ASTM D3557-02(2007)e1

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
Contact ASTM International (www.astm.org) for the latest information
´1
Designation: D3557 − 02(Reapproved 2007)
Standard Test Methods for
Cadmium in Water
This standard is issued under the fixed designation D3557; 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 (´) indicates an editorial change since the last revision or reapproval.
´ NOTE—Editorial changes were made throughout in September 2007.
1. Scope in Closed Conduits (Withdrawn 2003)
D1193Specification for Reagent Water
1.1 Thesetestmethodscoverthedeterminationofdissolved
D1687Test Methods for Chromium in Water
and total recoverable cadmium in water and wastewater by
D1688Test Methods for Copper in Water
atomic-absorption spectrophotometry and differential pulse
2 D1691Test Methods for Zinc in Water
anodic stripping voltammetry. Four test methods are included
D1886Test Methods for Nickel in Water
as follows:
D2777Practice for Determination of Precision and Bias of
Concentration
Sections
Applicable Test Methods of Committee D19 on Water
Range
Test Method A—Atomic Absorption, 0.05 to 2.0 7to15 D3370Practices for Sampling Water from Closed Conduits
Direct mg/L
D3558Test Methods for Cobalt in Water
Test Method B—Atomic Absorption, 5to200 µg/L 16to24
D3559Test Methods for Lead in Water
Chelation-Extraction
Test Method C—Differential Pulse 1to100 µg/L 25to34 D3919Practice for Measuring Trace Elements in Water by
Anodic Stripping Voltammetry
Graphite Furnace Atomic Absorption Spectrophotometry
Test Method D—Atomic Absorption, 2to10µg/L 35to43
D4841Practice for Estimation of Holding Time for Water
Graphite Furnace
Samples Containing Organic and Inorganic Constituents
1.2 Test Method B can be used to determine cadmium in
D5810Guide for Spiking into Aqueous Samples
brines. It is the user’s responsibility to ensure the validity of
D5847Practice for Writing Quality Control Specifications
these test methods for waters of untested matrices.
for Standard Test Methods for Water Analysis
1.3 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the
3. Terminology
responsibility of the user of this standard to establish appro-
3.1 Definitions: For definitions of terms used in these test
priate safety and health practices and determine the applica-
methods, refer to Terminology D1129.
bility of regulatory limitations prior to use.
3.2 Definitions of Terms Specific to This Standard:
3.2.1 spiking solution—the standard solution added to the
2. Referenced Documents
polarographic cell that is used to quantitate the sample.
2.1 ASTM Standards:
3.2.2 stripping peak potential—the applied potential versus
D858Test Methods for Manganese in Water
SCE at which the stripping peak current is a maximum.
D1066Practice for Sampling Steam
D1068Test Methods for Iron in Water
3.2.3 SCE—saturated calomel electrode.
D1129Terminology Relating to Water
3.2.4 stripping peak signal—the current measured at the
D1192Guide for Equipment for Sampling Water and Steam
stripping peak maximum for a metal.
4. Significance and Use
These test methods are under the jurisdiction of ASTM Committee D19 on
4.1 The test for cadmium is necessary because it is a
Water and are the direct responsibility of Subcommittee D19.05 on Inorganic
toxicant and because there is a limit specified for cadmium in
Constituents in Water.
Current edition approved Aug. 1, 2007. Published September 2007. Originally potable water in the National Interim Primary Drinking Water
approved in 1977. Last previous edition approved in 2002 as D3557–02. DOI:
Regulations. This test serves to determine whether the cad-
10.1520/D3557-02R07E01.
mium content of potable water is above or below the accept-
Platte,J.A.,andMarcy,V.M.,“ANewToolfortheWaterChemist,”Industrial
able limit.
Water Engineering, May 1965.
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 last approved version of this historical standard is referenced on
the ASTM website. www.astm.org.
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D3557 − 02 (2007)
5. Purity of Reagents (Test Methods D1687), cobalt (Test Methods D3558), copper
(Test Methods D1688), iron (Test Methods D1068), lead (Test
5.1 Reagent grade chemicals shall be used in all tests.
Methods D3559), manganese (Test Methods D858), and zinc
Unlessotherwiseindicated,itisintendedthatallreagentsshall
(Test Methods D1691).
conform to the specifications of the Committee on Analytical
Reagents of the American Chemical Society. Other grades
9. Interferences
may be used, provided it is first ascertained that the reagent is
of sufficiently high purity to permit its use without lessening 9.1 Calcium concentrations above 1000 mg/L suppress the
cadmiumabsorption.At2000mg/Lofcalciumthesuppression
the accuracy of the determination.
is 19%.
