1、Designation: D 5673 05Standard Test Method forElements in Water by Inductively Coupled PlasmaMassSpectrometry1This standard is issued under the fixed designation D 5673; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of l
2、ast 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. Scope*1.1 This test method covers the determination of dissolvedelements in ground water, surface water, and drinking water. It
3、may also be used for the determination of total-recoverableelements in these waters as well as wastewater.21.2 This test method should be used by analysts experiencedin the use of inductively coupled plasmamass spectrometry(ICP-MS), the interpretation of spectral and matrix interfer-ences and proced
4、ures for their correction.1.3 It is the users responsibility to ensure the validity of thetest method for waters of untested matrices.1.4 Table 1 lists elements for which the test method applies,with recommended masses and typical estimated instrumentaldetection limits using conventional pneumatic n
5、ebulization.Actual working detection limits are sample dependent and, asthe sample matrix varies, these detection limits may also vary.In time, other elements may be added as more informationbecomes available and as required.1.4.1 This method covers the analysis of mine dewateringgroundwater and was
6、tewater effluent in the range of 2120g/L dissolved antimony and 3200 g/L dissolved arsenic.1.5 This standard does not 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 practi
7、ces and determine the applica-bility of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:3D 1066 Practice for Sampling SteamD 1129 Terminology Relating to WaterD 1192 Specification for Equipment for Sampling Waterand Steam in Closed Conduits4D 1193 Specification for Reag
8、ent WaterD 2777 Practice for Determination of Precision and Bias ofApplicable Methods of Committee D19 on WaterD 3370 Practices for Sampling Water from Closed ConduitsD 5810 Guide for Spiking into Aqueous SamplesD 5847 Practice for the Writing Quality Control Specifica-tions for Standard Test Method
9、s for Water AnalysisE 691 Practice for Conducting an Interlaboratory Study toDetermine the Precision of a Test MethodE 1601 Practice for Conducting an Interlaboratory Study toEvaluate the Performance of an Analytical MethodE 1763 Guide for Interpretation and Use of Results fromInterlaboratory Testin
10、g of Chemical Analysis Methods3. Terminology3.1 DefinitionsFor definitions of other terms used in thistest method, refer to Terminology D 1129.3.2 Definitions of Terms Specific to This Standard:1This test method is under the jurisdiction of ASTM Committee D19 on Waterand is the direct responsibility
11、 of Subcommittee D19.05 on Inorganic Constituentsin Water.Current edition approved July 1, 2005. Published July 2005. Originally approvedin 1996. Last previous edition approved in 2003 as D 567303.2EPA Test Method: Determination of Trace Elements in Waters and Wastes byInductively Coupled PlasmaMass
12、 Spectrometry, Method 200.8.3For referenced 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.4Withdrawn.TABLE 1 Recommended An
13、alytical Mass and EstimatedInstrument Detection LimitsElementRecommendedAnalytical MassEstimated InstrumentDetection Limit, g/LAAluminum 27 0.05Antimony 121 0.08Arsenic 75 0.9Barium 137 0.5Beryllium 9 0.1Cadmium 111 0.1Chromium 52 0.07Cobalt 59 0.03Copper 63 0.03Lead 206, 207, 208 0.08Manganese 55 0
14、.1Molybdenum 98 0.1Nickel 60 0.2Selenium 82 5.0Silver 107 0.05Thallium 205 0.09Thorium 232 0.03Uranium 238 0.02Vanadium 51 0.02Zinc 66 0.2AInstrument detection limits (3s) estimated from seven replicate scans of theblank (1 % v/v HNO3) and three replicate integrations of a multi-element standard.1*A
15、 Summary of Changes section appears at the end of this standard.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.3.2.1 calibration blanka volume of water containing thesame acid matrix as the calibration standards (see 11.1).3.2.2 cali
16、bration standardsa series of known standardsolutions used by the analyst for calibration of the instrument(that is, preparation of the analytical curve) (see Section 11).3.2.3 calibration stock solutiona solution prepared fromthe stock standard solution(s) to verify the instrument responsewith respe
17、ct to analyte concentration.3.2.4 dissolvedthose elements that will pass through a0.45-m membrane filter.3.2.5 interference check sample (ICSA)a solution contain-ing matrix elements at environmental levels that result ininterferences on target low level analytes. The interferencesformed in the ICP c
18、an be corrected for by use of element-specific correction equations or collision cell technology withquadrupole-based ICP-MS, or high resolution ICP-MS.3.2.6 interference check sample (ICSAB)the ICSA solu-tion spiked with 20 g/L As and Sb.3.2.7 instrumental detection limit (IDL)the concentrationequi
19、valent to a signal, which is equal to three times thestandard deviation of the blank signal at the selected analyticalmass(es).3.2.8 internal standardpure analyte(s) added in knownamount(s) to a solution. This is used to measure the relativeinstrument response to the other analytes that are componen
20、tsof the same solution. The internal standards must be analytesthat are not a sample component.3.2.9 method detection limit (MDL)the minimum concen-tration of an analyte that can be identified, measured andreported with 99 % confidence that the analyte concentration isgreater than zero. This confide
21、nce level is determined fromanalysis of a sample in a given matrix containing the ana-lyte(s).3.2.10 quality control reference solution (QCS)a solutionwith the certified concentration(s) of the analytes, prepared byan independent laboratory, and used for a verification of theinstruments calibration.
