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1、BRITISH STANDARD BS EN 13651:2001 Soil improvers and growing media Extraction of calcium chloride/DTPA (CAT) soluble nutrients The European Standard EN 13651:2001 has the status of a British Standard ICS 65.080 NO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAW Licensed Copy: she
2、ffieldun sheffieldun, na, Mon Oct 30 01:39:37 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS EN 13651:2001 This British Standard, having been prepared under the direction of the Consumer Products and Services Sector Policy and Strategy Committee, was published under the authority of the Standards Pol
3、icy and Strategy Committee on 09 November 2001 BSI 09 November 2001 ISBN 0 580 38266 4 National foreword This British Standard is the official English language version of EN 13651:2001. The UK participation in its preparation was entrusted to Technical Committee AW/20, Top soil and other growing med
4、ia, which has the responsibility to: A list of organizations represented on this committee can be obtained on request to its secretary. Cross-references The British Standards which implement international or European publications referred to in this document may be found in the BSI Standards Catalog
5、ue under the section entitled “International Standards Correspondence Index”, or by using the “Find” facility of the BSI Standards Electronic Catalogue. A British Standard does not purport to include all the necessary provisions of a contract. Users of British Standards are responsible for their cor
6、rect application. Compliance with a British Standard does not of itself confer immunity from legal obligations. aid enquirers to understand the text; present to the responsible European committee any enquiries on the interpretation, or proposals for change, and keep the UK interests informed; monito
7、r related international and European developments and promulgate them in the UK. Summary of pages This document comprises a front cover, an inside front cover, the EN title page, pages 2 to 16, an inside back cover and a back cover. The BSI copyright date displayed in this document indicates when th
8、e document was last issued. Amendments issued since publication Amd. No. DateComments Licensed Copy: sheffieldun sheffieldun, na, Mon Oct 30 01:39:37 GMT+00:00 2006, Uncontrolled Copy, (c) BSI EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN 13651 September 2001 ICS 65.080 English version Soil i
9、mprovers and growing media - Extraction of calcium chloride/DTPA (CAT) soluble nutrients Amendements du sol et supports de culture - Extraction des lments nutritifs solubles dans le chlorure de calcium/DTPA (CAT) Bodenverbesserungsmittel und Kultursubstrate - Extraktion von in Calciumchlorid/DTPA (C
10、AT) lslichen Nhrstoffen This European Standard was approved by CEN on 11 August 2001. 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 standard without any alteration. Up-to-date lists
11、and bibliographical references concerning such national standards may be obtained on application to the Management Centre or to any CEN member. This European Standard exists in three official versions (English, French, German). A version in any other language made by translation under the responsibi
12、lity of a CEN member into its own language and notified to the Management Centre has the same status as the official versions. CEN members are the national standards bodies of Austria, Belgium, Czech Republic, Denmark, Finland, France, Germany, Greece, Iceland, Ireland, Italy, Luxembourg, Netherland
13、s, Norway, Portugal, Spain, Sweden, Switzerland and United Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZATION COMIT EUROPEN DE NORMALISATION EUROPISCHES KOMITEE FR NORMUNG Management Centre: rue de Stassart, 36 B-1050 Brussels 2001 CENAll rights of exploitation in any form and by any means reserved wor
14、ldwide for CEN national Members. Ref. No. EN 13651:2001 E Licensed Copy: sheffieldun sheffieldun, na, Mon Oct 30 01:39:37 GMT+00:00 2006, Uncontrolled Copy, (c) BSI EN 13651:2001 (E) 2 Contents page Foreword .3 1Scope4 2Normative references4 3Terms and definitions.4 4Principle .4 5Reagents 4 6Appara
15、tus.5 7Test sample5 8Procedure.6 9Determination of the extracted nutrients and elements6 10Expression of results6 11Precision 6 12Test report7 Annex A (informative) Results of an interlaboratory trial to determine calcium chloride/DTPA (CAT) soluble nutrients and elements.8 Annex B (informative) Met
16、hods of analysis used in the interlaboratory trial.15 Bibliography16 Licensed Copy: sheffieldun sheffieldun, na, Mon Oct 30 01:39:37 GMT+00:00 2006, Uncontrolled Copy, (c) BSI EN 13651:2001 (E) 3 Foreword This European Standard has been prepared by Technical Committee CEN/TC 223 “Soil improvers and
17、growing media“, the secretariat of which is held by BSI. 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 March 2002, and conflicting national standards shall be withdrawn at the latest by March 20
