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1、DD CEN/TS 15749:2008 ICS 65.080 NO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAW DRAFT FOR DEVELOPMENT Fertilizers Determination of sulfates content using three different methods Licensed Copy: London South Bank University, South Bank University, 16/11/2008 12:00, Uncontrolled
2、Copy, (c) BSI This Draft for Development was published under the authority of the Standards Policy and Strategy Committee on 30 September 2008 BSI 2008 ISBN 978 0 580 60739 4 Amendments/corrigenda issued since publication DateComments DD CEN/TS 15749:2008 National foreword This Draft for Development
3、 is the UK implementation of CEN/TS 15749:2008. This publication is not to be regarded 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 i
4、ts practical application can be obtained. Comments arising from the use of this Draft for Development are requested so that UK experience can be reported to the international organization responsible for its conversion to an international standard. A review of this publication will be initiated not
5、later than 3 years after its publication by the international organization so that a decision can be 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 r
6、eview period, the responsible BSI Committee will decide whether to support the conversion into an international 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 Hous
7、e, 389 Chiswick High Road, London W4 4AL. The UK participation in its preparation was entrusted to Technical 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 in
8、clude all the necessary provisions of a contract. Users are responsible for its correct application. Compliance with a British Standard cannot confer immunity from legal obligations. Licensed Copy: London South Bank University, South Bank University, 16/11/2008 12:00, Uncontrolled Copy, (c) BSI DD C
9、EN/TS 15749:2008 TECHNICAL SPECIFICATION SPCIFICATION TECHNIQUE TECHNISCHE SPEZIFIKATION CEN/TS 15749 July 2008 ICS 65.080 English Version Fertilizers - Determination of sulfates content using three different methods Engrais - Dosage des sulfates selon trois mthodes diffrentes Dngemittel - Bestimmun
10、g von Sulfat mit drei verschiedenen Verfahren This Technical Specification (CEN/TS) was approved by CEN on 11 May 2008 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
11、, particularly on the question whether the CEN/TS can be converted into a European Standard. 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 co
12、nflicting national standards in force (in parallel to the CEN/TS) until the final decision 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, German
13、y, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZATION COMIT EUROPEN DE NORMALISATION EUROPISCHES KOMITEE FR NORMUNG M
14、anagement Centre: rue de Stassart, 36 B-1050 Brussels 2008 CENAll rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. CEN/TS 15749:2008: E Licensed Copy: London South Bank University, South Bank University, 16/11/2008 12:00, Uncontrolled Copy, (c
15、) BSI DD CEN/TS 15749:2008 CEN/TS 15749:2008 (E) 2 Contents Page Foreword3 1 Scope 4 2 Normative references4 3 Terms and definitions .4 4 Principle4 5 Sampling and sample preparation.5 6 Method A Gravimetric method 5 7 Method B ICP-OES method6 8 Method C IC method.10 9 Precision of methods A, B and
16、C.16 10 Test report18 Annex A (informative) Statistical results of the inter-laboratory tests 19 Bibliography22 Licensed Copy: London South Bank University, South Bank University, 16/11/2008 12:00, Uncontrolled Copy, (c) BSI DD CEN/TS 15749:2008 CEN/TS 15749:2008 (E) 3 Foreword This document (CEN/TS
17、 15749:2008) has been prepared by Technical Committee CEN/TC 260 “Fertilizers and liming materials”, the secretariat of which is held by DIN. 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 res
18、ponsible for identifying any or all such patent rights. 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 following countries
19、are bound to announce this Technical Specification: 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, Slovenia, Spai
20、n, Sweden, Switzerland and the United Kingdom. Licensed Copy: London South Bank University, South Bank University, 16/11/2008 12:00, Uncontrolled Copy, (c) BSI DD CEN/TS 15749:2008 CEN/TS 15749:2008 (E) 4 1 Scope This document specifies three different methods (Methods A, B and C) for the determinat