22、3.2.11 reagent blanka volume of water containing thesame matrix as the calibration standards, carried through theentire analytical procedure.3.2.12 total-recoverablea term relating to forms of eachelement that are determinable by the digestion method includedin this procedure (see 12.2).3.2.13 tunin
23、g solutiona solution that is used to determineacceptable instrument performance prior to calibration andsample analysis.4. Summary of Test Method4.1 This test method describes the multi-element determi-nation of trace elements by inductively coupled plasmamassspectrometry (ICP-MS). Sample material i
24、n solution is intro-duced by pneumatic nebulization into a radiofrequency plasmawhere energy transfer processes cause desolvation, atomiza-tion, and ionization. The ions are extracted from the plasmathrough a differentially pumped vacuum interface and sepa-rated on the basis of their mass-to-charge
25、ratio by a quadrupolemass spectrometer. The ions transmitted through the quadru-pole are detected by a continuous dynode electron multiplierassembly and the ion information processed by a data handlingsystem. Interferences relating to the technique must be recog-nized and corrected for (see Section
26、7 on interferences). Suchcorrections must include compensation for isobaric elementalinterferences and interferences from polyatomic ions derivedfrom the plasma gas, reagents, or sample matrix. Instrumentaldrift as well as suppressions or enhancements of instrumentresponse caused by the sample matri
27、x must be corrected for bythe use of internal standardization.5. Significance and Use5.1 The test method is useful for the determination ofelement concentrations in many natural waters and wastewa-ters. It has the capability for the determination of up to 20elements. High analysis sensitivity can be
28、 achieved for someelements that are difficult to determine by other techniques.6. Interferences6.1 Several types of interference effects may contribute toinaccuracies in the determination of trace elements. Theseinterferences can be summarized as follows:6.1.1 Isobaric Elemental InterferencesIsobari
29、c elementalinterferences are caused by isotopes of different elementswhich form singly or doubly charged ions of the same nominalmass-to-charge ratio and which cannot be resolved by the massspectrometer in use. All elements determined by this testmethod have, at a minimum, one isotope free of isobar
30、icelemental interference. Of the analytical isotopes recom-mended for use with this test method (see Table 2), onlymolybdenum-98 (ruthenium) and selenium-82 (krypton) haveisobaric elemental interferences. If alternative analytical iso-topes having higher natural abundance are selected in order toach
31、ieve greater sensitivity, an isobaric interference may occur.All data obtained under such conditions must be corrected bymeasuring the signal from another isotope of the interferingTABLE 2 Recommended Analytical Isotopes and AdditionalMasses That Are Recommended To Be MonitoredIsotopeAElement of Int
32、erest27 Aluminum121, 123 Antimony75 Arsenic135, 137 Barium9 Beryllium106, 108, 111, 114 Cadmium52, 53 Chromium59 Cobalt63, 65 Copper206, 207, 208 Lead55 Manganese95, 97,98 Molybdenum60, 62 Nickel77, 82 Selenium107, 109 Silver203, 205 Thallium232 Thorium238 Uranium51 Vanadium66, 67, 68 Zinc83 Krypton
33、99 Ruthenium105 Palladium118 TinAIsotopes recommended for analytical determination are underlined. Thesemasses were recommended and are reflected in the precision and bias data.Alternate masses may be used but interferences must be documented.D 5673 052element and subtracting the appropriate signal
34、ratio from theisotope of interest. A record of this correction process shouldbe included with the report of the data. It should be noted thatsuch corrections will only be as accurate as the accuracy of theisotope ratio used in the elemental equation for data calcula-tions. Relevant isotope ratios an
35、d instrument bias factorsshould be established prior to the application of any correc-tions.6.1.2 Abundance SensitivityAbundance sensitivity is aproperty defining the degree to which the wings of a mass peakcontribute to adjacent masses. The abundance sensitivity isaffected by ion energy and quadrup
36、ole operating pressure.Wing overlap interferences may result when a small ion peakis being measured adjacent to a large one. The potential forthese interferences should be recognized and the spectrometerresolution adjusted to minimize them.6.1.3 Isobaric Polyatomic Ion InterferencesIsobaric poly-ato
