1、Designation: D5673 15D5673 16Standard Test Method forElements in Water by Inductively Coupled PlasmaMassSpectrometry1This standard is issued under the fixed designation D5673; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the yea
2、r 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*1.1 This test method covers the determination of dissolved elements in ground water, surface water, and drinking wat
3、er. It mayalso be used for the determination of total-recoverable elements in these waters as well as wastewater.21.2 This test method should be used by analysts experienced in the use of inductively coupled plasmamass spectrometry(ICP-MS), the interpretation of spectral and matrix interferences and
4、 procedures for their correction.1.3 It is the users responsibility to ensure the validity of the test 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 pn
5、eumatic nebulization. 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.1.4.1 This method covers the analysis of mine dewatering groundw
6、ater and wastewater effluent in the range of 2120 g/Ldissolved antimony and 3200 g/L dissolved arsenic.1.4.2 This method covers the analysis of metallurgical processing cyanide solutions in the range of 1500 g/L dissolved gold.1.5 The values stated in SI units are to be regarded as standard. No othe
7、r units of measurement are included in this standard.1 This test method is under the jurisdiction ofASTM Committee D19 on Water and is the direct responsibility of Subcommittee D19.05 on Inorganic Constituents in Water.Current edition approved July 1, 2015Feb. 1, 2016. Published August 2015June 2016
8、. Originally approved in 1996. Last previous edition approved in 20102015 asD5673 10.D5673 15. DOI: 10.1520/D5673-15.10.1520/D5673-16.2 EPA Test Method: Determination of Trace Elements in Waters and Wastes by Inductively Coupled PlasmaMass Spectrometry, Method 200.8.TABLE 1 Recommended Analytical Ma
9、ss and EstimatedInstrument Detection LimitsElement RecommendedAnalytical Mass Estimated 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 0.03Gold 197 0.01Lead 206, 207, 208 0.08Manganese
10、55 0.1Molybdenum 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 0.2A Instrument detection limits (3) estimated from seven replicate scans of the blank(1 % v/v HNO3) and three replicate integrations of a multi-element standard
11、.This document is not an ASTM standard 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 ed
12、itions as appropriate. In all cases only 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 19428-29
13、59. United States11.6 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 safety and health practices and determine the applicability of regulatorylimitations prior to use
14、.2. Referenced Documents2.1 ASTM Standards:3D1066 Practice for Sampling SteamD1129 Terminology Relating to WaterD1193 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 Clos
15、ed ConduitsD5810 Guide for Spiking into Aqueous SamplesD5847 Practice for Writing Quality Control Specifications for Standard Test Methods for Water AnalysisE691 Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test MethodE1601 Practice for Conducting an Interlaborato
16、ry Study to Evaluate the Performance of an Analytical MethodE1763 Guide for Interpretation and Use of Results from Interlaboratory Testing of Chemical Analysis Methods (Withdrawn2015)43. Terminology3.1 Definitions:3.1.1 For definitions of terms used in this standard, refer to Terminology D1129.3.2 D
17、efinitions of Terms Specific to This Standard:3.2.1 calibration blank, na volume of water containing the same acid matrix as is in the calibration standards (see 11.1).3.2.2 calibration standards, na series of known standard solutions used by the analyst for calibration of the instrument (thatis, pr
18、eparation of the analytical curve) (see Section 11).3.2.3 calibration stock solution, na solution prepared from the stock standard solution(s) to verify the instrument responsewith respect to analyte concentration.3.2.4 dissolved, adjcapable of passing through a 0.45-m membrane filter.3.2.5 interfer
19、ence check sample A (ICSA), na solution containing matrix elements at environmental levels that result ininterferences on target low level analytes.3.2.5.1 DiscussionICSA is different from the mixed element standards in 8.48.5, which are intended for instrument calibration, not for checkinginterfere
