1、BSI Standards PublicationBS EN ISO 17380:2013Soil quality Determinationof total cyanide and easilyliberatable cyanide Continuous-flow analysismethod (ISO 17380:2013)BS EN ISO 17380:2013 BRITISH STANDARDNational forewordThis British Standard is the UK implementation of EN ISO 17380:2013. It supersede
2、s BS ISO 17380:2004 which is withdrawn.The UK participation in its preparation was entrusted to Technical Committee EH/4, Soil quality.A list of organizations represented on this committee can be obtained on request to its secretary.This publication does not purport to include all the necessary prov
3、isions of a contract. Users are responsible for its correct application. The British Standards Institution 2013. Published by BSI Standards Limited 2013ISBN 978 0 580 76239 0 ICS 13.080.10 Compliance with a British Standard cannot confer immunity from legal obligations.This British Standard was publ
4、ished under the authority of the Standards Policy and Strategy Committee on 31 July 2013.Amendments issued since publicationDate Text affectedEUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN ISO 17380 June 2013 ICS 13.080.10 English Version Soil quality - Determination of total cyanide and easil
5、y liberatable cyanide - Continuous-flow analysis method (ISO 17380:2013) Qualit du sol - Dtermination des cyanures totaux et des cyanures aisment librables - Mthode danalyse en flux continu (ISO 17380:2013) Bodenbeschaffenheit - Bestimmung des Gehalts an gesamtem Cyanid und leicht freisetzbarem Cyan
6、id - Verfahren mittels kontinuierlicher Durchfluanalyse (ISO 17380:2013) This European Standard was approved by CEN on 8 June 2013. CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this European Standard the status of a national stan
7、dard 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 Standard exists in three official versions (English, French, German). A version in a
8、ny 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 national standards bodies of Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Rep
9、ublic, Denmark, Estonia, Finland, Former Yugoslav Republic of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and United Kingdom. EUROPEA
10、N 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 reserved worldwide for CEN national Members. Ref. No. EN ISO 17380:2013: EBS EN ISO 1738
11、0:2013EN ISO 17380:2013 (E) 3 Foreword 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 NEN. This European Standard shall be given
12、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 that some of the elements of this document may
13、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 implement this European Standard: Austria,
14、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, Slovakia, Slovenia, Spain, Sweden, Sw
15、itzerland, 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. BS EN ISO 17380:2013ISO 17380:2013(E) ISO 2013 All rights reserved iiiContents PageForeword ivIntroduction v1 Scope . 12 Normative reference
16、s 13 Terms and definitions . 14 Principle 24.1 Pretreatment of soil samples 24.2 Determination of total cyanide content . 24.3 Determination of easily-liberatable cyanide content 25 Reagents 25.1 General reagents 25.2 Reagents for determination of cyanide 35.3 Standard solutions for cyanide determin
17、ation . 46 Apparatus . 66.1 Standard laboratory glassware and laboratory equipment . 66.2 Continuous flow analysis system 66.3 Shaking machine 77 Sampling, sample preparation and extraction 88 Working range. 89 Procedure. 89.1 General . 89.2 Checking analysis system for correct function 89.3 Calibra
18、tion graph 99.4 Measurement of samples . 99.5 Cleaning of the analysis system . 1010 Calculation of the cyanide content in the sample 1011 Precision 1012 Test report 11Annex A (informative) Recovery and repeatability 12Annex B (informative) Information on continuous flow automatic distillation appar
19、atus .14Annex C (informative) Alternative distillation buffer (pH = 3,8) .15Bibliography .16BS EN ISO 17380:2013ISO 17380:2013(E)ForewordISO (the International Organization for Standardization) is a worldwide federation of national standards bodies (ISO member bodies). The work of preparing Internat
20、ional 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, governmental and non-governmental, in liaison with I
21、SO, also take part in the work. ISO collaborates closely with the International Electrotechnical Commission (IEC) on all matters of electrotechnical standardization.International Standards are drafted in accordance with the rules given in the ISO/IEC Directives, Part 2.The main task of technical com
22、mittees is to prepare International Standards. Draft International Standards adopted by the technical committees are circulated to the member bodies for voting. Publication as an International Standard requires approval by at least 75 % of the member bodies casting a vote.Attention is drawn to the p
