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1、BRITISH STANDARD BS EN 13366:2001 Fertilizers Treatment with a cation exchange resin for the determination of the chelated micro-nutrient content and of the chelated fraction of micro-nutrients The European Standard EN 13366:2001 has the status of a British Standard ICS 65.080 NO COPYING WITHOUT BSI
2、 PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAW Licensed Copy: sheffieldun sheffieldun, na, Mon Oct 30 01:39:19 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS EN 13366:2001 This British Standard, having been prepared under the direction of the Sector Committee for Materials and Chemicals, was publis
3、hed under the authority of the Standards Committee and comes into effect on 15 May 2001 BSI 05-2001 ISBN 0 580 37283 9 National foreword This British Standard is the official English language version of EN 13366:2001. The UK participation in its preparation was entrusted to Technical Committee CII/3
4、7, Fertilizers and related chemicals, 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
5、found in the BSI Standards Catalogue 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 Stand
6、ards are responsible for their correct 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
7、 the UK interests informed; monitor 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 11 and a back cover. The BSI copyright date displayed in this document indic
8、ates when the document was last issued. Amendments issued since publication Amd. No. DateComments Licensed Copy: sheffieldun sheffieldun, na, Mon Oct 30 01:39:19 GMT+00:00 2006, Uncontrolled Copy, (c) BSI EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN 13366 January 2001 ICS 65.080 English vers
9、ion Fertilizers Treatment with a cation exchange resin for the determination of the chelated micro-nutrient content and of the chelated fraction of micro-nutrients Engrais Traitement avec une rsine changeuse dions cationique pour la dtermination de la teneur en oligo- lments chlats et de la fraction
10、 chlate des oligo- lments Dngemittel Behandlung mit einem Kationenaustauscherharz zur Bestimmung des chelatisierten Spurennhrstoffgehaltes und des chelatgebundenen Anteils von Spurennhrstoffen This European Standard was approved by CEN on 1 January 2001. CEN members are bound to comply with the CEN/
11、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 and bibliographical references concerning such national standards may be obtained on application to the Management Centre or to any
12、 CEN 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 Management Centre has the same status as the official versions. CEN
13、members are the national standards bodies of Austria, Belgium, Czech Republic, Denmark, Finland, France, Germany, Greece, Iceland, Ireland, Italy, Luxembourg, Netherlands, Norway, Portugal, Spain, Sweden, Switzerland and United Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZATION COMIT EUROPEN DE NORMALI
14、SATION 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 worldwide for CEN national Members. Ref. No. EN 13366:2001 E Licensed Copy: sheffieldun sheffieldun, na, Mon Oct 30 01:39:19 GMT+00:00
15、 2006, Uncontrolled Copy, (c) BSI Page 2 EN 13366:2001 BSI 05-2001 Contents Foreword. 3 1Scope . 3 2Normative references . 4 3Terms and definitions. 4 4Principle. 4 5Interferences 5 6Apparatus 5 7Reagents 5 8Procedure 7 9Expression of results . 9 10Precision 9 11Test report . 10 Bibliography. 11 Lic
16、ensed Copy: sheffieldun sheffieldun, na, Mon Oct 30 01:39:19 GMT+00:00 2006, Uncontrolled Copy, (c) BSI Page 3 EN 13366:2001 BSI 05-2001 Foreword This European Standard has been prepared by Technical Committee CEN/TC 260, Fertilizers and liming materials, the Secretariat of which is held by DIN. Thi
17、s 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 July 2001, and conflicting national standards shall be withdrawn at the latest by July 2001. According to the CEN/CENELEC Internal Regulations, the nat
18、ional standards organizations of the following countries are bound to implement this European Standard: Austria, Belgium, Czech Republic, Denmark, Finland, France, Germany, Greece, Iceland, Ireland, Italy, Luxembourg, Netherlands, Norway, Portugal, Spain, Sweden, Switzerland and the United Kingdom.
