1、Designation: D1976 07D1976 12Standard Test Method forElements in Water by Inductively-Coupled Argon PlasmaAtomic Emission Spectroscopy1This standard is issued under the fixed designation D1976; the number immediately following the designation indicates the year oforiginal adoption or, in the case of
2、 revision, the year of last revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon () indicates an editorial change since the last revision or reapproval.1. Scope Scope*1.1 This test method covers the determination of dissolved, total-recoverable, or total elem
3、ents in drinking water, surface water,domestic, or industrial wastewaters.2, 31.2 It is the users responsibility to ensure the validity of the test method for waters of untested matrices.1.3 Table 1 lists elements for which this test method applies, with recommended wavelengths and typical estimated
4、 instrumentaldetection limits using conventional pneumatic nebulization.4 Actual working detection limits are sample dependent and as thesample matrix varies, these detection limits may also vary. In time, other elements may be added as more information becomesavailable and as required.1.4 The value
5、s 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 responsibilityof the user of this standard to establish appropriate sa
6、fety and health practices and determine the applicability of regulatorylimitations prior to use. For specific hazard statements, see Note 2 and Section 9.2. Referenced Documents2.1 ASTM Standards:5D1066 Practice for Sampling SteamD1129 Terminology Relating to WaterD1192 Guide for Equipment for Sampl
7、ing Water and Steam in Closed Conduits (Withdrawn 2003)6D1193 Specification for Reagent WaterD2777 Practice for Determination of Precision and Bias of Applicable Test Methods of Committee D19 on WaterD3370 Practices for Sampling Water from Closed ConduitsD4841 Practice for Estimation of Holding Time
8、 for Water Samples Containing Organic and Inorganic ConstituentsD5810 Guide for Spiking into Aqueous SamplesD5847 Practice for Writing Quality Control Specifications for Standard Test Methods for Water Analysis3. Terminology3.1 DefinitionsFor definitions of other terms used in this test method, refe
9、r to Terminology D1129.3.2 Definitions of Terms Specific to This Standard:3.2.1 calibration blank, na volume of water containing the same acid matrix as the calibration standards (see 11.1).1 This test method is under the jurisdiction ofASTM Committee D19 on Water and is the direct responsibility of
10、 Subcommittee D19.05 on Inorganic Constituents in Water.Current edition approved Aug. 1, 2007March 1, 2012. Published August 2007March 2012. Originally approved in 1991. Last previous edition approved in 20022007 asD1976 02.D1976 07. DOI: 10.1520/D1976-07.10.1520/D1976-12.2 The detailed report of EP
11、A Method Study 27, Method 200.7 is available from the National Technical Information Service, 5285 Port Royal Road, Springfield, VA. Asummary of the project is available from the U.S. Environmental Protection Agency, Environmental Monitoring and Support Laboratory, Cincinnati, OH.3 Fishman, M. J. an
12、d Friedman, L., “Methods for Determination of Inorganic Substances in Water and Fluvial Sediments”, U.S. Geological Survey Techniques ofWater-Resources Investigations, Book 5, Chapter Practice for Sampling Steam, Open File Report 85-495, 1985, p. 659671. Fishman, M. J. and Friedman, L., “Methods for
13、Determination of Inorganic Substances inWater and Fluvial Sediments”, U.S. Geological Survey Techniques of Water-Resources Investigations, Book 5, Chapter D1066, OpenFile Report 85-495, 1985, p. 659671.4 Winge, R. K., Fassel, V. A., Peterson, V. J. and Floyd, M. A.,“ Inductively Coupled Plasma-Atomi
14、c Emission Spectroscopy,” An Atlas of Spectral Information, ElsevierScience Publishing Co., Inc., NewYork, NY, 1985.Winge, R. K., Fassel,V.A., Peterson,V. J. and Floyd, M.A., “Inductively Coupled Plasma-Atomic Emission Spectroscopy,”An Atlas of Spectral Information, Elsevier Science Publishing Co.,
15、Inc., New York, NY, 1985.5 For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at serviceastm.org. For Annual Book of ASTM Standardsvolume information, refer to the standards Document Summary page on the ASTM website.This document is not an ASTM standar
16、d and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Becauseit may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases o
17、nly the current versionof the standard as published by ASTM is to be considered the official document.*A Summary of Changes section appears at the end of this standardCopyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States13.2.2 calibration s
18、tandards, na series of known standard solutions used by the analyst for calibration of the instrument(preparation of the analytical curve) (see 8.11).3.1.3 dissolved, adjthose elements that will pass through a 0.45 m membrane filter.3.2.3 instrumental detection limit, nthe concentration equivalent t
