1、January 2013 Translation by DIN-Sprachendienst.English price group 8No 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、 65.080!$gF“1936835www.din.deDDIN EN 16195Fertilizers Determination of chlorides in the absence of organic material;English version EN 16195:2012,English translation of DIN EN 16195:2013-01Dngemittel Bestimmung von Chlorid bei Abwesenheit organischer Stoffe;Englische Fassung EN 16195:2012,Englische
3、bersetzung von DIN EN 16195:2013-01Engrais Dosage des chlorures en labsence de matires organiques;Version anglaise EN 16195:2012,Traduction anglaise de DIN EN 16195:2013-01SupersedesDIN CEN/TS 16195(DIN SPEC 91268):2011-08www.beuth.deIn case of doubt, the German-language original shall be considered
4、 authoritative.Document comprises 11 pages 12.12 DIN EN 16195:2013-01 2 A comma is used as the decimal marker. National foreword The method specified in this standard is based upon Regulation (EC) No 2003/2003 relating to fertilizers, Annex IV, method 6.1 (see Bibliography). This document (EN 16195:
5、2012) has been prepared by Technical Committee CEN/TC 260 “Fertilizers and liming materials” (Secretariat: DIN, Germany) under the mandate M/335. The responsible German body involved in its preparation was the Normenausschuss Lebensmittel und landwirtschaftliche Produkte (Food and Agricultural Produ
6、cts Standards Committee), Working Committee NA 057-03-02 AA Dngemittel. The DIN Standard corresponding to the International Standard referred to in this document is as follows: ISO 5725-2 DIN ISO 5725-2 Amendments This standard differs from DIN CEN/TS 16195 (DIN SPEC 91268):2011-08 as follows: a) th
7、e status of the Technical Specification has been changed to that of a European Standard; b) the standard has been editorially revised. Previous editions DIN CEN/TS 16195 (DIN SPEC 91268): 2011-08 National Annex NA (informative) Bibliography DIN ISO 5725-2, Accuracy (trueness and precision) of measur
8、ement methods and results Part 2: Basic method for the determination of repeatability and reproducibility of a standard measurement method EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN 16195 November 2012 ICS 65.080 Supersedes CEN/TS 16195:2011English Version Fertilizers - Determination of ch
9、lorides in the absence of organic material Engrais - Dosage des chlorures en labsence de matires organiques Dngemittel - Bestimmung von Chlorid bei Abwesenheit organischer Stoffe This European Standard was approved by CEN on 6 October 2012. CEN members are bound to comply with the CEN/CENELEC Intern
10、al Regulations which stipulate 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 C
11、EN member. This European Standard 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 vers
12、ions. CEN members are the national 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,
13、Poland, Portugal, Romania, Slovakia, 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 2012 CEN All rights of exploitation in any f
14、orm and by any means reserved worldwide for CEN national Members. Ref. No. EN 16195:2012: EEN 16195:2012 (E) 2 Contents Page Foreword 31 Scope 42 Normative references 43 Terms and definitions .44 Principle 45 Sampling .46 Reagents .47 Apparatus .58 Procedure .58.1 Preparation of the test portion and
15、 the solution 58.2 Determination .58.3 Blank test 68.4 Control test .69 Calculation and expression of the results 610 Precision .610.1 Inter-laboratory test .610.2 Repeatability .610.3 Reproducibility .611 Test report 7Annex A (informative) Statistical results of the inter-laboratory test 8Bibliogra
16、phy 9DIN EN 16195:2013-01 EN 16195:2012 (E) 3 Foreword This document (EN 16195:2012) has been prepared by Technical Committee CEN/TC 260 “Fertilizers and liming materials”, the secretariat of which is held by DIN. This European Standard shall be given the status of a national standard, either by pub
17、lication of an identical text or by endorsement, at the latest by May 2013, and conflicting national standards shall be withdrawn at the latest by May 2013. Attention is drawn to the possibility that some of the elements of this document may be the subject of patent rights. CEN and/or CENELEC shall
18、not be held responsible for identifying any or all such patent rights. This document supersedes CEN/TS 16195:2011. The following changes have been made to the former edition: a) the CEN Technical Specification has been adopted as a European Standard; b) the document has been editorially revised. Thi
