1、Designation: D 4190 08Standard Test Method forElements in Water by Direct-Current Plasma AtomicEmission Spectroscopy1This standard is issued under the fixed designation D 4190; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the ye
2、ar 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.This standard has been approved for use by agencies of the Department of Defense.1. Scope1.1 This test method covers the det
3、ermination of dissolvedand total recoverable elements in water, which includes drink-ing water, lake water, river water, sea water, snow, and Type IIreagent water by direct current plasma atomic emission spec-troscopy (DCP).1.2 The information on precision and bias may not apply toother waters.1.3 T
4、his test method is applicable to the 15 elements listedin Annex A1 (Table A1.1) and covers the ranges in Table 1.1.4 This test method is not applicable to brines unless thesample matrix can be matched or the sample can be diluted bya factor of 200 up to 500 and still maintain the analyteconcentratio
5、n above the detection limit.1.5 The values stated in SI units are to be regarded asstandard. No other units of measurement are included in thisstandard.1.6 This standard does not purport to address all of thesafety concerns, if any, associated with its use. It is theresponsibility of the user of thi
6、s standard to establish appro-priate safety and health practices and determine the applica-bility of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:2D 1066 Practice for Sampling SteamD 1129 Terminology Relating to WaterD 1193 Specification for Reagent WaterD 2777 Pract
7、ice for Determination of Precision and Bias ofApplicable 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 Sa
8、mplesD 5847 Practice for Writing Quality Control Specificationsfor Standard Test Methods for Water AnalysisE 1097 Guide for Direct Current Plasma-Atomic EmissionSpectrometry Analysis3. Terminology3.1 Definitions For definitions of terms used in this testmethod, refer to Terminology D 1129.3.2 Defini
9、tions of Terms Specific to This Standard:3.2.1 LCS, nlaboratory control standard.3.2.2 total recoverable element, na term relating to formsof each element that are determinable by the digestion methodthat is included in this test method.4. Summary of Test Method4.1 Elements are determined, either se
10、quentially or simul-taneously, by DCP.4.2 Matrix enhancement or suppression of the emissionsignal can be minimized by the addition of 2000 mg/L oflithium ion to all standards, samples, and blanks.4.3 Dissolved elements are determined by atomizing afiltered and acidified sample directly with no pretr
11、eatment.4.4 If the sample is clear, total recoverable elements aredetermined in the same manner as dissolved elements exceptthat sample is unfiltered and acidified.1This test method is under the jurisdiction of ASTM Committee D19 on Waterand is the direct responsibility of Subcommittee D19.05 on Ino
12、rganic Constituentsin Water.Current edition approved Oct. 1, 2008. Published October 2008. Originallyapproved in 1982. Last previous edition approved in 2003 as D 4190 03.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Ann
13、ual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.TABLE 1 Solutions for AnalysisElement PSolutions for Analysis, g/L123Al 50 100 190Be 50 500 1000B 50 500 1000Cd 1000 50 500Cr 500 1000 50Co 50 500 1000Cu 1000 50 500Fe 500 1000 50Pb 500 200
14、1000Mn 800 50 300Hg 500 1000 200Ni 50 300 800Sr 600 50 300V 1000 50 400Zn 500 1000 501Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.4.5 If there are large particles (non-colloidal) the totalrecoverable elements are determined on a p
15、ortion of the sampleafter a hydrochloric-nitric acid digestion (12.2-12.5). The samedigestion procedure is used to determine all total recoverableelements in this test method.NOTE 1The volatility of mercury3,4compounds, especially the chlo-rides, makes it necessary to use considerable care in digest
16、ing samplescontaining these elements. The samples must not be boiled unlessprovision is made to prevent loss by volatilization.5. Significance and Use5.1 This test method is useful for the determination ofelement concentrations in many natural waters. It has thecapability for the simultaneous determ
17、ination of up to 15separate elements. High analysis sensitivity can be achievedfor some elements, such as boron and vanadium.6. Interferences6.1 For commonly occurring matrix elements the followingspectral interferences have been observed:6.1.1 Calcium, magnesium, and boron interfere with lead at405
18、.78 nm.6.1.2 Calcium interferes with chromium at 425.43 nm.6.1.3 Magnesium interferes with cadmium at 214.44 nm.6.1.4 Iron interferes with cobalt at 345.35 and 240.73 nm.6.1.5 Cobalt interferes with nickel at 341.48 nm.NOTE 2The exact magnitude of these interferences has not beendetermined since it
