ASTM D3697-12
(Test Method)Standard Test Method for Antimony in Water
Standard Test Method for Antimony in Water
SIGNIFICANCE AND USE
5.1 Because of the association with lead and arsenic in industry, it is often difficult to assess the toxicity of antimony and its compounds. In humans, complaints referable to the nervous system have been reported. In assessing human cases, however, the possibility of lead or arsenic poisoning must always be borne in mind. Locally, antimony compounds are irritating to the skin and mucous membranes.
SCOPE
1.1 This test method covers the determination of dissolved and total recoverable antimony in water by atomic absorption spectroscopy.2
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 The values stated in either SI units or inch-pound units are to be regarded separately as standard. The values stated in each system are mathematical conversions and may not be exact equivalents; therefore, each system shall be used independently of the other.
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.
General Information
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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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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: D3697 − 12
Standard Test Method for
1
Antimony in Water
This standard is issued under the fixed designation D3697; 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* D4841 Practice for Estimation of Holding Time for Water
Samples Containing Organic and Inorganic Constituents
1.1 This test method covers the determination of dissolved
D5847 Practice for Writing Quality Control Specifications
and total recoverable antimony in water by atomic absorption
2 for Standard Test Methods for Water Analysis
spectroscopy.
1.2 This test method is applicable in the range from 1 to 15
3. Terminology
µg/L of antimony. The range may be extended by less scale
3.1 Definitions:For definitions of terms used in this test
expansion or by dilution of the sample.
method, refer to Terminology D1129.
1.3 The precision and bias data were obtained on reagent
3.2 Definitions of Terms Specific to This Standard:
water, tap water, salt water, and two untreated wastewaters.
3.2.1 total recoverable antimony, n—an arbitrary analytical
The information on precision and bias may not apply to other
term relating to forms of antimony that are determinable by the
waters.
digestion method which is included in the procedure; some
1.4 The values stated in either SI units or inch-pound units
organic compounds may not be completely recovered.
are to be regarded separately as standard. The values stated in
3.2.2 laboratory control sample, n—a solution with a certi-
each system are mathematical conversions and may not be
fied concentration of the antimony.
exact equivalents; therefore, each system shall be used inde-
pendently of the other.
4. Summary of Test Method
1.5 This standard does not purport to address all of the
4.1 Organic antimony-containing compounds are decom-
safety concerns, if any, associated with its use. It is the
posed by adding sulfuric and nitric acids and repeatedly
responsibility of the user of this standard to establish appro-
evaporating the sample to fumes of sulfur trioxide. The
priate safety and health practices and determine the applica-
antimony so produced, together with inorganic antimony
bility of regulatory limitations prior to use.
originally present, is subsequently reacted with potassium
iodide and stannous chloride, and finally with sodium borohy-
2. Referenced Documents
dride to form stibine. The stibine is removed from solution by
3
2.1 ASTM Standards:
aeration and swept by a flow of nitrogen into a hydrogen flame
D1129 Terminology Relating to Water
where it is determined by atomic absorption at 217.6 nm.
D1193 Specification for Reagent Water
D2777 Practice for Determination of Precision and Bias of
5. Significance and Use
Applicable Test Methods of Committee D19 on Water
5.1 Because of the association with lead and arsenic in
D3370 Practices for Sampling Water from Closed Conduits
industry, it is often difficult to assess the toxicity of antimony
D4691 Practice for Measuring Elements in Water by Flame
and its compounds. In humans, complaints referable to the
Atomic Absorption Spectrophotometry
nervous system have been reported. In assessing human cases,
however, the possibility of lead or arsenic poisoning must
1 always be borne in mind. Locally, antimony compounds are
This test method is under the jurisdiction of ASTM Committee D19 on Water
and is the direct responsibility of Subcommittee D19.05 on Inorganic Constituents
irritating to the skin and mucous membranes.
in Water.
