1、BSI Standards PublicationBS ISO 17586:2016Soil quality Extraction oftrace elements using dilutenitric acidBS ISO 17586:2016 BRITISH STANDARDNational forewordThis British Standard is the UK implementation of ISO 17586:2016.The UK participation in its preparation was entrusted to TechnicalCommittee EH
2、/4, Soil quality.A list of organizations represented on this committee can beobtained on request to its secretary.This publication does not purport to include all the necessaryprovisions of a contract. Users are responsible for its correctapplication. The British Standards Institution 2016. Publishe
3、d by BSI StandardsLimited 2016ISBN 978 0 580 79518 3ICS 13.080.10Compliance with a British Standard cannot confer immunity fromlegal obligations.This British Standard was published under the authority of theStandards Policy and Strategy Committee on 31 March 2016.Amendments issued since publicationD
4、ate Text affectedBS ISO 17586:2016 ISO 2016Soil quality Extraction of trace elements using dilute nitric acidQualit du sol Extraction dlments traces laide dacide nitrique diluINTERNATIONAL STANDARDISO17586First edition2016-02-15Reference numberISO 17586:2016(E)BS ISO 17586:2016ISO 17586:2016(E)ii IS
5、O 2016 All rights reservedCOPYRIGHT PROTECTED DOCUMENT ISO 2016, Published in SwitzerlandAll 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, including photocopying, or posting on t
6、he 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 officeCh. de Blandonnet 8 CP 401CH-1214 Vernier, Geneva, SwitzerlandTel. +41 22 749 01 11Fax +41 22 749 09
7、47copyrightiso.orgwww.iso.orgBS ISO 17586:2016ISO 17586:2016(E)Foreword iv1 Scope . 12 Normative references 13 Terms and definitions . 14 Principle 15 Interferences 26 Reagents 27 Apparatus . 28 Procedure. 38.1 Sample preparation 38.2 Determining water content 38.3 Extraction 38.4 Phase separation .
8、 48.5 Blank test . 48.6 Measurement of trace elements . 49 Calculation 410 Expression of results 511 Test report . 5Annex A (informative) Precision . 7Annex B (informative) Notes on homogenization, initial sample mass and extraction .13Bibliography .14 ISO 2016 All rights reserved iiiContents PageBS
9、 ISO 17586:2016ISO 17586:2016(E)ForewordISO (the International Organization for Standardization) is a worldwide federation of national standards bodies (ISO member bodies). The work of preparing International Standards is normally carried out through ISO technical committees. Each member body intere
10、sted in a subject for which a technical committee has been established has the right to be represented on that committee. International organizations, governmental and non-governmental, in liaison with ISO, also take part in the work. ISO collaborates closely with the International Electrotechnical
11、Commission (IEC) on all matters of electrotechnical standardization.The procedures used to develop this document and those intended for its further maintenance are described in the ISO/IEC Directives, Part 1. In particular the different approval criteria needed for the different types of ISO documen
12、ts should be noted. This document was drafted in accordance with the editorial rules of the ISO/IEC Directives, Part 2 (see www.iso.org/directives).Attention 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
13、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 and/or on the ISO list of patent declarations received (see www.iso.org/patents).Any trade name used in this document is information given for the
14、 convenience of users and does not constitute an endorsement.For an explanation on the meaning of ISO specific terms and expressions related to conformity assessment, as well as information about ISOs adherence to the WTO principles in the Technical Barriers to Trade (TBT), see the following URL: Fo
15、reword Supplementary information.The committee responsible for this document is ISO/TC 190, Soil quality, Subcommittee SC 3, Chemical methods and soil characteristics.iv ISO 2016 All rights reservedBS ISO 17586:2016INTERNATIONAL STANDARD ISO 17586:2016(E)Soil quality Extraction of trace elements usi
16、ng dilute nitric acidWARNING Users of this International Standard should be familiar with usual laboratory practice. This International Standard does not address all of the safety problems, if any, associated with its use. It is the responsibility of the user to establish appropriate safety and heal
17、th practices and to ensure compliance with any national regulatory conditions.IMPORTANT It is absolutely essential that tests conducted according to this International Standard be carried out by suitably trained staff.1 ScopeThis International Standard specifies a method of extracting trace elements