19、s document has been prepared under a mandate given to CEN by the European Commission and the European Free Trade Association. According to the CEN/CENELEC Internal Regulations, the national standards organisations of the following countries are bound to implement this European Standard: Austria, Bel
20、gium, 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, Switz
21、erland, Turkey and the United Kingdom. DIN EN 16195:2013-01 EN 16195:2012 (E) 4 1 Scope This European Standard specifies a method for the determination of chlorides in the absence of organic material. The method is applicable to all fertilizers which are free from organic material. 2 Normative refer
22、ences The 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 any amendments) applies. E
23、N 1482-2, Fertilizers and liming materials Sampling and sample preparation Part 2: Sample preparation EN 12944-1:1999, Fertilizers and liming materials and soil improvers Vocabulary Part 1: General terms EN 12944-2:1999, Fertilizers and liming materials and soil improvers Vocabulary Part 2: Terms re
24、lating to fertilizers 3 Terms and definitions For the purposes of this document, the terms and definitions given in EN 12944 1:1999 and EN 12944-2:1999 apply. 4 Principle The chlorides, dissolved in water, are precipitated in an acid medium by an excess of standard solution of silver nitrate. The ex
25、cess is titrated with a solution of ammonium thiocyanate in the presence of ferric ammonium sulfate (Volhards method). 5 Sampling Sampling is not part of the method specified in this document. A recommended sampling method is given in EN 1482-1. Sample preparation shall be carried out in accordance
26、with EN 1482-2. Grinding of the laboratory sample is recommended for homogeneity reasons. 6 Reagents Use only reagents of recognised analytical grade. 6.1 Water, distilled or demineralised and free from chlorides. 6.2 Nitrobenzene or diethyl ether. 6.3 Nitric acid, c = 10 mol/l. 6.4 Indicator soluti
27、on. Dissolve 40 g of ferric ammonium sulfate Fe2(SO4)3. (NH4)2SO4. 24H2O, in water and make up to 1 l. DIN EN 16195:2013-01 EN 16195:2012 (E) 5 6.5 Silver nitrate standard solution, c = 0,1 mol/l. Preparation: since this salt is hygroscopic and cannot be dried without risk of decomposition, it is ad
28、visable to weigh out an amount of approximately 18 g, dissolve in water and make up the volume to 1 l. Adjust to c = 0,1 mol/l substance concentration by titration of ammonium thiocyanate 0,1 mol/l. Silver nitrate standard solution is also readily available commercially and may be used instead. 6.6
29、Ammonium thiocyanate, standard solution, c = 0,1 mol/l. Preparation: since ammonium thiocyanate is hygroscopic and cannot be dried without risk of decomposition, it is advisable to weigh out an amount of approximately 9 g, dissolve in water and make up the volume to 1 l. Adjust to c = 0,1 mol/l subs
30、tance concentration by titration of silver nitrate 0,1 mol/l. Ammonium thiocyanate standard solution is also readily available commercially, and may be used instead. 7 Apparatus 7.1 Standard laboratory equipment. 7.2 Rotary shaker, 35 to 40 min-1. 7.3 Burettes. 7.4 Graduated flask, capacity 500 ml a
31、nd 1 000 ml. 7.5 Conical (Erlenmeyer) flask, capacity 250 ml. 8 Procedure 8.1 Preparation of the test portion and the solution Place 5 g of the laboratory sample, weighed to the nearest 0,001 g, in a graduated flask (7.4) and add 450 ml of water (6.1). Mix for 0,5 h on the shaker (7.2), make up to 5
32、00 ml with water (6.1), mix and filter into a beaker. 8.2 Determination Take an aliquot part of the test solution containing not more than 0,150 g of chloride: for example 25 ml (0,25 g), 50 ml (0,5 g) or 100 ml (1 g). If the amount of the test solution taken is smaller than 50 ml it is necessary to
33、 make up the volume to 50 ml with water (6.1). Add 5 ml of nitric acid (6.3), 20 ml of the indicator solution (6.4), and two drops of ammonium thiocyanate standard solution (6.6) (this latter reagent is added with a burette adjusted to zero for this purpose). With a burette (7.3) then add silver nit
34、rate standard solution (6.5) until there is an excess of 2 ml to 5 ml. Add 5 ml of nitrobenzene or 5 ml of diethyl ether (6.2) and shake well to agglomerate the precipitate. Titrate the excess silver nitrate with ammonium thiocyanate (6.6) until a red-brown colour appears which remains after the fla
