1、June 2009DEUTSCHE NORM English price group 11No part of this standard 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 65.080!$X8h“1532169www.di
2、n.deDDIN EN 15559Fertilizers Determination of nitric and ammoniacal nitrogen according to ArndEnglish version of DIN EN 15559:2009-06Dngemittel Bestimmung von Nitrat- und Ammoniumstickstoff nach ArndEnglische Fassung DIN EN 15559:2009-06SupersedesDIN CEN/TS 15559:2007-06www.beuth.deDocument comprise
3、s pages17DIN EN 15559:2009-06 2 National foreword This standard 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
4、 landwirtschaftliche Produkte (Food and Agricultural Products Standards Committee), Technical Committee NA 057-03-02 AA Dngemittel. The method specified in this standard is based upon Regulation (EC) No 2003/2003 relating to fertilizers, Annex IV, method 2.2.2 (see Bibliography). Amendments This sta
5、ndard differs from DIN CEN/TS 15559:2007-06 as follows: a) In Table 3, 1stline, the F value has been corrected to read 0,175 (instead of 0,75). b) In Table 3, 5thline, the F value has been corrected to read 1,400 (instead of 1,00). c) Normative references have been updated. d) The standard has been
6、brought in line with the current rules of presentation. Previous editions DIN CEN/TS 15559: 2007-06 EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN 15559 January 2009 ICS 65.080 Supersedes CEN/TS 15559:2007English Version Fertilizers Determination of nitric and ammoniacal nitrogen according to
7、Arnd Engrais Dosage de lazote nitrique et ammoniacal selon Arnd Dngemittel Bestimmung von Nitrat- und Ammoniumstickstoff nach Arnd This European Standard was approved by CEN on 6 December 2008. CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions f
8、or 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 Management Centre or to any CEN member. This European Standard exists in three offic
9、ial versions (English, French, German). A version in any other language made by translationunder the responsibility of a CEN member into its own language and notified to the CEN Management Centre has the same status as the official versions. CEN members are the national standards bodies of Austria,
10、Belgium, Bulgaria, Cyprus, Czech Republic, Denmark, Estonia, Finland, France,Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania,Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom. EUROPEAN COMMITTEE F
11、OR STANDARDIZATION COMIT EUROPEN DE NORMALISATION EUROPISCHES KOMITEE FR NORMUNG Management Centre: rue de Stassart, 36 B-1050 Brussels 2009 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN 15559:2009: EEN 15559:2009 (E) 2 Contents
12、Page Foreword 3 1 Scope 4 2 Normative references 4 3 Terms and definitions .4 4 Principle 4 5 Reagents .4 6 Apparatus .6 7 Sampling and sample preparation 11 8 Procedure 11 9 Calculation and expression of the result . 14 10 Test report . 14 Bibliography . 15 DIN EN 15559:2009-06 EN 15559:2009 (E) 3
13、Foreword This document (EN 15559:2009) 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 publication of an identical text or by endorsemen
14、t, at the latest by July 2009, and conflicting national standards shall be withdrawn at the latest by July 2009. 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 not be held responsible for identifying any
15、or all such patent rights. This document supersedes CEN/TS 15559:2007. This 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 organizations of the follo
16、wing countries are bound to implement this European Standard: Austria, Belgium, Bulgaria, Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slov
17、enia, Spain, Sweden, Switzerland and the United Kingdom. DIN EN 15559:2009-06 EN 15559:2009 (E) 4 1 Scope This European Standard specifies a method for the determination of nitric and ammoniacal nitrogen with reduction according to Arnd (modified for each of the variants a, b and c). The method is a
18、pplicable to all nitrogenous fertilizers, including compound fertilizers, in which nitrogen is found exclusively in nitrate form, or in ammoniacal and nitrate form. 2 Normative references The following referenced documents are indispensable for the application of this document. For dated references,
19、 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 12944-1:1999, Fertilizers and liming materials and soil
20、 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 3696:1987) 3 Terms and definitions For the purpo
21、ses of this document, the terms and definitions given in EN 12944-1:1999 and EN 12944-2:1999 apply. 4 Principle Reduction of nitrates and nitrites to ammonia in a neutral aqueous solution by means of a metallic alloy composed of 60 % Cu and 40 % Mg (Arnds alloy) in the presence of magnesium chloride
22、. Distillation of the ammonia and determination of the yield in a known volume of standard sulfuric acid solution. Titration of the excess acid by means of a standard solution of sodium or potassium hydroxide. 5 Reagents 5.1 General Use only reagents of recognized analytical grade and distilled or d
23、emineralized water, free from carbon dioxide and all nitrogenous compounds (grade 3 according to EN ISO 3696:1995). 5.2 Diluted hydrochloric acid Mix one volume of concentrated hydrochloric acid solution, (HCl) = 1,18 g/ml, with one volume of water. DIN EN 15559:2009-06 EN 15559:2009 (E) 5 5.3 Sulfu
24、ric acid (for variant a), c = 0,05 mol/l. 5.4 Sodium or potassium hydroxide solution (for variant a), carbonate free, c = 0,1 mol/l. 5.5 Sulfuric acid (for variant b, see NOTES in 8.2), c = 0,1 mol/l. 5.6 Sodium or potassium hydroxide solution (for variant b, see NOTES in 8.2), carbonate free, c = 0
25、,2 mol/l. 5.7 Sulfuric acid (for variant c, see NOTES in 8.2), c = 0,25 mol/l. 5.8 Sodium or potassium hydroxide solution (for variant c, see NOTES in 8.2), carbonate free, c = 0,5 mol/l. 5.9 Sodium hydroxide solution, approximately c = 2 mol/l. 5.10 Arnds alloy, powdered so as to pass through a sie
26、ve with apertures less than 1 mm square. 5.11 Magnesium chloride solution, = 20 %. Dissolve 200 g of magnesium chloride (MgCl2.6H2O) in approximately 600 ml to 700 ml of water in a 1 l flat-bottomed flask. To prevent frothing, add 15 g of magnesium sulfate (MgSO4.7H2O). After dissolution add 2 g of
27、magnesium oxide and a few anti-bump granules of pumice stone and concentrate the suspension to 200 ml by boiling, thus expelling any trace of ammonia from the reagents. Cool, make up the volume to 1 l and filter. 5.12 Indicator solutions 5.12.1 Mixed indicator Solution A: Dissolve 1 g of methyl red
28、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 neutral solution and green in alk
29、aline 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 specified in 5.12.1. 5.12.3 Co
30、ngo red indicator solution Dissolve 3 g of Congo red in 1 l of warm water and filter if necessary after cooling. This indicator may be used, instead of that specified in 5.12.1.or 5.12.2, in the neutralization of acid extracts before distillation, using 0,5 ml per 100 ml of liquid to be neutralized.
