ASTM D3697-07

Standard Test Method for Antimony in Water

SIGNIFICANCE AND USE
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.
1.2 This test method is applicable in the range from 1 to 15 g/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.
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

• Status: Historical
• Publication Date: 31-Jul-2007
• ICS: 13.060.50 - Examination of water for chemical substances
• Technical Committee: D19 - Water
• Drafting Committee: D19.05 - Inorganic Constituents in Water

Relations

• Replaces: ASTM D3697-02 - Standard Test Method for Antimony in Water
• Effective Date: 01-Aug-2007
• Replaced By: ASTM D3697-12 - Standard Test Method for Antimony in Water
• Effective Date: 01-Sep-2012
• Referred By: ASTM D1971-16(2021)e1 - Standard Practices for Digestion of Water Samples for Determination of Metals by Flame Atomic Absorption, Graphite Furnace Atomic Absorption, Plasma Emission Spectroscopy, or Plasma Mass Spectrometry
• Effective Date: 01-Aug-2007

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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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 − 07
StandardTest 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 3. Terminology
3.1 Definitions:For definitions of terms used in this test
1.1 This test method covers the determination of dissolved
method, refer to Terminology D1129.
and total recoverable antimony in water by atomic absorption
2
3.2 Definitions of Terms Specific to This Standard:
spectroscopy.
3.2.1 total recoverable antimony—an arbitrary analytical
1.2 This test method is applicable in the range from 1 to 15
term relating to forms of antimony that are determinable by the
µg/L of antimony. The range may be extended by less scale
digestion method which is included in the procedure. Some
expansion or by dilution of the sample.
organic compounds may not be completely recovered.
1.3 The precision and bias data were obtained on reagent
3.2.2 laboratory control sample, n—a solution with a certi-
water, tap water, salt water, and two untreated wastewaters.
fied concentration of the antimony.
The information on precision and bias may not apply to other
4. Summary of Test Method
waters.
4.1 Organic antimony-containing compounds are decom-
1.4 This standard does not purport to address all of the
posed by adding sulfuric and nitric acids and repeatedly
safety concerns, if any, associated with its use. It is the
evaporating the sample to fumes of sulfur trioxide. The
responsibility of the user of this standard to establish appro-
antimony so produced, together with inorganic antimony
priate safety and health practices and determine the applica-
originally present, is subsequently reacted with potassium
bility of regulatory limitations prior to use.
iodide and stannous chloride, and finally with sodium borohy-
dride to form stibine. The stibine is removed from solution by
2. Referenced Documents
aeration and swept by a flow of nitrogen into a hydrogen flame
3
2.1 ASTM Standards:
where it is determined by atomic absorption at 217.6 nm.
D1129 Terminology Relating to Water
D1193 Specification for Reagent Water
5. Significance and Use
D2777 Practice for Determination of Precision and Bias of
5.1 Because of the association with lead and arsenic in
Applicable Test Methods of Committee D19 on Water
industry, it is often difficult to assess the toxicity of antimony
D3370 Practices for Sampling Water from Closed Conduits
and its compounds. In humans, complaints referable to the
D4691 Practice for Measuring Elements in Water by Flame
nervous system have been reported. In assessing human cases,
Atomic Absorption Spectrophotometry
however, the possibility of lead or arsenic poisoning must
D4841 Practice for Estimation of Holding Time for Water
always be borne in mind. Locally, antimony compounds are
Samples Containing Organic and Inorganic Constituents
irritating to the skin and mucous membranes.
D5847 Practice for Writing Quality Control Specifications
for Standard Test Methods for Water Analysis
6. Interference
6.1 Since the stibine is freed from the original sample
matrix, interferences in the flame are minimized.
1
This test method is under the jurisdiction of ASTM Committee D19 on Water
6.2 Selenium and arsenic, which also form hydrides, do not
and is the direct responsibility of Subcommittee D19.05 on Inorganic Constituents
in Water. interfere at concentrations of 100 µg/L. Higher concentrations
Current edition approved Aug. 1, 2007. Published August 2007. Originally
were not tested.
approved in 1978. Last previous edition approved in 2002 as D3697 – 02. DOI:
10.1520/D3697-07.
7. Apparatus
2
Platte, J.A., and Marcy,V. M., “ANewTool for theWater Chemist,” Industrial
Water Engineering, IWEGA, May 1965.
7.1 Atomic Absorption Spectrophotometer , for use at 217.6
3
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
nm with a scale expansion of approximately 3.Ageneral guide
contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM
for the use of flame atomic absorption applications is given in
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. Practice D4691.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1

---------------------- Page: 1 ----------------------
D3697 − 07
8.4 Antimony Solution, Intermediate (1.00 mL = 10 µg
Sb)—Dilute 50.0 mL of antimony stock solution to 500.0 mL
with water.
8.5 Antimony Solution, Standard (1.0 mL = 0.10 µg Sb)—
Dilute 5.0 mL of antimony intermediate solution to 5
...