DIN EN ISO 17380-2013 Soil quality - Determination of total cyanide and easily liberatable cyanide - Continuous-flow analysis method (ISO 17380 2013) German version EN ISO 17380 20.pdf

1、October 2013Translation by DIN-Sprachendienst.English price group 12No part of this translation may be reproduced without prior permission ofDIN Deutsches Institut fr Normung e. V., Berlin. Beuth Verlag GmbH, 10772 Berlin, Germany,has the exclusive right of sale for German Standards (DIN-Normen).ICS

2、 13.080.10!%)d“2066594www.din.deDDIN EN ISO 17380Soil quality Determination of total cyanide and easily liberatable cyanide Continuous-flow analysis method (ISO 17380:2013);English version EN ISO 17380:2013,English translation of DIN EN ISO 17380:2013-10Bodenbeschaffenheit Bestimmung des Gehalts an

3、Gesamtcyanid und leicht freisetzbarem Cyanid Verfahren mittels kontinuierlicher Durchflussanalyse (ISO 17380:2013);Englische Fassung EN ISO 17380:2013,Englische bersetzung von DIN EN ISO 17380:2013-10Qualit du sol Dtermination des cyanures totaux et des cyanures aisment librables Mthode danalyse en

4、flux continu (ISO 17380:2013);Version anglaise EN ISO 17380:2013,Traduction anglaise de DIN EN ISO 17380:2013-10SupersedesDIN ISO 17380:2006-05www.beuth.deIn case of doubt, the German-language original shall be considered authoritative.Document comprises 24 pages09.13 DIN EN ISO 17380:2013-10 2 A co

5、mma is used as the decimal marker. National foreword This document (EN ISO 17380:2013) has been prepared by Technical Committee ISO/TC 190 “Soil quality” (Secretariat: NEN, Netherlands) and has been taken over by Technical Committee CEN/TC 345 “Charac-terization of soils” (Secretariat: NEN, Netherla

6、nds). The responsible German body involved in its preparation was the Normenausschuss Wasserwesen (Water Practice Standards Committee), Working Committees NA 119-01-02-02-04 AK Elementanalytik and NA 119-01-02-02 UA Chemische und physikalische Verfahren. The DIN Standards corresponding to the Intern

7、ational Standards referred to in this document are as follows: ISO 3696 DIN ISO 3696 ISO 11262 DIN ISO 11262 ISO 11465 DIN ISO 11465 ISO 14507 DIN ISO 14507 This document contains a national footnote to Subclause 5.1.7, NOTE. In accordance with the result of the parallel voting procedure within the

8、scope of the Agreement on technical cooperation between ISO and CEN (Vienna Agreement), International Standard ISO 17380:2013 has been adopted as a European Standard. This standard includes safety requirements. Amendments This standard differs from DIN ISO 17380:2006 as follows: a) normative referen

9、ces have been updated; b) the standard has been editorially revised; c) a second NOTE has been added under 3.2; d) Subclause 5.2.6 “Rinse solution for the sampler” has been added; e) Table 2 has been deleted; f) in Figure 1, the numerical values of items 3, 5, 6, 7, 8 and 9 have been changed; g) in

10、Subclause 9.2.7, the values specified for thiocyanate have been changed. Previous editions DIN ISO 17380: 2006-05 DIN EN ISO 17380:2013-10 3 National Annex NA (informative) Bibliography DIN ISO 3696, Water for analytical laboratory use Specification and test methods DIN ISO 11262, Soil quality Deter

11、mination of total cyanide DIN ISO 11465, Soil quality Determination of dry matter and water content on a mass basis Gravimetric method DIN ISO 14507, Soil quality Pretreatment of samples for determination of organic contaminants DIN EN ISO 17380:2013-10 4 This page is intentionally blank EUROPEAN ST

12、ANDARD NORME EUROPENNE EUROPISCHE NORM EN ISO 17380 June 2013 ICS 13.080.10 English Version Soil quality - Determination of total cyanide and easily liberatable cyanide - Continuous-flow analysis method (ISO 17380:2013) Qualit du sol - Dtermination des cyanures totaux et des cyanures aisment librabl

13、es - Mthode danalyse en flux continu (ISO 17380:2013) Bodenbeschaffenheit - Bestimmung des Gehalts an Verfahren mittels kontinuierlicher DurchflussanalyseThis European Standard was approved by CEN on 8 June 2013. CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipula

14、te the conditions for giving this European Standard the status of a national standard without any alteration. Up-to-date lists and bibliographical references concerning such national standards may be obtained on application to the CEN-CENELEC Management Centre or to any CEN member. This European Sta