37、mic ion interferences are caused by ions consisting of morethan one atom that have the same nominal mass-to-charge ratioas the isotope of interest, and which cannot be resolved by themass spectrometer in use. These ions are commonly formed inthe plasma or interface system from support gases or sampl
38、ecomponents. Most of the common interferences have beenidentified, and these are listed in Table 3 together with themethod elements affected. Such interferences must be recog-nized, and when they cannot be avoided by the selection of analternative analytical isotope, appropriate corrections must bem
39、ade to the data. Equations for the correction of data should beestablished at the time of the analytical run sequence as thepolyatomic ion interferences will be highly dependent on thesample matrix and chosen instrument conditions.6.1.4 Physical InterferencesPhysical interferences are as-sociated wi
40、th the physical processes that govern the transportof the sample into the plasma, sample conversion processes inthe plasma, and the transmission of ions through the plasmamass spectrometer interface. These interferences may result indifferences between instrument responses for the sample andthe cali
41、bration standards. Physical interferences may occur inthe transfer of solution to the nebulizer (for example, viscosityeffects), at the point of aerosol formation and transport to theplasma (for example, surface tension), or during excitation andionization processes within the plasma itself. High le
42、vels ofdissolved solids in the sample may contribute deposits ofmaterial on the extraction, or skimmer cones, or both, reducingthe effective diameter of the orifices and, therefore, iontransmission. Dissolved solids levels not exceeding 0.2 %(w/v) have been recommended to reduce such effects. Intern
43、alstandardization may be effectively used to compensate formany physical interference effects. Internal standards shouldhave similar analytical behavior to the elements being deter-mined.6.1.5 Memory InterferencesMemory interferences resultwhen isotopes of elements in a previous sample contribute to
44、the signals measured in a new sample. Memory effects canresult from sample deposition on the sampler and skimmercones, and from the buildup of sample material in the plasmatorch and spray chamber. The site where these effects occur isdependent on the element and can be minimized by flushing thesyste
45、m with a rinse blank consisting of HNO3(1+49) in waterbetween samples. The possibility of memory interferencesshould be recognized within an analytical run and suitable rinsetimes should be used to reduce them. The rinse times necessaryfor a particular element should be estimated prior to analysis.T
46、his may be achieved by aspirating a standard containingelements corresponding to ten times the upper end of the linearrange for a normal sample analysis period, followed byTABLE 3 Common Molecular Ion InterferencesBackground Molecular IonsMolecular Ion Mass Element InterferenceANH+15 .OH+17 .OH2+18
47、.C2+24 .CN+26 .CO+28 .N2+28 .N2H+29 .NO+30 .NOH+31 .O2+32 .O2H+33 .36ArH+37 .36ArH+39 .40ArH+41 .CO2+44 .CO2H+45 ScArC+,ArO+52 CrArN+54 CrArNH+55 MnArO+56 .ArOH+57 .40Ar36Ar+76 Se40Ar38Ar+78 Se40Ar2+80 SeMatrix Molecular IonsChloride35ClO+51 V35ClOH+52 Cr37ClO+53 Cr37ClOH+54 CrAr35Cl+75 AsAr37Cl+77
48、SeSulphate32SO+48 .32SOH+49 .34SO+50 V, Cr34SOH+51 VSO2+,S2+64 ZnAr32S+72 .Ar34S+74 .PhosphatePO+47 .POH+48 .PO2+63 CuArP+71 .Group I, II MetalsArNa+63 CuArK+79 .ArCa+80 .Matrix OxidesBTiO 62 to 66 Ni, Cu, ZnZrO 106 to 112 Ag, CdMoO 108 to 116 CdAMethod elements or internal standards affected by mol
49、ecular ions.BOxide interferences will normally be very small and will only impact the methodelements when present at relatively high concentrations. Some examples of matrixoxides are listed of which the analyst should be aware. It is recommended that Tiand Zr isotopes be monitored if samples are likely to contain high levels of theseelements. Mo is monitored as a method analyte.D 5673 053analysis of the rinse blank at designated intervals.The length oftime required to reduce analyte signals to within a factor of tenof the method detection limit shoul
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