Standard Practice for Sample Digestion Using Closed Vessel Microwave Heating Technique for the Determination of Total Metals in Water

SIGNIFICANCE AND USE
5.1 The analysis of many types of water for metals using flame atomic absorption spectrophotometry, inductively coupled plasma emission spectrophotometry, direct current plasma emission spectrophotometry, or graphite furnace atomic absorption spectrophotometry necessitates the use of a digestion practice in order to ensure the proper statistical recovery of the metals from the sample matrix. The use of closed vessel microwave techniques will speed the complete recovery of metals from the water matrices and eliminate sample contamination from external sources.
SCOPE
1.1 This practice covers the general considerations for quantitative sample digestion for total metals in water using closed vessel microwave heating technique. This practice is applicable to surface, saline, domestic, and industrial wastewater.  
1.2 Because of the differences among various makes and models of satisfactory instruments, no detailed operating instructions can be provided. Instead, the analyst should follow the instructions provided by the manufacturer of the particular instrument.  
1.3 This practice can be used with the following ASTM standards, providing the user determines precision and bias based on this digestion practice: Test Method D857, Test Methods D858, Test Methods D1068, Test Methods D1687, Test Methods D1688, Test Methods D1691, Test Methods D1886, Test Method D1976, Practices D3370, Test Methods D3557, Test Methods D3559, Practice D3919, Test Method D4190, Practice D4453, Practice D4691, and Test Method D5673.  
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 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 Section 9.

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Publication Date
29-Feb-2012
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English language
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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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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: D4309 − 12
Standard Practice for
Sample Digestion Using Closed Vessel Microwave Heating
1
Technique for the Determination of Total Metals in Water
This standard is issued under the fixed designation D4309; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision.Anumber in parentheses indicates the year of last reapproval.A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
1. Scope* 2. Referenced Documents
2
2.1 ASTM Standards:
1.1 This practice covers the general considerations for
D857Test Method for Aluminum in Water
quantitative sample digestion for total metals in water using
D858Test Methods for Manganese in Water
closed vessel microwave heating technique. This practice is
D1068Test Methods for Iron in Water
applicable to surface, saline, domestic, and industrial waste-
D1129Terminology Relating to Water
water.
D1193Specification for Reagent Water
1.2 Because of the differences among various makes and
D1687Test Methods for Chromium in Water
models of satisfactory instruments, no detailed operating in-
D1688Test Methods for Copper in Water
structions can be provided. Instead, the analyst should follow
D1691Test Methods for Zinc in Water
the instructions provided by the manufacturer of the particular
D1886Test Methods for Nickel in Water
instrument.
D1976Test Method for Elements in Water by Inductively-
1.3 This practice can be used with the following ASTM
Coupled Argon Plasma Atomic Emission Spectroscopy
standards, providing the user determines precision and bias D3370Practices for Sampling Water from Closed Conduits
based on this digestion practice: Test Method D857, Test
D3557Test Methods for Cadmium in Water
Methods D858, Test Methods D1068, Test Methods D1687, D3559Test Methods for Lead in Water
Test Methods D1688, Test Methods D1691, Test Methods
D3856Guide for Management Systems in Laboratories
D1886, Test Method D1976, Practices D3370, Test Methods Engaged in Analysis of Water
D3557, Test Methods D3559, Practice D3919, Test Method
D3919Practice for Measuring Trace Elements in Water by
D4190, Practice D4453, Practice D4691, and Test Method
Graphite Furnace Atomic Absorption Spectrophotometry
D5673. D4190TestMethodforElementsinWaterbyDirect-Current
Plasma Atomic Emission Spectroscopy
1.4 The values stated in SI units are to be regarded as
D4453Practice for Handling of High Purity Water Samples
standard. No other units of measurement are included in this
D4691Practice for Measuring Elements in Water by Flame
standard.
Atomic Absorption Spectrophotometry
1.5 This standard does not purport to address all of the
D5673Test Method for Elements in Water by Inductively
safety concerns, if any, associated with its use. It is the
Coupled Plasma—Mass Spectrometry
3
responsibility of the user of this standard to establish appro-
2.2 U.S. Code of Federal Regulations:
priate safety and health practices and determine the applica-
CFR 1.030.10Code of Federal Regulations, Volume 21
3
bility of regulatory limitations prior to use. For specific hazard
2.3 Federal Communications Commission Standard:
statements, see Section 9.
Code of Federal Regulations,Volume 47, FCC Rule Part 18
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
1
This practice is under the jurisdiction ofASTM Committee D19 on Water and contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
is the direct responsibility of Subcommittee D19.05 on Inorganic Constituents in Standards volume information, refer to the standard’s Document Summary page on
Water. the ASTM website.
3
Current edition approved March 1, 2012. Published March 2012. Originally AvailablefromU.S.GovernmentPrintingOfficeSuperintendentofDocuments,
approved in 1991. Last previous edition approved in 2007 as D4309–02 (2007). 732 N. Capitol St., NW, Mail Stop: SDE, Washington, DC 20401, http://
DOI: 10.1520/D4309-12. www.access.gpo.gov.
*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 ----------------------
D4309 − 12
4
2.4 U.S. EPA Method: heating. Safety interlocks, to shut off magnetron power output,
U.S. EPAMethod:Methods for ChemicalAnalysis of Water must be contained in the oven door opening mechanism. The
and Waste—March 1979, “Total Metals Digestion Proce- unit may contain a temperature control device capable of
dure” 4.1.3, page Metals 6 controlling vessel temperatures to 200°C and/or a pressure
U.S. EPA Method: SW 846 Method 3015Microwave As- control device capable of controlling vessel pressures to a
sisted Acid Digestion of Aqueous Samples and Extracts minimum 100 psi
...

