatography resins con-
bility of regulatory limitations prior to use.
sist of inert porous beads coated with selective extractants.
3.2.4 spectral interference—an interference caused by the
2. Referenced Documents
emission from a species other than the analyte of interest.
2.1 ASTM Standards:
D7035
D1193 Specification for Reagent Water
3.2.5 surface wipe—refers either to a wetted wipe, as
D1356 Terminology Relating to Sampling and Analysis of
defined in Practice D6966, or to a dry wipe, as defined in
Atmospheres
Practice D7296, used to gather material from a surface for
D6966 Practice for Collection of Settled Dust Samples
subsequent analysis.
Using Wipe Sampling Methods for Subsequent Determi-
3.2.5.1 Discussion—The terms wipe sampling, swipe
nation of Metals
sampling, and smear sampling describe the techniques used to
D7035 Test Method for Determination of Metals and Met-
assess surface contamination on the skin, work surfaces, and
alloids in Airborne Particulate Matter by Inductively
PPE surfaces (for example, gloves, respirators, aprons, etc.)
3.2.6 vacuum box—container used to maintain a vacuum on
This practice is under the jurisdiction ofASTM Committee D22 on Air Quality
a resin or column sample in order to increase the rate of flow
and is the direct responsibility of Subcommittee D22.04 on WorkplaceAir Quality.
of liquid through the column. Other vacuum sources such as an
Current edition approved April 1, 2008. Published May 2008. DOI: 10.1520/
aspirator may be used.
D7441-08.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Standards volume information, refer to the standard’s Document Summary page on The boldface numbers in parentheses refer to a list of references at the end of
the ASTM website. this standard.
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D7441 − 08
4. Summary of Practice 6.1.2 2-mL cartridges of beryllium extraction chromatogra-
phy resin ,
4.1 This practice is based on using extraction chromatogra-
6.1.3 Syringe barrel (or similar size reservoir),
phy resin to separate beryllium ions from other metal ions in
6.1.4 Vacuum box, with fittings compatible with the
extracts and digestates of surface wipe samples.
cartridges,
4.2 Surface wipe samples are collected using Practice
6.1.5 Delivery pipet, 5 mL or 10 mL,
D6966 or Practice D7296, and are then digested or extracted
6.2 Reagents:
into solution by mineral acids.
(See Note 1.)
4.3 The pH of the solution is adjusted to between 1 and 2
6.2.1 DeionizedWater,Type I orType II in accordance with
with sodium acetate.
Practice D1193,
6.2.2 Nitric Acid (HNO ), concentrated, ρ~1.42 g/mL
4.4 The sample is then loaded onto the extraction chroma-
tography resin column, where beryllium is retained. Matrix (~70 % m/m),
6.2.3 Boric Acid (H BO ),
interferencesarerinsedfromthecolumnwith0.2Mnitricacid.
3 3
6.2.4 Ammonium Oxalate monohydrate (NH C H O),
4 2 4
4.5 Beryllium is selectively eluted from the resin with 4 M
6.2.5 Sodium acetate trihydrate (C H O Na· H O),
2 3 2 3 2
nitric acid and is available for analysis using the spectroscopic
6.2.6 Methyl Violet (indicator grade).
techniques such as ICP-AES (See Test Method D7035).
NOTE1—Purity of Reagents—Reagentgradechemicalsshallbeusedin
5. Significance and Use
all tests. Unless otherwise indicated, it is intended that all reagents
conform to the specifications of the Committee onAnalytical Reagents of
5.1 Beryllium is an important analyte in industrial hygiene
the American Chemical Society where such specifications are available.
because of the risk of exposed workers developing Chronic
Other grades may be used, provided it is first ascertained that the reagent
Beryllium Disease (CBD). CBD is a granulomatous lung
is of sufficiently high purity to permit its use without lessening the
disease that is caused by the body’s immune system response accuracy of the determination.
to inhaled dust or fumes containing beryllium, a human
6.3 Solutions:
carcinogen (2). Surface wipe samples and air filter samples are
6.3.1 3.4 M Sodium acetate + 0.2 M Ammonium oxalate +
collected to monitor the workplace.This practice addresses the
(0.2 M Boric acid): To a l-L volumetric flask, add 500 mL of
problem of spurious results caused by the presence of interfer-
deionized water. Add 12.37 grams of Boric acid and mix until
ing elements in the solution analyzed. The practice has been
dissolved. Add 28.42 grams of Ammonium oxalate monohy-
evaluated for all elements having emission spectra near the
drate and mix until dissolved. Add 462.68 grams of Sodium
313.042 and 313.107 nm beryllium lines, as well as elements
acetate trihydrate and mix. Fill to 1 Lwith deionized water and
ofgeneralconcernincludingaluminum,calcium,ironandlead.
mix until dissolved.
