1、BS ISO 14869-3:2017Soil quality Dissolution forthe determination of totalelement contentPart 3: Dissolution with hydrofluoric,hydrochloric and nitric acids usingpressurised microwave techniqueBSI Standards PublicationWB11885_BSI_StandardCovs_2013_AW.indd 1 15/05/2013 15:06BS ISO 14869-3:2017 BRITISH
2、 STANDARDNational forewordThis British Standard is the UK implementation of ISO 14869-3:2017. The UK participation in its preparation was entrusted to TechnicalCommittee EH/4, Soil quality.A list of organizations represented on this committee can be obtained on request to its secretary.This publicat
3、ion does not purport to include all the necessary provisions of a contract. Users are responsible for its correct application. The British Standards Institution 2017.Published by BSI Standards Limited 2017ISBN 978 0 580 84002 9 ICS 13.080.10 Compliance with a British Standard cannot confer immunity
4、from legal obligations.This British Standard was published under the authority of the Standards Policy and Strategy Committee on 28 February 2017.Amendments/corrigenda issued since publicationDate T e x t a f f e c t e dBS ISO 14869-3:2017 ISO 2017Soil quality Dissolution for the determination of to
5、tal element content Part 3: Dissolution with hydrofluoric, hydrochloric and nitric acids using pressurised microwave techniqueQualit du sol Mise en solution pour la dtermination des teneurs lmentaires totales Partie 3: Mise en solution par lacide fluorhydrique, lacide chlorhydrique et lacide nitriqu
6、e laide de la technique de micro-ondes pressurisesINTERNATIONAL STANDARDISO14869-3First edition2017-02Reference numberISO 14869-3:2017(E)BS ISO 14869-3:2017ISO 14869-3:2017(E)ii ISO 2017 All rights reservedCOPYRIGHT PROTECTED DOCUMENT ISO 2017, Published in SwitzerlandAll rights reserved. Unless oth
7、erwise 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 the internet or an intranet, without prior written permission. Permission can be requested from either ISO at the address
8、 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 47copyrightiso.orgwww.iso.orgBS ISO 14869-3:2017ISO 14869-3:2017(E)Foreword ivIntroduction v1 Scope . 12 Normative refer
9、ences 13 Terms and definitions . 14 Safety remarks 25 Principle 26 Interferences and sources of errors . 27 Reagents 38 Apparatus . 39 Sampling and sample pre-treatment 49.1 Sample pre-treatment . 49.2 Pre-treatment of test portion . 410 Procedure. 410.1 Blank test . 410.2 Test portion 510.3 Dissolu
10、tion 511 Quality control 612 Test report . 613 Performance characteristics 6Annex A (informative) Validation data . 7Bibliography 9 ISO 2017 All rights reserved iiiContents PageBS ISO 14869-3:2017ISO 14869-3:2017(E)ForewordISO (the International Organization for Standardization) is a worldwide feder
11、ation 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 technical committee has been established has the right to be represented on that commit
12、tee. 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 of electrotechnical standardization.The procedures used to develop this document and
13、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 was drafted in accordance with the editorial rules of the ISO/IEC Directives, Part
14、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 patent rights. Details of any patent rights identified during the development of t
15、he 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 not constitute an endorsement.For an explanation on the meaning of ISO specific
16、terms and expressions related to conformity assessment, as well as information about ISOs adherence to the World Trade Organization (WTO) principles in the Technical Barriers to Trade (TBT) see the following URL: www .iso .org/ iso/ foreword .html.This document was prepared by Technical Committee IS
17、O/TC 190, Soil quality, Subcommittee SC 3, Chemical methods and soil characteristics.A list of all parts in the ISO 14869 series can be found on the ISO website.iv ISO 2017 All rights reservedBS ISO 14869-3:2017ISO 14869-3:2017(E)IntroductionThis document is a module for analysis of inorganic parame
18、ters in soil and soil material. This document concerns the complete dissolution for the subsequent analysis of elements.An acid mixture based on nitric acid, hydrofluoric acid and hydrochloric acid will be used to totally dissolve most soils and similar materials. The resulting solutions can be dete
19、rmined separately or after combination with atomic absorption spectrometry (AAS) techniques, inductively coupled plasma optical emission spectrometry (ICP-OES) or inductively coupled plasma mass spectrometry (ICP-MS) determination methods. ISO 2017 All rights reserved vBS ISO 14869-3:2017BS ISO 1486