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: D4309 − 02 (Reapproved 2007) D4309 − 12
Standard Practice for
Sample Digestion Using Closed Vessel Microwave Heating
1
Technique for the Determination of Total Metals in Water
This standard is issued under the fixed designation D4309; 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 practice covers the general considerations for quantitative sample digestion for total metals in water using closed vessel
microwave heating technique. This practice is applicable to surface, saline, domestic, and industrial wastewater.
1.2 Because of the differences among various makes and models of satisfactory instruments, no detailed operating instructions
can be provided. Instead, the analyst should follow the instructions provided by the manufacturer of the particular instrument.
1.3 This practice can be used with the following ASTM standards, providing the user determines precision and bias based on
this digestion practice: Test MethodsMethod D857, Test Methods D858, Test Methods D1068, Specification D1192, Test Methods
D1687, Test Methods D1688, Test Methods D1691, Test Methods D1886, Test Method D1976, Practices D3370, Test Methods
D3557, Test Methods D3559, Practice D3919, Test MethodsMethod D4190, Practice D4453, and Practice D4691, and Test Method
D5673.
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 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 Section 9.
2. Referenced Documents
2
2.1 ASTM Standards:
D857 Test Method for Aluminum in Water
D858 Test Methods for Manganese in Water
D1068 Test Methods for Iron in Water
D1129 Terminology Relating to Water
3
D1192 Guide for Equipment for Sampling Water and Steam in Closed Conduits (Withdrawn 2003)
D1193 Specification for Reagent Water
D1687 Test Methods for Chromium in Water
D1688 Test Methods for Copper in Water
D1691 Test Methods for Zinc in Water
D1886 Test Methods for Nickel in Water
D1976 Test Method for Elements in Water by Inductively-Coupled Argon Plasma Atomic Emission Spectroscopy
D3370 Practices for Sampling Water from Closed Conduits
D3557 Test Methods for Cadmium in Water
D3559 Test Methods for Lead in Water
D3856 Guide for Management Systems in Laboratories Engaged in Analysis of Water
D3919 Practice for Measuring Trace Elements in Water by Graphite Furnace Atomic Absorption Spectrophotometry
D4190 Test Method for Elements in Water by Direct-Current Plasma Atomic Emission Spectroscopy
D4453 Practice for Handling of High Purity Water Samples
D4691 Practice for Measuring Elements in Water by Flame Atomic Absorption Spectrophotometry
1
This practice 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 June 15, 2007March 1, 2012. Published June 2007March 2012. Originally approved in 1991. Last previous edition approved in 20022007 as
D4309 – 02.D4309 – 02 (2007). DOI: 10.1520/D4309-02R07.10.1520/D4309-12.
2
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 ----------------------
D4309 − 12
D5673 Test Method for Elements in Water by Inductively Coupled Plasma—Mass Spectrometry
3
2.2 U.S. Code of Federal Regulations:
CFR 1.030.10 Code of Federal Regulations, Volume 21
3
2.3 Federal Communications Commission Standard:
Code of Federal Regulations, Volume 47, FCC Rule Part 18
4
2.4 U.S. EPA Method:
U.S. EPA Method: Methods for Chemical Analysis of Water and Waste—March 1979, “Total Metals Digestion Procedure” 4.1.3,
page Metals 6
U.S. EPA Method: SW 846 Method 3015 Microwave Ass
...