5.2 Unless otherwise indicated, references to water shall be
9.2 Sodium, potassium, sulfate, and chloride (9000 mg/L
understood to mean reagent water conforming to Specification
each),magnesium(4500mg/L),iron(4000mg/L),nitrate(100
D1193, Type I. Other reagent water types may be used,
mg/L), and nickel, lead, copper, zinc, cobalt, and chromium
provided it is first ascertained that the water is of sufficiently
(10 mg/L each), do not interfere.
high purity to permit its use without adversely affecting the
bias and precision of the test method. Type II water was
9.3 Background correction or a chelation-extraction proce-
specified at the time of round-robin testing of this test method.
dure (see Test Method B) may be necessary to determine low
levels of cadmium in some waters.
6. Sampling
NOTE 1—Instrument manufacturer’s instructions for use of the specific
6.1 Collect the samples in accordance with the applicable
correction technique should be followed.
ASTM standard as follows: Practices D3370, Practice D1066,
and Specification D1192.
10. Apparatus
6.2 Samples shall be preserved with HNO (sp gr 1.42) to a
10.1 Atomic Absorption Spectrophotometer , for use at
pH of 2 or less immediately at the time of collection, normally
228.8 nm.
about 2 mL/L of HNO . If only dissolved cadmium is to be
NOTE 2—The manufacturer’s instructions shall be followed for all
determined,thesampleshallbefilteredthrougha0.45-µm(No.
instrumental parameters.Awavelength other than 228.8 nm may be used
325)membranefilterbeforeacidification.Theholdingtimefor
if it has been determined to be equally suitable.
samplesmaybecalculatedinaccordancewithPracticeD4841.
10.2 Cadmium Light Source—Either cadmium hollow-
TEST METHOD A—ATOMIC ABSORPTION, DIRECT cathode lamps or multielement hollow-cathode lamps, or
electrodeless-discharge lamps.
7. Scope
10.3 Pressure-Reducing Valves—The supplies of fuel and
7.1 This test method covers the determination of dissolved
oxidant shall be maintained at pressures somewhat higher than
and total recoverable cadmium in most waters and wastewa-
the controlled operating pressure of the instrument by suitable
ters.
valves.
7.2 This test method is applicable in the range from 0.05 to
11. Reagents and Materials
2.0 mg/L of cadmium. The range may be extended to concen-
trations greater than 2.0 mg/L by dilution of the sample.
11.1 Cadmium Solution, Stock (1 mL=1.0 mg Cd)—
Dissolve 1.000 g of cadmium metal in a minimum quantity of
7.3 This test method has been used successfully with
reagentgradewater,riverwater,wastewater,groundwater,tap HNO (sp gr 1.42) and dilute to 1 L.
water, lake water, and refinery effluent. The information on
11.2 Cadmium Solution, Standard (1 mL=0.1 mg Cd)—
precisionandbiasmaynotapplytootherwater.Itistheuser’s
Dilute 100.0 mL of the cadmium stock solution and 1 mL of
responsibility to ensure the validity of this test method for
HNO (sp gr 1.42) to 1000 mL with water.
waters of other matrices.
11.3 Hydrochloric Acid (sp gr 1.19)—Concentrated hydro-
chloric acid (HCl).
8. Summary of Test Method
8.1 Cadmium is determined by atomic absorption spectro- NOTE 3—If the reagent blank concentration is greater than the method
detectionlimit,distilltheHClorusespectrogradeacid.(Warning—When
photometry. Dissolved cadmium is determined by aspirating a
HCl is distilled, an azeotropic mixture is obtained (approximately 6 N
portion of the filtered sample directly with no pretreatment.
HCl). Therefore, whenever concentrated HCl is specified for the prepara-
Total recoverable cadmium is determined by aspirating the
tion of a reagent or in the procedure, use double the volume specified if
sample following hydrochloric-nitric acid digestion and filtra-
distilled acid is used.)
tion. The same digestion procedure may be used to determine
11.4 Nitric Acid (sp gr 1.42)—Concentrated nitric acid
total recoverable nickel (Test Methods D1886), chromium
(HNO ).
NOTE 4—If the reagent blank concentration is greater than the method
Reagent Chemicals, American Chemical Society Specifications, American
detection limit, distill the HNO or use a spectrograde acid.
Chemical Society, Washington, DC. For Suggestions on the testing of reagents not
listed by the American Chemical Society, see Annual Standards for Laboratory 11.5 Nitric Acid (1+499)—Add 1 volume of HNO (sp gr
Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
1.42) to 499 volumes of water.
and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,
MD. 11.6 Oxidant:
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D3557 − 02 (2007)
11.6.1 Air,whichhasbeenpassedthroughasuitablefilterto 14. Calculation
remove oil, water, and other foreign substances is the usual
14.1 Calculate the concentration of cadmium in the sample,
oxidant.
in milligrams per litre, using the analytical curve prepared in
12.4.