35、sk has been shaken slightly. NOTE Nitrobenzene or diethyl ether (but above all nitrobenzene) prevents the silver chloride from reacting with thiocyanate ions. Thus a clear colour change is obtained. DIN EN 16195:2013-01 EN 16195:2012 (E) 6 8.3 Blank test Carry out a blank test (omitting the test por
36、tion) under the same conditions and allow for it when calculating the final result. 8.4 Control test Before carrying out the estimations check the accuracy of the method by using an aliquot part of a freshly prepared solution of potassium chloride, such that this part contains a known quantity in th
37、e order of 100 mg of chloride. 9 Calculation and expression of the results Express the result of the analysis as a percentage of chloride contained in the sample as it has been received for analysis. Calculate the mass fraction of chlorides (Cl), wCl, in percent according to Formula (1). 100)()(5460
38、,003caaCZZCl=MVVVVw (1) where Vz is the amount of silver nitrate 0,1 mol/l, in millilitres; Vcz is the amount of silver nitrate 0,1 mol/l, used in the blank test, in millilitres; Va is the amount of ammonium thiocyanate 0,1 mol/l, in millilitres; Vca is the amount of ammonium thiocyanate 0,1 mol/l,
39、used in the blank test, in millilitres; M is the mass, in grams, of the test portion taken (8.1). 10 Precision 10.1 Inter-laboratory test An inter-laboratory test has been carried out in 2009 with 14/13 participating laboratories and two different samples. The repeatability and reproducibility were
40、calculated according to ISO 5725-2. The values derived from these inter-laboratory tests may not be applicable to concentration ranges and matrices other than those given in Annex A. 10.2 Repeatability The absolute difference between two independent single test results, obtained with the same method
41、 on identical test material in the same laboratory by the same operator using the same equipment within a short interval of time, will in not more than 5 % of the cases exceed the values of r given in Table 1. 10.3 Reproducibility The absolute difference between two single test results, obtained wit
42、h the same method on identical test material in different laboratories by different operators using different equipment, will not exceed values of R given in Table 1 in more than 5 % of the cases. DIN EN 16195:2013-01 EN 16195:2012 (E) 7 Table 1 Mean values, repeatability and reproducibility limits
43、Sample x % r % R % Patent kali 2,781 0,066 0,284 NPK2 (12-11-18+4+8) 0,478 0,076 0,312 11 Test report The test report shall contain at least the following information: a) all information necessary for the complete identification of the sample; b) the test method used with reference to this document;
44、 c) the 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 fulfilled; g) all operating details not specified in this document, or regarded as optional, together with deta
45、ils of any incidents occurred when performing the method, which might have influenced the test result(s). DIN EN 16195:2013-01 EN 16195:2012 (E) 8 Annex A (informative) Statistical results of the inter-laboratory test The precision of the method was established in 2009 by Working Group 7 “Chemical a
46、nalysis” of CEN/TC 260 “Fertilizers and liming materials” in an inter-laboratory test evaluated in accordance with ISO 5725-2. The statistical results are given in Table A.1. Table A.1 Statistical results of the inter-laboratory test Parameter Sample Patent kali NPK2 (12-11-18+4+8) Number of partici
47、pating laboratories 14 13 Number of laboratories after elimination of outliers (accepted test results) 11 13Mean value x (%) 2,781 0,478 Repeatability standard deviation sr(%) 0,024 0,027RSDr(%) 0,9 6,0 Repeatability limit r (%) 0,066 0,076Reproducibility standard deviation sR(%) 0,101 0,111 RSDR(%)
48、 3,6 23,0Reproducibility limit R (%) 0,284 0,312 DIN EN 16195:2013-01 EN 16195:2012 (E) 9 Bibliography 1 EN 1482-1, Fertilizers and liming materials Sampling and sample preparation Part 1: Sampling 2 ISO 5725-2, Accuracy (trueness and precision) of measurement methods and results Part 2: Basic method for the determination of repeatability and reproducibility of a standard measurement method 3 Regulation (EC) No 2003/2003 of the European Parliament and of the Council of 13
