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ASTM D4309-02

(Practice)

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

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

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 Methods D 857, Test Methods D 858, Test Methods D 1068, Specification D 1192, Test Methods D 1687, Test Methods D 1688, Test Methods D 1691, Test Methods D 1886, Practices D 3370, Test Methods D 3557, Test Methods D 3559, Practice D 3919, Test Methods D 4190, Practice D 4453, and Practice D 4691.
1.4 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.

General Information

Status
Historical
Publication Date
09-Jan-2002
ICS
13.060.50 - Examination of water for chemical substances
Technical Committee
D19 - Water
Drafting Committee
D19.05 - Inorganic Constituents in Water
Current Stage
Ref Project

Relations

Replaces
ASTM D4309-96 - Standard Practice for Sample Digestion Using Closed Vessel Microwave Heating Technique for the Determination of Total Metals in Water
Effective Date
10-Jan-2002
Replaced By
ASTM D4309-02(2007) - Standard Practice for Sample Digestion Using Closed Vessel Microwave Heating Technique for the Determination of Total Metals in Water
Effective Date
15-Jun-2007
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
10-Jan-2002
Referred By
ASTM D7876-13(2018) - Standard Practice for Practice for Sample Decomposition Using Microwave Heating (With or Without Prior Ashing) for Atomic Spectroscopic Elemental Determination in Petroleum Products and Lubricants
Effective Date
10-Jan-2002
Referred By
ASTM F2931-19a - Standard Guide for Analytical Testing of Substances of Very High Concern in Materials and Products
Effective Date
10-Jan-2002

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ASTM D4309-02 - Standard Practice for Sample Digestion Using Closed Vessel Microwave Heating Technique for the Determination of Total Metals in WaterASTM D4309-02 - Standard Practice for Sample Digestion Using Closed Vessel Microwave Heating Technique for the Determination of Total Metals in Water
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ASTM D4309-02 - Standard Practice for Sample Digestion Using Closed Vessel Microwave Heating Technique for the Determination of Total Metals in Water
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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:D 4309–02
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 D 4309; 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 (e) indicates an editorial change since the last revision or reapproval.
2
1. Scope D1688 Test Methods for Copper in Water
2
D1691 Test Methods for Zinc in Water
1.1 This practice covers the general considerations for
2
D1886 Test Methods for Nickel in Water
quantitative sample digestion for total metals in water using
D3370 Practices for Sampling Water from Closed Con-
closed vessel microwave heating technique. This practice is
2
duits
applicable to surface, saline, domestic, and industrial waste-
2
D3557 Test Methods for Cadmium in Water
water.
2
D3559 Test Methods for Lead in Water
1.2 Because of the differences among various makes and
D3856 Guide for Good Laboratory Practices in Laborato-
models of satisfactory instruments, no detailed operating in-
2
ries Engaged in Sampling and Analysis of Water
structions can be provided. Instead, the analyst should follow
D3919 Practice for Measuring Trace Elements in Water by
the instructions provided by the manufacturer of the particular
2
Graphite Furnace Atomic Absorption Spectrophotometry
instrument.
D4190 Test Methods for Elements in Water by Direct-
1.3 This practice can be used with the following ASTM
2
Current Argon Plasma Atomic Emission Spectroscopy
standards, providing the user determines precision and bias
2
D4453 PracticeforHandlingofUltra-PureWaterSamples
based on this digestion practice: Test Methods D857, Test
D4691 PracticeforMeasuringElementsinWaterbyFlame
Methods D858, Test Methods D1068, Specification D1192,
2
Atomic Absorption Spectrophotometry
Test Methods D1687, Test Methods D1688, Test Methods
2.2 U.S. Code of Federal Regulations:
D1691,TestMethodsD1886,PracticesD3370,TestMethods
3
CFR 1.030.10 Code of Federal Regulations, Volume 21
D3557, Test Methods D3559, Practice D3919, Test Methods
2.3 Federal Communications Commission Standard:
D4190, Practice D4453, and Practice D4691.
Code of Federal Regulations, Volume 47, FCC Rule Part
1.4 This standard does not purport to address all of the
3
18
safety concerns, if any, associated with its use. It is the
2.4 U.S. EPA Method:
responsibility of the user of this standard to establish appro-
U.S.EPAMethod: MethodsforChemicalAnalysisofWater
priate safety and health practices and determine the applica-
and Waste—March 1979, “Total Metals Digestion Proce-
bility of regulatory limitations prior to use. For specific hazard
4
dure” 4.1.3, page Metals 6
statements, see Section 9.
U.S. EPA Method: SW 846 Method 3015 Microwave As-
4
2. Referenced Documents sisted Acid Digestion of Aqueous Samples and Extracts
2.1 ASTM Standards:
3. Terminology
2
D857 Test Methods for Aluminum in Water
2 3.1 Definitions—For definitions of terms used in this prac-
D858 Test Methods for Manganese in Water
2
tice, refer to Terminology D1129.
D1068 Test Methods for Iron in Water
2
D1129 Terminology Relating to Water
4. Summary of Practice
D1192 Specification for Equipment for Sampling Water
2
4.1 A representative aliquot of a homogeneous sample is
and Steam in Closed Conduits
2 digested with acid in a closed microwave transparent vessel,
D1193 Specification for Reagent Water
2
using microwave heating. The digestate or a filtered digestate
D1687 Test Methods for Chromium in Water
is then analyzed by direct aspiration or injection by flame
1
This practice is under the jurisdiction ofASTM Committee D19 on Water and
3
is the direct responsibility of Subcommittee D19.05 on Inorganic Constituents in Available from Office of the Federal Register, National Archives Records
Water. Administration, Superintendent of Documents, U.S. Government Printing Office,
Current edition approved Jan. 10, 2002. Published April 2002. Originally Washington, DC 20401.
4
published as D 4309 – 91. Last previous edition D 4309 – 96. Available from National Technical Information Service, 5285 Port Royal Rd.,
2
Annual Book of ASTM Standards, Vol 11.01. Springfield, VA 22161.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
1