18、 from soil at approximately pH 0,5 using a dilute nitric acid solution. Using this method the potential environmental available trace elements as defined in ISO 17402 is extracted.The method is applicable for all soils and soil like materials.2 Normative referencesThe following documents, in whole o
19、r in part, are normatively referenced in this document and are indispensable for its application. For dated references, only the edition cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies.ISO 11464, Soil quality Pretreatment of sam
20、ples for physico-chemical analysisISO 11465, Soil quality Determination of dry matter and water content on a mass basis Gravimetric method3 Terms and definitionsFor the purposes of this document, the following terms and definitions apply.3.1test portionanalytical portionquantity of material, of prop
21、er size, for measurement of the concentration or other property of interest, removed from the test sampleNote 1 to entry: The test portion may be taken from the field sample or from the laboratory sample directly if no preparation of the sample is required (e.g. with liquids), but usually it is take
22、n from the prepared test sample.Note 2 to entry: A unit or increment of proper homogeneity, size, and fineness, needing no further preparation, may be a test portion.SOURCE: ISO 11074:2005, 4.3.134 PrincipleThe soil sample with particle size of 2 mm exceeds 5 % (mass fraction), the entire oversized
23、fraction shall be separated by sieving (7.9) and crushed with suitable crushing equipment (7.8) to grain size 2 mm.The drying temperature shall not exceed 40 C.On no account the material shall be finely ground.8.2 Determining water contentDetermine the water content as specified in ISO 11465 using a
24、 separate test sample portion.8.3 Extraction8.3.1 Using a pipette or dispenser, add 100,0 ml of (0,43 0,02) mol/l nitric acid solution (6.4) to (10 0,1) g of the soil test portion (8.1) into a suitable test tube (7.2).8.3.2 Add, with a pipette, drop by drop, 0,50 ml of 5 mol/l nitric acid (6.4) for
25、each mass fraction of calcium carbonate in percent which is above 5 %.8.3.3 Close the test tube with a screw cap, mount it to an end-over-end shaker (7.3) and extract the soil at room temperature (20 2) C and (25 10) revolutions per min for (240 10) min.NOTE After the addition of nitric acid, in cas
26、e of effervescence, allow the foaming to stop; then continue. ISO 2016 All rights reserved 3BS ISO 17586:2016ISO 17586:2016(E)8.4 Phase separation8.4.1 Place the closed test tubes into a centrifuge and separate the solid phase by centrifugation at 1 000 g or higher for 10 min.8.4.2 Rinse the membran
27、e filter and the syringe with at least 1 ml of extract solution and discard the rinsing solution.8.4.3 Filter a suitable amount for following analysis (e.g. 10 ml) of the supernatant solution directly from the sample test tube by pushing it through a syringe equipped with a 0,45 m disposable in-line
28、 membrane filter.8.4.4 Store the acid extract in a clean conical test tube.NOTE Because the extract is already acid, extra addition for stabilization is not necessary.8.5 Blank testSubject at least one blank to the same extraction procedure.8.6 Measurement of trace elementsTo determine the element f
29、raction extracted with 0,43 mol/l nitric acid solution, the extract solution should be analysed with a sufficiently sensitive analytical method capable to determine concentrations down to the g/l level. Use inductively coupled plasma atomic emission spectrometry described in ISO 22036 or inductively
30、 coupled plasma mass spectrometry in ISO 17294-2, atomic absorption methods in ISO 11047 or ISO 20280. Carefully designed temperature programmes in connection with appropriate matrix modifier should be used with ET-AAS determination. Apply matrix matching in calibration solutions. Always expect non-
31、negligible blank concentrations which shall be taken into account.9 CalculationSubtract the blank concentration of an element from the concentration in the sample solution. Calculate the extractable element mass fraction according to Formula (1) for air-dried samples or Formula (2) for wet-field sam
32、ple.Air-dried sample:wVF wmxairo=+()BHO2100100(1)Wet-field sample. The equation corrects for the dilution by the water present in the sample:wFVmwxwet=+BdHOHO22100(2)Determine the water content according to ISO 11465 and calculate using Formula (3).4 ISO 2016 All rights reservedBS ISO 17586:2016ISO
33、17586:2016(E)Water content in %:wmmmHO2=odd100 (3)wherewxairor wxwetis the nitric acid extractable mass fraction of an element (x) in soil, in micro-grams per kilogram, g/kg;Bis the blank-corrected concentration of the element (x), in micrograms per litre, g/l;V is the volume of nitric acid added to
34、 the soil sample, in litres (nominal 0,1 l);F is the dilution factor, Vend/Vi: Vialiquot taken of nitric acid, diluted to volume Vendof analysis solution;mois the initial mass of air-dried or fresh-field sample, in kilograms, kg;mdis the mass of soil, dried according to ISO 11465, in kilograms, kg;w
