1、Designation: D5673 10D5673 15Standard 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 This test method is under the jurisdiction ofASTM Committee D19 on Wate
7、r and is the direct responsibility of Subcommittee D19.05 on Inorganic Constituents in Water.Current edition approved Aug. 1, 2010July 1, 2015. Published September 2010August 2015. Originally approved in 1996. Last previous edition approved in 20052010as D5673 05.D5673 10. DOI: 10.1520/D5673-10.10.1
8、520/D5673-15.2 EPA Test Method: Determination of Trace Elements in Waters and Wastes by Inductively Coupled PlasmaMass Spectrometry, Method 200.8.TABLE 1 Recommended Analytical Mass and EstimatedInstrument Detection Limitschar=“.“ colwidth=“38.68*“/COLSPECElementElement RecommendedAnalytical MassEst
9、imated InstrumentDetection Limit, g/L 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 55 0.1Molybdenum 98 0.1Nickel 60 0.2Selenium 82 5.0Silver 107 0.05Thallium 20
10、5 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.This document is not an ASTM standard and is intended only to provide the us
11、er 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 only the current versionof the standard a
12、s 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 States11.5 The values stated in SI units are to be regarded as sta
13、ndard. No other units of measurement are included in this standard.1.6 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 ap
14、plicability of regulatorylimitations prior to use.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
15、WaterD3370 Practices for Sampling Water from Closed 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 Met
16、hodE1601 Practice for Conducting an Interlaboratory 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 DefinitionsFor definitions of other terms used in
17、 this test method, refer to Terminology D1129.3.1 Definitions:3.1.1 For definitions of terms used in this standard, refer 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 is in the calibration stand
18、ards (see 11.1).3.2.2 calibration standards, na series of known standard solutions used by the analyst for calibration of the instrument (thatis, preparation of the analytical curve) (see Section 11).3.2.3 calibration stock solution, na solution prepared from the stock standard solution(s) to verify
19、 the instrument responsewith respect to analyte concentration.3.2.4 dissolved, nadjthose elements that will pass capable of passing through a 0.45-m membrane filter.3.2.5 interference check sample A (ICSA), na solution containing matrix elements at environmental levels that result ininterferences on
20、 target low level analytes.3.2.5.1 DiscussionICSA is different from the mixed element standards in 8.4, which are intended for instrument calibration, not for checkinginterferences. The interferences formed in the ICP can be corrected for by use of element-specific correction equations orequations,
21、collision cell technology with quadrupole-based ICP-MS, or high resolution 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 instrumental detection limit (IDL), nthe concentration equivalent to a signal, whichthat is equal to
22、 three times thestandard deviation of the blank signal at the selected analytical mass(es).3.2.8 internal standard, npure analyte(s)element(s) added in known amount(s) to a solution.3.2.8.1 DiscussionThis The internal standard is used to measure the relative instrument response relative to the other