Current edition approved Sept. 1, 2012. Published September 2012. Originally
6. Interference
approved in 1978. Last previous edition approved in 2007 as D3697 – 07. DOI:
10.1520/D3697-12.
6.1 Since the stibine is freed from the original sample
2
Platte, J.A., and Marcy,V. M., “ANewTool for theWater Chemist,” Industrial
matrix, interferences in the flame are minimized.
Water Engineering, IWEGA, May 1965.
3
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
6.2 Selenium and arsenic, which also form hydrides, do not
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
interfere at concentrations of 100 µg/L. Higher concentrations
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. were not tested.
*A Summary of Changes section appears at the end of this standard
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1
---------------------- Page: 1 ----------------------
D3697 − 12
8.3 Antimony Solution, Stock (1.00 mL = 100 µg Sb)—
Dissolve 274.3 mg of antimony potassium tartrat
...
This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Because
it may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current version
of the standard as published by ASTM is to be considered the official document.
Designation: D3697 − 07 D3697 − 12
Standard Test Method for
1
Antimony in Water
This standard is issued under the fixed designation D3697; 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 Scope*
1.1 This test method covers the determination of dissolved and total recoverable antimony in water by atomic absorption
2
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 The values stated in either SI units or inch-pound units are to be regarded separately as standard. The values stated in each
system are mathematical conversions and may not be exact equivalents; therefore, each system shall be used independently of the
other.
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.
2. Referenced Documents
3
2.1 ASTM Standards:
D1129 Terminology Relating to Water
D1193 Specification for Reagent Water
D2777 Practice for Determination of Precision and Bias of Applicable Test Methods of Committee D19 on Water
D3370 Practices for Sampling Water from Closed Conduits
D4691 Practice for Measuring Elements in Water by Flame Atomic Absorption Spectrophotometry
D4841 Practice for Estimation of Holding Time for Water Samples Containing Organic and Inorganic Constituents
D5847 Practice for Writing Quality Control Specifications for Standard Test Methods for Water Analysis
3. Terminology
3.1 Definitions:For definitions of terms used in this test method, refer to Terminology D1129.
3.2 Definitions of Terms Specific to This Standard:
3.2.1 total recoverable antimony—antimony, n—an arbitrary analytical term relating to forms of antimony that are determinable
by the digestion method which is included in the procedure. Someprocedure; some organic compounds may not be completely
recovered.
3.2.2 laboratory control sample, n—a solution with a certified concentration of the antimony.
4. Summary of Test Method
4.1 Organic antimony-containing compounds are decomposed by adding sulfuric and nitric acids and repeatedly evaporating
the sample to fumes of sulfur trioxide. The antimony so produced, together with inorganic antimony originally present, is
1
This test method is under the jurisdiction of ASTM Committee D19 on Water and is the direct responsibility of Subcommittee D19.05 on Inorganic Constituents in Water.
Current edition approved Aug. 1, 2007Sept. 1, 2012. Published August 2007September 2012. Originally approved in 1978. Last previous edition approved in 20022007
as D3697 – 02.D3697 – 07. DOI: 10.1520/D3697-07.10.1520/D3697-12.
2
Platte, J. A., and Marcy, V. M., “A New Tool for the Water Chemist,” Industrial Water Engineering, IWEGA, May 1965.
3
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 ASTM website.
*A Summary of Changes section appears at the end of this standard
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1
---------------------- Page: 1 ----------------------
D3697 − 12
FIG. 1 Stibine Vapor Analyzer
subsequently reacted with potassium iodide and stannous chloride, and finally with sodium borohydride to form stibine. The stibine
is removed from solution by aeration and swept by a flow of nitrogen into a hydrogen flame where it is determined by atomic
absorption at 217.6 nm.
5. Significance and Use
5.1 Because of the association with lead and arsenic in industry, it is often difficult to assess the toxicity of antimony and its
compounds. In humans, complaints referable to the nervous system have been reported. In assessing human cases, however, the
possibility of lead or arsenic poisoning must always be borne in mind. Locally, antimony compounds are irrita
...
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