ASTM D1976-2007 Standard Test Method for Elements in Water by Inductively-Coupled Argon Plasma Atomic Emission Spectroscopy《用电感耦合氩等离子原子发射光谱法对水中元素的标准试验方法》.pdf

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1、Designation: D 1976 07Standard Test Method forElements in Water by Inductively-Coupled Argon PlasmaAtomic Emission Spectroscopy1This standard is issued under the fixed designation D 1976; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revis

2、ion, 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 This test method covers the determination of dissolved,total-recoverable, or total elements in drink

3、ing water, surfacewater, domestic, or industrial wastewaters.2, 31.2 It is the users responsibility to ensure the validity of thetest method for waters of untested matrices.1.3 Table 1 lists elements for which this test method applies,with recommended wavelengths and typical estimated instru-mental

4、detection limits using conventional pneumatic nebuli-zation.4Actual working detection limits are sample dependentand as the sample matrix varies, these detection limits may alsovary. In time, other elements may be added as more informa-tion becomes available and as required.1.4 This standard does no

5、t purport to address all of thesafety concerns, if any, associated with its use. It is theresponsibility of the user of this standard to establish appro-priate safety and health practices and determine the applica-bility of regulatory limitations prior to use. For specific hazardstatements, see Note

6、 2 and Section 9.2. Referenced Documents2.1 ASTM Standards:5D 1066 Practice for Sampling SteamD 1129 Terminology Relating to WaterD 1192 Guide for Equipment for Sampling Water andSteam in Closed Conduits6D 1193 Specification for Reagent WaterD 2777 Practice for Determination of Precision and Bias of

7、Applicable Test Methods of Committee D19 on WaterD 3370 Practices for Sampling Water from Closed ConduitsD 4841 Practice for Estimation of Holding Time for WaterSamples Containing Organic and Inorganic ConstituentsD 5810 Guide for Spiking into Aqueous SamplesD 5847 Practice for Writing Quality Contr

8、ol Specificationsfor Standard Test Methods for Water Analysis3. Terminology3.1 Definitions of Terms Specific to This Standard:1This test method is under the jurisdiction of ASTM Committee D19 on Waterand is the direct responsibility of Subcommittee D19.05 on Inorganic Constituentsin Water.Current ed

9、ition approved Aug. 1, 2007. Published August 2007. Originallyapproved in 1991. Last previous edition approved in 2002 as D 1976 02.2The detailed report of EPA Method Study 27, Method 200.7 is available fromthe National Technical Information Service, 5285 Port Royal Road, Springfield, VA.A summary o

10、f the project is available from the U.S. Environmental ProtectionAgency, Environmental Monitoring and Support Laboratory, Cincinnati, OH.3Fishman, M. J. and Friedman, L., “Methods for Determination of InorganicSubstances in Water and Fluvial Sediments”, U.S. Geological Survey Techniques ofWater-Reso

11、urces Investigations, Book 5, Chapter , Open File Report 85-495, 1985,p. 659671.4Winge, R. K., Fassel, V. A., Peterson, V. J. and Floyd, M. A.,“ InductivelyCoupled Plasma-Atomic Emission Spectroscopy,” An Atlas of Spectral Information,Elsevier Science Publishing Co., Inc., New York, NY, 1985.5For re

12、ferenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.6Withdrawn.TABLE 1 Suggested Wavelengths and EstimatedDetection Limi

13、ts4Element Wavelength, nmAEstimated detection limit,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 202.03

14、0 8Nickel 231.604 15Selenium 196.026 75Silver 328.068 7Thallium 190.864 40Vanadium 292.402 8Zinc 213.856 2AThe wavelengths listed are recommended because of their sensitivity andoverall acceptance. Other wavelengths may be substituted if they can provide theneeded sensitivity and are treated with th

15、e same corrective techniques for spectralinterference (see 6.1.1).BThe 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-depe

16、ndent and may vary as the sample matrix varies (see 3.1.4).1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.3.1.1 calibration blank, na volume of water containingthe same acid matrix as the calibration standards (see 11.1).3.1.2 calib

17、ration standards, na series of known standardsolutions 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 througha 0.45 m membrane filter.3.1.4 instrumental detection limit, nthe concentrationequival

18、ent to a signal, due to the analyte, that is equal to threetimes the standard deviation of a series of ten replicatemeasures of a reagent blank signal at the same wavelength.3.1.5 reagent blank, na volume of water containing thesame matrix as the calibration standards, carried through theentire anal