21、ion of sulfur present in fertilizers extracts in the form of sulfates. Method A specifies the gravimetric procedure. Method B specifies the method using inductively coupled plasma optical spectrometry (ICP-OES). Method C specifies the method using ion chromatography (IC). 2 Normative references The
22、following referenced documents are indispensable for the application 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 - Samplin
23、g 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 relating to fertilizers. EN ISO 3696:1995,
24、 Water for analytical laboratory use - Specification and test methods (ISO 3696:1987) 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 4.1 Method A: Gravimetric method Sulfur is extracted from the sam
25、ple according to the methods described in 1, 2, 3, or 4 and determined based on the gravimetric determination as barium sulfate. 4.2 Method B: ICP-OES Sulfur is extracted from the sample according to the methods described in 1, 2, 3, or 4 and its concentration in the extract is measured by inductive
26、ly coupled plasma-optical emission spectrometry (ICP- OES). 4.3 Method C: IC Sulfur is extracted from the fertilizer according to the methods described in 1, 2, 3, or 4 in the form of sulfate. The sulfate concentration of the extract is measured by ion chromatography (IC) equipped with a suppressor
27、device and a conductivity detector. Licensed Copy: London South Bank University, South Bank University, 16/11/2008 12:00, Uncontrolled Copy, (c) BSI DD CEN/TS 15749:2008 CEN/TS 15749:2008 (E) 5 5 Sampling and sample preparation Sampling is not part of the methods specified in this Technical Specific
28、ation. A recommended sampling method is given in EN 1482-1 5. Sample preparation shall be carried out in accordance with EN 1482-2. 6 Method A Gravimetric method 6.1 Reagents 6.1.1 General Use only reagents of recognized analytical grade and distilled or demineralized water (grade 3 according to EN
29、ISO 3696:1995). 6.1.2 Diluted hydrochloric acid Mix one volume of (HCl) = 1,18 g/ml with one volume of water. 6.1.3 Barium chloride solution, (BaCl2.2 H2O) = 122 g/l; 6.1.4 Silver nitrate solution, = 5 g/l. 6.2 Apparatus 6.2.1 Porcelain crucibles 6.2.2 Hot water bath 6.2.3 Drying oven, set at 105 C
30、1 C; 6.2.4 Electric oven, set at 800 C 50 C. 6.3 Procedure 6.3.1 Sampling of the solution Pipette an aliquot part of one of the extraction solutions containing between 20 mg and 100 mg of sulfur or 50 mg and 250 mg of SO3. Place this aliquot in a beaker of suitable capacity. Add 20 ml of diluted hyd
31、rochloric acid (6.1.2). Make up to about 300 ml with water. 6.3.2 Preparation of the precipitate Bring the solution to the boil. Add, drop by drop, about 20 ml of the barium chloride solution (6.1.3) while stirring the solution vigorously. Boil for a few minutes. Place the beaker, covered with a wat
32、ch glass, in a boiling hot water bath (6.2.2) for 1 h. Then leave standing hot ( 60 C) until the supernatant liquor is clear. Decant the clear solution through a slow filtration ash-free filter. Wash the precipitate several times with hot water. Continue to wash the precipitate on the filter until t
33、he filtrate is chloride free. This can be checked by using a silver nitrate solution (6.1.4). Licensed Copy: London South Bank University, South Bank University, 16/11/2008 12:00, Uncontrolled Copy, (c) BSI DD CEN/TS 15749:2008 CEN/TS 15749:2008 (E) 6 6.3.3 Incineration and weighing of the precipita
34、te Place the filter paper and precipitate in a porcelain crucible (6.2.1) previously weighed to the nearest 0,1 mg. Dry in the oven (6.2.3) and ash at approximately 800 C for half an hour (6.2.4). Allow to cool in a desiccator and weigh to 0,1 mg. 6.4 Calculation and expression of the result 1 mg of
35、 barium sulfate corresponds to 0,137 mg of sulfur or to 0,343 mg of SO3. Calculate the sulfates content, wS, as mass fraction in percent of the fertilizer according to equation (1): 22 1 1S 0,0137 mv v mw = (1) Calculate the SO3 content, wSO3, as mass fraction in percent of the fertilizer according
36、to equation (2): 2,5 SSO3 = ww (2) where m1 is the mass of the barium sulfate precipitate, in milligrams; m2 is the mass of the test portion, in grams; v1 is the volume of the extraction solution, in millilitres; v2 is the aliquot volume, in millilitres. 7 Method B ICP-OES method 7.1 Reagents 7.1.1
37、General Use only reagents of recognized analytical grade, and water conforming to grade 2 of EN ISO 3696:1995. Stock solutions shall be replaced after a maximum of one year, but the standard solution shall be freshly prepared monthly as a minimum. 7.1.2 Hydrochloric acid, approximately 1,18 g/ml; 7.