15、ndard exists in three official versions (English, French, German). A version in any other language made by translation under the responsibility of a CEN member into its own language and notified to the CEN-CENELEC Management Centre has the same status as the official versions. CEN members are the na

16、tional standards bodies of Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, Former Yugoslav Republic of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, S

17、lovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and United Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZATION COMIT EUROPEN DE NORMALISATION EUROPISCHES KOMITEE FR NORMUNG Management Centre: Avenue Marnix 17, B-1000 Brussels 2013 CEN All rights of exploitation in any form and by any means reserve

18、d worldwide for CEN national Members. Ref. No. EN ISO 17380:2013: E(ISO 17380:2013) Gesamtcyanid und leicht freisetzbarem Cyanid - Contents Page Foreword . 3 Introduction . 4 1 Scope . 5 2 Normative references. 5 3 Terms and definitions 5 4 Principle 6 4.1 Pretreatment of soil samples 6 4.2 Determin

19、ation of total cyanide content 6 4.3 Determination of easily-liberatable cyanide content 6 5 Reagents . 6 5.1 General reagents 6 5.2 Reagents for determination of cyanide 7 5.3 Standard solutions for cyanide determination . 8 6 Apparatus 10 6.1 Standard laboratory glassware and laboratory equipment

20、. 10 6.2 Continuous flow analysis system 10 6.3 Shaking machine 11 7 Sampling, sample preparation and extraction 12 8 Working range 12 9 Procedure 12 9.1 General 12 9.2 Checking analysis system for correct function 12 9.3 Calibration graph 13 9.4 Measurement of samples 13 9.5 Cleaning of the analysi

21、s system . 14 10 Calculation of the cyanide content in the sample 14 11 Precision . 14 12 Test report . 15 Annex A (informative) Recovery and repeatability . 16 Annex B (informative) Information on continuous flow automatic distillation apparatus . 18 Annex C (informative) Alternative distillation b

22、uffer (pH = 3,8) 19 Bibliography 20 2DIN EN ISO 17380:2013-10EN ISO 17380:2013 (E) This document (EN ISO 17380:2013) has been prepared by Technical Committee ISO/TC 190 “Soil quality” in collaboration with Technical Committee CEN/TC 345 “Characterization of soils” the secretariat of which is held by

23、 NEN. This European Standard shall be given the status of a national standard, either by publication of an identical text or by endorsement, at the latest by December 2013, and conflicting national standards shall be withdrawn at the latest by December 2013. Attention is drawn to the possibility tha

24、t some of the elements of this document may be the subject of patent rights. CEN and/or CENELEC shall not be held responsible for identifying any or all such patent rights. According to the CEN-CENELEC Internal Regulations, the national standards organizations of the following countries are bound to

25、 implement this European Standard: Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, Former Yugoslav Republic of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Ro

26、mania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and the United Kingdom. Endorsement notice The text of ISO 17380:2013 has been approved by CEN as EN ISO 17380:2013 without any modification. Foreword3DIN EN ISO 17380:2013-10 EN ISO 17380:2013 (E) IntroductionCyanides may be present in s

27、oil as cyanide ions and as complex cyanides. They can be determined as easily-liberatable cyanide or as total cyanide. Complex cyanide can be calculated by subtracting the easily-liberatable cyanide result from the total cyanide result. This International Standard specifies the determination of easi

28、ly-liberatable cyanide, complex cyanides and total cyanide.Methods using flow analysis automate wet chemical procedures and are particularly suitable for the processing of many analytes in water or soil extracts in large sample series at a high analysis frequency. The continuous flow analysis (CFA)

29、method uses an automated dosage of the sample into a flow system (manifold) where the analytes in the sample react with the reagent solution on their way through the manifold. The sample preparation may be integrated in the manifold. The reaction product is measured in a photometric detector (e.g. f

30、low cell photometer).1,2In ISO 11262 a manual method for the photometric and volumetric determination of total cyanide in soil samples is described. It should be noted that the total cyanide results in soil samples as described in ISO 11262 may show slight differences from this International Standar

31、d. These differences are not considered to be very significant for this analysis. The easily-liberatable cyanide test has been removed from ISO 11262 because the validation data for this method were very poor.For the analysis of cyanide in water ISO 14403-16and ISO 14403-27can be applied. The analyt

32、ical procedure described in ISO 14403-27is identical to the one specified in this International Standard.4DIN EN ISO 17380:2013-10EN ISO 17380:2013 (E) WARNING Cyanide solutions are highly toxic. Appropriate measures shall be taken to avoid ingestion. Care should be taken in the disposal of these so

33、lutions.1 ScopeThis International Standard specifies a method for the photometric determination of the total cyanide and easily-liberatable cyanide content in soil using automated distillation/continuous-flow analysis.The International Standard applies to all types of soil with cyanide contents abov

