BS DD CEN TS 15705-2009 肥料.使用高性能液体色谱法(HPLC)测定尿素冷凝物.异丁叉二脲和巴豆叉二脲(方法A)和亚甲脲低聚物(方法B).pdf
《BS DD CEN TS 15705-2009 肥料.使用高性能液体色谱法(HPLC)测定尿素冷凝物.异丁叉二脲和巴豆叉二脲(方法A)和亚甲脲低聚物(方法B).pdf》由会员分享,可在线阅读,更多相关《BS DD CEN TS 15705-2009 肥料.使用高性能液体色谱法(HPLC)测定尿素冷凝物.异丁叉二脲和巴豆叉二脲(方法A)和亚甲脲低聚物(方法B).pdf(24页珍藏版)》请在三一文库上搜索。
1、 This Draft for Development was published under the authority of the Standards Policy and Strategy Committee on 31 March 2009 - W - - - - - - - - - - - 7 -8 7 8 7 7 8- 787 7 $ - - -$- - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - W W D - w - - - - CEN/TS 15705:2009 (E) 2 Conten
2、ts Page Foreword 3 1Scope 4 2Normative references 4 3Terms and definitions .4 4Sampling and sample preparation .4 5Method A: Determination of CDU and IBDU .4 6Method B: Determination of methylen-urea oligomers (MU) 7 7Precision method A and method B . 12 8Test report . 13 Annex A (informative) Resul
3、ts of the inter-laboratory tests 14 Annex B (informative) Chromatogram and calibration curves method A 16 Annex C (informative) Chromatogram and calibration curves method B 18 Bibliography . 21 CEN/TS 15705:2009 (E) 3 Foreword This document (CEN/TS 15705:2009) has been prepared by Technical Committe
4、e 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 responsible for identifying any or all such patent righ
5、ts. 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 are bound to announce this Technical Specification:
6、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, Spain, Sweden, Switzerland and the United Kingdom. CEN/T
7、S 15705:2009 (E) 4 1 Scope This document specifies methods for the determination of isobutylidenediurea (IBDU), crotonylidenediurea (CDU) (method A) and methylene-urea oligomers (MU) (method B) in fertilizers using high-performance liquid chromatography (HPLC). The method is applicable for all ferti
8、lizers which do not contain interfering organic compounds. 2 Normative references The 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 (in
9、cluding 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 improvers Vocabulary Part 1: General terms EN 12944-2:1999, Fertilizers and liming materials and soil imp
10、rovers 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 purposes of this document, the terms and definitions given in EN 12944-1:1999 and EN 12944-2:1999 apply. 4 Samp
11、ling and sample preparation Sampling is not part of the method specified in this document. A recommended sampling method is given in EN 1482-1 1. Sample preparation shall be carried out in accordance with EN 1482-2. 5 Method A: Determination of CDU and IBDU 5.1 Principle The sample is extracted with
12、 water and, after appropriate dilution, analyzed using a suitable HPLC system. 5.2 Reagents 5.2.1 General Use only reagents of recognized analytical grade and distilled or demineralized water (grade 3 according to EN ISO 3696:1995). CEN/TS 15705:2009 (E) 5 5.2.2 Acetonitrile, p.a., HPLC-grade; 5.2.3
13、 Isobutylidenediurea and crotonylidenediurea, in their pure form. 5.3 Apparatus 5.3.1 Laboratory equipment and glassware, for preparation of solutions and dilutions; 5.3.2 Analytical balance, capable for weighing to an accuracy of 0,1 mg; 5.3.3 HPLC-system, with UV-detector; 5.3.4 Ultrasonic bath; 5
14、.3.5 Magnetic stirrer; 5.3.6 Disposible filter, 0,45 m. 5.4 Procedure 5.4.1 System parameters of HPLC Analytical/separating column: silica column with C18 reverse phase 1 Detection wavelength: 200 nm Eluent: acetonitrile/water: 10/90 (volume fraction) Flow rate: 1 ml/min Temperature: ambient tempera
15、ture Injection volume: 20 l 5.4.2 Calibration 5.4.2.1 Stock solution IBDU (IBDU) = 100 mg/l Weigh 100/R mg of IBDU (5.2.3), where R is the purity of IBDU, into a 1 000 ml flask and add about 900 ml of water (5.2.1). Dissolve in an ultrasonic bath (5.3.4) for about 10 min, followed by stirring on a m
16、agnetic stirrer (5.3.5) for about 1 h. Make up to volume. Filtration is not necessary. 5.4.2.2 Stock solution CDU (CDU) = 100 mg/l Weigh 100/R mg of CDU (5.2.3) , where R is the purity of CDU, into a 1 000 ml flask and add about 900 ml of water (5.2.1). Dissolve in an ultrasonic bath (5.3.4) for abo
17、ut 10 min, followed by stirring on a magnetic stirrer (5.3.5) for about 1 h. Make up to volume. Filtration is not necessary. 1 E.g. LiChrosorb RP-18 7m 250/4 mm or equivalent. CEN/TS 15705:2009 (E) 6 5.4.2.3 Calibration solution For calibration, prepare three solutions according to Table 1 using one
18、-mark (bulb) pipettes and dilute to the mark with water (5.2.1). For the determination of the retention time, dilute 10 ml of the stock solution 5.4.2.1 or respectively 5.4.2.2 into two 100 ml flasks and make up to volume with water (5.2.1). The evaluation of calibration is carried out manually or b
19、y means of a suitable PC-aided (computerized) calculation method. Table 1 Preparation of calibration solutions Parameter Amount of stock solution IBDU/CDU ml (to be added to the 100 ml flask) Content of IBDU mg/l Content of CDU mg/l Standard1 10 10,0 10,0 Standard 2 25 25,0 25,0 Standard 3 50 50,0 5
20、0,0 5.4.3 Preparation of the test portion Weigh 1 g of the sample grounded to 0,2 mm to the nearest 0,1 mg and flush into a 1 000 ml volumetric flask with water (5.2.1). Fill the flask to an amount of approximately 900 ml and treat it for 10 min in the ultrasonic bath (5.3.4). Then make up to the ma
21、rk and stir for 1 h at room temperature on a magnetic stirrer (5.3.5). Dilute 10 ml of the solution in a 100 ml volumetric flask and filter into the HPLC injection vial through a disposable filter (5.3.6). 5.4.4 Measurement Measurement is performed manually or by means of an automatic sample loading
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