19、ytical procedure.3.1.6 total, nthe concentration determined on an unfil-tered sample following vigorous digestion (see 12.3).3.1.7 total-recoverable, adja term relating to forms ofeach element that are determinable by the digestion methodthat is included in this procedure (see 12.2).3.1.8 laboratory

20、 control sample, na solution with thecertified concentration(s) of the analytes.3.2 DefinitionsFor definitions of other terms used in thistest method, refer to Terminology D 1129.4. Summary of Test Method4.1 Elements are determined, either sequentially or simul-taneously, by inductively-coupled argo

21、n plasma optical emis-sion spectroscopy.4.2 A background correction technique may be used tocompensate for variable background contribution from highconcentrations of major and trace elements.5. Significance and Use5.1 This test method is useful for the determination ofelement concentrations in many

22、 natural waters and wastewa-ters. It has the capability for the simultaneous determination ofup to 20 elements. High sensitivity analysis can be achieved forsome elements that are difficult to determine by other tech-niques such as Flame Atomic Absorption.6. Interferences6.1 Several types of interfe

23、rence effects may contribute toinaccuracies in the determination of trace elements. Theseinterferences can be summarized as follows:6.1.1 Spectral interferences can be categorized as (1) over-lap of a spectral line from another element; (2) unresolvedoverlap of molecular band spectra; (3) background

24、 contributionfrom continuous or recombination phenomena; and (4) back-ground contribution from stray light from line emission of highconcentration elements.6.1.1.1 The effects described in 6.1.1 can be compensatedfor by utilizing a computer correction of the raw data, requiringthe monitoring and mea

25、surement of the interfering element.The second effect may require selection of an alternate wave-length. The third and fourth effects can usually be compensatedfor by a background correction adjacent to the analyte line.6.1.1.2 Table 2 lists some interference effects for the rec-ommended wavelengths

26、 given in Table 1. The data in Table 2are intended for use only as a rudimentary guide for theindication of potential spectral interferences. For this purpose,linear relations between concentration and intensity for theanalytes and the interferents can be assumed.6.1.1.3 Only those interferents list

27、ed in Table 2 were inves-tigated. The blank spaces in Table 2 indicate that measurableinterferences were not observed for the interferent concentra-tions listed in Table 3. Generally, interferences were consideredas discernible if the interferent produced interference peaks orbackground shifts that

28、corresponded to 2 to 5 % of the peaksgenerated by the analyte concentrations also listed in Table 3.TABLE 2 Analyte Concentration Equivalents, mg/L, Arising from Interferents at the 100 mg/L LevelAAnalyte Wavelength, nmInterferentAl Ca Cr Cu Fe Mg Mn Ni Ti VAluminum 308.215 . . . . . . 0.21 . . 1.4A

29、ntimony 206.833 0.47 . 2.9 . 0.08 . . . 0.25 0.45Arsenic 193.696 1.3 . 0.44 . . . . . . 1.1Barium 455.403 . . . . . . . . . .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 0.0

30、3Chromium 267.716 . . . . 0.003 . 0.04 . . 0.04Cobalt 228.616 . . 0.03 . 0.005 . . 0.03 0.15 .Copper 324.754 . . . . 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

31、 . 0.002 . . . . .Molybdenum 202.030 0.05 . . . 0.03 . . . . .Nickel 231.604 . . . . . . . . . .Selenium 196.026 0.23 . . . 0.09 . . . . .Silicon 288.158 . . 0.07 . . . . . . 0.01Sodium 588.995 . . . . . . . . 0.08 .Thallium 190.864 0.30 . . . . . . . . .VanadiumZinc292.402213.856.0.05.0.140.005.0.2

32、90.02.ASee Table 3 for concentrations used.D 1976 0726.1.2 Physical interferences are generally considered to beeffects associated with the sample nebulization and transportprocesses. Such properties as change in viscosity and surfacetension can cause significant inaccuracies, especially insamples t

33、hat may contain high dissolved solids or acid con-centrations, or both. The use of a peristaltic pump may lessenthese interferences. If these types of interferences are opera-tive, they must be reduced by dilution of these samples orutilization of standard addition techniques, or both.6.1.2.1 Salt b

34、uildup at the tip of the nebulizer is anotherproblem that can occur from high dissolved solids. This saltbuildup affects aerosol flow rate that can cause instrumentaldrift. To control this problem, wet the argon prior to nebuliza-tion, use a tip washer, or dilute the sample.NOTE 1Periodic inspection

