D 3223 – 02 ;RDMYMJM_.doc
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2、n American National StandardStandard Test Method forTotal Mercury in Water1This standard is issued under the fixed designation D 3223; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last revision. A number in parenthes
3、es indicates the year of last reapproval. Asuperscript 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. Scope1.1 This test method2 covers the determination of total mercury in water in
4、the range from 0.5 to 10.0 g Hg/L (1). 3The test method is applicable to fresh waters, saline waters, and some industrial and sewage effluents. It is the users responsi- bility to ensure the validity of this test method for waters of untested matrices.1.1.1 The analyst should recognize that the prec
5、ision 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 (sedi- ments, biological materials, tis
6、sues, 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 procedur
7、e if they are first converted to mercuric ions. Using potassium persulfate and potassium permanganate as oxidants, and a digestion temperature of95C, approximately 100 % recovery of organomercury com- pounds can be obtained (2,4).1.3 The range of the test method may be changed by instrument or recor
8、der 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
9、 of this standard to establish appro- priate safety and health practices and determine the applica-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 March 10,
10、 2002. Published May 2002. Originally published as D 322379. Last previous edition D 3223 95.2 Adapted from research investigations by the U. S. Environmental ProtectionAgencys Analytical Quality Control Laboratory, Cincinnati, OH, and Region IV Surveillance and Analysis Division, Chemical Services
11、Branch, Athens, GA.3 The boldface numbers in parentheses refer to the references at the end of thistest method.bility of regulatory limitations prior to use. For specific hazardstatements, see 7.8 and 10.8.2.2. Referenced Documents2.1 ASTM Standards:D 512 Test Methods for Chloride Ion in Water4D 112
12、9 Terminology Relating to Water4D 1193 Specification for Reagent Water4D 1245 Practice for Examination of Water-Formed Deposits by Chemical Microscopy5D 1252 Test Methods for Chemical Oxygen Demand(Dichromate Oxygen Demand) of Water5D 1426 Test Methods for Ammonia Nitrogen in Water4D 2777 Practice f
13、or Determination of Precision and Bias ofApplicable Methods of Committee D19 on Water4D 3370 Practices for Sampling Water from Closed Con- duits4D 4691 Practice for Measuring Elements in Water by FlameAtomic Absorption Spectrophotometry4D 4841 Practice for Estimation of Holding Time for WaterSamples
14、 Containing Organic and Inorganic Constituents4D 5810 Guide for Spiking into Aqueous Samples4D 5847 Practice for Writing Quality Control Specifications for Standard Test Methods for Water Analysis53. Terminology3.1 DefinitionsFor definitions of terms used in this test method, refer to Terminology D
15、1129.4. Summary of Test Method4.1 The test method consists of a wet chemical oxidation which converts all mercury to the mercuric ion; reduction of mercuric ions to metallic mercury, followed by a cold vapor atomic absorption analysis (1,2). A general guide for flame and vapor generation atomic abso
16、rption applications is given in Practice D 4691.4.2 Cold vapor atomic absorption analysis is a physical method based on the absorption of ultraviolet radiation at a wavelength of 253.7 nm by mercury vapor. The mercury is4 Annual Book of ASTM Standards, Vol 11.01.5 Annual Book of ASTM Standards, Vol
17、11.02.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.1D 3223 02reduced to the elemental state and aerated from solution ineither a closed recirculating system or an open one-pass system. The mercury vapor passes through a cell positi
18、oned in the light path of an atomic absorption spectrophotometer. Absorbance is measured as a function of mercury concentra- tion.5. Significance and Use5.1 The presence of mercury in industrial discharge, domes- tic discharge, and potable water is of concern to the public because of its toxicity. R
19、egulations 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.6. Interference6.1 Possible interference from sulfide is eliminated by the addition of potassium permanganate. Concentra
20、tions as high as20 mg/L of sulfide as sodium sulfide do not interfere with therecovery of added inorganic mercury from distilled water (2). AReaction flaskGHollow cathode mercury lamp6.2 Copper has also been reported to interfere; however,copper concentrations as high as 10 mg/L have no effect on th
21、e recovery of mercury from spiked samples (2).6.3 Seawaters, brines, and industrial effluents high in chlo- rides require additional permanganate (as much as 25 mL). During the oxidation step chlorides are converted to free chlorine which will also absorb radiation at 253.7 nm. Care must be taken to
22、 assure that free chlorine is absent before mercury is reduced and swept into the cell. This may be accomplished by using an excess of hydroxylamine sulfate reagent (25 mL). The dead air space in the reaction flask must also be purged before the addition of stannous sulfate. Both inorganic and organ
23、ic mercury spikes have been quantitatively recovered from sea water using this technique (2).6.4 Volatile organic materials that could interfere will be removed with sample digestion as described in 11.2 through11.4.7. ApparatusNOTE 1Take care to avoid contamination of the apparatus with mercury. So
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