1、 ISO 2013 Soil quality Determination of trace elements using inductively coupled plasma mass spectrometry (ICP-MS) Qualit du sol Dtermination des lments en traces par spectromtrie de masse avec plasma induit par haute frquence (ICP-MS) TECHNICAL SPECIFICATION ISO/TS 16965 First edition 2013-09-15 Re
2、ference number ISO/TS 16965:2013(E) ISO/TS 16965:2013(E)ii ISO 2013 All rights reserved COPYRIGHT PROTECTED DOCUMENT ISO 2013 All rights reserved. Unless otherwise specified, no part of this publication may be reproduced or utilized otherwise in any form or by any means, electronic or mechanical, in
3、cluding photocopying, or posting on the internet or an intranet, without prior written permission. Permission can be requested from either ISO at the address below or ISOs member body in the country of the requester. ISO copyright office Case postale 56 CH-1211 Geneva 20 Tel. + 41 22 749 01 11 Fax +
4、 41 22 749 09 47 E-mail copyrightiso.org Web www.iso.org Published in Switzerland ISO/TS 16965:2013(E) ISO 2013 All rights reserved iii Contents Page Foreword iv Introduction v 1 Scope . 1 2 Normative references 1 3 Principle 1 4 Interferences 2 4.1 General . 2 4.2 Spectral interferences . 2 5 Reage
5、nts 3 6 Apparatus . 5 6.1 General requirements . 5 6.2 Mass spectrometer 6 6.3 Mass-flow controller 6 6.4 Nebuliser with variable speed peristaltic pump 6 6.5 Gas supply . 6 6.6 Storage bottles, for the stock, standard, calibration and sample solutions 6 7 Procedure. 7 7.1 Test sample solution 7 7.2
6、 Test portion solution 7 7.3 Instrument set up . 7 7.4 Calibration 8 7.5 Sample measurement 8 8 Calculation 9 9 Expression of results 9 10 Performance characteristics .10 10.1 General 10 10.2 Blank .10 10.3 Calibration check 10 10.4 Internal standard response .10 10.5 Interference 10 10.6 Recovery 1
7、0 10.7 Precision 10 11 Test report 11 Annex A (informative) Selected isotopes and spectral interferences for quadrupole ICP- MS instruments .12 Bibliography .13 ISO/TS 16965:2013(E) Foreword ISO (the International Organization for Standardization) is a worldwide federation of national standards bodi
8、es (ISO member bodies). The work of preparing International Standards is normally carried out through ISO technical committees. Each member body interested in a subject for which a technical committee has been established has the right to be represented on that committee. International organizations
9、 governmental and non-governmental, in liaison with ISO, also take part in the work. ISO collaborates closely with the International Electrotechnical Commission (IEC) on all matters of electrotechnical standardization. The procedures used to develop this document and those intended for its further
10、maintenance are described in the ISO/IEC Directives, Part 1. In particular the different approval criteria needed for the different types of ISO documents should be noted. This document was drafted in accordance with the editorial rules of the ISO/IEC Directives, Part 2. www.iso.org/directives Atten
11、tion is drawn to the possibility that some of the elements of this document may be the subject of patent rights. ISO shall not be held responsible for identifying any or all such patent rights. Details of any patent rights identified during the development of the document will be in the Introduction
12、 and/or on the ISO list of patent declarations received. www.iso.org/patents Any trade name used in this document is information given for the convenience of users and does not constitute an endorsement. For an explanation on the meaning of ISO specific terms and expressions related to conformity as
13、sessment, as well as information about ISOs adherence to the WTO principles in the Technical Barriers to Trade (TBT) see the following URL: Foreword - Supplementary information The committee responsible for this document is ISO/TC 190, Soil quality, Subcommittee SC 3, Chemical methods and soil chara
14、cteristics.iv ISO 2013 All rights reserved ISO/TS 16965:2013(E) Introduction ISO/TS 16965 is based upon CEN/TS 16171, Sludge, treated biowaste and soil Determination of elements using inductively coupled plasma mass spectrometry (ICP-MS), which was developed by CEN/TC 400, Project Committee Horizont
15、al standards in the fields of sludge, biowaste and soil. This Technical Specification is applicable and validated for several types of matrices as indicated in Table 1. Table 1 Matrices for which this Technical Specification is applicable and validated Matrix Materials used for validation Sludge Mun
16、icipal sludge Biowaste Compost Soil Sludge-amended soils ISO 2013 All rights reserved v Soil quality Determination of trace elements using inductively coupled plasma mass spectrometry (ICP-MS) WARNING Persons using this Technical Specification should be familiar with usual laboratory practice. This
17、Technical Specification does not purport to address all of the safety problems, if any, associated with its use. It is the responsibility of the user to establish appropriate safety and health practices and to ensure compliance with any national regulatory conditions. IMPORTANT It is absolutely esse
18、ntial that tests conducted according to this Technical Specification be carried out by suitably trained staff. 1 Scope This Technical Specification specifies a method for the determination of the following elements in aqua regia or nitric acid digests or other extraction solutions of sludge, treated