35、 and cleaning of the nebulizer and torchcomponents are highly recommended.6.1.2.2 Reports indicate that better control of the argon flowrate improves instrument performance. This control of theargon flow rate can be accomplished with the use of mass flowcontrollers.6.1.3 Chemical interferences are c

36、haracterized by molecularcompound formation, ionization effects, and solute vaporiza-tion effects. Normally these effects are not pronounced with theICPtechnique; however, if observed, they can be minimized bycareful selection of operating conditions (incident power,plasma observation position, and

37、so forth), by buffering thesample, by matrix matching, and by standard addition proce-dures. These types of interferences can be highly dependent onmatrix type and the specific analyte.7. Apparatus7.1 See the manufacturers instruction manual for installa-tion and operation of inductively-coupled arg

38、on plasma spec-trometers.8. Reagents and Materials8.1 Purity of ReagentsReagent grade chemicals shall beused in all tests. Unless otherwise indicated, it is intended thatreagents shall conform to the specifications of the Committeeon Analytical Reagents of the American Chemical Society.7The high sen

39、sitivity of inductively-coupled argon plasmaatomic emission spectrometry may require reagents of higherpurity. Stock standard solutions are prepared from high puritymetals, oxides, or nonhydroscopic reagent grade salts usingTypes I, II, and III reagent water, and ultrapure acids. Othergrades may be

40、used, provided it is first ascertained that thereagent is of sufficient purity to permit its use without lesseningthe accuracy of the determination.8.2 Purity of WaterUnless otherwise indicated, referenceto water shall be understood to mean reagent water conformingto Type I, II, or III of Specificat

41、ion D 1193. It is the analystsresponsibility to assure that water is free of interferences. Otherreagent water types may be used provided it is first ascertainedthat the water is of sufficiently high purity to permit its usewithout adversely affecting the precision and bias of the testmethod. Type I

42、I water was specified at the time of round robintesting of this test method.8.3 Aqua RegiaMix three parts hydrochloric acid (sp gr1.19) and one part concentrated nitric acid (sp gr 1.42) justbefore use.NOTE 2Exercise caution when mixing this reagent.8.4 ArgonWelding grade equivalent or better.8.5 Hy

43、drochloric Acid (sp gr 1.19)Concentrated hydro-chloric acid, ultrapure or equivalent.8.6 Hydrochloric Acid (1 + 1)Add 1 vol of hydrochloricacid (sp gr 1.19) to 1 vol of water.8.7 Nitric Acid (sp gr 1.42)Concentrated nitric acid,ultrapure or equivalent.8.8 Nitric Acid (1 + 1)Add 1 vol of nitric acid

44、(sp gr 1.42)to 1 vol of water.8.9 Nitric Acid (1 + 499)Add 1 vol of nitric acid (sp gr1.42) to 499 vol of water.8.10 Stock SolutionsPreparation of stock solutions foreach element is listed in Table 4.8.11 Mixed Calibration Standard SolutionsPrepare mixedcalibration standard solutions by combining ap

45、propriate vol-umes of the stock solutions in volumetric flasks (see Note 3).Prior to preparing mixed standards, each stock solution shouldbe analyzed separately to determine possible spectral interfer-ence or the presence of impurities. Care should be taken whenpreparing the mixed standards to ensur

46、e the elements arecompatible and stable.NOTE 3Mixed calibration standards will vary depending on thenumber of elements being determined. An example of mixed calibrationstandards for the simultaneous determination of 20 elements is as follows:7Reagent Chemicals, American Chemical Society Specificatio

47、ns, AmericanChemical Society, Washington, DC. For suggestions on the testing of reagents notlisted by the American Chemical Society, see Analar Standards for LaboratoryChemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeiaand National Formulary, U.S. Pharmacopeial Convention, I

48、nc. (USPC), Rockville,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 10V1Zn 10AThis table in

49、dicates concentrations used for interference measurements inTable 2.D 1976 073Mixed Standard Solution Imanganese, beryllium, cadmium, lead, and zincMixed Standard Solution IIcopper, vanadium, iron, and cobaltMixed Standard Solution IIImolybdenum, arsenic, and seleniumMixed Standard Solution IValuminum, chromium, and nickelMixed Standard Solution Vantimony, boron, magnesium, silver, and thallium8.12 Reagent BlankThis must contain all the reagents andbe the same volume as used in the processing of the samples.The reagent blank must be car