---------------------- Page: 1 ----------------------
D 4309–02
atomic absorption spectrophotometry (FAAS), inductively 8. Reagents
coupled plasma emission techniques (ICP), direct current
8.1 Purity of Reagents—Reagent grade chemicals shall be
plasma emission techniques (DCP), or graphite furnace atomic
used in this practice. Unless otherwise indicated, it is intended
absorption spec
...

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5.1 This test method has been developed by U.S. EPA Region 5 Chicago Regional Laboratory (CRL).  
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1.2 The Detection Verification Level (DVL) and Reporting Range for the carbamates are listed in Table 1.    
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Standard Test Method for Determination of Bisphenol A in Environmental Waters by Liquid Chromatography/Tandem Mass Spectrometry

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5.1 The first reported synthesis of BPA was by the reaction of phenol with acetone by Zincke.4 BPA has become an important high volume industrial chemical used in the manufacture of polycarbonate plastic and epoxy resins. Polycarbonate plastic and resins are used in numerous products including electrical and electronic equipment, automobiles, sports and safety equipment, reusable food and drink containers, electrical laminates for printed circuit boards, composites, paints, adhesives, dental sealants, protective coatings and many other products.5  
5.2 The environmental source of BPA is predominantly from the decomposition of polycarbonate plastics and resins. BPA is not classified as bio-accumulative by the U.S. Environmental Protection Agency and will biodegrade. BPA has been reported to have adverse effects in aquatic organisms and may be released into environmental waters directly at trace levels through landfill leachate and POTW effluents. This method has been investigated for use with surface water and secondary and tertiary POTW effluent samples therefore, it is applicable to these matrices only. It has not been investigated for use with salt water or solid sample matrices.
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5.1 Pesticides may be used in various agricultural and household products. These products may enter waterways at low levels through run-off or misuse near water resources. Hence, there is a need for quick, easy and robust method to determine pesticide concentration in water matrices for understanding the sources and concentration levels in affected areas.  
5.2 This method has been single-laboratory validated in reagent water and surface waters (Tables 12-14).
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1.2 A full collaborative study to meet the requirements of Practice D2777 has not been completed. This standard contains single-operator precision and bias based on single-operator data. Publication of standards that have not been fully validated is done to make the current technology accessible to users of standards, and to solicit additional input from the user community.  
1.3 A reporting limit check sample (RLCS) is analyzed during every batch to ensure that if an analyte was present in a sample at or near the reporting limit it would be positively identified and accurately quantitated within set quality control limits. A method detection limit (MDL) study was not done for this method, the method detection limits would be much lower than the reporting limits in this method and would be irrelevant. A RLCS was determined to be more applicable for this standard. If this method is adapted to report much lower or near the MDL then a MDL study would be warranted.  
1.4 Units—The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.5 The Reporting Range for the target analytes are listed in Table 1.  
1.5.1 The reporting limit in this test method is the minimum value below which data are documented as non-detects. The reporting limit is calculated from the concentration of the Level 1 calibration standard as shown in Table 6 after taking into account an 8 mL water sample volume and a final diluted sample volume of 10 mL (80 % water/20 % methanol).  
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, health, and environmental practices and determine the applicability of regulatory limitations prior to use.  
1.7 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.

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Standard Test Method for Determination of Nonylphenol, p-tert-Octylphenol, Nonylphenol Monoethoxylate and Nonylphenol Diethoxylate in Environmental Waters by Liquid Chromatography/Tandem Mass Spectrometry

SIGNIFICANCE AND USE
5.1 NP and OP have been shown to have toxic effects in aquatic organisms. The source of NP and OP is prominently from the use of common commercial surfactants. The most widely used surfactant is nonylphenol ethoxylate (NPEO) which has an average ethoxylate chain length of nine. The ethoxylate chain is readily biodegraded to form NP1EO, NP2EO, nonylphenol carboxylate (NPEC) and, under anaerobic conditions, NP. NP will also biodegrade, but may be released into environmental waters directly at trace levels. This method has been investigated and is applicable for environmental waters, including seawater.
SCOPE
1.1 This test method covers the determination of nonylphenol (NP), nonylphenol ethoxylate (NP1EO), nonylphenol diethoxylate (NP2EO), and octylphenol (OP), extracted from water utilizing solid phase extraction (SPE), separated using liquid chromatography (LC) and detected with tandem mass spectrometry (MS/MS). These compounds are qualitatively and quantitatively determined by this method. This method adheres to single reaction monitoring (SRM) mass spectrometry.  
1.2 The method detection limit (MDL) and reporting limit (RL) for NP, NP1EO, NP2EO, and OP are listed in Table 1.    
1.3 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.4 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, health, and environmental practices and determine the applicability of regulatory limitations prior to use.  
1.5 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.

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