19、o a signal, due to the analyte, that is equal to three times thestandard deviation of a series of ten replicate measures of a reagent blank reagent-blank signal at the same wavelength.3.2.4 laboratory control sample, na solution with the certified concentration(s) of the analytes.3.2.5 reagent blank
20、, na volume of water containing the same matrix as the calibration standards, carried through the entireanalytical procedure.3.2.6 total, nthe concentration determined on an unfiltered sample following vigorous digestion (see 12.3).3.2.7 total-recoverable, adja term relating to forms of each element
21、 element forms that are determinable by the digestionmethod that is included in this procedure (see 12.2).3.1.8 laboratory control sample, na solution with the certified concentration(s) of the analytes.TABLE 1 Suggested Wavelengths and EstimatedDetection Limits4Element Wavelength, nmA Estimated det
22、ection limit,g/Llimit, g/LBAluminum 308.215 45Arsenic 193.696 53Antimony 206.833 32Beryllium 313.042 0.3Boron 249.773 5Cadmium 226.502 4Chromium 267.716 7Cobalt 228.616 7Copper 324.754 6Iron 259.940 7Lead 220.353 42Magnesium 279.079 30Manganese 257.610 2Molybdenum 202.030 8Nickel 231.604 15Selenium
23、196.026 75Silver 328.068 7Thallium 190.864 40Vanadium 292.402 8Zinc 213.856 2A The wavelengths listed are recommended because of their sensitivity and overallacceptance. Other wavelengths may be substituted if they can provide the neededsensitivity and are treated with the same corrective techniques
24、 for spectralinterference (see 6.1.1).B The estimated detection limits as shown are taken from Winge, Fassel, et al.4They are given as a guide for approximate detection limits for the listed wave-lengths. The actual test method instrumental detection limits are sample-dependent and may vary as the s
25、ample matrix varies (see 3.1.43.2.3).D1976 1223.2 DefinitionsFor definitions of other terms used in this test method, refer to Terminology D1129.4. Summary of Test Method4.1 Elements are determined, either sequentially or simultaneously, by inductively-coupled argon plasma optical emissionspectrosco
26、py.4.2 A background correction technique may be used to compensate for variable background contribution from highconcentrations of major and trace elements.5. Significance and Use5.1 This test method is useful for the determination of element concentrations in many natural waters and wastewaters. It
27、 hasthe capability for the simultaneous determination of up to 20 elements. High sensitivity analysis can be achieved for some elementsthat are difficult to determine by other techniques such as Flame Atomic Absorption.6. Interferences6.1 Several types of interference effects may contribute to inacc
28、uracies in the determination of trace elements. Theseinterferences can be summarized as follows:6.1.1 Spectral interferences can be categorized as (1) overlap of a spectral line from another element; (2) unresolved overlapof molecular band spectra; (3) background contribution from continuous or reco
29、mbination phenomena; and (4) backgroundcontribution from stray light from line emission of high concentration elements.6.1.1.1 The effects described in 6.1.1 can be compensated for by utilizing a computer correction of the raw data, requiring themonitoring and measurement of the interfering element.
30、 The second effect may require selection of an alternate wavelength. Thethird and fourth effects can usually be compensated for by a background correction adjacent to the analyte line.6.1.1.2 Table 2 lists some interference effects for the recommended wavelengths given in Table 1. The data in Table
31、2 areintended for use only as a rudimentary guide for the indication of potential spectral interferences. For this purpose, linear relationsbetween concentration and intensity for the analytes and the interferents can be assumed.6.1.1.3 Only those interferents listed in Table 2 were investigated. Th
32、e blank spaces in Table 2 indicate that measurableinterferences were not observed for the interferent concentrations listed in Table 3. Generally, interferences were considered asdiscernible if the interferent produced interference peaks or background shifts that corresponded to 2 to 5 % of the peak
33、s generatedby the analyte concentrations also listed in Table 3.6.1.2 Physical interferences are generally considered to be effects associated with the sample nebulization and transportprocesses. Such properties as change in viscosity and surface tension can cause significant inaccuracies, especiall
34、y in samples thatmay contain high dissolved solids or acid concentrations, or both. The use of a peristaltic pump may lessen these interferences.If these types of interferences are operative, they must be reduced by dilution of these samples or utilization of standard additiontechniques, or both.TAB
35、LE 2 Analyte Concentration Equivalents, mg/L, Arising from Interferents at the 100 mg/L LevelAAnalyte Wavelength, nm InterferentAl Ca Cr Cu Fe Mg Mn Ni Ti VAluminum 308.215 . . . . . . 0.21 . . 1.4Antimony 206.833 0.47 . 2.9 . 0.08 . . . 0.25 0.45Arsenic 193.696 1.3 . 0.44 . . . . . . 1.1Barium 455.