19、 biowaste and soil: Aluminium (Al), antimony (Sb), arsenic (As), barium (Ba), beryllium (Be), bismuth (Bi), boron (B), cadmium (Cd), calcium (Ca), cerium (Ce), cesium (Cs), chromium (Cr), cobalt (Co), copper (Cu), dysprosium (Dy), erbium (Er), europium (Eu), gadolinium (Gd), gallium (Ga), germanium
20、Ge), gold (Au), hafnium (Hf), holmium (Ho), indium (In), iridium (Ir), iron (Fe), lanthanum (La), lead (Pb), lithium (Li), lutetium (Lu), magnesium (Mg), manganese (Mn), mercury (Hg), molybdenum (Mo), neodymium (Nd), nickel (Ni), palladium (Pd), phosphorus (P), platinum (Pt), potassium (K), praseod
21、ymium (Pr), rhenium (Re), rhodium (Rh), rubidium (Rb), ruthenium (Ru), samarium (Sm), scandium (Sc), selenium (Se), silicon (Si), silver (Ag), sodium (Na), strontium (Sr), sulfur (S), tellurium (Te), terbium (Tb), thallium (Tl), thorium (Th), thulium (Tm), tin (Sn), titanium (Ti), tungsten (W), uran
22、ium (U), vanadium (V), ytterbium(Yb), yttrium (Y), zinc (Zn) and zirconium (Zr). The working range depends on the matrix and the interferences encountered. The limit of detection is between 0,1 mg/kg dry matter and 2,0 mg/kg dry matter for most elements. The limit of detection will be higher in case
23、s where the determination is likely to have interferences (see Clause 4) or in the case of memory effects (see e.g. 8.2 of ISO 17294-1:2004). 2 Normative references The following documents, in whole or in part, are normatively referenced in this document and are indispensable for its application. Fo
24、r dated references, only the edition cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies. ISO 11466, Soil quality Extraction of trace elements soluble in aqua regia ISO 16729, Soil quality Digestion of nitric acid soluble fractions
25、of elements ISO 3696, Water for analytical laboratory use Specification and test methods ISO 17294-1:2004, Water quality Application of inductively coupled plasma mass spectrometry (ICP- MS) Part 1: General guidelines 3 Principle Digests with nitric acid or aqua regia of samples of sludge, treated b
26、iowaste or soil (see ISO 11466 and ISO 16729) are analysed by ICP-MS to get a multi-elemental determination of analytes. TECHNICAL SPECIFICATION ISO/TS 16965:2013(E) ISO 2013 All rights reserved 1 ISO/TS 16965:2013(E) The method measures ions produced by a radio-frequency inductively coupled plasma.
27、 Analyte species originating in the digest solution are nebulised and the resulting aerosol is transported by argon gas into the plasma. The ions produced by the high temperatures of the plasma are entrained in the plasma gas and introduced, by means of an interface, into a mass spectrometer, sorted
28、 according to their mass- to-charge ratios and quantified with a detector (e.g. channel electron multiplier). 4 Interferences 4.1 General Interferences shall be assessed and valid corrections applied. Interference correction shall include compensation for background ions contributed by the plasma ga
29、s, reagents, and constituents of the sample matrix. Detailed information on spectral and non-spectral interferences is given in Clause 6 of ISO 17294-1:2004. 4.2 Spectral interferences 4.2.1 Isobaric elemental interferences Isobaric elemental interferences are caused by isotopes of different element
30、s of closely matched nominal mass-to-charge ratio and which cannot be separated due to an insufficient resolution of the mass spectrometer in use (e.g. 114 Cd and 114 Sn). Element interferences from isobars may be corrected by taking into account the influence from the interfering element (see ISO 1
31、7294-1:2004). The isotopes used for correction shall be free of interference if possible. Correction options are often included in the software supplied with the instrument. Common isobaric interferences are given in Table A.1. 4.2.2 Isobaric molecular and doubly-charged ion interferences Isobaric m
32、olecular and doubly-charged ion interferences in ICP-MS are caused by ions consisting of more than one atom or charge, respectively. Examples include 40 Ar 35 Cl +and 40 Ca 35 Cl +ion on the 75 As signal or 98 Mo 16 O +ions on the 114 Cd +signal. Natural isotope abundances are available from the lit
33、erature. The accuracy of correction equations is based upon the constancy of the observed isotopic ratios for the interfering species. Corrections that presume a constant fraction of a molecular ion relative to the “parent” ion have not been found to be reliable, e.g. oxide levels can vary with oper
34、ating conditions. If a correction for an oxide ion is based upon the ratio of parent-to-oxide ion intensities, this shall be determined by measuring the interference solution just before the sequence is started. The validity of the correction coefficient should be checked at regular intervals within
35、 a sequence. Another possibility to remove isobaric molecular interferences is the use of an instrument with collision/reaction cell technology. The use of high resolution ICP-MS avoids these interferences and additionally double-charged ion interferences. The response of the analyte of interest sha
36、ll be corrected for the contribution of isobaric molecular and doubly-charged interferences if their impact can be higher than three times the detection limit or higher than half the lowest concentration to be reported. More information about the use of correction factors is given in ISO 17294-1. 4.