38、1.3 Diluted hydrochloric acid, mix 40 ml of hydrochloric acid (7.1.2) in 1 l of water; 7.1.4 Sulfur stock solution, corresponding to 1 000 mg/l sulfur. Dry in a pre-treatment step some grams of sodium sulfate (Na2SO4) at 105 C for 1 h. Let cool in a desiccator. Weigh to the nearest 0,1 mg, approxima
39、tely 4,4375 g of sodium sulfate (Na2SO4). Dissolve the weighted mass in a small quantity of water in volumetric flasks of nominal capacity of 1 000 ml, fill to the mark with water, The solution is stable for several months if stored at 4 C to 6 C. Licensed Copy: London South Bank University, South B
40、ank University, 16/11/2008 12:00, Uncontrolled Copy, (c) BSI DD CEN/TS 15749:2008 CEN/TS 15749:2008 (E) 7 NOTE Sulfur stock solution of 1 000 mg/l is also readily available commercially, and may be used instead. 7.2 Apparatus 7.2.1 General Common laboratory equipment and glassware, in particular equ
41、ipment according to 7.2.2 to 7.2.3. 7.2.2 Analytical balance, capable of weighing to an accuracy of 0,1 mg 7.2.3 Inductively coupled plasma Optical emission spectrometer Inductively Coupled Plasma Optical Emission Spectrometer (ICP-OES) with radial viewing of the plasma and simultaneous measurement
42、of emission signals. For measuring sulfur at wavelengths below 190 nm the optical system shall be evacuated or be filled or continuously flushed with an inert gas as recommended by the instrument manufacturer to obtain high and stable signal intensities. The instrument shall be equipped with radial
43、plasma as a minimum requirement; axial plasma is equally acceptable, as long as it can be shown that the results are statistically equal to the results obtained with radial plasma. Background correction shall also be performed. Settings of the working conditions (e. g. viewing height, gas flows, RF
44、or plasma power, sample uptake rate, integration time, number of replicates) shall be optimized according the manufacturers instructions. 7.3 Preparation of the extract The sulfur is extracted from the sample according to one of the methods described in 1, 2, 3, or 4. 7.4 Procedure 7.4.1 General Cal
45、ibration shall be performed by means of the standard addition technique. This method allows the analysis of fertilizers with unknown matrix composition or with a matrix that cannot be synthetically imitated easily. 7.4.2 Preparation of the test solution Dilute the extraction solution with the dilute
46、d hydrochloric acid (7.1.2) to obtain a concentration between 10 mg/l and 150 mg/l of sulfur. 7.4.3 Preparation of the blank test solution Carry out a blank test at the same time as the extraction, with only the reagents. 7.4.4 Preparation of the calibration solutions The additions to the test solut
47、ion, prior to the dilution step, should be about 20 %, 50 % and 100 % of the expected sulfur content. After the additions, dilute each of the samples with the diluted hydrochloric acid (7.1.2). A (external) calibration curve method can also be used instead of the standard addition method where the a
48、nalytical results are demonstrated to be statistically equal. Appropriate matrix matching of the calibration solutions shall be performed if an (external) calibration method is used. Licensed Copy: London South Bank University, South Bank University, 16/11/2008 12:00, Uncontrolled Copy, (c) BSI DD C
49、EN/TS 15749:2008 CEN/TS 15749:2008 (E) 8 7.5 Determination 7.5.1 General Set up the instrument according to the manufacturers instructions using appropriate conditions, and with the suitable background correction system in operation. For each instrument used, selectivity, limits of detection and quantification, precision, linear working area, and interference shall be established separately. 7.5.2 Determination by ICP-OES Aspirate the blank test solution (7.4.3), the test solution (7.4.2), and the var
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