35、HO2is the percentage of water in soil sample, determined according to ISO 11465;HO2is the density of water, usually taken as 1 kg/l.Additionally, the concentration of the extracted element M, in g/dm3, determined as specified in ISO 11465 may be calculated according to Formula (4).Md=wx(4)where dis
36、the bulk density of dry soil, determined in a separate analysis, in kilograms per cubic decimetre (kg/dm3).10 Expression of resultsReport the results expressed in g/kg.EXAMPLE 1 wPb= 20,3 g/kg.EXAMPLE 2 wCd= 1,3 g/kg.The number of decimal places reported will generally depend on the precision of the
37、 analytical method used or on the limits of determination. As a rule, the contents should be reported with three significant decimal places, but only in two or even one in the vicinity of the limit of determination.11 Test reportThe test report shall contain at least the following information:a) a r
38、eference to this International Standard, i.e. ISO 17586;b) the identification of the sample;c) details of sample pre-treatment, indicating whether the sample was used as collected from the field (wet or air-dried); ISO 2016 All rights reserved 5BS ISO 17586:2016ISO 17586:2016(E)d) the dry matter con
39、tent according to ISO 11465;e) the result of the determination of trace elements according to the analytical method used;f) any details not specified in this standard or that are optional, and any circumstances that may have affected the result.6 ISO 2016 All rights reservedBS ISO 17586:2016ISO 1758
40、6:2016(E)Annex A (informative) PrecisionAn inter-laboratory comparison on the determination of trace elements by extraction with diluted nitric acid according to this International Standard has been carried out in the beginning of 2015. The extracts were measured using the method applied in the indi
41、vidual laboratories. Most elements were analysed using ICP with AES or MS detection. One laboratory has used AAS including deuterium background correction and for arsenic the hydride technique. The final results are given in Tables A.2 and A.3. A more detailed report is available on www.wepal.nl.The
42、 statistical test was carried out according to the ISO 5725 series. Six samples were used that are part of the WEPAL proficiency scheme and distributed to 17 participating laboratories. Each soil sample should be extracted four times according to ISO 17586 and measured according the analytical proce
43、dures available in the laboratory.Six soil samples have been used with different soil properties (Table A.1) and content of trace elements (Tables A.2 and A.3):Table A.1 Consensus values of general soil parameters in the analysed soilsParameter 1 2 3 4 5 6Clay (%) 13,3 25,2 22,0 26,7 13,6 8,9Organic
44、 matter (LOI) (%) 5,6 5,3 5,3 12,0 3,0 2,1CaCO3(%) 9,0 8,4 2,8 8,4 0 1,8All materials used were homogenized and grinded materials. They were sieved over 0,5 mm and distributed in pots to contain 100 g of soil. Before sending, it was checked if the soils were homogenous distributed in the pots using
45、previous test results and specific analysis of total concentrations in a random selection of 10 pots. Participants have submitted their results electronically by www.wepal.nl.Outliers were identified using Cochrans test and Grubbs test described in ISO 5725-2. Although the laboratories were asked to
46、 analyse four replicates, two laboratories measured two replicates and one laboratory analysed three replicates. The results of the validation are summarized in Tables A.2 and A.3. In these tables, we have added the total concentration measured using aqua regia. The concentration measured after extr
47、action using ISO 17586 is a part of the total concentration.Table A.2 describes the results with more than four participating laboratories. For most elements, the repeatability and reproducibility are as expected for such an analysis, and the method is validated for these elements (all elements in T
48、able A.2 with exception of B, Mo and Se). Higher values are obtained for B, Mo and Se. For Mo and Se this is caused by the low concentrations and the higher values for B shows that the method is less suitable for this element.Table A.3 summarizes the results for elements with four or less than four
49、participating laboratories. Repeatability and reproducibility of the elements in Table A.3 are indicative. High values of repeatability and reproducibility are obtained for Sn.For all elements presented in Tables A.2 and A.3, it has to be considered that they are the results of a chemical method and more precisely, the amount that can be extracted with a mild acid extraction (approximately pH 0,5). If this amount is representative for the bioavailable, fraction has to be prove
