1、BSI Standards PublicationBS ISO 17318:2015Fertilizers and soil conditioners Determination of arsenic,cadmium, chromium, lead andmercury contentsBS ISO 17318:2015 BRITISH STANDARDNational forewordThis British Standard is the UK implementation of ISO 17318:2015.The UK participation in its preparation
2、was entrusted to TechnicalCommittee CII/37, Fertilisers and related chemicals.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 correct
3、application. The British Standards Institution 2015. Published by BSI StandardsLimited 2015ISBN 978 0 580 76270 3ICS 65.080Compliance with a British Standard cannot confer immunity fromlegal obligations.This British Standard was published under the authority of theStandards Policy and Strategy Commi
4、ttee on 30 June 2015.Amendments issued since publicationDate Text affectedBS ISO 17318:2015 ISO 2015Fertilizers and soil conditioners Determination of arsenic, cadmium, chromium, lead and mercury contentsMatires fertilisantes Dtermination de larsenic, du cadmium, du plomb, du chrome et du mercure da
5、ns les engraisINTERNATIONAL STANDARDISO17318First edition2015-06-01Reference numberISO 17318:2015(E)BS ISO 17318:2015ISO 17318:2015(E)ii ISO 2015 All rights reservedCOPYRIGHT PROTECTED DOCUMENT ISO 2015, Published in SwitzerlandAll rights reserved. Unless otherwise specified, no part of this publica
6、tion may be reproduced or utilized otherwise in any form or by any means, electronic or mechanical, including 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
7、 of the requester.ISO copyright officeCh. de Blandonnet 8 CP 401CH-1214 Vernier, Geneva, SwitzerlandTel. +41 22 749 01 11Fax +41 22 749 09 47copyrightiso.orgwww.iso.orgBS ISO 17318:2015ISO 17318:2015(E)Foreword iv1 Scope . 12 Normative references 13 Principle 14 Reagents 15 Apparatus and materials 2
8、6 Procedure. 26.1 Sample preparation 26.2 Preparation of the test solution 26.3 Preparation of the blank test solution 26.4 Preparation of the working standard solution 26.5 Determination of arsenic, cadmium, chromium, lead and mercury contents by inductively coupled plasma optical emission spectros
9、copy (ICP-OES) 36.6 Calculation and expression of the results 47 Precision . 47.1 Ring test 47.2 Repeatability . 47.3 Reproducibility . 48 Test report . 4Annex A (informative) Interlaboratory testing . 6Bibliography .30 ISO 2015 All rights reserved iiiContents PageBS ISO 17318:2015ISO 17318:2015(E)F
10、orewordISO (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 interested in a subject for which a tec
11、hnical 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 Commission (IEC) on all matters o
12、f 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 documents should be noted. This document
13、 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 for identifying any or all such p
14、atent 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 convenience of users and does no
15、t 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: Foreword Supplementary information
16、.The committee responsible for this document is ISO/TC 134, Fertilizers and soil conditioners.iv ISO 2015 All rights reservedBS ISO 17318:2015Fertilizers and soil conditioners Determination of arsenic, cadmium, chromium, lead and mercury contents1 ScopeThis International Standard specifies the test
17、methods for determination of metals soluble in nitric acid: arsenic, cadmium, chromium, lead, and mercury contents in fertilizers.This International Standard is applicable to the analysis of arsenic, cadmium, chromium, lead, and mercury contents in fertilizers. Special attention should be given when
18、 analysing some micro-nutrients fertilizers.2 Normative referencesThe following documents, in whole or 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 t
19、he referenced document (including any amendments) applies.ISO 3696, Water for analytical laboratory use Specification and test methods3 PrincipleArsenic, cadmium, chromium, lead, and mercury in the test portion are extracted by means of nitric acid digestion in a microwave digestion system. The dige
20、sted solution will be measured by inductively coupled plasma optical emission spectroscopy (ICP-OES). Indium will be used as internal standard substance when chromium or lead is determined.NOTE An internal standard is recommended for metals to correct for solution matrix differences between the cali