34、e 1 mg/kg on the basis of dry matter, expressed as cyanide ion.NOTE Sulfide concentrations in the sample higher than 40 mg/kg dry matter cause interference. This effect can be recognized by the split peaks and as a slow decrease of the detector signal and can only be prevented by diluting the sample

35、 extract.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 the referenced document (including a

36、ny amendments) applies.ISO 3696, Water for analytical laboratory use Specification and test methodsISO 9297,Water quality Determination of chloride Silver nitrate titration with chromate indicator (Mohrs method)ISO 11262, Soil quality Determination of total cyanideISO 11465, Soil quality Determinati

37、on of dry matter and water content on a mass basis Gravimetric methodISO 14507:2003, Soil quality Pretreatment of samples for determination of organic contaminants3 Terms and definitionsFor the purposes of this document, the following terms and definitions apply.3.1total cyanide contentcontent of in

38、organic cyanide compounds consisting of the sum of the contents of easily-liberatable cyanide species and cyanide bound to metal cyanides, with the exception of thiocyanate ions and only partial breakdown of the cyanide bound in cobalt, gold, palladium and platinum cyanide complexes3.2easily-liberat

39、able cyanidecontent of inorganic cyanide compounds consisting of the sum of the contents of the easily-liberatable cyanide ions and the cyanide bound in simple metal cyanides (all expressed as CN) which are determined under the conditions of the method described in this International StandardNote 1

40、to entry: The weakly complexed cyanide contained in tetracyanonickelate(II) and dicyanomercurate(II) is determined with the method for easily-liberatable cyanide. Up to 5 % of the strongly complexed cyanide in iron(III) hexacyanoferrate(II), hexacyanoferrate(III) and hexocyanoferrate(II) is determin

41、ed with the method for easily-liberatable cyanide. Organic cyanide compounds (such as acetonitrile) are not determined.5DIN EN ISO 17380:2013-10 EN ISO 17380:2013 (E) Note 2 to entry: In connection with waste from the production of gold, “easily liberatable cyanide” is named “weak acid dissociable c

42、yanide”8.3.3complex cyanide contenttotal cyanide content less than the easily-liberatable cyanide content4 Principle4.1 Pretreatment of soil samplesThe soil sample is extracted with 2,5 mol/l sodium hydroxide solution for 16 h. The extract is diluted 100 times, after which analysis of total and/or e

43、asily-liberatable cyanide is performed.4.2 Determination of total cyanide contentComplex bound cyanide, present in the diluted extract (0,025 mol/l NaOH), is decomposed in a continuously flowing stream after addition of a buffer solution, with an initial pH of 3,8, by the effect of UV light. An UV-B

44、 lamp and decomposition coil of borosilicate glass are used. UV light with a wavelength of less than 290 nm is absorbed by the glass, preventing the photolytic conversion of thiocyanate into cyanide. The hydrogen cyanide present at these conditions is separated by in-line distillation at a heating b

45、ath temperature of 125 C 2 C and then determined photometrically. The photometric determination is based on the reaction of cyanide with chloramine-T resulting in the formation of cyanogen chloride. This reacts with pyridine-4-carboxylic acid and 1,3-dimethylbarbituric acid to give a purple colour.

46、The absorbance at 606 nm is then measured to determine the cyanide content. When an interference filter is used, a peak wavelength of 600 nm 10 nm can be used.NOTE Addition of the buffer solution, with an initial pH of 3,8 (5.2.1), to the sample flow containing 0,025 mol/l NaOH (ratio 1,0 sample : 0

47、,42 buffer) leads to a final pH of 4,0. Varying the pH of the distillation between 3,8 and 5,7 leads to very small fluctuations in the recovery of hydrogen cyanide (only a few percent).4.3 Determination of easily-liberatable cyanide contentBefore distillation, and without UV decomposition, a zinc su

48、lfate solution is added to the sample flow, such that any complex iron cyanide(s) present are precipitated as zinc-cyanoferrate complexes. The hydrogen cyanide present during these conditions is separated by distillation at a temperature of 125 C and photometrically determined as described under 4.2

49、.NOTE The added zinc sulfate replaces a water reagent (see Table 1) used in the determination of total cyanide content.5 ReagentsOnly use reagents of recognized analytical grade and demineralized water or distilled water according to ISO 3696, Grade 1 or 2.5.1 General reagents5.1.1 Hydrochloric acid w(HCl) = 37 %.5.1.2 Hydrochloric acid c(HCl) = 1 mol/l.Dilute 83 ml of hydrochloric acid (5.1.1) with water to 1 000 ml.5.1.3 Hydrochlo