20、9-3:2017Soil quality Dissolution for the determination of total element content Part 3: Dissolution with hydrofluoric, hydrochloric and nitric acids using pressurised microwave technique1 ScopeThis document specifies a method for microwave-assisted dissolution of soil samples for determination of to
21、tal element contents ofAl, As, Ba, Ca, Cd, Co, Cr, Cs, Cu, Fe, Hg, K, Li, Mg, Mn, Na, Ni, P, Pb, S, Se, Sb, Sr, Tl, V, Znusing an acid mixture of nitric acid (HNO3), hydrofluoric acid (HF) and hydrochloric acid (HCl). This method is applicable to all types of soil and soil material.The main field of
22、 application is geological and pedological survey.The acid mixture is suitable for total dissolution of element contents in soil (major, minor and trace), but some refractory compounds such as SiO2, TiO2, spinel, Al2O3or other compounds may remain as a residue. In such a case, the use of alkaline fu
23、sion, following ISO 14869-2, is recommended to determine the true total element content.NOTE 1 In environmental studies, usually, aqua regia extraction is applied using ISO 12914 or ISO 11466.Solutions produced by the microwave method are suitable for analysis, for example, by using atomic absorptio
24、n spectrometry (FAAS, HGAAS, CVAAS, GFAAS), inductively coupled plasma optical emission spectrometry (ICP-OES) and inductively coupled plasma mass spectrometry (ICP-MS).NOTE 2 Due to the presence of chloride in the digestion solution, limitations for the application of some analytical techniques can
25、 occur.2 Normative referencesThe following documents are referred to in the text in such a way that some or all of their content constitutes requirements of this document. For dated references, only the edition cited applies. For undated references, the latest edition of the referenced document (inc
26、luding any amendments) applies.ISO 3696, Water for analytical laboratory use Specification and test methodsISO 11074, Soil quality VocabularyISO 11464, Soil quality Pretreatment of samples for physico-chemical analysisISO 11465, Soil quality Determination of dry matter and water content on a mass ba
27、sis Gravimetric method3 Terms and definitionsFor the purposes of this document, the terms and definitions given in ISO 11074, ISO 11464 and ISO 11465 apply.INTERNATIONAL STANDARD ISO 14869-3:2017(E) ISO 2017 All rights reserved 1BS ISO 14869-3:2017ISO 14869-3:2017(E)ISO and IEC maintain terminologic
28、al databases for use in standardization at the following addresses: IEC Electropedia: available at h t t p :/ www .electropedia .org/ ISO Online browsing platform: available at h t t p :/ www .iso .org/ obp4 Safety remarksAll this work has to be performed by trained persons.The reagents used within
29、this document are strongly corrosive and potentially very harmful. Safety precautions are absolutely necessary due to strong corrosive reagents, high temperature and high pressure.All procedures have to be performed in a hood or in closed force-ventilated equipment. By the use of strong oxidising re
30、agents, the formation of explosive organic intermediates is possible, especially when dealing with samples with a high-organic content. Do not open pressurised vessels before they have cooled down. Avoid contact with the chemicals and the gaseous reaction products.DANGER Hydrofluoric acid is dangero
31、us if inhaled as vapour or by direct contact with skin and mucosa. It should be noted that the effects of exposure to HF may not be apparent for several hours, particularly for skin, after which effective treatment can be difficult. Users of this document should familiarize themselves with the neces
32、sary precautions, taking professional and medical advice where appropriate. The use of an efficient exhaust hood, rubber gloves, glasses or face protection and protected pipetting devices is essential. Observe safety precaution for handling hydrofluoric acid.WARNING Several stages of the procedure a
33、re potentially hazardous, especially those involving concentrated acids under pressurized conditions. Users of this document should familiarize themselves with the necessary safety precautions and, where appropriate, any legal requirements for their use. If in doubt, seek professional advice.5 Princ
34、ipleThe laboratory sample shall be treated in accordance with the principles of ISO 11464 in order to produce a homogeneous test sample from which a representative test portion can be sub-sampled and completely dissolved in an acid mixture by microwave-assisted heating.6 Interferences and sources of
