ASTM D3697-92(1996)
(Test Method)Standard Test Method for Antimony in Water
Standard Test Method for Antimony in Water
SCOPE
1.1 This test method covers the determination of dissolved and total recoverable antimony in water by atomic absorption spectroscopy.
1.2 This test method is applicable in the range from 1 to 15 μg/L of antimony. The range may be extended by less scale expansion or by dilution of the sample.
1.3 The precision and bias data were obtained on reagent water, tap water, salt water, and two untreated wastewaters. The information on precision and bias may not apply to other waters.
1.4 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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Standards Content (Sample)
NOTICE: This standard has either been superseded and replaced by a new version or
withdrawn.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.
Designation: D 3697 – 92 (Reapproved 1996)
AMERICAN SOCIETY FOR TESTING AND MATERIALS
100 Barr Harbor Dr., West Conshohocken, PA 19428
Reprinted from the Annual Book of ASTM Standards. Copyright ASTM
Standard Test Method for
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Antimony in Water
This standard is issued under the fixed designation D 3697; 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 (e) indicates an editorial change since the last revision or reapproval.
1. Scope organic compounds may not be completely recovered.
2
1.1 This test method covers the determination of dissolved
4. Summary of Test Method
and total recoverable antimony in water by atomic absorption
4.1 Organic antimony-containing compounds are decom-
spectroscopy.
posed by adding sulfuric and nitric acids and repeatedly
1.2 This test method is applicable in the range from 1 to 15
evaporating the sample to fumes of sulfur trioxide. The
μg/L of antimony. The range may be extended by less scale
antimony so produced, together with inorganic antimony
expansion or by dilution of the sample.
originally present, is subsequently reacted with potassium
1.3 The precision and bias data were obtained on reagent
iodide and stannous chloride, and finally with sodium borohy-
water, tap water, salt water, and two untreated wastewaters.
dride to form stibine. The stibine is removed from solution by
The information on precision and bias may not apply to other
aeration and swept by a flow of nitrogen into a hydrogen flame
waters.
where it is determined by atomic absorption at 217.6 nm.
1.4 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the
5. Significance and Use
responsibility of the user of this standard to establish appro-
5.1 Because of the association with lead and arsenic in
priate safety and health practices and determine the applica-
industry, it is often difficult to assess the toxicity of antimony
bility of regulatory limitations prior to use. For specific
and its compounds. In humans, complaints referable to the
precautionary statements, see 5.1 and 8.12.
nervous system have been reported. In assessing human cases,
however, the possibility of lead or arsenic poisoning must
2. Referenced Documents
always be borne in mind. Locally, antimony compounds are
2.1 ASTM Standards:
irritating to the skin and mucous membranes.
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D 1129 Terminology Relating to Water
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D 1193 Specification for Reagent Water
6. Interference
D 2777 Practice for Determination of Precision and Bias of
6.1 Since the stibine is freed from the original sample
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Applicable Test Methods of Committee D-19 on Water
matrix, interferences in the flame are minimized.
D 3370 Practices for Sampling Water from Closed Con-
6.2 Selenium and arsenic, which also form hydrides, do not
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duits
interfere at concentrations of 100 μg/L. Higher concentrations
D 4691 Practice for Measuring Elements in Water by Flame
were not tested.
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Atomic Absorption Spectrophotometry
D 4841 Practice for Estimation of Holding Time for Water 7. Apparatus
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Samples Containing Organic and Inorganic Constituents
7.1 Atomic Absorption Spectrophotometer, for use at 217.6
nm with a scale expansion of approximately 3. A general guide
3. Terminology
for the use of flame atomic absorption applications is given in
3.1 Definitions: For definitions of terms used in this test
Practice D 4691.
method, refer to Terminology D 1129.
3.2 Definition of Term Specific to This Standard: NOTE 1—The manufacturer’s instructions should be followed for all
instrumental parameters.
3.2.1 total recoverable antimony—an arbitrary analytical
term relating to forms of antimony that are determinable by the
7.1.1 Antimony Electrodeless Discharge Lamp.
digestion method which is included in the procedure. Some
7.2 Recorder or Digital Readout— Any multirange variable
speed recorder or digital readout accessory, or both, that is
compatible with the atomic absorption spectrophotometer is
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This test method is under the jurisdiction of ASTM Committee D-19 on Water
suitable.
and is the direct responsibility of Subcommittee D19.05 on Inorganic Constituents
7.3 Stibine Vapor Analyzer, assembled as shown in Fig. 1.
in Water.
Current edition approved June 15, 1992. Published October 1992. Originally
NOTE 2—A static system, such as one using a balloon, has been found
published as D 3697 – 78. Last previous edition D 3697 – 86.
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to be satisfactory. See McFarren, E. F., “New, Simplified Method for
Platte, J. A., and Marcy, V. M., “A New Tool for the Water Chemist,” Industrial
Metal Analysis,” Journal of American Water Works Assoc., JAWWA, Vol
Water Engineering, IWEGA, May 1965.
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Annual Book of ASTM Standards, Vol 11.01.
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