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1、DRAFT FOR DEVELOPMENT DD CEN/TS 15560:2007 Fertilizers Determination of total nitrogen in calcium cyanamide nitrate free ICS 65.080 ? Licensed Copy: London South Bank University, London South Bank University, Wed May 16 04:10:38 GMT+00:00 2007, Uncontrolled Copy, (c) BSI DD CEN/TS 15560:2007 This Dr
2、aft for Development was published under the authority of the Standards Policy and Strategy Committee on 31 May 2007 BSI 2007 ISBN 978 0 580 50718 2 National foreword This Draft for Development was published by BSI. It is the UK implementation of CEN/TS 15560:2007. This publication is not to be regar
3、ded as a British Standard. It is being issued in the Draft for Development series of publications and is of a provisional nature. It should be applied on this provisional basis, so that information and experience of its practical application can be obtained. Comments arising from the use of this Dra
4、ft for Development are requested so that UK experience can be reported to the European organization responsible for its conversion to a European standard. A review of this publication will be initiated not later than 3 years after its publication by the European organization so that a decision can b
5、e taken on its status. Notification of the start of the review period will be made in an announcement in the appropriate issue of Update Standards. According to the replies received by the end of the review period, the responsible BSI Committee will decide whether to support the conversion into a Eu
6、ropean Standard, to extend the life of the Technical Specification or to withdraw it. Comments should be sent to the Secretary of the responsible BSI Technical Committee at British Standards House, 389 Chiswick High Road, London W4 4AL. The UK participation in its preparation was entrusted to Techni
7、cal Committee CII/37, Fertilisers and related chemicals. 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 provisions of a contract. Users are responsible for its correct application. Amen
8、dments issued since publication Amd. No. DateComments Licensed Copy: London South Bank University, London South Bank University, Wed May 16 04:10:38 GMT+00:00 2007, Uncontrolled Copy, (c) BSI TECHNICAL SPECIFICATION SPCIFICATION TECHNIQUE TECHNISCHE SPEZIFIKATION CEN/TS 15560 April 2007 ICS 65.080 E
9、nglish Version Fertilizers - Determination of total nitrogen in calcium cyanamide nitrate free Engrais - Dtermination de lazote total dans la cyanamide calcique exempte de nitrate Dngemittel - Bestimmung von Gesamtstickstoff in nitratfreiem Kalkstickstoff This Technical Specification (CEN/TS) was ap
10、proved by CEN on 1 January 2007 for provisional application. The period of validity of this CEN/TS is limited initially to three years. After two years the members of CEN will be requested to submit their comments, particularly on the question whether the CEN/TS can be converted into a European Stan
11、dard. CEN members are required to announce the existence of this CEN/TS in the same way as for an EN and to make the CEN/TS available promptly at national level in an appropriate form. It is permissible to keep conflicting national standards in force (in parallel to the CEN/TS) until the final decis
12、ion about the possible conversion of the CEN/TS into an EN is reached. CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Neth
13、erlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, 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 2007 CENAll rights of exploitatio
14、n in any form and by any means reserved worldwide for CEN national Members. Ref. No. CEN/TS 15560:2007: E Licensed Copy: London South Bank University, London South Bank University, Wed May 16 04:10:38 GMT+00:00 2007, Uncontrolled Copy, (c) BSI 2 Contents Page Foreword3 1 Scope 4 2 Normative referenc
15、es4 3 Terms and definitions .4 4 Principle4 5 Reagents.4 6 Apparatus .6 7 Sampling and sample preparation.11 8 Procedure .11 9 Calculation and expression of the result 13 10 Test report14 Bibliography15 CEN/TS 15560:2007 Licensed Copy: London South Bank University, London South Bank University, Wed
16、May 16 04:10:38 GMT+00:00 2007, Uncontrolled Copy, (c) BSI 3 Foreword This document (CEN/TS 15560:2007) has been prepared by Technical Committee CEN/TC 260 “Fertilizers and liming materials”, the secretariat of which is held by DIN. This document has been prepared under a mandate given to CEN by the
17、 European Commission and the European Free Trade Association. According to the CEN/CENELEC Internal Regulations, the national standards organizations of the following countries are bound to announce this Technical Specification: Austria, Belgium, Bulgaria, Cyprus, Czech Republic, Denmark, Estonia, F