This document is not anASTM standard and is intended only to provide the user of anASTM 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:D4309–02 (Reapproved 2007) Designation:D4309–12
Standard Practice for
Sample Digestion Using Closed Vessel Microwave Heating
1
Technique for the Determination of Total Metals in Water
This standard is issued under the fixed designation D4309; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision.Anumber 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 Thispracticecoversthegeneralconsiderationsforquantitativesampledigestionfortotalmetalsinwaterusingclosedvessel
microwave heating technique. This practice is applicable to surface, saline, domestic, and industrial wastewater.
1.2 Because of the differences among various makes and models of satisfactory instruments, no detailed operating instructions
can be provided. Instead, the analyst should follow the instructions provided by the manufacturer of the particular instrument.
1.3 This practice can be used with the followingASTM standards, providing the user determines precision and bias based on
this digestion practice: Test Methods D857, Test Methods D858, Test Methods D1068, Specification D1192, Test Method D1976,
Test Methods D1687, Test Methods D1688, Test Methods D1691, Test Methods D1886, Practices D3370, Test Methods D3557,
Test Methods D3559, Practice D3919, Test Methods D4190, Practice D4453, and Practice , Practice D4691, and Test Method
D5673.
1.4
1.4 The values stated in either SI or inch-pound units are to be regarded as the standard. The values given in parentheses are
for information only.
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 Section 9.
2. Referenced Documents
2
2.1 ASTM Standards:
D857 Test Method for Aluminum in Water
D858 Test Methods for Manganese in Water
D1068 Test Methods for Iron in Water
D1129 Terminology Relating to Water D1192Guide for Equipment for Sampling Water and Steam in Closed Conduits
D1193 Specification for Reagent Water
D1687 Test Methods for Chromium in Water
D1688 Test Methods for Copper in Water
D1691 Test Methods for Zinc in Water
D1886 Test Methods for Nickel in Water
D1976 Test Method for Elements in Water by Inductively-Coupled Argon Plasma Atomic Emission Spectroscopy
D3370 Practices for Sampling Water from Closed Conduits
D3557 Test Methods for Cadmium in Water
D3559 Test Methods for Lead in Water
D3856 Guide for Management Systems in Laboratories Engaged in Analysis of Water
D3919 Practice for Measuring Trace Elements in Water by Graphite Furnace Atomic Absorption Spectrophotometry
D4190 Test Method for Elements in Water by Direct-Current Plasma Atomic Emission Spectroscopy
D4453 Practice for Handling of High Purity Water Samples
D4691 Practice for Measuring Elements in Water by Flame Atomic Absorption Spectrophotometry Practice for Measuring
Elements in Water by Flame Atomic Absorption Spectrophotometry
1
This practice is under the jurisdiction ofASTM Committee D19 on Water and is the direct responsibility of Subcommittee D19.05 on Inorganic Constituents in Water.
Current edition approved June 15, 2007. Published June 2007. Originally approved in 1991. Last previous edition approved in 2002 as D4309–02. DOI:
10.1520/D4309-02R07.
Current edition approved March 1, 2012. Published March, 2012. Originally approved in 1991. Last previous edition approved in 2007 as D4309–02(2007). DOI:
10.1520/D4309-12.
2
ForreferencedASTMstandards,visittheASTMwebsite,www.astm.org,orcontactASTMCustomerServiceatservice@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 ----------------------
D4309–12
D5673 Test Method for Elements in Water by Inductively Coupled PlasmaMass Spectrometry
3
2.2 U.S. Code of Federal Regulations:
CFR 1.030.10 Code of Federal Regulations, Volume 21
3
2.3 Federal Communications Commission Standard:
Code of Federal Regulations, Volume 47, FCC Rule Part 18
4
2.4 U.S. EPA Method:
U.S. EPA Method: Method
...

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