D 1971 – 02 ;RDE5NZE_.doc
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2、n American National StandardStandard Practices forDigestion of Water Samples for Determination of Metals by Flame Atomic Absorption, Graphite Furnace Atomic Absorption, Plasma Emission Spectroscopy, or PlasmaMass Spectrometry1This standard is issued under the fixed designation D 1971; the number imm
3、ediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon (e) indicates an editorial change since the last revision or reapproval.1. Scope1.1 Mo
4、st atomic absorption and plasma emission spectros- copy, and plasma-mass spectrometric test methods require that the metals of interest be dissolved in a liquid phase before being introduced into the spectrophotometer. These practices describe digestion or dissolution procedures whereby analyte meta
5、ls associated with the solid fraction of a sample can be brought into solution for subsequent analysis. The following practices are included:Sections1.7 This standard does not purport to address all of thesafety concerns, if any, associated with its use. It is the responsibility of the user of this
6、standard to establish appro- priate safety and health practices and determine the applica- bility of regulatory limitations prior to use. Specific hazard statements are given in Section 6.2. Referenced Documents2.1 ASTM Standards:D 511 Test Methods for Calcium and Magnesium in Water2Practice ADigest
7、ion with Mineral Acids andElevated PressurePractice BDigestion with Mineral Acids andHeating at Atmospheric Pressure8 through 1314 through 19D 857 Test Methods for Aluminum in Water2D 858 Test Methods for Manganese in Water2D 1068 Test Methods for Iron in Water2Practice CIn-bottle digestion with Min
8、eral Acids20 through 251.2 These practices have been demonstrated to be applicable to a wide variety of sample types and sample matrices, and in many cases, will give complete dissolution of the analyte metals of interest. They are by no means the only digestion procedures available.1.3 The user of
9、these practices should be cautioned that these practices may not completely dissolve all portions of a samples solid phase and may not give complete recovery of the desired analyte metals. In these cases, other digestion techniques are available that will effect complete dissolution ofa sample. It i
10、s the users responsibility to ensure the validity of these practices for use on their particular sample matrix, for their metals of interest.1.4 This practice assumes that the criteria established inGuide D 3856 can be met.1.5 These digestion procedures have been selected for their wide application,
11、 low cost, and ease of use.1.6 The values stated in SI units are to be regarded as the standard. The values given in parentheses are for information only.1 These practices are under the jurisdiction of ASTM Committee D19 on Water and is the direct responsibility of Subcommittee D19.05 on Inorganic C
12、onstituents in Water.D 1129 Terminology Relating to Water2D 1192 Specification for Equipment for Sampling Water and Steam in Closed Conduits2D 1193 Specification for Reagent Water2D 1687 Test Methods for Chromium in Water2D 1688 Test Methods for Copper in Water2D 1691 Test Methods for Zinc in Water2
13、D 1886 Test Methods for Nickel in Water2D 1976 Test Method for Elements in Water by Inductively- Coupled Argon Plasma Atomic Emission Spectroscopy2D 3370 Practices for Sampling Water from Closed Con- duits2D 3372 Test Method for Molybdenum in Water2D 3557 Test Methods for Cadmium in WaterD 3558 Test
14、 Methods for Cobalt in Water2D 3559 Test Method for Lead in Water2D 3645 Test Method for Beryllium in Water2D 3856 Guide for Good Laboratory Practices in Laborato- ries Engaged in Sampling and Analysis of Water2D 3866 Test Methods for Silver in Water2D 3919 Practices for Measuring Trace Elements in
15、Water byGraphite Furnace Atomic Absorption Spectrophotometry2D 4190 Test Method for Elements in Water by Direct- Current Argon Plasma Atomic Emission Spectroscopy2D 4191 Test Method for Sodium in Water by AtomicCurrent edition approved March 10, 2002. Published June 2002. Originally published as D 1
16、971 91. Last previous edition D 1971 95.2 Annual Book of ASTM Standards, Vol 11.01.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.1Absorption Spectrophotometry2D 1971 02effluents; river and lake waters; and plant and animal tissues.D
17、 4192 Test Method for Potassium in Water by AtomicAbsorption Spectrophotometry2D 4309 Practice for Sample Digestion Using Closed Vessel Microwave Heating Technique for Determination of Total Recoverable Metals in Water2D 4691 Practice for Measuring Elements in Water by FlameAtomic Absorption Spectro
18、photometry2D 5673 Test Method for Elements in Water by InductivelyCoupled Plasma-Mass Spectrometry32.2 U.S. EPA Method:EPA-600/4-79-020 Methods for Chemical Analysis of Wa- ter and Wastes4EPA-600/R-94/111 Methods for the Determination of Met- als in Environmental SamplesSupplement 142.3 U.S. Geologi
19、cal Survey Method:U.S. Geological Survey Open File Report 96225: Methods of Analysis by the U.S. Geological Survey National Water Quality LaboratoryIn-Bottle Acid Digestion of Whole Water Samples5Quality LaboratoryIn-Bottle Acid Digestion of WholeWater Samples53. Terminology3.1 Definitions: For defi
20、nitions of terms used in these practices, refer to Terminology D 1129.3.2 Definitions of Terms Specific to This Standard:3.2.1 digestiontreating a sample with the use of heat or elevated pressures, or both, usually in the presence of chemical additives, to bring analytes of interest into solution or
21、 to remove interfering matrix components, or both.3.2.2 total recoverablethe amount of a metal analyte measurable by atomic absorption spectrophotometry, plasma emission spectroscopy or plasma mass spectrometry after applying the digestion procedure in either Practice A, Practice B, or Practice C. T
22、he choice of Practice A, B, or C shall be noted in reporting resultant data.4. Significance and Use4.1 The determination of metals in water often requires the measurement of total (suspended and dissolved) metals as well as soluble (dissolved) metals. In such cases, consistent and dependable digesti
23、on procedures must be used so that data derived for the total metals content is reliable.4.2 The practices given are applicable to a wide variety of sample types for the purpose of preparing a sample for metals analyses by atomic absorption spectrophotometry or plasma emission spectroscopy (see Test
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