ASTM D3697-17
(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.
5.2 ICP-MS may also be appropriate but at a higher instrument cost. See Test Method D5673.
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 SI units are to be regarded as standard. The values given in parentheses are mathematical conversion to inch-pound units that are provided for information only and are not considered standard.
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.
1.6 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
General Information
Relations
Standards Content (Sample)
This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
Designation: D3697 − 17
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* D2777 Practice for Determination of Precision and Bias of
Applicable Test Methods of Committee D19 on Water
1.1 This test method covers the determination of dissolved
D3370 Practices for Sampling Water from Closed Conduits
and total recoverable antimony in water by atomic absorption
2 D4691 Practice for Measuring Elements in Water by Flame
spectroscopy.
Atomic Absorption Spectrophotometry
1.2 This test method is applicable in the range from 1 to 15
D4841 Practice for Estimation of Holding Time for Water
µg/L of antimony. The range may be extended by less scale
Samples Containing Organic and Inorganic Constituents
expansion or by dilution of the sample.
D5673 Test Method for Elements in Water by Inductively
1.3 The precision and bias data were obtained on reagent Coupled Plasma—Mass Spectrometry
D5810 Guide for Spiking into Aqueous Samples
water, tap water, salt water, and two untreated wastewaters.
The information on precision and bias may not apply to other D5847 Practice for Writing Quality Control Specifications
for Standard Test Methods for Water Analysis
waters.
1.4 The values stated in SI units are to be regarded as
3. Terminology
standard. The values given in parentheses are mathematical
conversion to inch-pound units that are provided for informa-
3.1 Definitions:
tion only and are not considered standard.
3.1.1 For definitions of terms used in this standard, refer to
Terminology D1129.
1.5 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the
3.2 Definitions of Terms Specific to This Standard:
responsibility of the user of this standard to establish appro-
3.2.1 continuing calibration blank, n—a solution contain-
priate safety and health practices and determine the applica-
ing no analytes (of interest) which is used to verify blank
bility of regulatory limitations prior to use.
response and freedom from carryover.
1.6 This international standard was developed in accor-
3.2.2 continuing calibration verification, n—a solution (or
dance with internationally recognized principles on standard-
setofsolutions)ofknownconcentrationusedtoverifyfreedom
ization established in the Decision on Principles for the
from excessive instrumental drift; the concentration is to cover
Development of International Standards, Guides and Recom-
the range of calibration curve.
mendations issued by the World Trade Organization Technical
3.2.3 laboratory control sample, n—a solution with a certi-
Barriers to Trade (TBT) Committee.
fied concentration of the antimony.
2. Referenced Documents
3.2.4 total recoverable antimony, n—a descriptive term
3
2.1 ASTM Standards: relating to forms of antimony that are determinable by the
D1129 Terminology Relating to Water digestion method which is included in the procedure; some
D1193 Specification for Reagent Water organic compounds may not be completely recovered.
4. Summary of Test Method
1
This test method is under the jurisdiction of ASTM Committee D19 on Water
4.1 Organic antimony-containing compounds are decom-
and is the direct responsibility of Subcommittee D19.05 on Inorganic Constituents
in Water.
posed by adding sulfuric and nitric acids and repeatedly
Current edition approved June 1, 2017. Published June 2017. Originally
evaporating the sample to fumes of sulfur trioxide. The
approved in 1978. Last previous edition approved in 2012 as D3697 – 12. DOI:
antimony so produced, together with inorganic antimony
10.1520/D3697-17.
2
originally present, is subsequently reacted with potassium
Platte, J.A., and Marcy,V. M., “ANewTool for theWater Chemist,” Industrial
Water Engineering, IWEGA, May 1965.
iodide and stannous chloride, and finally with sodium borohy-
3
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
dride to form stibine. The stibine is removed from solution by
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
aeration and swept by a flow of nitrogen into a hydrogen flame
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. where it is determined by atomic absorption at 217.6 nm.
*A Summary of Changes section appears at the end of this standard
Copyright © ASTM International, 100 Barr Harbo
...
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 − 12 D3697 − 17
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*
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 statedgiven
in each system are mathematical conversions and may not be exact equivalents; therefore, each system shall be used independently
of the other.parentheses are mathematical conversion to inch-pound units that are provided for information only and are not
considered standard.
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.
1.6 This international standard was developed in accordance with internationally recognized principles on standardization
established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued
by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
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
D5673 Test Method for Elements in Water by Inductively Coupled Plasma—Mass Spectrometry
D5810 Guide for Spiking into Aqueous Samples
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.
3.1 Definitions:
3.1.1 For definitions of terms used in this standard, refer to Terminology D1129.
3.2 Definitions of Terms Specific to This Standard:
3.2.1 continuing calibration blank, n—a solution containing no analytes (of interest) which is used to verify blank response and
freedom from carryover.
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 Sept. 1, 2012June 1, 2017. Published September 2012June 2017. Originally approved in 1978. Last previous edition approved in 20072012 as
D3697 – 07.D3697 – 12. DOI: 10.1520/D3697-12.10.1520/D3697-17.
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 − 17
FIG. 1 Stibine Vapor Analyzer
3.2.2 continuing calibration verification, n—a solution (or set of solutions) of known concentration used to verify freedom from
excessive instrumental drift; the concentration is to cover the range of calibration curve.
3.2.3 laboratory control sample, n—a solution with a certified concentration of the antimony.
3.2.4 total recoverable antimony, n—an arbitrary analytical a descriptive term relating to forms of antimony that are
determinable by
...
Questions, Comments and Discussion
Ask us and Technical Secretary will try to provide an answer. You can facilitate discussion about the standard in here.