18、inland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom. CEN/TS 15560:2007 Licensed Copy: London South Bank University, London South Bank
19、 University, Wed May 16 04:10:38 GMT+00:00 2007, Uncontrolled Copy, (c) BSI 4 1 Scope This Technical Specification specifies a method for the determination of total nitrogen in nitrate-free calcium cyanamide. 2 Normative references The following referenced documents are indispensable for the applica
20、tion of this document. For dated references, only the edition cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies. EN 1482-2, Fertilizers and liming materials sampling and sample preparation Part 2: Sample preparation EN 12944-1:199
21、9, 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 relating to fertilizers EN ISO 3696:1995, Water for analytical laboratory use Specification and test methods (ISO 3696
22、:1987) 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 Digestion in sulfuric acid with the aid of a catalyst. Distillation of the ammonia from an alkaline solution, absorption in an excess of standar
23、d sulfuric acid solution and back-titration with standard sodium or potassium hydroxide solution. 5 Reagents 5.1 General Use only reagents of recognized analytical grade and distilled or demineralized water, free from carbon dioxide and all nitrogenous compounds (grade 3 according to EN ISO 3696:199
24、5). 5.2 Diluted sulfuric acid Mix one volume of sulfuric acid, = 1,84 g/ml, with one volume of water. 5.3 Potassium sulphate p.a. 5.4 Catalyst Use 0,3 g to 0,4 g of copper(II)oxide or 0,95 g to 1,25 g of copper(II)sulfate pentahydrate for each determination. CEN/TS 15560:2007 Licensed Copy: London S
25、outh Bank University, London South Bank University, Wed May 16 04:10:38 GMT+00:00 2007, Uncontrolled Copy, (c) BSI 5 5.5 Sodium hydroxide solution 30 % mass concentration, of approximately (NaOH) = 1,33 g/ml, ammonia free 5.6 Sulfuric acid c = 0,05 mol/l 5.7 Sodium or potassium hydroxide solution ca
26、rbonate free, c = 0,1 mol/l 5.8 Sulfuric acid c = 0,1 mol/l 5.9 Sodium or potassium hydroxide solution carbonate free, c = 0,2 mol/l 5.10 Sulfuric acid c = 0,25 mol/l 5.11 Sodium or potassium hydroxide solution carbonate free, c = 0,5 mol/l 5.12 Indicator solutions 5.12.1 Mixed indicator Solution A:
27、 Dissolve 1 g of methyl red in 37 ml of sodium hydroxide solution c = 0,1 mol/l and make up to 1 l with water. Solution B: Dissolve 1 g of methylene blue in water and make up to 1 l. Mix one volume of solution A with two volumes of solution B. This indicator is violet in acid solution, grey in neutr
28、al solution and green in alkaline solution. Use 0,5 ml (10 drops) of this indicator solution. 5.12.2 Methyl red indicator solution Dissolve 0,1 g of methyl red in 50 ml of 95 % ethanol. Make up to 100 ml with water and filter if necessary. This indicator may be used (4 to 5 drops) instead of that sp
29、ecified in 5.12.1. 5.13 Anti-bump granules of pumice stone washed in hydrochloric acid and calcined 5.14 Potassium thiocyanate p.a. CEN/TS 15560:2007 Licensed Copy: London South Bank University, London South Bank University, Wed May 16 04:10:38 GMT+00:00 2007, Uncontrolled Copy, (c) BSI 6 6 Apparatu
30、s 6.1 Distillation apparatus consisting of a round-bottomed flask of suitable capacity connected to a condenser by means of a splash head. The equipment is made of borosilicate glass. NOTE The different types of equipment recommended for this determination are reproduced, showing all the features of
31、 construction, in Figures 1, 2, 3 and 4. An automatic distillation apparatus may also be used, provided that the results are statistically equivalent. CEN/TS 15560:2007 Licensed Copy: London South Bank University, London South Bank University, Wed May 16 04:10:38 GMT+00:00 2007, Uncontrolled Copy, (
32、c) BSI 7 Dimensions in millimetres Key 1 round-bottomed, long-necked flask of 1 000 ml capacity 2 distillation tube with a splash head, connected to the condenser by means of a spherical joint (No 18) (the spherical joint for the connection to the condenser may be replaced by an appropriate rubber c
33、onnection) 3 funnel with a polytetrafluoroethylene (PTFE) tap (6) for the addition of sodium hydroxide (the tap may likewise be replaced by a rubber connection with a clip) 4 six-bulb condenser with spherical joint (No 18) at the entrance, and joined at the issue to a glass extension tube by means o
34、f a small rubber connection (when the connection to the distillation tube is effected by means of a rubber tube, the spherical joint may be replaced by a suitable rubber bung) 5 500 ml flask in which the distillate is collected 6 PTFE-tap a hole Figure 1 Distillation apparatus 1 CEN/TS 15560:2007 Li