23、 analytes that are componentsof the same solution. The internal standards must be analyteselements that are not a sample component.3.2.9 method detection limit (MDL), nthe minimum concentration of an analyte analyte concentration that can be identified,measured and reported with 99 %99 % confidence
24、that the analyte concentration is greater than zero.3.2.9.1 Discussion3 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
25、 website.4 The last approved version of this historical standard is referenced on www.astm.org.D5673 152This confidence level is determined from analysis of a sample in a given matrix containing the analyte(s).3.2.10 quality control reference solution (QCS), na solution with the certified concentrat
26、ion(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 stock standard solution, na
27、 concentrated solution containing one or more analytes, obtained as a certified solution froma reputable source or prepared as described in Table 4.3.2.13 total-recoverable, nadja term relating to forms of each element that are determinable by the digestion methodincluded in this procedure (see 12.2
28、).TABLE 2 Recommended Analytical Isotopes and AdditionalMasses That Are Recommended To Be Monitoredcolname=“col2“ colwidth=“1.88in“Isotope A Element of Interest27 Aluminum121, 123 Antimony75 Arsenic135, 137 Barium9 Beryllium106, 108, 111, 114 Cadmium52, 53 Chromium59 Cobalt63, 65 Copper206, 207, 208
29、 Lead55 Manganese95, 97,98 Molybdenum60, 62 Nickel77, 82 Selenium107, 109 Silver203, 205 Thallium232 Thorium238 Uranium51 Vanadium66, 67, 68 Zinc83 Krypton99 Ruthenium105 Palladium118 TinTABLE 2 Recommended Analytical Isotopes and AdditionalMasses That Are Recommended To Be MonitoredIsotopeA Element
30、 of Interest27 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
31、Krypton99 Ruthenium105 Palladium118 TinA Isotopes 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.D5673 153TABLE 3 Common Molecular Ion Interferenc
32、escolwidth=“37.54*“/COLSPECBackground Molecular IonsMolecularMolecularIon MassElementInterference InterferenceANH + 15 .NH+ 15 .OH + 17 .OH+ 17 .OH2+ 18 .C2+ 24 .CN + 26 .CN+ 26 .CO + 28 .CO+ 28 .N2+ 28 .N2H + 29 .N2H+ 29 .NO + 30 .NOH + 31 .NOH+ 31 .O2+ 32 .O2H + 33 .O2H+ 33 .36ArH + 37 .36ArH+ 37
33、.36ArH + 39 .36ArH+ 39 .40ArH + 41 .40ArH+ 41 .CO2+ 44 .CO2H + 45 ScCO2H+ 45 ScArC +, ArO + 52 CrArC +, ArO+ 52 CrArN + 54 CrArNH + 55 MnArO + 56 .ArOH + 57 .40Ar 36Ar + 76 Se40Ar 36Ar+ 76 Se40Ar 38Ar + 78 Se40Ar 38Ar+ 78 Se40Ar2+ 80 Se118Ta16O+ 197 AuMatrix Molecular IonsChloride35ClO + 51 V35ClO+
34、51 V35ClOH + 52 Cr35ClOH+ 52 Cr37ClO + 53 Cr37ClO+ 53 Cr37ClOH + 54 Cr37ClOH+ 54 CrAr 35Cl + 75 AsAr35Cl+ 75 AsAr 37Cl + 77 SeAr37Cl+ 77 SeSulphate32SO + 48 .32SO+ 48 .32SOH + 49 .32SOH+ 49 .34SO + 50 V, Cr34SO+ 50 V, Cr34SOH + 51 V34SOH+ 51 VSO2+, S2+ 64 ZnAr 32S + 72 .Ar 32S+ 72 .Ar 34S + 74 .Ar 3
35、4S+ 74 .PhosphatePO + 47 .PO+ 47 .POH + 48 .POH+ 48 .D5673 154Background Molecular IonsMolecularMolecularIon MassElementInterference InterferenceAPO2+ 63 CuArP + 71 .ArP+ 71 .Group I, II MetalsArNa + 63 CuArNa+ 63 CuArK + 79 .ArK+ 79 .ArCa + 80 .ArCa+ 80 .Matrix Oxides BMatrix OxidesBTiO 62 to 66 Ni
36、, Cu, ZnZrO 106 to 112 Ag, CdMoO 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
37、 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.TABLE 4 Preparation of Metal Stock Solutions Acolwidth=“64.29*“/COLSPECElement orCompoundWeight,g SolventAl 0.1000 10
38、 mL ofHCl (sp gr1.19) + 2mL ofHNO3 (spgr1.42)Sb 0.1000 0.5 mL ofHCl (sp gr1.19) + 2mL ofHNO3(1 + 1)As2O3 0.1320 1 mL ofNH4OH (spgr0.902) + 50mL of H2OBaCO3 0.1437 2 mL ofHNO3 (spgr1.42) + 10mL of H2OBeSO44H2O 1.9650 50 mL ofH2O, add 1mL ofHNO3 (spgr 1.42)Bi2O3 0.1115 5 mL ofHNO3 (spgr 1.42)Cd 0.1000