Below is a table listing each possible spectrally interfering
NOTE 2—Boric acid is added to combat the effect of HF used in
element:
digestion. If HF is not used, the Boric acid may be omitted.
Cerium Chromium Hafnium Molybdenum
6.3.2 Ammonium Oxalate, 0.25 M: To a l-L volumetric
Niobium Thorium Titanium Thulium
flask, add 500 mL of deionized water. Add 35.53 grams of
Uranium Vanadium Uranium
Ammonium oxalate monohydrate and mix until dissolved. Fill
Measurement of beryllium on the order of 1 ppb (0.003 µg to 1 L with deionized water and mix until dissolved.
Be/100 cm wipe sample) has been successfully accomplished
6.3.3 Nitric Acid, 0.2 M: To a 1-Lvolumetric flask, add 200
in the presence of spectrally interfering elements on the order mL of deionized water. Add 12.5 mL of concentrated (70%)
of hundreds of ppm. This method has been validated on
nitric acid (trace metal grade) and mix. Fill to 1 L with
matrices containing 10 mg of each of the above elements. In deionized water and mix thoroughly.
some cases including interferents such as chromium and
6.3.4 Nitric Acid, 4.0 M: To a 1-Lvolumetric flask, add 200
calcium, the single 2 mLberyllium extraction chromatography mL of deionized water. Add 250 mL of concentrated (70 %)
resin can handle >100 mg of total dissolved solids and still
nitric acid (trace metal grade) and mix. Fill to 1 L with
deliver >90 % beryllium yield. Should the matrix contain deionized water and mix thoroughly.
greater amounts of contaminants, additional resin may be used
6.3.5 Methyl Violet, 0.1 % solution, in deionized water: 0.1
or, more likely, a combination of different resins may be used. gm Methyl Violet per 100 mL of water.
(3,4).
6. Reagents and Materials Beryllium extraction chromatography resin cartridge: 2 mL bed volume,
50-100 micron beads, bis (2-ethylhexyl) methanediphosphonic acid sorbed onto
6.1 Equipment:
acrylic ester beads (3, 4, 5). Quality control parameters for the resin are stated in
6.1.1 50-mL polypropylene centrifuge tubes, subsection 8.6.
D7441 − 08
7. Procedure 7.2.3 Rinse the beryllium extraction chromatography resin
cartridge with 15 mLof 0.25 M ammonium oxalate (see 6.3.2)
7.1 Wipe Digest Preparation:
at 2 mL/min. Discard the eluate.
7.1.1 Prepare resin load solution in accordance with the
7.2.4 Rinse the beryllium extraction chromatography resin
chemical reagents normally used to digest beryllium surface
cartridge with 15 mL of 0.2 M HNO (see 6.3.3) at 2 mL/min.
wipes.
Discard the eluate.
7.2.5 Equip the vacuum box (see 6.1.4) with a 50-mL
NOTE 3—Example methods for sample preparation may be found in
Test Method D7035.
polypropylene centrifuge tube for each beryllium extraction
chromatography resin cartridge.
7.1.2 Transfer extract from digested filter or wipe to a 50
7.2.6 Elute the beryllium with 15 mL of 4.0 M HNO (see
mL polypropylene centrifuge tube (see 6.1.1). The volume 3
6.3.4) at 1 mL/min. Collect the eluate in a 50-mL polypropyl-
should be less than 20 mL at this point. If a larger volume is
enecentrifugetube.Agreatervolumeof4Mnitricacidmaybe
requiredtoadequatelydigestthesample,checkberylliumyield
usedtoincreaseberylliumyield
...
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