19、Licensed Copy: sheffieldun sheffieldun, na, Mon Oct 30 01:39:19 GMT+00:00 2006, Uncontrolled Copy, (c) BSI Page 4 EN 13366:2001 BSI 05-2001 1 Scope This standard defines a method for the treatment with a cation exchange resin for the determination of the chelated micro-nutrient content and the chela
20、ted fraction of the micro-nutrients (trace elements) cobalt, copper, iron, manganese, and zinc in fertilizers. This method applies to fertilizers containing one or more of the micro-nutrients cobalt, copper, iron, manganese, and zinc, chelated by one or more chelating agents of the group of the poly
21、amino polycarboxylic acids, previously determined according to EN 13368-1 and EN 13368-2, either alone or in combination with primary (N, P, K) and/or secondary (S, Na, Ca, Mg) nutrients. The limit of determination of the chelated micro-nutrient content varies between 0,005 % in simple matrices with
22、 high amounts of chelated micro-nutrients, and 0,5 % in more complex cases (see 7.2). 2 Normative references This European standard incorporates by dated or undated reference, provisions from other publications. These normative references are cited at the appropriate places in the text, and the publ
23、ications 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 it by amendment or revision. For undated references, the latest edition of the publication referred to applies (including
24、amendments). EN 1482, Sampling of solid fertilizers and liming materials. EN 13368-1, Fertilizers Determination of chelating agents in fertilizers by ion chromatography Part 1:EDTA, HEDTA and DTPA. EN 13368-2, Fertilizers Determination of chelation agents in fertilizers by ion chromatography Part 2:
25、EDDHA and EDDHMA. EN ISO 3696, Water for analytical laboratory use Specification and test methods (ISO 3696:1987). 3 Terms and definitions For the purposes of this standard the following terms and definitions apply: 3.1 chelated fraction chelated content of a micro-nutrient, divided by its total con
26、tent, and expressed as a percentage 4 Principle The sample is extracted with water and the extract adjusted to a neutral pH. The chelated forms of an element thus having a negative and/or neutral charge are not retained by an ion exchange resin of the strong sulfonated cationic type, and are separat
27、ed from the non-chelated forms, having a cationic nature. The chelated forms are collected and their content determined by spectrometry, as well as the total element content. Licensed Copy: sheffieldun sheffieldun, na, Mon Oct 30 01:39:19 GMT+00:00 2006, Uncontrolled Copy, (c) BSI Page 5 EN 13366:20
28、01 BSI 05-2001 5 Interferences Any substance combining with a micro-nutrient to form a stable, negative or uncharged compound (chelate or complex) at neutral pH, will prevent the retention by the resin, and account for a certain degree of chelation. This is the case for many complexing agents, e.g.
29、amino acids, citrate, and for chelating agents other than ethylenediaminetetraacetic acid (EDTA), hydroxyethylethylenediaminetetraacetic acid (HEDTA), diethylenetriaminepentaacetic acid (DTPA), ethylenediamine-di-(o-hydroxyphenyl)acetic acid (EDDHA) and ethylenediamine-di-(o-hydroxy-p-methylphenyl)a
30、cetic acid (EDDHMA). NOTE In order to confirm the presence of the statutory chelating agents in the sample, EN 13368-1 and EN 13368-2 should be applied. In some cases, especially where complex fertilizer matrices with high amounts of phosphate are handled, or where micro-nutrients with a low chelate
31、d fraction are present, slow precipitation reactions can occur during the contact with the resin, causing equilibrium shifts, adsorption, decreasing the exchange capacity and leading to inaccurate and imprecise results. It is advised to proceed as soon as possible with all steps. Highly unstable sol
32、utions cannot be considered. 6 Apparatus NOTEAll glassware, filters, and equipment parts coming in contact with samples and solutions, should be appropriate for micro-nutrient analysis, be very clean and free from contamination, especially by the elements Co, Cu, Fe, Mn and Zn. Usual laboratory equi
33、pment and in particular: 6.1 Sieve, sieve having a plastic body and a nylon mesh of aperture size less than the minimum diameter of the resin particles. The mass of the dry sieve shall be determined to within 0,01 g. 6.2 Tumbling shaker, tumbling or rotary shaker operating at a rotational speed betw
34、een 30 min-1 and 40 min-1, at a temperature of 18 C to 22 C. 6.3 Conductivity meter, equipped with a conductivity cell and a temperature controller. The cell shall be rinsed and dried before immersion, and calibrated with a 0,01 mol/l potassium chloride solution, having a specific conductivity at 20