39、 5 mL ofHNO3(1 + 1)CrO3 0.1923 1 mL ofHNO3 (sp1.42) + 10mL H2OCo 0.1000 5 mL ofHNO3(1 + 1)Cu 0.1000 5 mL ofHNO3(1 + 1)Au 0.1000 20 mLH2O, ad 8mL of HCL= 5 mLHNO3(1 + 1)In 0.1000 10 mL ofHNO3(1 + 1)PbNO3 0.1599 5 mL ofHNO3(1 + 1)MgO 0.1658 10 mL ofHNO3(1 + 1)Mn 0.1000 5 mL ofHNO3(1 + 1)MoO3 0.1500 1
40、mL ofNH4OH (spgr0.902) + 10mL of H2ONi 0.1000 5 mL ofHNO3 (spgr 1.42)Sc2O3 0.1534 5 mL ofHNO3(1 + 1)SeO2 0.1405 20 mL ofH2OD5673 1553.2.14 tuning solution, na solution that is used to determine acceptable instrument performance prior to calibration and sampleanalysis.3.3 Acronyms:3.3.1 ICSA, ninterf
41、erence 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, nquality-control reference solution4. Summary of Test Method4.1 This test method describes the multi-element determination of trace elements by inductive
42、ly coupled plasmamassspectrometry (ICP-MS). Sample material in solution is introduced by pneumatic nebulization into a radiofrequency plasma whereenergy transfer processes cause desolvation, atomization, and ionization. The ions are extracted from the plasma through adifferentially pumped vacuum int
43、erface and separated on the basis of their mass-to-charge ratio by a quadrupole mass spectrometer.The ions transmitted through the quadrupole are detected by a continuous dynode electron multiplier assembly and the ioninformation processed by a data handling system. Interferences relating to the tec
44、hnique must be recognized and corrected for (seeSection 6 on interferences). Such corrections must include compensation for isobaric elemental interferences and interferencesfrom polyatomic ions derived from the plasma gas, reagents, or sample matrix. Instrumental drift as well as suppressions orenh
45、ancements of instrument response caused by the sample matrix must be corrected for by the use of internal standardization.5. Significance and Use5.1 The test method is useful for the determination of element concentrations in many natural waters waters, metallurgicalprocess cyanide solutions and was
46、tewaters. It has the capability for the determination of up to 2021 elements. High analysissensitivity can be achieved for some elements that are difficult to determine by other techniques.6. Interferences6.1 Several types of interference effects may contribute to inaccuracies in the determination o
47、f trace elements. Theseinterferences can be summarized as follows:6.1.1 Isobaric Elemental 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 m
48、assspectrometer in use. use by ICP-MS.All elements determined by this test method have, at a minimum, one isotope free of isobaricElement orCompoundWeight,g SolventAg 0.1000 5 mL ofHNO3(1 + 1)Tb4O7 0.1176 5 mL ofHNO3 (spgr 1.42)TlNO3 0.1303 1 mL ofHNO3 (spgr1.42) + 10mL of H2OTh(NO3)44H2O 0.2380 20
49、mL ofH2OUO2(NO3)26H2O 0.2110 20 mL ofH2OV 0.1000 5 mL ofHNO2(1 + 1)Y2O3 0.1270 5 mL ofHNO3(1 + 1)Zn 0.1000 5 mL ofHNO3(1 + 1)A Metal stock solutions, 1.00 mL = 1000 g of metal. Dissolve the listed weights ofeach metal or compound as specified in Table 4, then dilute to 100 mL with water.The metals may require heat to increase rate of dissolution. Commerciallyavailable standards of known purity may be used. Alternate salts or oxides mayalso be used.D5673 156elemental interference. Of the analytical isotopes recommended for us
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