36、403 . . . . . . . . . .Beryllium 313.042 . . . . . . . . 0.04 0.05Boron 249.773 0.04 . . . 0.32 . . . . .Cadmium 226.502 . . . . 0.03 . . 0.02 . .Calcium 317.933 . . 0.08 . 0.01 0.01 0.04 . 0.03 0.03Chromium 267.716 . . . . 0.003 . 0.04 . . 0.04Cobalt 228.616 . . 0.03 . 0.005 . . 0.03 0.15 .Copper 3
37、24.754 . . . . 0.003 . . . 0.05 0.02Iron 259.940 . . . . . 0.12 0.12 . . .Lead 220.353 0.17 . . . . . . . . .Magnesium 279.079 . 0.02 0.11 . 0.13 0.002 0.25 . 0.07 0.12Manganese 257.610 0.005 . 0.01 . 0.002 . . . . .Molybdenum 202.030 0.05 . . . 0.03 . . . . .Nickel 231.604 . . . . . . . . . .Seleni
38、um 196.026 0.23 . . . 0.09 . . . . .Silicon 288.158 . . 0.07 . . . . . . 0.01Sodium 588.995 . . . . . . . . 0.08 .Thallium 190.864 0.30 . . . . . . . . .VanadiumZinc292.402213.856.0.05.0.140.005.0.290.02.A See Table 3 for concentrations used.D1976 1236.1.2.1 Salt buildup at the tip of the nebulizer
39、is another problem that can occur from high dissolved solids. This salt buildupaffects aerosol flow rate that can cause instrumental drift. To control this problem, wet the argon prior to nebulization, use a tipwasher, or dilute the sample.NOTE 1Periodic inspection and cleaning of the nebulizer and
40、torch components are highly recommended.6.1.2.2 Reports indicate that better control of the argon flow rate improves instrument performance. This control of the argonflow rate can be accomplished with the use of mass flow controllers.6.1.3 Chemical interferences are characterized by molecular compou
41、nd formation, ionization effects, and solute vaporizationeffects. Normally these effects are not pronounced with the ICPtechnique; however, if observed, they can be minimized by carefulselection of operating conditions (incident power, plasma observation position, and so forth), by buffering the sam
42、ple, by matrixmatching, and by standard addition procedures. These types of interferences can be highly dependent on matrix type and thespecific analyte.7. Apparatus7.1 See the manufacturers instruction manual for installation and operation of inductively-coupled argon plasma spectrometers.8. Reagen
43、ts and Materials8.1 Purity of ReagentsReagent grade chemicals shall be used in all tests. Unless otherwise indicated, it is intended thatreagents shall conform to the specifications of the Committee onAnalytical Reagents of theAmerican Chemical Society.6 The highsensitivity of inductively-coupled ar
44、gon plasma atomic emission spectrometry may require reagents of higher purity. Stockstandard solutions are prepared from high purity metals, oxides, or nonhydroscopic reagent grade salts using Types I, II, and IIIreagent water, and ultrapure acids. Other grades may be used, provided it is first asce
45、rtained that the reagent is of sufficient purityto permit its use without lessening the accuracy of the determination.8.2 Purity of WaterUnless otherwise indicated, reference to water shall be understood to mean reagent water conforming toType I, II, or III of Specification D1193. It is the analysts
46、 responsibility to assure that water is free of interferences. Other reagentwater types may be used provided it is first ascertained that the water is of sufficiently high purity to permit its use withoutadversely affecting the precision and bias of the test method. Type II water was specified at th
47、e time of round robin testing of thistest method.8.3 Aqua RegiaMix three parts hydrochloric acid (sp gr 1.19) and one part concentrated nitric acid (sp gr 1.42) just beforeuse.NOTE 2Exercise caution when mixing this reagent.6 Reagent Chemicals, American Chemical Society Specifications, American Chem
48、ical Society, Washington, DC. For Suggestions on the testing of reagents not listed bythe American Chemical Society, see Annual Standards for Laboratory Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia and NationalFormulary, U.S. Pharmacopeial Convention, Inc. (USPC), Roc
49、kville, MD.TABLE 3 Interferent and Analyte Elemental ConcentrationsAAnalytes mg/L Interferents mg/LAl 10 Al 1 000As 10 Ca 1 000B 10 Cr 200Ba 1 Cu 200Be 1 Fe 1 000Ca 1 Mg 1 000Cd 10 Mn 200Co 1 Ni 200Cr 1 Ti 200Cu 1 V 200Fe 1Mg 1Mn 1Na 10Ni 10Pb 10Sb 10Se 10Si 1Tl 10V 1Zn 10A This table indicates concentrations used for interference measurements in Table2.D1976 1248.4 ArgonWelding grade equivalent or better.8.5 Hydrochloric Acid (sp gr 1.19)Concentrated hydrochloric acid, ultrapure or equivalent.8.6 Hydrochloric Acid (1 + 1)Add 1 vol of hy