35、censed Copy: London South Bank University, London South Bank University, Wed May 16 04:10:38 GMT+00:00 2007, Uncontrolled Copy, (c) BSI 8 Dimensions in millimetres Key 1 round-bottomed, short-necked flask of 1 000 ml capacity with a spherical joint (No 35) 2 distillation tube with a splash head, equ
36、ipped with a spherical joint (No 35) at the entrance and a spherical joint (No 18) at the issue, connected at the side to a funnel with a polytetrafluoroethylene (PTFE) tap (5) for the addition of sodium hydroxide 3 six-bulb condenser with a spherical joint (No 18) at the entrance and joined at the
37、issue to a glass extension tube by means of a small rubber connection 4 500 ml flask in which the distillate is collected 5 PTFE-tap a enlarged description Figure 2 Distillation apparatus 2 CEN/TS 15560:2007 Licensed Copy: London South Bank University, London South Bank University, Wed May 16 04:10:
38、38 GMT+00:00 2007, Uncontrolled Copy, (c) BSI 9 Dimensions in millimetres Key 1 round-bottomed, long-necked flask of 750 ml or 1 000 ml capacity with, a bell mouth 2 distillation tube with a splash head and a spherical joint (No 18) at the issue 3 elbow tube with a spherical joint (No 18) at the ent
39、rance and a drip cone (the connection to the distillation tube may be effected by means of a rubber tube instead of a spherical joint) 4 six-bulb condenser joined at the issue to a glass extension tube by means of a small rubber connection 5 500 ml flask in which the distillate is collected Figure 3
40、 Distillation apparatus 3 CEN/TS 15560:2007 Licensed Copy: London South Bank University, London South Bank University, Wed May 16 04:10:38 GMT+00:00 2007, Uncontrolled Copy, (c) BSI 10 Dimensions in millimetres Key 1 round-bottomed, long-necked flask of 1 000 ml capacity with a bell mouth 2 distilla
41、tion tube with a splash head and a spherical joint (No 18), at the issue, connected at the side to a funnel with a polytetrafluoroethylene (PTFE) tap (5) for the addition of sodium hydroxide (a suitable rubber bung may be used instead of the spherical joint; the tap may be replaced by a rubber conne
42、ction with an appropriate clip) 3 six-bulb condenser with a spherical joint (No 18) at the entrance, joined at the issue, by a rubber connection, to a glass extension tube (when the connection to the distillation tube is effected by means of a rubber tube, the spherical joint may be replaced by a su
43、itable rubber bung) 4 500 ml flask for the collection of the distillate 5 PTFE-tap Figure 4 Distillation apparatus 4 CEN/TS 15560:2007 Licensed Copy: London South Bank University, London South Bank University, Wed May 16 04:10:38 GMT+00:00 2007, Uncontrolled Copy, (c) BSI 11 6.2 Kjeldahl flask long
44、necked and of suitable capacity 6.3 Pipettes of capacity 50 ml, 100 ml and 200 ml 6.4 Graduated flask capacity 250 ml 7 Sampling and sample preparation Sampling is not part of the method specified in this Technical Specification. A recommended sampling method is given in EN 1482-1. Sample preparatio
45、n shall be carried out in accordance with EN 1482-2. 8 Procedure 8.1 Preparation of the solution Weigh, to the nearest 0,001 g, 1 g of the sample and place it in the Kjeldahl flask. Add 50 ml of diluted sulfuric acid (5.2), 10 g to 15 g of potassium sulfate (5.3) and the appropriate amount of cataly
46、st (5.4). Heat slowly to drive off the water, boil gently for 2 h, allow to cool and dilute with 100 ml to 150 ml of water. Cool again, transfer quantitatively the suspension to a graduated 250 ml flask, and make up the volume with water, shake and filter through a dry filter into a dry flask. 8.2 A
47、nalysis of the solution According to the variant chosen, place in the receiving flask a measured quantity of standard sulfuric acid as indicated in Table 1, Table 2 or Table 3. Add the appropriate quantity of the chosen indicator solution (5.12.1 or 5.12.2) and, if necessary, water in order to obtai
48、n a volume of at least 50 ml. The end of the extension tube of the condenser shall be below the surface of the solution. With a pipette, transfer, according to the variant chosen, 50 ml, 100 ml or 200 ml of the solution obtained as described in 8.1, and distil the ammonia as described below, adding
49、sufficient NaOH solution (5.5) to ensure a considerable excess. Add water in order to obtain a total volume of about 350 ml and several grains of pumice in order to control the boiling. Assemble the distillation apparatus, and taking care to avoid any loss of ammonia, add to the contents of the distillation flask 10 ml of concentrated sodium hydroxide solution (5.5). Gradually warm the flask, to avoid boiling vigorously. When boiling commences, distil at the rate of about 100 ml in 1