35、 errorsDuring trace element determinations, contaminations shall be avoided. The container in which the sample is delivered and stored can be a source of errors. The containers material shall be chosen such that it does not absorb the elements to be determined (e.g. elemental Hg can penetrate polyet
36、hylene walls very fast in both directions).Grinding or milling samples includes a risk of contamination of the sample by the environment (e.g. air, dust, wear of milling equipment). Due to the volatility of some compounds, it is important to take care that the sample is not heated before the dissolu
37、tion and that the volatile reaction products which might be formed during the dissolution are not allowed to escape.For the determination of elements forming volatile compounds (e.g. Hg, As, Cr, Se), special care shall be taken during sample pre-treatment and pressurized digestions.High acid and hig
38、h dissolved matrix element concentrations in the dissolution solution may cause interferences in the analytical method.Depending on the concentration of the elements of interest, particular attention needs to be paid to the cleaning of the laboratory equipment. It is recommended to thoroughly clean
39、all laboratory equipment and as a minimum, leave the equipment standing over night in 5 % nitric acid.2 ISO 2017 All rights reservedBS ISO 14869-3:2017ISO 14869-3:2017(E)Some elements of interest can be lost due to precipitation with ions present in the digestion solution, e.g. low-solubility chlori
40、de, fluoride or sulfate compounds. Before starting filtration, boric acid should be added to bind excess hydrofluoric acid and re-dissolve insoluble fluorides. During filtration, avoid introduction of contaminants.7 ReagentsUse only reagents of recognized analytical grade.7.1 Water.Deionised or dist
41、illed water used shall conform at least to grade 2 of ISO 3696.It is recommended that the same batch of water be used throughout a given batch of determinations. Blank tests are carried out in each series of sample determination.7.2 Hydrochloric acid, c(HCl) = 12 mol/l; = 1,18 g/ml; w(HCl) = 36 %.7.
42、3 Nitric acid, c(HNO3) = 14,3 mol/l; = 1,4 g/ml; not less than w(HNO3) = 65 %.7.4 Nitric acid, diluted, c(HNO3) = 0,5 mol/l, dilute 35 ml nitric acid (7.3) to 1 l with water (7.1).7.5 Hydrofluoric acid, c(HF) = 22,6 mol/l, = 1,13 g/ml, w(HF) = 40 %.7.6 Antifoaming agent.For example, n-dodecane (C12H
43、26) or polyethyleneglycol p-(1,1,3,3-tetramethylbutyl)-phenyl ether (C14H22O(C2H4O)n) is suitable.7.7 Boric acid solution, w(H3BO3) approximately 4 %.Dissolve 20 g boric acid (H3BO3) in 450 ml of water and dilute to 500 ml with water. Store in a polyethylene bottle. Solubility limit of H3BO3is 49 g
44、in 1 000 ml of water.8 ApparatusAll glassware and plasticware shall be adequately cleaned and stored in order to avoid any contamination.8.1 Microwave-assisted dissolution system.8.1.1 Microwave apparatus requirements, microwave apparatus for pressurised digestions preferably a temperature-regulated
45、 device, in combination with pressure measurement for laboratory use only. A laboratory-grade microwave unit cavity shall be well ventilated and corrosion resistant. All electronics shall be protected against corrosion for safe operation. The temperature performance requirements necessitate that the
46、 microwave decomposition system is able to sense the temperature with an accuracy of 2,5 C and automatically adjust the microwave field output power within 2 s of sensing. Temperature sensors should be accurate to 2 C including at the final reaction temperature of (175 5) C. Temperature feedback con
47、trol provides the primary performance mechanism for the method. Due to the variability in sample matrices and microwave equipment (i.e. different vessel types and microwave designs), control of the temperature during the dissolution process is important for ensuring reproducible microwave heating fo
48、r different units. ISO 2017 All rights reserved 3BS ISO 14869-3:2017ISO 14869-3:2017(E)The accuracy of the temperature measurement system shall be periodically tested at an elevated temperature according to the manufacturers instructions. If the temperature deviates by more than 2,5 C from the tempe
49、rature measured by an external calibrated temperature measurement system, the microwave temperature measurement system should be calibrated.8.1.2 Rotating turntable.The speed of the turntable should be a minimum of 3 r/min. Other types of equipment used to assist in achieving uniformity of the microwave field may also be appropriate.8.1.3 Microwave dissolution vessels.Digestion vessels shall be made of materials that are microwave transparent and resistant to reagents and temperature, such as fluoroc
