BS DD CEN TS 13130-16-2005 和食品接触的材料和物品.受限制的塑料物质.食品模拟物中己内酰胺和己内酰胺盐的测定.pdf
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1、DRAFT FOR DEVELOPMENT DD CEN/TS 13130-16:2005 Materials and articles in contact with foodstuffs Plastics substances subject to limitation Part 16: Determination of caprolactam and caprolactam salt in food simulants ICS 67.250 DD CEN/TS 13130-16:2005 This Draft for Development was published under the
2、 authority of the Standards Policy and Strategy Committee on 16 September 2005 BSI 16 September 2005 ISBN 0 580 46071 1 National foreword This Draft for Development is the official English language version of CEN/TS 13130-10:2005. This publication is not to be regarded as a British Standard. It is b
3、eing issued in the Draft for Development series of publications and is of a provisional nature because the method was not evaluated using recognized ring trial procedures. As a consequence there are no reproducibility data for the method. It should be applied on this provisional basis, so that infor
4、mation and experience of its practical application may be obtained. Comments arising from the use of this Draft 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
5、 initiated 2 years after its publication by the European organization so that a decision can be taken on its status at the end of its 3-year life. 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 rec
6、eived by the end of the review period, the responsible BSI Committee will decide whether to support the conversion into a European Standard, to extend the life of the Technical Specification or to withdraw it. Comments should be sent in writing to the Secretary of BSI Subcommittee CW/47/1 Migration
7、from plastics, at British Standards House, 389 Chiswick High Road, London W4 4AL, giving the document reference and clause number and proposing, where possible, an appropriate revision of the text. A list of organizations represented on this subcommittee can be obtained on request to its secretary.
8、Cross-references The British Standards which implement international or European publications referred to in this document may be found in the BSI Catalogue under the section entitled “International Standards Correspondence Index”, or by using the “Search” facility of the BSI Electronic Catalogue or
9、 of British Standards Online. This publication does not purport to include all the necessary provisions of a contract. Users are responsible for its correct application. Summary of pages This document comprises a front cover, an inside front cover, the CEN/TS title page, pages 2 to 16, an inside bac
10、k cover and a back cover. The BSI copyright notice displayed in this document indicates when the document was last issued. Amendments issued since publication Amd. No. DateComments W - - - - - - - - - - 7 - - 7- - - - - 7- - - - - 7 - - - - - - - - 98 % (GC). 4.1.2 Aza-2-cyclononanone, (8-aminooctan
11、oic acid lactam; 8-Caprylolactam), C8H15NO molecular weight 141,2, purity 99 %. 4.2 Chemicals 4.2.1 Ethanol, absolute 4.2.2 n-Heptane 4.2.3 Methanol 4.2.4 Water, deionized 4.3 Solutions 4.3.1 Ethanol/water = 1:2 Measure 200 ml ethanol (4.2.1) and make up with water (4.2.4) to 600 ml. 4.3.2 Standard
12、stock solution of caprolactam in methanol (0,5 mg/ml) Weigh to the nearest 0,1 mg approximately 50 mg of caprolactam (4.1.1) into a 100 ml volumetric flask. Dissolve the caprolactam in methanol and make up to the mark with methanol (4.2.3). Calculate the exact concentration in milligrams of caprolac
13、tam per millilitre solution. Repeat the procedure to obtain a second stock solution. NOTE The solution can be stored in a well-closed container in the dark for a maximum period of 3 months at any temperature between - 20 C to + 20 C. 4.3.3 Internal standard stock solution of caprylolactam in methano
14、l (0,35 mg/ml) Weigh to the nearest 0,1 mg approximately 70 mg of caprylolactam (4.1.2) into a 200 ml volumetric flask. Dissolve the caprylolactam in methanol and make up to the mark with methanol (4.2.3). Calculate the exact concentration in milligrams caprylolactam per millilitre of solution. NOTE
15、 The solution can be stored in a well-closed container in the dark for a maximum period of 3 months at any temperature between - 20 C and + 20 C. 4.3.4 Diluted internal standard solution of caprylolactam in methanol (0,07 mg/ml) Transfer by pipette 10,0 ml of the internal standard stock solution (4.
16、3.3) into a 50 ml volumetric flask and make up to the mark with methanol (4.2.3). Calculate the concentration in milligrams of caprylolactam per millilitre of solution. DD CEN/TS 13130-16:2005 8 4.3.5 Standard solutions Add to a series of 25 ml volumetric flasks, 0 ml, 1 ml, 2 ml, 4 ml, 6 ml and 8 m
17、l of the standard stock solution of caprolactam (4.3.2). Add to each of the flasks 5,0 ml of the internal standard stock solution of caprylolactam (4.3.3) and make up to the mark with methanol (4.2.3). The standards thus obtained contain approximately 0 g/ml, 20 g/ml, 40 g/ml, 80 g/ml, 120 g/ml and
18、160 g/ml of caprolactam and 70 g of caprylolactam per millilitre of methanol. Calculate the exact concentrations in micrograms per millilitre of methanol. Repeat the procedure using the second standard stock solution to obtain a second series of standard solutions. 5 Apparatus NOTE An instrument or
19、item of apparatus is listed only where it is special or made to a particular specification, usual laboratory glassware and equipment being assumed to be available. 5.1 Gas chromatograph, equipped with a flame ionization detector and preferably with an automatic injection sampler, capable of separati
20、ng caprolactam fully from caprylolactam as well as from peaks originating from simulants and/or solvents used. Appropriate operating conditions shall be established for the specific equipment used for the determination. NOTE 1 The following chromatographic columns and conditions have been found to b
21、e satisfactory: Column 1 25 m x 0,32 mm fused silica WCOT provided with a 1,2 m thick layer of 7 % cyanopropyl, 7 % phenyl, 85 % methyl and 1 % vinylpolysiloxane. DD CEN/TS 13130-16:2005 9 GC parameters: Column oven 200 C Injector 240 C Detector 250 C Carrier gas helium Inlet pressure 150 kPa Flow 3
22、 ml/min Injector split (split ratio 1:14) Injection volume: 0.5 l FID gasses optimized according to the manufacturers specifications. GC apparatus should be optimized according to manufacturers instruction. Occasionally, double peaks for caprolactam have been observed. Reasons for this phenomenon sh
23、ould be found in the injection system. Cleaning or exchange of the injector liner is recommended to overcome the problem. In any case, double peaks should not be evaluated. NOTE 2 Other columns that have been found to be suitable are as follows: Column 2 50 m x 0,2 mm fused silica coated with 0,5 m
24、methylsilicone. Temperature programme 2 min at 80 C then ramped at 5 C per minute to 230 C Carrier gas helium at 220,6 kPa Injection temperature 250 C Detector temperature 280 C Column 3 2 m x 2 mm stainless steel column, packed with Gaschrom Q 100 mesh to 120 mesh coated with 10 % of polyethylenegl
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