19、depends on the concentration of the calibrationstandards used and the sample matrix.6.2 Some additional possible interferences are listed inAnnexA2 (TableA2.1) so that the analyst may be aware of andtest for them.7. Apparatus7.1 See the manufacturers instruction manual for installa-tion and operatio
20、n of DCP spectrometers, refer to GuideE 1097 for information on DCP spectrometers.8. Reagents8.1 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
21、the American Chemical Society5where such specifications are available. Other grades may beused, provided it is first ascertained that the reagent is ofsufficient purity to permit its use without lessening the accu-racy of the determination.8.2 Purity of Water Unless otherwise indicated, referenceto
22、water shall be understood to mean reagent water conformingto Type I of Specification D 1193. Other reagent water typesmay be used, provided it is first ascertained that the water is ofsufficiently high purity to permit its use without lessening thebias and precision of the determination. Type II wat
23、er wasspecified at the time of round robin testing of this test method.8.3 Stock Solutions Preparation of stock solutions foreach element is listed in Annex A3 (Table A3.1)orusecommercially available, ICP Grade, stock standards.8.4 High Purity Hydrochloric Acid, (HCl), (sp gr 1.19),concentrated hydr
24、ochloric acid.8.5 Hydrochloric Acid, (1 + 1) Add one volume of HCl(sp gr 1.19) to one volume of water.8.6 Lithium Carbonate, ultrapure.8.7 Lithium Solution (40 000 mg/L)Dissolve 213 g ofultrapure lithium carbonate in a minimum amount of HCl (spgr 1.19) and dilute to 1 L with water.8.8 Concentrated N
25、itric Acid, (HNO3), (sp gr 1.42)High-purity acid can be prepared by distillation of concentrated nitricacid from a sub-boiling quartz still or it can be commerciallypurchased.8.9 Dilute Nitric Acid, (1+1)Add one volume of HNO3(sp. gr. 1.42) to one volume of water.8.10 Dilute Nitric Acid, (1 + 499) A
26、dd one volume ofHNO3(sp gr 1.42) to 499 volumes of water.NOTE 3If a high reagent blank is obtained on either HNO3or HCl,distill the acid or use high purity acid. When HCl is distilled, an azeotropicmixture is obtained (approximately 6 N HCl); therefore, wheneverconcentrated HCl is specified in the p
27、reparation of a reagent or in theprocedure, use double the amount if distilled acid is used.9. Precautions9.1 Emission intensities are affected by changing viscosityso it is important to control the viscosity of blanks, standards,and samples within reasonable limits. Reagent water standardsshould no
28、t be used to analyze oil field brines. Alternatively,matrix matching or the method of additions can be used.9.2 Organic solvents, such as alcohol, acetone, and methylethyl ketone have been observed to enhance emission intensity.This enhancement effect must be compensated for whenorganic solvents are
29、 known to be present. Alternatively, matrixmatching or the method of additions can be used.10. Sampling10.1 Collect the samples in accordance with the applicablestandards, Practice D 1066 or Practices D 3370.10.2 Preserve the samples by immediately adding highpurity nitric acid to adjust the pH to t
30、wo at the time ofcollection. Normally 2 mL of HNO3is required per liter ofsample. If only dissolved elements are to be determined, (Note4) filter the sample through a 0.45 m membrane filter beforeacidification. The holding time for the sample may be calcu-lated in accordance with Practice D 4841.NOT
31、E 4Depending on the manufacturer, these filters have been foundto be contaminated to various degrees with heavy metals. Care should beexercised in selecting a source of these filters. A good practice is to washthe filters with nitric acid and reagent water before filtering a sample.3Standard Methods
32、 of Chemical Analysis, Editor, N. H. Furman, Vol 1, SixthEdition, pp. 107 and 657.4Smith, G. F., The Wet Chemical Oxidation of Organic Compositions, The G.Frederick Smith Chemical Co., 1965.5Reagent Chemicals, American Chemical Society Specifications, AmericanChemical Society, Washington, DC. For Su
33、ggestions on the testing of reagents notlisted by the American Chemical Society, see Annual Standards for LaboratoryChemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeiaand National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,MD.D419008211. Calibration and
34、 Standardization11.1 Prepare 100 mL of a blank and at least four standardsolutions to bracket the expected concentration range of thesamples to be analyzed by diluting 5.0 mL of lithium solution(see 8.7) and an appropriate volume of stock solution withHNO3(1 + 499). Prepare the blank and standards e