37、2.3 Non-spectral interferences Physical interferences are associated with sample nebulisation and transport processes as well as with ion-transmission efficiencies. Nebulisation and transport processes can be affected if a matrix component causes a change in surface tension or viscosity. Changes in
38、matrix composition can cause 2 ISO 2013 All rights reserved ISO/TS 16965:2013(E) significant signal suppression or enhancement. Solids can be deposited on the nebuliser tip of a pneumatic nebuliser and on the cones. It is recommended to keep the level of total dissolved solids below 0,2 % (2 000 mg/
39、l) to minimize deposition of solids in the sample introduction system of the plasma torch. An internal standard can be used to correct for physical interferences if it is carefully matched to the analyte, so that the two elements are similarly affected by matrix changes. Other possibilities to minim
40、ize non-spectral interferences are matrix matching, particularly matching of the acid concentration, and standard addition. When intolerable physical interferences are present in a sample, a significant suppression of the internal standard signals (to less than 30 % of the signals in the calibration
41、 solution) will be observed. Dilution of the sample (e.g. fivefold) usually eliminates the problem. 5 Reagents For the determination of elements at trace and ultra trace level, the reagents shall be of adequate purity. The concentration of the analyte or interfering substances in the reagents and th
42、e water should be negligible compared to the lowest concentration to be determined. Preferably, nitric acid preservation should be applied in order to minimize interferences by chloropolyatom molecules. Bi, Hg, Hf, Mo, Sn, Sb, Te, W and Zr may need hydrochloric acid for preservation. 5.1 Water, grad
43、e 1 as specified in ISO 3696 for all sample preparations and dilutions. 5.2 Nitric acid, c(HNO 3 ) = 15 mol/l. NOTE Nitric acid is available both as c(HNO 3 ) 1,4 g/ml w(HNO 3 ) = 650 g/kg and c(HNO 3 ) = 1,42 g/ml w(HNO 3 ) 720 g/kg. Both are suitable for use in this method, provided the content of
44、 the analytes of interest is minimal. 5.3 Hydrochloric acid, c(HCl) = 12 mol/l, 1,18 g/ml. 5.4 Single-element standard stock solutions For Ag, Al, As, Au, B, Ba, Be, Bi, Ca, Cd, Ce, Co, Cr, Cs, Cu, Dy, Er, Eu, Fe, Ga, Gd, Ge, Hf, Hg, Ho, In, Ir, K, La, Li, Lu, Mg, Mn, Mo, Na, Nd, Ni, P, Pb, Pd, Pr,
45、Pt, Rb, Re, Rh, Ru, S, Sb, Sc, Se, Si, Sm, Sn, Sr, Tb, Te, Th, Ti, Tl, Tm, U, V, W, Y, Yb, Zn, Zr, = 1 000 mg/l each. Both single-element standard stock solutions and multi-element standard stock solutions with adequate specification stating the acid used and the preparation technique are commercial
46、ly available. These solutions are considered to be stable for more than one year, but in reference to guaranteed stability, the recommendations of the manufacturer should be considered. 5.5 Anion standard stock solutions = 1 000 mg/l each. Prepare these solutions from the respective acids. The solut
47、ions are commercially available. These solutions are considered to be stable for more than one year, but in reference to guaranteed stability, the recommendations of the manufacturer should be considered. 5.6 Multi-element standard stock solutions Depending on the scope, different multi-element stan
48、dard stock solutions may be necessary. In general, when combining multi-element standard stock solutions, their chemical compatibility and the possible ISO 2013 All rights reserved 3 ISO/TS 16965:2013(E) hydrolysis of the components shall be regarded. Care shall be taken to prevent chemical reaction
49、s (e.g. precipitation). The multi-element standard stock solutions are considered to be stable for several months if stored in the dark. This does not apply to multi-element standard stock solutions that are prone to hydrolysis, in particular solutions of Bi, Mo, Sn, Sb, Te, W, Hf and Zr. Mercury standard stock solutions can be stabilized by adding 1 mg/l Au in nitric acid (5.2) or by adding hydrochloric acid (5.3) up to 0,6 %. NOTE When Au is to be used as modifier, the instrument is no
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