31、 5.13 Anti-bump granules, for example pumice stone, washed in hydrochloric acid and reclaimed. 5.14 Sodium nitrate, p.a. DIN EN 15559:2009-06 EN 15559:2009 (E) 6 6 Apparatus 6.1 Distillation apparatus Consisting of a round-bottomed flask of suitable capacity connected to a condenser by means of a sp
32、lash 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 construction, in Figures 1, 2, 3 and 4. An automatic distillation apparatus may also be used, provided that the results are sta
33、tistically equivalent. DIN EN 15559:2009-06 EN 15559:2009 (E) 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 t
34、he condenser may be replaced by an appropriate rubber connection) 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 j
35、oined at the issue to a glass extension tube by means of 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
36、 Figure 1 Distillation apparatus 1 DIN EN 15559:2009-06 EN 15559:2009 (E) 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, equipped with a spherical joint (No 35) at the entrance and a sph
37、erical 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 issue to a glass extension tube by means of a small rubber con
38、nection 4 500 ml flask in which the distillate is collected 5 PTFE-tap a enlarged description Figure 2 Distillation apparatus 2 DIN EN 15559:2009-06 EN 15559:2009 (E) 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
39、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 entrance 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
40、a glass extension tube by means of a small rubber connection 5 500 ml flask in which the distillate is collected Figure 3 Distillation apparatus 3 DIN EN 15559:2009-06 EN 15559:2009 (E) 10 Dimensions in millimetres Key 1 round-bottomed, long-necked flask of 1 000 ml capacity with a bell mouth 2 dist
41、illation 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 c
42、onnection 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
43、a suitable rubber bung) 4 500 ml flask for the collection of the distillate 5 PTFE-tap Figure 4 Distillation apparatus 4 DIN EN 15559:2009-06 EN 15559:2009 (E) 11 6.2 Pipettes, of capacity 10 ml, 20 ml, 25 ml, 50 ml, 100 ml and 200 ml. 6.3 Graduated flask, of capacity 500 ml. 6.4 Rotary shaker, 35 t
44、o 40 turns per minute. 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 preparation shall be carried out in accordance with EN 1482-2. 8 Procedure 8.1 Preparation of the solutio
45、n 8.1.1 General Carry out a solubility test on the sample in water at room temperature and in the proportion of 2 % (mass concentration). Weigh to 0,001 g, according to the indications given in Table 1, a quantity of 5 g or 7 g or 10 g of the prepared sample and place it in a 500 ml graduated flask.
46、 According to the result of the solubility test, proceed as follows: 8.1.2 Products completely soluble in water Add to the flask the quantity of water needed to dissolve the sample; shake, and when completely dissolved, make up the volume and mix thoroughly. 8.1.3 Products not completely soluble in
47、water Add to the flask 50 ml of water and then 20 ml of hydrochloric acid (5.2). Shake and leave undisturbed until the evolution of carbon dioxide has ceased. Add 400 ml of water and shake for half an hour with the rotary shaker (6.4). Make up the volume with water, mix and filter through a dry filt
48、er into a dry receptacle. 8.2 Analysis of the solution According to the chosen variant, place in the receiving flask the exactly measured quantity of standard sulfuric acid as indicated in Table 1, Table 2 or Table 3. Add the appropriate quantity of chosen indicator solution (5.12.1 or 5.12.2) and f
49、inally, sufficient water to give a volume of at least 50 ml. The end of the extension tube of the condenser shall be below the surface of the solution. Using a precision pipette, take, according to Table 1, Table 2 or Table 3, an adequate aliquot of the clear solution. Place it in the distillation flask. DIN EN 15559:2009-06 EN 15559:2009 (E) 12 Add sufficient water to obtain a total volume of about 350 ml (see NOTE 1), 10 g of Arnds alloy (5.10), 50 ml of magnesium chloride solution (5.11) and a few fragments of pumice stone (5.13). Rapidl
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