18、02. The annexes A and B are informative. According to the CEN/CENELEC Internal Regulations, the national standards organizations of the following countries are bound to implement this European Standard: Austria, Belgium, Czech Republic, Denmark, Finland, France, Germany, Greece, Iceland, Ireland, It
19、aly, Luxembourg, Netherlands, Norway, Portugal, Spain, Sweden, Switzerland and the United Kingdom. Licensed Copy: sheffieldun sheffieldun, na, Mon Oct 30 01:39:37 GMT+00:00 2006, Uncontrolled Copy, (c) BSI EN 13651:2001 (E) 4 SAFETY PRECAUTIONS Care should be taken when handling samples that may con
20、tain sharps or is of a dusty nature. 1 Scope This European Standard specifies an extraction method for the routine determination of calcium chloride/DTPA (CAT-method) extractable nutrients and elements (as listed in annex B) in soil improvers or growing media. The method is not applicable to liming
21、materials and preformed materials such as mineral wool slabs and foam slabs. NOTEThe requirements of the standard may differ from the national legal requirements for the declaration of the products concerned. 2 Normative references This European Standard incorporates by dated or undated reference, p
22、rovisions from other publications. These normative references are cited at the appropriate places in the text, and the publications are listed hereafter. For dated references, subsequent amendments to or revisions of any of these publications apply to this European Standard only when incorporated in
23、 it by amendment or revision. For undated references the latest edition of the publication referred to applies (including amendments). EN ISO 3696, Water for analytical laboratory use - Specification and test methods (ISO 3696:1987). EN 13040:1999, Soil improvers and growing media - Sample preparati
24、on for chemical and physical tests, determination of dry matter content, moisture content and laboratory compacted bulk density. 3 Terms and definitions For the purposes of this standard the terms and definitions given in EN 13040 apply. 4 Principle A sample is extracted with calcium chloride/DTPA a
25、t 22 ?C ? 3 ?C in an extraction volume ratio of 1+5. The extracted nutrients are determined by various methods as appropriate (see annex B). 5 Reagents 5.1 General All reagents used shall be of recognised analytical quality and water of grade 2 according to EN ISO 3696. 5.2 Dihydrated calcium chlori
26、de, CaCl2.2H2O. 5.3 Diethylenetriaminepentaacetic acid (DTPA), C14H23N3O10. 5.4 Concentrated extracting solution CaCl2/DTPA, (CAT), dissolve 14,7 g CaCl2.2H2O (5.2) and 7,88 g DTPA (5.3) in 800 ml hot water (temperature approximately 80 ?C) with stirring on a magnetic stirrer in a 1000 ml beaker. At
27、 75 ?C ? 10 ?C the reagents will dissolve within 2 h. Allow to cool to ambient temperature. Transfer the solution to a 1000 ml flask and dilute to the mark with water. The Licensed Copy: sheffieldun sheffieldun, na, Mon Oct 30 01:39:37 GMT+00:00 2006, Uncontrolled Copy, (c) BSI EN 13651:2001 (E) 5 s
28、olution is stable at room temperature for several weeks. Any precipitation that occurs will disappear with warming and stirring. 5.5 Extracting solution CaCl2/DTPA, (CAT), dilute the concentrated extracting solution (5.4) with water in the proportions one part concentrated solution with nine parts w
29、ater. The final concentration of the extracting solution should be 0,01 mol/l CaCl2 and 0,002 mol/l DTPA. The pH of the extracting solution should be adjusted if necessary to be between 2,6 and 2,65. 5.6 Nitric acid, c(HNO3) = 15 mol/l: ? ? 1,42 g/ml; not less than 65 % mass/volume. 5.7 Nitric acid,
30、 c(HNO3) = 0,5 mol/l, dilute 35 ml nitric acid (5.6) to one litre with water. 6 Apparatus 6.1 General NOTEIt has been found convenient to keep separate sets of glassware for the determinations given in annex B, in order to reduce the possibility of within-laboratory contamination. All glass apparatu
31、s and plastic vessels used in the procedure should be subject to an appropriate preparation procedure in order to keep the risk of contamination as low as possible. It is recommended that all vessels (glass and plastic) are cleansed by carefully immersing in warm nitric acid (5.6) for a minimum of 6
32、 h and then rinsed in water. Rubber stoppers, which may contain traces of metals shall not be used. It is recommended to use plastic or any other stopper free of all substances to be analyzed. Borosilicate glassware shall not be used if boron is to be determined. The apparatus consists of the usual
33、laboratory apparatus, and in particular the following : 6.2 Plastic bottles or containers, sufficiently large (500 ml to 1500 ml) with screw cap to accommodate the volume of the sample, extractant and at least 10 % air volume. 6.3 Shaking or mixing machine, capable of holding the plastic bottles or
34、containers (6.2) and maintaining the sample in suspension without damaging the structure of the sample. The use of a horizontal table shaker is recommended. 6.4 Filter paper, cellulose-based ashless types, with a medium pore size of approximately 8 ?m and diameter of 150 mm. NOTECentrifugation is an