20、nces. The interferences formed in the ICP can be corrected for by use of element-specific correction equations, collisioncell technology with quadrupole-based ICP-MS, or high-resolution ICP-MS.3.2.6 interference check sample B (ICSAB), nthe ICSA solution spiked with 20 g/L each As and Sb.3.2.7 instr
21、umental detection limit (IDL), nthe concentration equivalent to a signal, that is equal to three times the standarddeviation of the blank signal at the selected analytical mass(es).3.2.8 internal standard, npure element(s) added in known amount(s) to a solution.3.2.8.1 DiscussionThe internal standar
22、d is used to measure the instrument response relative to the other analytes that are components of the samesolution. The internal standards must be elements that are not a sample component.3.2.9 method detection limit (MDL), nthe minimum analyte concentration that can be identified, measured and rep
23、orted with99 % confidence that the analyte concentration is greater than zero.3.2.9.1 DiscussionThis confidence level is determined from analysis of a sample in a given matrix containing the analyte(s).3 For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Servi
24、ce at serviceastm.org. For Annual Book of ASTM Standardsvolume information, refer to the standards Document Summary page on the ASTM website.4 The last approved version of this historical standard is referenced on www.astm.org.D5673 1623.2.10 quality control reference solution (QCS), na solution wit
25、h the certified concentration(s) of the analytes, prepared byan independent laboratory, and used for a verification of the instruments calibration.3.2.11 reagent blank, na volume of water containing the same matrix as the calibration standards, carried through the entireanalytical procedure.3.2.12 s
26、tock standard solution, na concentrated solution containing one or more analytes, obtained as a certified solution froma reputable source or prepared as described in Table 42.3.2.13 total-recoverable, adjdeterminable by the digestion method included in this procedure (see 12.2).3.2.14 tuning solutio
27、n, na solution that is used to determine acceptable instrument performance prior to calibration and sampleanalysis.3.3 Acronyms:3.3.1 ICSA, ninterference check sample A3.3.2 ICSAB, ninterference check sample B3.3.3 IDL, ninstrumental detection limit3.3.4 MDL, nmethod detection limit3.3.5 QCS, nquali
28、ty-control reference solution4. Summary of Test Method4.1 This test method describes the multi-element determination of trace elements by inductively coupled plasmamassspectrometry (ICP-MS). Sample material in solution is introduced by pneumatic nebulization into a radiofrequency plasma whereenergy
29、transfer processes cause desolvation, atomization, and ionization. The ions are extracted from the plasma through adifferentially pumped vacuum interface and separated on the basis of their mass-to-charge ratio by a quadrupole mass spectrometer.The ions transmitted through the quadrupole are detecte
30、d by a continuous dynode electron multiplier assembly and the ioninformation processed by a data handling system. Interferences relating to the technique must be recognized and corrected for (seeSection 6 on interferences). Such corrections must include compensation for isobaric elemental interferen
31、ces and interferencesfrom polyatomic ions derived from the plasma gas, reagents, or sample matrix. Instrumental drift as well as suppressions orenhancements of instrument response caused by the sample matrix must be corrected for by the use of internal standardization.5. Significance and Use5.1 The
32、test method is useful for the determination of element concentrations in many natural waters, metallurgical processcyanide solutions and wastewaters. It has the capability for the determination of up to 21 elements. High analysis sensitivity canbe achieved for some elements that are difficult to det
33、ermine by other techniques.TABLE 23 Recommended Analytical Isotopes and AdditionalMasses That Are Recommended To Be MonitoredIsotopeA Element of Interest27 Aluminum121, 123 Antimony75 Arsenic135, 137 Barium9 Beryllium106, 108, 111, 114 Cadmium52, 53 Chromium59 Cobalt63, 65 Copper206, 207, 208 Lead55
34、 Manganese95, 97,98 Molybdenum60, 62 Nickel77, 82 Selenium107, 109 Silver203, 205 Thallium232 Thorium238 Uranium51 Vanadium66, 67, 68 Zinc83 Krypton99 Ruthenium105 Palladium118 TinA Isotopes recommended for analytical determination are underlined. Thesemasses were recommended and are reflected in th
