ASTM D3697-02
(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.
General Information
Relations
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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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 3697–02
Standard Test Method for
1
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 3.2 Definition of Term Specific to This Standard:
2 3.2.1 total recoverable antimony—an arbitrary analytical
1.1 This test method covers the determination of dissolved
term relating to forms of antimony that are determinable by the
and total recoverable antimony in water by atomic absorption
digestion method which is included in the procedure. Some
spectroscopy.
organic compounds may not be completely recovered.
1.2 This test method is applicable in the range from 1 to 15
3.2.2 laboratory control sample, n—a solution with a cer-
µg/L of antimony. The range may be extended by less scale
tified concentration of the antimony.
expansion or by dilution of the sample.
1.3 The precision and bias data were obtained on reagent
4. Summary of Test Method
water, tap water, salt water, and two untreated wastewaters.
4.1 Organic antimony-containing compounds are decom-
The information on precision and bias may not apply to other
posed by adding sulfuric and nitric acids and repeatedly
waters.
evaporating the sample to fumes of sulfur trioxide. The
1.4 This standard does not purport to address all of the
antimony so produced, together with inorganic antimony
safety concerns, if any, associated with its use. It is the
originally present, is subsequently reacted with potassium
responsibility of the user of this standard to establish appro-
iodide and stannous chloride, and finally with sodium borohy-
priate safety and health practices and determine the applica-
dride to form stibine. The stibine is removed from solution by
bility of regulatory limitations prior to use.
aeration and swept by a flow of nitrogen into a hydrogen flame
2. Referenced Documents where it is determined by atomic absorption at 217.6 nm.
2.1 ASTM Standards:
5. Significance and Use
3
D 1129 Terminology Relating to Water
3
5.1 Because of the association with lead and arsenic in
D 1193 Specification for Reagent Water
industry, it is often difficult to assess the toxicity of antimony
D 2777 Practice for Determination of Precision and Bias of
3 and its compounds. In humans, complaints referable to the
Applicable Test Methods of Committee D-19 on Water
nervous system have been reported. In assessing human cases,
D 3370 Practices for Sampling Water from Closed Con-
3 however, the possibility of lead or arsenic poisoning must
duits
always be borne in mind. Locally, antimony compounds are
D 4691 Practice for Measuring Elements inWater by Flame
3 irritating to the skin and mucous membranes.
Atomic Absorption Spectrophotometry
D 4841 Practice for Estimation of Holding Time for Water
6. Interference
3
Samples Containing Organic and Inorganic Constituents
6.1 Since the stibine is freed from the original sample
D 5847 Practice for the Writing Quality Control Specifica-
4 matrix, interferences in the flame are minimized.
tions for Standard Test Methods for Water Analysis
6.2 Selenium and arsenic, which also form hydrides, do not
3. Terminology interfere at concentrations of 100 µg/L. Higher concentrations
were not tested.
3.1 Definitions: For definitions of terms used in this test
method, refer to Terminology D 1129.
7. Apparatus
7.1 Atomic Absorption Spectrophotometer, for use at 217.6
1
This test method is under the jurisdiction of ASTM Committee D19 on Water
nm with a scale expansion of approximately 3.Ageneral guide
and is the direct responsibility of Subcommittee D19.05 on Inorganic Constituents
for the use of flame atomic absorption applications is given in
in Water.
Current edition approved May 10, 2002. Published June 2002. Originally Practice D 4691.
published as D 3697 – 78. Last previous edition D 3697 – 92 (1996).
2
NOTE 1—The manufacturer’s instructions should be followed for all
Platte, J.A., and Marcy,V. M., “ANewTool for theWater Chemist,” Industrial
instrumental parameters.
Water Engineering, IWEGA, May 1965.
3
Annual Book of ASTM Standards, Vol 11.01.
7.1.1 Antimony Electrodeless Discharge Lamp.
4
Annual Book of ASTM Standards, Vol 11.02.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
1
---------------------- Page: 1 ----------------------
D 3697–02
8.6 Hydrochloric Acid (sp gr 1.19)— Concentrated hydro-
chloric acid (HCl).
8.7 Nitric Acid (sp gr 1.42)— Concentrated nitric acid
(HNO ).
3
8.8 NitricAcid (1 + 1)—Add 250 mLof concentrated nitric
acid (sp gr 1.42) to 250 mL of water.
8.9 Potassium Iodid
...
Questions, Comments and Discussion
Ask us and Technical Secretary will try to provide an answer. You can facilitate discussion about the standard in here.