ISO-10504-1998.pdf
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1、A Reference number ISO 10504:1998(E) INTERNATIONAL STANDARD ISO 10504 First edition 1998-10-01 Starch derivatives Determination of the composition of glucose syrups, fructose syrups and hydrogenated glucose syrups Method using high-performance liquid chromatography Produits drivs de lamidon Dtermina
2、tion de la composition des sirops de glucose, des sirops de fructose, et des sirops de glucose hydrogns Mthode par chromatographie en phase liquide haute performance ISO 10504:1998(E) ISO 1998 All rights reserved. Unless otherwise specified, no part of this publication may be reproduced or utilized
3、in any form or by any means, electronic or mechanical, including photocopying and microfilm, without permission in writing from the publisher. International Organization for Standardization Case postale 56 CH-1211 Genve 20 Switzerland Internetisoiso.ch Printed in Switzerland ii Foreword ISO (the Int
4、ernational Organization for Standardization) is a worldwide federation of national standards bodies (ISO member bodies). The work of preparing International Standards is normally carried out through ISO technical committees. Each member body interested in a subject for which a technical committee ha
5、s been established has the right to be represented on that committee. International organizations, governmental and non- governmental, in liaison with ISO, also take part in the work. ISO collaborates closely with the International Electrotechnical Commission (IEC) on all matters of electrotechnical
6、 standardization. Draft International Standards adopted by the technical committees are circulated to the member bodies for voting. Publication as an International Standard requires approval by at least 75 % of the member bodies casting a vote. International Standard ISO 10504 was prepared by Techni
7、cal Commitee ISO/TC 93, Starch (including derivatives and by-products). Annex A of this International Standard is for information only. -,-,- INTERNATIONAL STANDARD ISOISO 10504:1998(E) 1 Starch derivatives Determination of the composition of glucose syrups, fructose syrups and hydrogenated glucose
8、syrups Method using high-performance liquid chromatography 1Scope This International Standard describes a high-performance liquid chromatographic (HPLC) method for measuring the composition of dextrose solutions, glucose syrups, fructose-containing syrups, hydrogenated glucose syrups, sorbitol, mann
9、itol and maltitol. The constituents are mainly glucose, maltose, maltotriose, fructose, sorbitol, mannitol, maltitol and malto-oligosaccharides. The use of a column packed with cation-exchange resin is essential. 2Normative references The following standards contain provisions which, through referen
10、ce in this text, constitute provisions of this International Standard. At the time of the publication, the editions indicated were valid. All standards are subject to revision, and parties to agreements based on this International Standard are encouraged to investigate the possibility of applying th
11、e most recent editions of the standards indicated below. Members of IEC and ISO maintain registers of currently valid International Standards. ISO 3696:1987,Water for analytical laboratory use Specification and test methods. ISO 5381:1983,Starch hydrolysis products Determination of water content Mod
12、ified Karl Fischer method. 3Principle Saccharide components are separated using high-performance liquid chromatography. Separation is achieved using a cation-exchange column with water as the eluent. The eluted components are detected by means of a differential refractometer, and quantified using an
13、 electronic integrator. 4Reagents All reagents used shall be of recognized analytical reagent grade. 4.1Special distilled water The water used may be double-distilled of quality grade 1 in accordance with ISO 3696. The most suitable is demineralized water, which prevents contamination of the ion-exc
14、hange resin. -,-,- ISO 10504:1998(E) ISO 2 The water should be filtered by passage through a 0,22 m filter. Also, it should be degassed by treatment under vacuum, or by use of an in-line degassing unit. The water should be maintained under an inert atmosphere, and preferably at 70 C to inhibit micro
15、bial growth. NOTE Some commercial water-purification devices produce water which is both filtered and degassed. 4.2Primary standard solutions Prepare solutions (see annex A) containing 10 % (or less) dry matter, according to the sensitivity of the refractometer, with compositions as close as possibl
16、e to that of the samples to be analysed. NOTE Suitable reference materials for the constituents listed in clause 1 can be obtained from established chemical companies. 4.3Ion-exchange resins, for off-line demineralization of samples. Salts present in the sample will co-elute from the column, and wil
17、l be detected by the refractometer, causing errors in the determination. These salts shall first be removed by ion-exchange resins. The most convenient way is to have an in-line guard column cartridge system (5.5), but this may also be carried out off-line using the following resins. a) Cation type:
18、 strong cation exchanger, 4 % cross-linked polystyrene divinylbenzene, in the H+ form; 200 mesh to 400 mesh in the dry form. b) Anion type: weak anion exchanger, 4 % cross-linked polystyrene divinylbenzene support containing tertiary amine groups, in the free base form; 200 mesh to 400 mesh in the d
19、ry form. NOTE While resins meeting these specifications are available from more than one supplier, their performance is variable. Experience in several laboratories shows that the resins sold by Bio-Rad 1) (AG50W - X4, AG3 - X4) perform satisfactorily. 5Apparatus 5.1 Liquid chromatograph, equipped w
20、ith the following: a pump, pulseless, that delivers a constant flow, at the rate required; a differential refractometer, thermostatically controlled; a thermostatically controlled column oven, capable of maintaining the column at temperatures up to 95 C, to within 0,5 C. 5.2 Sample injector, compris
21、ing a loop injector (manual or part of autosampler) with a capacity of 20 l or less. 5.3 Integrator, comprising an electronic integrator with calculating and recording capabilities, compatible with the voltage output of the detector. 5.4 Separation column, comprising a pre-packed cation-exchange col
22、umn in the form best suited for the analysis. 1) This information is given for the convenience of users of this International Standard and does not constitute an endorsement by ISO of these products. Equivalent products may be used if they can be shown to lead to the same results. ISOISO 10504:1998(
23、E) 3 The recommended resin is 6 % to 8 % cross-linked sulfonated polystyrene divinylbenzene with a bead diameter of 9 m to 25 m. NOTE Acceptable columns are available from several major column suppliers. 5.5 Guard columns, custom-prepared dual-cartridge system, inserted unheated in-line, to deminera
24、lize the sample. NOTE There are a few systems available but with varying efficiency. The Bio-Rad 2) guard cartridges 125-0118 have been shown in several laboratories to be the most effective in all respects. 5.6 Sample filtration system, comprising a syringe to which suitable membrane disc filters c
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