11.7 Fuel:
11.7.1 Acetylene—Standard, commercially available acety-
15. Precision and Bias
lene is the usual fuel. Acetone, always present in acetylene
cylinders, can affect analytical results. The cylinder should be 15.1 The precision of this test method was tested by 17
replaced at 50 psig (345 kPa). (Warning —“Purified” grade
laboratories in reagent water, river water, wastewater, ground
acetylene containing a special proprietary solvent rather than water, tap water, lake water, and refinery effluent. The overall
acetone should not be used with poly(vinyl chloride) tubing as
bias and precision of this test method, within its designated
weakening of the tubing walls can cause a potentially hazard- range, varies with the quantity being measured in accordance
ous situation.)
with Table 1.
15.2 These data may not apply to waters of the matrices,
12. Standardization
therefore, it is the responsibility of the analyst to ensure the
validity of the test method in other matrices.
12.1 Prepare 100 mL each of a blank and at least four
standard solutions to bracket the expected cadmium concen-
15.3 Precision and bias for this test method conforms to
tration range of the samples to be analyzed by diluting the
Practice D2777–77, which was in place at the time of
standard cadmium solution (11.2) with HNO (1+499). Pre-
collaborative testing. Under the allowances made in 1.4 of
pare the standards each time the test is to be performed.
Practice D2777–06, these precision and bias data meet
existing requirements for interlaboratory studies of Committee
12.2 When determining total recoverable cadmium, add 0.5
D19 test methods.
mL of HNO (sp gr 1.42) to each blank and standard solution
and proceed as directed in 13.2 through 13.4. After the
TEST METHOD B—ATOMIC ABSORPTION,
digestion of the blank and standard solutions has been com-
CHELATION-EXTRACTION
pleted in 13.4, return to 12.3 to complete the standardization
for total recoverable determinations. When determining dis-
16. Scope
solved cadmium, proceed with 12.3.
16.1 Thistestmethodcoversthedeterminationofdissolved
12.3 Aspirate the blank and standards and record the instru-
and total recoverable cadmium in most waters and brines.
ment readings. Aspirate HNO (1+499) between each stan-
16.2 This test method is applicable in the range from 5 to
dard.
200 µg/L of cadmium. The range may be extended to concen-
12.4 Prepare an analytical curve by plotting the absorbance
trations greater than 200 µg/L by dilution of the sample.
versus the concentration for each standard on the instrument
16.3 This test method has been used successfully with
software. Alternatively, read directly in concentration if this
reagentgradewater,riverwater,wastewater,groundwater,tap
capability is provided with the instrument.
water, lake water, and refinery effluent. The information on
precision and bias may not apply to other water.
13. Procedure
16.4 It is the responsibility of the analyst to determine the
13.1 Measure 100.0 mL of a well-mixed acidified sample
acceptability of this test method when analyzing other matri-
into a 125-mL beaker or flask.
ces.
NOTE 5—If only dissolved cadmium is to be determined, start with
13.5.
13.2 Add 5 mL of HCl (sp gr 1.19) to each sample.
13.3 Heat the samples on a steam bath or hotplate in a 6
Supporting data have been filed atASTM International Headquarters and may
well-ventilated hood until the volume has been reduced to 15 be obtained by requesting Research Report RR:D19-1030.
to 20 mL, making certain that the samples do not boil.
TABLE 1 Determination of Bias and Precision for Cadmium by
NOTE 6—For samples containing appreciable amounts of suspended
Atomic Absorption, Direct
matterordissolvedsolids,theamountofreductioninvolumeislefttothe
Statistically
discretion of the analyst.
Amount Added, Amount
S , mg/L S , mg/L % Bias Significant,
T O
mg/L Found, mg/L
95 % Level
13.4 Cool and filter the samples through a suitable filter
Reagent Water
such as fine-textured, acid-washed, ashless, paper into 100-mL
0.20 0.200 0.033 0.033 0.0 No
volumetricflasks.Washthefilterpapertwoorthreetimeswith
0.60 0.592 0.034 0.026 −1.3 No
1.60 1.521 0.111 0.061 −4.9 Yes
water and adjust to volume.
Water of Choice
0.20 0.200 0.033 0.033 0.0 No
13.5 Aspirate each filtered and acidified sample and deter-
0.60 0.589 0.040 0.026 −1.8 No
mine its absorbance or concentration at 228.8 nm. Aspirate
1.60 1.511 0.114 0.061 −5.6 Yes
HNO (1+499) between each sample.
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D3557 − 02 (2007)
17. Summary of Test Method 20.12 Materials—Use materials from 11.6 and 11.7.
17.1 Cadmium is determined by atomic absorption spectro-
21. Standardization
photometry.The element, either dissolved or total recoverable,
is chelated with pyrro
...