23、ossibility 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.ISO 17380 was prepared by Technical Committee ISO/TC 190, Soil quality, Subcommittee SC 3, Chemical methods and soil characterist
24、ics.This second edition cancels and replaces the first edition (ISO 17380:2004), which has been technically revised.iv ISO 2013 All rights reservedBS EN ISO 17380:2013ISO 17380:2013(E)IntroductionCyanides may be present in soil as cyanide ions and as complex cyanides. They can be determined as easil
25、y-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 easily-liberatable cyanide, complex cyanides and total cyanide.Methods using flo
26、w 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) method uses an automated dosage of the sample into a flow system (manifold)
27、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. flow cell photometer).1,2In ISO 11262 a manual method for the photometric and
28、 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 Standard. These differences are not considered to be very significant for this anal
29、ysis. 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 analytical procedure described in ISO 14403-27is identical to the one specified in
30、 this International Standard. ISO 2013 All rights reserved vBS EN ISO 17380:2013BS EN ISO 17380:2013Soil quality Determination of total cyanide and easily liberatable cyanide Continuous-flow analysis methodWARNING Cyanide solutions are highly toxic. Appropriate measures shall be taken to avoid inges
31、tion. Care should be taken in the disposal of these solutions.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 a
32、pplies to all types of soil with cyanide contents above 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 s
33、ignal and can only be prevented by diluting the sample 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
34、latest edition of the referenced document (including any 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 Determinati
35、on of total cyanideISO 11465, Soil quality Determination 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 d
36、efinitions apply.3.1total cyanide contentcontent of inorganic 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, pal
37、ladium and platinum cyanide complexes3.2easily-liberatable 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
38、method described in this International StandardNote 1 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), hexa
39、cyanoferrate(III) and hexocyanoferrate(II) is determined with the method for easily-liberatable cyanide. Organic cyanide compounds (such as acetonitrile) are not determined.INTERNATIONAL STANDARD ISO 17380:2013(E) ISO 2013 All rights reserved 1BS EN ISO 17380:2013ISO 17380:2013(E)Note 2 to entry: In
40、 connection with waste from the production of gold, “easily liberatable cyanide” is named “weak acid dissociable cyanide”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
41、mol/l sodium hydroxide solution for 16 h. The extract is diluted 100 times, after which analysis of total and/or easily-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
42、 flowing stream after addition of a buffer solution, with an initial pH of 3,8, by the effect of UV light. An UV-B 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
43、into cyanide. The hydrogen cyanide present at these conditions is separated by in-line distillation at a heating bath 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 cyanog
44、en chloride. This reacts with pyridine-4-carboxylic acid and 1,3-dimethylbarbituric acid to give a purple colour. 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
45、 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 : 0,42 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
46、.3 Determination of easily-liberatable cyanide contentBefore distillation, and without UV decomposition, a zinc sulfate 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 condi
47、tions is separated by distillation at a temperature of 125 C and photometrically determined as described under 4.2.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 demi
48、neralized 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 Hydrochloric acid c(HCl) = 0,1 mol/l.Dilute 100 ml of 1 mol
49、/l hydrochloric acid (5.1.2) with water to 1 000 ml.2 ISO 2013 All rights reservedBS EN ISO 17380:2013ISO 17380:2013(E)5.1.4 Sodium hydroxide solution c(NaOH) = 2,5 mol/l.Dissolve 100 g of NaOH in water and dilute with water to 1 000 ml. Store in a polyethylene bottle.5.1.5 Sodium hydroxide solution c(NaOH) = 1 mol/l.Dissolve 40 g of NaOH in water and dilute with water to 1 000 ml. Store in a polyethylene bottle.5.1.6 Sodium hydroxide solution c(NaOH) = 0,025 mol/l.Dilute 25 ml of 1 mol/l sodium hydroxide (5.1.5) wit
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