ASTM D3223-12
(Test Method)Standard Test Method for Total Mercury in Water
Standard Test Method for Total Mercury in Water
SIGNIFICANCE AND USE
5.1 The presence of mercury in industrial discharge, domestic discharge, and potable water is of concern to the public because of its toxicity. Regulations and standards have been established that require the monitoring of mercury in water. This test method provides an analytical procedure to measure total mercury in water.
SCOPE
1.1 This test method2 covers the determination of total mercury in water in the range from 0.5 to 10.0 μg Hg/L (1).3 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 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.5 A method for the disposal of mercury-containing wastes is also presented (Appendix X1) (5).
1.6 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.
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Designation: D3223 − 12
Standard Test Method for
1
Total Mercury in Water
This standard is issued under the fixed designation D3223; 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.
This standard has been approved for use by agencies of the U.S. Department of Defense.
1. Scope* 1.6 This standard does not purport to address all of the
2 safety concerns, if any, associated with its use. It is the
1.1 This test method covers the determination of total
3 responsibility of the user of this standard to establish appro-
mercury in water in the range from 0.5 to 10.0 µg Hg/L (1).
priate safety and health practices and determine the applica-
Thetestmethodisapplicabletofreshwaters,salinewaters,and
bility of regulatory limitations prior to use. For specific hazard
some industrial and sewage effluents. It is the user’s responsi-
statements, see 7.8 and 10.8.2.
bility to ensure the validity of this test method for waters of
untested matrices.
2. Referenced Documents
1.1.1 The analyst should recognize that the precision and
4
2.1 ASTM Standards:
bias of this standard may be affected by the other constituents
D512 Test Methods for Chloride Ion In Water
inallwaters,astap,industrial,river,andwastewaters.Thecold
D1129 Terminology Relating to Water
vaporatomicabsorptionmeasurementportionofthismethodis
D1193 Specification for Reagent Water
applicable to the analysis of materials other than water
D1245 Practice for Examination of Water-Formed Deposits
(sediments,biologicalmaterials,tissues,etc.)if,andonlyif,an
by Chemical Microscopy
initial procedure for digesting and oxidizing the sample is
D1252 Test Methods for Chemical Oxygen Demand (Di-
carried out, ensuring that the mercury in the sample is
chromate Oxygen Demand) of Water
converted to the mercuric ion, and is dissolved in aqueous
D1426 Test Methods for Ammonia Nitrogen In Water
media (2, 3).
D2777 Practice for Determination of Precision and Bias of
1.2 Both organic and inorganic mercury compounds may be
Applicable Test Methods of Committee D19 on Water
analyzed by this procedure if they are first converted to
D3370 Practices for Sampling Water from Closed Conduits
mercuric ions. Using potassium persulfate and potassium
D4691 Practice for Measuring Elements in Water by Flame
permanganate as oxidants, and a digestion temperature of
Atomic Absorption Spectrophotometry
95°C, approximately 100 % recovery of organomercury com-
D4841 Practice for Estimation of Holding Time for Water
pounds can be obtained (2, 4).
Samples Containing Organic and Inorganic Constituents
D5810 Guide for Spiking into Aqueous Samples
1.3 The range of the test method may be changed by
D5847 Practice for Writing Quality Control Specifications
instrument or recorder expansion or both, and by using a larger
for Standard Test Methods for Water Analysis
volume of sample.
1.4 The values stated in SI units are to be regarded as
3. Terminology
standard. No other units of measurement are included in this
3.1 Definitions—For definitions of terms used in this test
standard.
method, refer to Terminology D1129.
1.5 Amethod for the disposal of mercury-containing wastes
4. Summary of Test Method
is also presented (Appendix X1) (5).
4.1 The test method consists of a wet chemical oxidation
which converts all mercury to the mercuric ion; reduction of
1
This test method is under the jurisdiction of ASTM Committee D19 on Water
mercuric ions to metallic mercury, followed by a cold vapor
and is the direct responsibility of Subcommittee D19.05 on Inorganic Constituents
atomicabsorptionanalysis (1, 2).Ageneralguideforflameand
in Water.
Current edition approved Sept. 1, 2012. Published September 2012. Originally
vapor generation atomic absorption applications is given in
ε1
approved in 1979. Last previous edition approved in 2002 as D3223 – 02 (2007) .
Practice D4691.
DOI: 10.1520/D3223-12.
2
Adapted from research investigations by the U. S. Environmental Protection
4
Agency’s Analytical Quality Control Laboratory, Cincinnati, OH, and Region IV For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Surveillance and Analysis Division, Chemical Services Branch, Athens, GA. contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
3
The boldface numbers in parentheses refer to the references at the end of this Standards volume information, refer to the standard’s Document Summary page on
test method. 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 State
...
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.
´1
Designation: D3223 − 02 (Reapproved 2007) D3223 − 12
Standard Test Method for
1
Total Mercury in Water
This standard is issued under the fixed designation D3223; 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.
This standard has been approved for use by agencies of the Department of Defense.
1
εNOTE—Reference to Practice D2777 – 77 was editorially updated to D2777 – 06 in August 2007.
1. Scope Scope*
2 3
1.1 This test method covers the determination of total mercury in water in the range from 0.5 to 10.0 μg 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 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.5 A method for the disposal of mercury-containing wastes is also presented (Appendix X1) (5).
1.6 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.
2. Referenced Documents
4
2.1 ASTM Standards:
D512 Test Methods for Chloride Ion In Water
D1129 Terminology Relating to Water
D1193 Specification for Reagent Water
D1245 Practice for Examination of Water-Formed Deposits by Chemical Microscopy
D1252 Test Methods for Chemical Oxygen Demand (Dichromate Oxygen Demand) of Water
D1426 Test Methods for Ammonia Nitrogen In 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
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 2007 September 2012. Originally approved in 1979. Last previous edition approved in 2002 as
D3223 – 02.D3223 – 02(2007)E01. DOI: 10.1520/D3223-02R07E01.
2
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
The boldface numbers in parentheses refer to the references at the end of this test method.
4
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
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D3223 − 12
D5810 Guide for Spiking into Aqueous Samples
D
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