ASTM D3223-02

Standard Test Method for Total Mercury in Water

SCOPE
1.1 This test method covers the determination of total mercury in water in the range from 0.5 to 10.0 g Hg/L (1). The test method is applicable to fresh waters, saline waters, and some industrial and sewage effluents. It is the user's responsibility to ensure the validity of this test method for waters of untested matrices.
1.1.1 The analyst should recognize that the precision and bias of this standard may be affected by the other constituents in all waters, as tap, industrial, river, and wastewaters. The cold vapor atomic absorption measurement portion of this method is applicable to the analysis of materials other than water (sediments, biological materials, tissues, etc.) if, and only if, an initial procedure for digesting and oxidizing the sample is carried out, ensuring that the mercury in the sample is converted to the mercuric ion, and is dissolved in aqueous media (2,3).
1.2 Both organic and inorganic mercury compounds may be analyzed by this procedure if they are first converted to mercuric ions. Using potassium persulfate and potassium permanganate as oxidants, and a digestion temperature of 95°C, approximately 100 % recovery of organomercury compounds can be obtained (2,4).
1.3 The range of the test method may be changed by instrument or recorder expansion or both, and by using a larger volume of sample.
1.4 A method for the disposal of mercury-containing wastes is also presented (Appendix X1) (5).
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. For specific hazard statements, see 7.8 and 10.8.2.

General Information

• Status: Historical
• Publication Date: 09-Mar-2002
• 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 D3223-95 - Standard Test Method for Total Mercury in Water
• Effective Date: 10-Mar-2002
• Replaced By: ASTM D3223-02(2007)e1 - Standard Test Method for Total Mercury in Water
• Effective Date: 01-Aug-2007
• Referred By: ASTM D4691-17 - Standard Practice for Measuring Elements in Water by Flame Atomic Absorption Spectrophotometry
• Effective Date: 10-Mar-2002
• Referred By: ASTM D1252-06(2020) - Standard Test Methods for Chemical Oxygen Demand (Dichromate Oxygen Demand) of Water
• Effective Date: 10-Mar-2002
• Referred By: ASTM D8006-16 - Standard Guide for Sampling and Analysis of Residential and Commercial Water Supply Wells in Areas of Exploration and Production (E&P) Operations
• Effective Date: 10-Mar-2002

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 3223–02
Standard Test Method for
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Total Mercury in Water
This standard is issued under the fixed designation D 3223; 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.
This standard has been approved for use by agencies of the Department of Defense.
1. Scope bility of regulatory limitations prior to use. For specific hazard
2 statements, see 7.8 and 10.8.2.
1.1 This test method covers the determination of total
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mercury in water in the range from 0.5 to 10.0 µg Hg/L (1).
2. Referenced Documents
Thetestmethodisapplicabletofreshwaters,salinewaters,and
2.1 ASTM Standards:
some industrial and sewage effluents. It is the user’s responsi-
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D 512 Test Methods for Chloride Ion in Water
bility to ensure the validity of this test method for waters of
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D 1129 Terminology Relating to Water
untested matrices.
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D 1193 Specification for Reagent Water
1.1.1 The analyst should recognize that the precision and
D1245 PracticeforExaminationofWater-FormedDeposits
bias of this standard may be affected by the other constituents
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by Chemical Microscopy
inallwaters,astap,industrial,river,andwastewaters.Thecold
D 1252 Test Methods for Chemical Oxygen Demand
vaporatomicabsorptionmeasurementportionofthismethodis
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(Dichromate Oxygen Demand) of Water
applicable to the analysis of materials other than water (sedi-
4
D 1426 Test Methods for Ammonia Nitrogen in Water
ments, biological materials, tissues, etc.) if, and only if, an
D 2777 Practice for Determination of Precision and Bias of
initial procedure for digesting and oxidizing the sample is
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Applicable Methods of Committee D19 on Water
carried out, ensuring that the mercury in the sample is
D 3370 Practices for Sampling Water from Closed Con-
converted to the mercuric ion, and is dissolved in aqueous
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duits
media (2,3).
D 4691 Practice for Measuring Elements inWater by Flame
1.2 Both organic and inorganic mercury compounds may be
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Atomic Absorption Spectrophotometry
analyzed by this procedure if they are first converted to
D 4841 Practice for Estimation of Holding Time for Water
mercuric ions. Using potassium persulfate and potassium
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Samples Containing Organic and Inorganic Constituents
permanganate as oxidants, and a digestion temperature of
4
D 5810 Guide for Spiking into Aqueous Samples
95°C, approximately 100 % recovery of organomercury com-
D 5847 Practice for Writing Quality Control Specifications
pounds can be obtained (2,4).
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for Standard Test Methods for Water Analysis
1.3 The range of the test method may be changed by
instrument or recorder expansion or both, and by using a larger
3. Terminology
volume of sample.
3.1 Definitions—For definitions of terms used in this test
1.4 Amethod for the disposal of mercury-containing wastes
method, refer to Terminology D 1129.
is also presented (Appendix X1) (5).
1.5 This standard does not purport to address all of the
4. Summary of Test Method
safety concerns, if any, associated with its use. It is the
4.1 The test method consists of a wet chemical oxidation
responsibility of the user of this standard to establish appro-
which converts all mercury to the mercuric ion; reduction of
priate safety and health practices and determine the applica-
mercuric ions to metallic mercury, followed by a cold vapor
atomic absorption analysis (1,2).Ageneral guide for flame and
1 vapor generation atomic absorption applications is given in
This test method is under the jurisdiction of ASTM Committee D19 on Water
Practice D 4691.
and is the direct responsibility of Subcommittee D19.05 on Inorganic Constituents
in Water.
4.2 Cold vapor atomic absorption analysis is a physical
Current edition approved March 10, 2002. Published May 2002. Originally
method based on the absorption of ultraviolet radiation at a
published as D 3223–79. Last previous edition D 3223 – 95.
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wavelength of 253.7 nm by mercury vapor. The mercury is
Adapted from research investigations by the U. S. Environmental Protection
Agency’s Analytical Quality Control Laboratory, Cincinnati, OH, and Region IV
Surveillance and Analysis Division, Chemical Services Branch, Athens, GA.
3 4
The boldface numbers in parentheses refer to the references at the end of this Annual Book of ASTM Standards, Vol 11.01.
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test method. 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.
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D 3223–02
reduced to the elemental state and aerated from solution in
either a closed recirculating system or an open one-pass
system. T
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