21、bration standards and the fertilizer digests, any other internal standard materials with equal effect could be utilized, provided none of these are contained in the fertilizer samples.4 ReagentsWARNING Nitric acid is corrosive and oxidizer. The related operations shall be performed in fume hood. Thi
22、s standard does not point out all possible safety problems, and the user shall bear the responsibility to take proper safety and health measures, and ensure the operations compliant with the conditions stipulated by the related laws and regulations of the state.Use only reagents of recognized analyt
23、ical grade, and water conforming to grade 3 of ISO 3696:1987.4.1 Nitric acid, d = 1,40 g/ml, recommend to use trace element grade nitric acid.4.2 Nitric acid solution, add 1 volume of nitric acid to 9 volume of water.4.3 Standard stock solution of arsenic, cadmium, chromium, lead, mercury, 1 000 mg/
24、l certificated substance.4.4 Indium standard stock solution, 1 000 mg/l.Weigh In(NO3)3 H2O containing 0,262 0 g In(NO3)3 to a 100 ml beaker, dissolved by nitric acid solution (4.2), then transfer to a 100 ml volumetric flask, fill to the mark with nitric acid solution (4.2), and mix.INTERNATIONAL ST
25、ANDARD ISO 17318:2015(E) ISO 2015 All rights reserved 1BS ISO 17318:2015ISO 17318:2015(E)4.5 Indium standard solution, 5 mg/l. Dilute 1 000 mg/l Indium standard stock solution with nitric acid solution (4.2) to 5 mg/l.4.6 High-purity argon, content 99,999 %.5 Apparatus and materialsOrdinary laborato
26、ry apparatus and the following:5.1 Microwave digestion system.5.2 Inductively coupled plasma optical emission spectroscopy (ICP-OES), with a mixing device to add an internal standard.5.3 Sieve, with the aperture size of 0,50 mm.6 Procedure6.1 Sample preparationTake a representative fertilizer subsam
27、ple of 100 g. Grind it until it passes through a sieve of aperture size 0,5 mm, mix thoroughly for reasons of homogeneity, place in a clean, and dry bottle with lid.6.2 Preparation of the test solutionThe replicate experiments shall be done for the determination.Weigh 1 g sample (accurate to 0,1 mg,
28、 for fertilizer containing liming material or organic matrixes, reduce the weight properly) and transfer into a digestion vessel, keep the sample from adhering to sides of vessel. Place the digestion vessel into a fume hood, and add 10 ml of nitric acid (4.1). Predigest at room temperature until vig
29、orous foaming subsides. Then seal the vessel and put into the microwave digestion system.The ramped temperature program should be set under the instruction of the instrument manual. Ramping temperature from ambient to 160 C slowly in 10 min, and then hold at 160 C for another 10 min. Cool vessels to
30、 room temperature, vent, and transfer digests to a 100 ml volumetric flask, fill to the mark with water, and mix. Then the solution should be filtered through a dry, folded filter paper. Discard the first few millilitres portions of filter solution.6.3 Preparation of the blank test solutionThe exper
31、iment steps are the same as the preparation of the test solution, with the exception of adding the sample.6.4 Preparation of the working standard solutionPipet appropriate amount of element standard stock solution (4.3), dilute with nitric acid solution (4.2) into volumetric flasks according to Tabl
32、e 1, prepare blended multi-element standard solution series.Table 1 Typical concentrations of blended multi-element standard solutions (mg/l)Element standardAs Cd Cr Pb HgNo. 0 0 0 0 0 02 ISO 2015 All rights reservedBS ISO 17318:2015ISO 17318:2015(E)Element standardAs Cd Cr Pb HgNo. 1 0,02 0,02 0,02
33、 0,02 0,02No. 2 0,1 0,1 0,1 0,1 0,1No. 3 0,5 0,5 0,5 0,5 0,5No. 4 2,0 2,0 2,0 2,0 2,0No. 5 5,0 5,0 5,0 5,0 5,0NOTE Useful concentrations for standardization can be quite different for different instrument types.6.5 Determination of arsenic, cadmium, chromium, lead and mercury contents by inductively
34、 coupled plasmaoptical emission spectroscopy (ICP-OES)Before the determination, refer to the instrument operation manual. Select the best operation conditions in accordance with the elements properties. The recommended operating conditions of ICP are listed in Table 2. Other conditions which can ach
35、ieve the same results can also be used.Table 2 Recommended operating conditions of ICPWavelength As 189,042 nm, Cd 228,802 nm, Pb 220,353 nm, Cr 283,563 nm, Hg 184,950 nm, In 230,606 nm.Maximum integration time Low wavelength scale: 10 s, High wavelength scale: 10 sFlush velocity ofsample pump50 r/m