35、ach time thetest is to be run.11.2 Atomize the blank and standards and record the emis-sion intensity or concentration. Atomize HNO3(1 + 499)between each standard.11.3 Using the instrument software verify that the instru-ment calibration is within user acceptable QC limits.12. Procedure12.1 To deter
36、mine dissolved elements, add 5.0 mL oflithium solution (see 8.7) to a 100.0 mL volumetric flask andbring to volume with the well-mixed acidified sample. Proceedwith 12.6.12.2 When determining total recoverable elements in solu-tions containing suspended matter or large particles (that is,noncolloida
37、l), add 5.0 mL of HNO3(sp. gr. 1.42) and 5.0 mLof lithium solution to a 100.0-mL sample.NOTE 5When digestion is necessary, subject the standards, sample,and blank to the same procedure.12.3 Add 5.0 mL of HCl (sp. gr. 1.19) to each sample.12.4 Heat the samples in a covered beaker on a steam bathor ho
38、t plate until the volume has been reduced to 15 or 20 mL.Take care to see that the samples do not boil. Loss of samplecould result from bumping or spattering.NOTE 6For samples with high levels of dissolved solids, the amountof reduction in volume is left to the discretion of the analyst.12.5 Cool an
39、d filter the samples, if necessary, through a fineashless filter paper into 100.0 mL volumetric flasks. Wash thefilter paper three times with water and adjust to volume.12.6 Atomize each solution and record its emission intensityor concentration. Atomize HNO3(1 + 499) between samples.13. Calculation
40、13.1 Calculate the concentration of elements in eachsample, in mg/L, using the calibrations established in 11.3.Modern DCP instruments will provide the results in thecalibrated concentration units.13.2 Multiply the results for dissolved elements by thedilution factor of 1.05 to correct for the requi
41、red addition oflithium solution (12.1).14. Precision and Bias614.1 To facilitate handling and distribution for round robintesting, three concentrated solutions were prepared. These wereacidified solutions of 15 elements.14.2 The concentrated solutions, when diluted according todirections, yielded so
42、lutions for analysis with the compositionas shown in Table 1. A total of eight laboratories and thirteenoperators participated in this study.14.2.1 Type II water was specified at the time of round robintesting of this test method.14.3 PrecisionThe precision of this test method for theelements tested
43、 within their respective ranges of concentrationgiven in Table 1 may be expressed as given in Table 2.14.4 BiasSee Table 3.14.5 This section on precision and bias conforms to PracticeD 2777 77 which was in place at the time of collaborativetesting. Under the allowances made in 1.4 of PracticeD 2777
44、06, these precision and bias data do meet existingrequirements of interlaboratory studies of Committee D19 testmethods.15. Quality Control (QC)15.1 In order to be certain that analytical values obtainedusing these test methods are valid and accurate within theconfidence limits of the test, the follo
45、wing QC procedures mustbe followed when analyzing each element.15.2 Calibration and Calibration Verification15.2.1 Analyze at least four working standards containingconcentrations of each element that bracket the expectedsample concentration, prior to analysis of samples, to calibratethe instrument.
46、 The calibration correlation coefficient shall beequal to or greater than 0.990. In addition to the initialcalibration blank, a calibration blank shall be analyzed at theend of the batch run to ensure contamination was not a problemduring the batch analysis.15.2.2 Verify instrument calibration after
47、 standardization byanalyzing a standard at the concentration of one of the6Supporting data have been filed at ASTM International Headquarters and maybe obtained by requesting Research Report RR: D191079.TABLE 2 PrecisionElement Reagent Water Water of ChoiceAl ST= 0.093X 0.301 ST= 0.108X + 0.424SO= 0
48、.051X + 0.497 SO= 0.044X + 3.18Be ST= 0.066X + 0.354 ST= 0.059X + 2.15SO= 0.025X 0.250 SO= 0.042X 1.43B ST= 0.045X + 9.34 ST= 0.045X + 2.87SO= 0.022X + 3.70 SO= 0.021X + 5.12Cd ST= 0.044X + 6.08 ST= 0.066X + 2.99SO= 0.025X + 4.96 SO= 0.037X + 7.99Cr ST= 0.060X + 2.13 ST= 0.038X + 4.56SO= 0.032X + 1.
49、20 SO= 0.027X + 3.86Co ST= 0.062X + 4.59 ST= 0.085X + 9.55SO= 0.032X + 4.11 SO= 0.040X + 3.99Cu ST= 0.038X + 5.58 ST= 0.049X + 2.75SO= 0.031X + 0.956 SO= 0.039X + 0.644Fe ST= 0.051X + 14.3 ST= 0.053X + 15.7SO= 0.013X + 10.7 SO= 0.034X + 12.2Pb ST= 0.038X + 9.69 ST= 0.037X + 18.3SO= 0.027X + 5.36 SO= 0.016X + 20.7Mn ST= 0.058X + 2.35 ST= 0.034X + 1.98SO= 0.023X + 3.30 SO= 0.018X + 3.79Hg ST= 0.008X + 22.3 ST= 0.009X + 28.0SO= 0.003X + 14.7 SO= 0.009X + 23.7Ni ST= 0.078X + 5.47 ST= 0.088X + 3.38SO= 0.029X + 7.17 SO= 0.039X 5.54Sr ST= 0.073X + 1.47 ST= 0.0
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