35、e precision and bias data.Alternate masses may be used but interferences must be documented.D5673 1636. Interferences6.1 Several types of interference effects may contribute to inaccuracies in the determination of trace elements. Theseinterferences can be summarized as follows:6.1.1 Isobaric Element
36、al InterferencesIsobaric elemental interferences are caused by isotopes of different elements whichform singly or doubly charged ions of the same nominal mass-to-charge ratio and which cannot be resolved by the massspectrometer in use by ICP-MS. All elements determined by this test method have, at a
37、 minimum, one isotope free of isobaricelemental interference. Of the analytical isotopes recommended for use with this test method (see Table 23), only molybdenum-98TABLE 34 Common Molecular Ion InterferencesBackground Molecular IonsMolecular Ion Mass Element InterferenceANH+ 15 .OH+ 17 .OH2+ 18 .C2
38、+ 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 .40Ar 36Ar+ 76 Se40Ar 38Ar+ 78 Se40Ar2+ 80 Se118Ta16O+ 197 AuMatrix Molecular IonsChloride35ClO+ 51 V35ClOH+ 52 C
39、r37ClO+ 53 Cr37ClOH+ 54 CrAr35Cl+ 75 AsAr37Cl+ 77 SeSulphate32SO+ 48 .32SOH+ 49 .34SO+ 50 V, Cr34SOH+ 51 VSO2+, S2+ 64 ZnAr 32S+ 72 .Ar 34S+ 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
40、108 to 116 CdA Method elements or internal standards affected by molecular ions.B Oxide 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
41、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.D5673 164(ruthenium) and selenium-82 (krypton) have isobaric elemental interferences. If alternative analytical isotopes having highernatural abundanc
42、e are selected in order to achieve greater sensitivity, an isobaric interference may occur. All data obtained undersuch conditions must be corrected by measuring the signal from another isotope of the interfering element and subtracting theappropriate signal ratio from the isotope of interest. A rec
43、ord of this correction process should be included with the report of thedata. It should be noted that such corrections will only be as accurate as the accuracy of the isotope ratio used in the elementalequation for data calculations. Relevant isotope ratios and instrument bias factors should be esta
44、blished prior to the application ofany corrections.6.1.2 Abundance SensitivityAbundance sensitivity is a property defining the degree to which the wings of a mass peakcontribute to adjacent masses.The abundance sensitivity is affected by ion energy and quadrupole operating pressure.Wing overlapinter
45、ferences may result when a small ion peak is being measured adjacent to a large one. The potential for these interferencesshould be recognized and the spectrometer resolution adjusted to minimize them.6.1.3 Isobaric Polyatomic Ion InterferencesIsobaric polyatomic ion interferences are caused by ions
46、 consisting of more thanone atom that have the same nominal mass-to-charge ratio as the isotope of interest, and which cannot be resolved by the massspectrometer in use. These ions are commonly formed in the plasma or interface system from support gases or sample components.Most of the common interf
47、erences have been identified, and these are listed in Table 34 together with the method elements affected.Such interferences must be recognized, and when they cannot be avoided by the selection of an alternative analytical isotope,appropriate corrections must be made to the data. Equations for the c
48、orrection of data should be established at the time of theanalytical run sequence as the polyatomic ion interferences will be highly dependent on the sample matrix and chosen instrumentconditions.6.1.4 Physical InterferencesPhysical interferences are associated with the physical processes that gover
49、n the transport of thesample into the plasma, sample conversion processes in the plasma, and the transmission of ions through the plasmamassspectrometer interface. These interferences may result in differences between instrument responses for the sample and thecalibration standards. Physical interferences may occur in the transfer of solution to the nebulizer (for example, viscosity effects),at the point of aerosol formation and transport to the plasma (for example, surface tension), or during excitation and ionizationprocesses with
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