35、 C of 1,28 mS/cm. 6.4 Shaking flasks, polyethylene flasks, each having a capacity of 50 ml and a stopper. 6.5 Membrane filters, micromembrane filters resistent to aqueous solutions, with porosity of 0,45 m. 7 Reagents 7.1 General a) all water used should conform to EN ISO 3696 and be degassed by boi
36、ling before use; b) all reagents should be of recognized analytical grade. Licensed Copy: sheffieldun sheffieldun, na, Mon Oct 30 01:39:19 GMT+00:00 2006, Uncontrolled Copy, (c) BSI Page 6 EN 13366:2001 BSI 05-2001 7.2 Sulfonated cationic exchange resin 7.2.1 General Polystyrene divinylbenzene (PS-D
37、VB) copolymer, slightly crosslinked (mass fraction of DVB less than or equal to 8 %), in sodic or protonic form, free from Co, Cu, Fe, Mn, and Zn1). 7.2.2 Preparation and determination of exchange capacity Protonate the resin prior to use, transform to the sodic form, to eliminate any contamination
38、and measure the cationic exchange capacity (CEC) of the sodic resin in wet form as follows: Transfer 50 g of resin to a 500 ml beaker and add 250 ml of hydrochloric acid solution (7.4). Place on a magnetic stirrer. After 1 h of moderate stirring, the suspension is transferred onto the sieve (6.1). T
39、he resin is recovered and transferred back to the beaker. The acidification and separation operations are repeated as described. At the end of the second operation, the protonated resin present on the sieve is washed thoroughly with water until the rinsing water is free from chloride when tested wit
40、h silver nitrate. Transfer the wet protonated resin into a 500 ml beaker and add 250 ml of sodium chloride solution (7.5). While stirring on a magnetic stirrer and using a pH meter, titrate the resin using the sodium hydroxide solution (7.6) until a stable pH of 7,0 is obtained. Let Vo be the requir
41、ed volume of NaOH (7.6), in millilitres. Transfer quantitatively the resin that is now in sodic form onto the sieve (6.1). Rinse thoroughly with water until the rinsing water is free from chloride (silver nitrate test). Once rinsing is complete, allow the resin to drain. Weigh the drained wet resin
42、to within 0,01 g. Let P be the mass in grams. The wet sodic resin can be stored in a stoppered opaque flask at ambient temperature for 2 years. The cationic exchange capacity of the resin is given by the following formula: CEC = 2 Vo / P where: CECis the cationic exchange capacity, in millimoles per
43、 gram of wet resin 7.3 Hydrochloric acid, c(HCl) 6 mol/l Hydrochloric acid, diluted 1 + 1 with water. 7.4 Hydrochloric acid solution, c(HCl) = 1 mol/l Dilute 165 ml of hydrochloric acid solution (7.3) to 1 l. 1) Dowex 50 x 4-400, Amberlite IR 120 or equivalent are examples of suitable products avail
44、able commercially. This information is given for the convenience of users of this European Standard and does not constitute an endorsement by CEN of these products. Licensed Copy: sheffieldun sheffieldun, na, Mon Oct 30 01:39:19 GMT+00:00 2006, Uncontrolled Copy, (c) BSI Page 7 EN 13366:2001 BSI 05-
45、2001 7.5 Sodium chloride solution, c(NaCl) = 1 mol/l Dissolve 58,4 g of NaCl in water and dilute to 1 l. 7.6 Sodium hydroxide solution, c(NaOH) = 2 mol/l Carefully dissolve 80,0 g of NaOH in water and dilute to 1 l. 7.7 Sodium hydroxide solution, c(NaOH) = 0,1 mol/l Dilute 25 ml of the sodium hydrox
46、ide solution (7.6) to 500 ml. 7.8 Nitric acid solution, c(HNO3) = 0,1 mol/l Carefully dilute 6,9 ml of nitric acid (65 % HNO3 , ? = 1,40 g/ml) to 1 l. 7.9 Sodium hydroxide solution, c(NaOH) = 0,01 mol/l Dilute 50 ml of the sodium hydroxide solution (7.7) to 500 ml. 7.10 Nitric acid solution, c(HNO3)
47、 = 0,01 mol/l Dilute 50 ml of the nitric acid solution (7.8) to 500 ml. 8 Procedure 8.1 Preparation of the sample Prepare the sample according to EN 1482. NOTE 1Sample may also be prepared according to method 1 (see 1 of bibliography). NOTE 2For the size reduction of samples with a high amount of ch
48、elating agents, it is not recommended to use a high speed laboratory mill. It is more convenient to grind the sample in a mortar to a particle size less than 1 mm. 8.2 Extraction of the sample Weigh an amount of sample, depending on the declared content of water soluble micro-nutrient, to within 1 m
49、g, into a volumetric flask of 250 ml or 500 ml, according to Table 1: Table 1 Sample mass/volume ratios Micro-nutrient content (%) 5 Mass of sample E (g)1052 Volume of the extract V (ml)250500500 Add about 200 ml of water for a 250 ml flask, or about 400 ml for a 500 ml flask. Stopper the flask, shake well to disperse the matter, and put on the tumbling shaker (6.2) for 30 min. Adjust to the mark with water, homogenize, and filter. Licensed Copy: sheffieldun sheffieldun, na