36、inAnalysis velocity of sample pump 50 r/minSample pump stable time 5 sLight source Radiofrequency, power of 1 150 WFlow rate of auxiliary gas 0,5 l/minFlow rate of gas within the nebu-lizer0,5 l/minNOTE Special attention should be given on the wavelength resolution of ICP instrument, the use of a se
37、cond or third wavelength for confirmation purposes may be recommended, if appropriate.Determine the working standard solutions (6.4), the blank test solution (6.3), and the test solutions (6.2) in order. When the concentration of Cr or Pb are determined, use the 5mg/l indium standard solution (4.5)
38、as the internal standard substance, mix the internal standard substance solution and test solution (1:5 V/V) by a mixing device. If the concentration of the element in the test solution exceeds the concentration range of the standard curve, dilute the test solution to a certain ratio with nitric aci
39、d solution (4.2) for re-determination.Table 1 (continued) ISO 2015 All rights reserved 3BS ISO 17318:2015ISO 17318:2015(E)6.6 Calculation and expression of the resultsThe determination results of elements (mg/kg) are calculated as follows:XD=()ccm0100(1)whereC is the concentration in mg/l, of the de
40、termined element in the test solution;c0is the concentration in mg/l, of the determined element in the blank test solution;100 is the total volume in ml, of the test solution;D is the dilution ratio of the test solution when required, otherwise D is removed or assigned a value of 1;m is the mass in
41、g, of the test portion.The determination result is the arithmetic average of the parallel determination results.7 Precision7.1 Ring testDetails of Ring test on the precision of the method are summarized in Annex A.7.2 RepeatabilityElement As Cd Cr Pb HgRepeatability limit, r, mg/kg0,227x0,6210,173x0
42、,586 20,145x0,755 20,100x0,849 90,252x0,582 47.3 ReproducibilityElement As Cd Cr Pb HgReproducibility limit, R, mg/kg0,316x0,8090,048x1,116 71,017x0,521 90,499x0,643 20,374x0,771 58 Test reportThe test report shall contain at least the following information:a) all information necessary for the compl
43、ete identification of the sample;b) test method used with reference to this International Standard (i.e. ISO 17318);c) test results obtained;d) date of sampling and sampling procedure (if known);e) date when the analysis was finished;f) whether the requirement of the repeatability limit has been ful
44、filled.4 ISO 2015 All rights reservedBS ISO 17318:2015ISO 17318:2015(E)All operating details not specified in this standard, or regarded as optional, together with details of any incidents occurred when performing the method, which might have influenced the test results. ISO 2015 All rights reserved
45、 5BS ISO 17318:2015ISO 17318:2015(E)Annex A (informative) Interlaboratory testingA.1 OverviewThe International Laboratories Ring Tests of this International Standard have been accomplished from Sep. 2012 to Dec. 2012. There are 14 laboratories participating in the two parallel tests on each four sam
46、ples. This international ring test was conducted by Shanghai Research Institute of Chemical Industry, P. R. China, the statistician analysis and final report was prepared by Shanghai Research Institute of Chemical Industry, P. R. China.The following are the14 laboratories participating in the two pa
47、rallel tests on each four samples. Shanghai Research Institute of Chemical Industry, Testing Center, China CF Industries Laboratory, USA Jiangsu Province Products Quality Supervising and Testing Institute, China Hunan Province Products Quality Supervising and Testing Institute, China Shandong Provin
48、ce Products Quality Supervising and Testing Institute, China Guizhou Province Products Quality Supervising and Testing Institute, China Guizhou Kailin Quality Testing Center, China Guangxi Zhuang Autonomous Region Products Quality Supervising and Testing Institute, China Heilongjiang Province Produc
49、ts Quality Supervising and Testing Institute, China Xingjiang Uygur Autonomous Region Products Quality Supervising and Testing Institute, China Yunnan Province Chemical Products Quality Supervising and Testing Center, China Shanghai Entry-Exit Inspection and Quarantine Bureau, China Yunnan Province Products Quality Supervising and Testing Institute, China Shenyang Fertilizer Quality Supervising and Testing Center, Ministry of Agriculture, ChinaNOTE The above sequence has nothing to do with the order of the tes