35、 acceptable alternative. 6.5 Analytical balance with an accuracy of 10 mg. 7 Test sample Prepare the laboratory sample in accordance with EN 13040:1999, clause 8, and determine the laboratory compacted bulk density of the sample in accordance with EN 13040:1999, annex A. Licensed Copy: sheffieldun s
36、heffieldun, na, Mon Oct 30 01:39:37 GMT+00:00 2006, Uncontrolled Copy, (c) BSI EN 13651:2001 (E) 6 8 Procedure 8.1 Extraction 8.1.1 Test samples passing through a 20 mm sieve Take a weight equivalent to 60 ml of the sample volume (EN 13040:1999, clause 8.5) to the nearest 1 g and transfer to the con
37、tainer (6.2). Add 300 ml of extracting solution (5.5), secure the cap and shake for 1 h on the shaking machine (6.3) at 22 ?C ? 3 ?C. 8.1.2 Test samples passing through a 40 mm sieve Take a weight equivalent to 250 ml of the sample volume (EN 13040:1999, clause 8.3) to the nearest 1 g and transfer t
38、o the container (6.2). Add 1250 ml of extracting solution (5.5), secure the cap and shake for 1 h on the shaking machine (6.3) at 22 ?C ? 3 ?C. 8.1.3 Filtration Filter through filter paper (6.4) discarding at least the first 10 ml. In some cases paper filtration is too slow or even impossible. In su
39、ch cases alternative procedures for obtaining a clear supernatant are acceptable and the technique used shall be reported. The filtered extract is stable for three days in a hermetically closed polyethylene bottle if stored in a refrigerator at 0 ?C to 5 ?C. The filtrate can be stored for longer per
40、iods in a deep freezer at about ? 18 ?C. NOTEBefore using a solution that has been frozen, the thawed solution shall be thoroughly mixed to eliminate gradient separation that occurs on freezing and subsequent thawing. 8.2 Blank The reagent blank test shall be carried out in parallel with the determi
41、nation, by the same procedure as outlined in 8.1.1 or 8.1.2 and 8.1.3, using the same quantities of all the reagents as in the determination but omitting the test portion. NOTEThe measurement of a blank is introduced to determine the contribution of the extracting solution, glassware and filter pape
42、r used. 9 Determination of the extracted nutrients and elements See annex B. 10 Expression of results Subtract the values determined for the reagent blank from those obtained for the samples. All results shall be calculated using the determined compacted laboratory bulk density and expressed in mg/l
43、 substrate as received basis. 11 Precision The repeatability and reproducibility of the calcium chloride DTPA soluble nutrient content in separately prepared samples should be in accordance with Tables A.1 to A.6. A summary of the results of an interlaboratory trial to determine the precision of the
44、 method, in accordance with ISO 5725 2, is given in annex A. NOTEThe values derived from this interlaboratory trial may not be applicable to concentrations and matrices other than those tested. Licensed Copy: sheffieldun sheffieldun, na, Mon Oct 30 01:39:37 GMT+00:00 2006, Uncontrolled Copy, (c) BSI
45、 EN 13651:2001 (E) 7 12 Test report The test report shall contain the following information: a) a reference to this European Standard; b) all information necessary for complete identification of the sample; c) all the analytical methods used; d) the results of the determination, expressed as mg/l fr
46、esh sample; e) details of any operations not specified in the European Standard or regarded as optional, as well as any factor which may have affected the results; f) the laboratory compacted bulk density result. Licensed Copy: sheffieldun sheffieldun, na, Mon Oct 30 01:39:37 GMT+00:00 2006, Uncontr
47、olled Copy, (c) BSI EN 13651:2001 (E) 8 Annex A (informative) Results of an interlaboratory trial to determine calcium chloride/DTPA (CAT) soluble nutrients and elements An interlaboratory trial was organized in 1997 under the auspices of the European Committee for Standardization, to test the proce
48、dures specified in this European Standard. In this trial the number of laboratories given in the Tables A.1 to A.6 determined the calcium chloride/DTPA soluble nutrient and elements content in six sample types. All results are reported on a fresh basis. Licensed Copy: sheffieldun sheffieldun, na, Mo
49、n Oct 30 01:39:37 GMT+00:00 2006, Uncontrolled Copy, (c) BSI EN 13651:2001 (E) 9 A summary of the results of the interlaboratory trial for the determination of calcium chloride/DTPA (CAT) soluble nutrients and elements in six sample types is given in Tables A.1 to A.6. Table A.1 - Composted bark ElementNo. of labs after eliminating outliers No. of outliers (labs) Mean value mg/l Repeatability sr Repeatability Std Dev % Repeatability limit r = 2,8 sr Reproducibility sR Reproducibility Std Dev % Reproducibility limit R = 2,8 sR NH4-N1901220,149,1911,29137,72248,5257,03695
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