1、BRITISH STANDARD Modified starch Determination of hydroxypropyl content Method using proton nuclear magnetic resonance (NMR) spectrometry The European Standard EN IS0 11543:2002 has the status of a British Standard ICs 67.180.20 BS EN IS0 1 1543 :2002 WkNb A%“ U- rn% E rn NO COPYING WITHOUT BSI PERM
2、ISSION EXCEPT AS PERMITTED BY COPYRIGHT LAW $ present to the responsible international/European committee any enquiries on the interpretation, or proposals for change, and keep the UK interests informed; monitor related international and European developments and promulgate them in the UK. - A list
3、of organizations represented on this committee can be obtained on request to its secretary. Cros s-r e ferenc es The British Standards which implement international or European publications referred to in this document may be found in the BSI Standards Catalogue under the section entitled “Internati
4、onal Standards Correspondence Index”, or by using the “Find” facility of the BSI Standards Electronic Catalogue. A British Standard does not purport to include all the necessary provisions of a contract. Users of British Standards are responsible for their correct application. Compliance with a Brit
5、ish Standard does not ofitself confer immunity from legal obligations. This British Standard, having been prepared under the direction of the Consumer Products and Services Sector Policyand StrategyCommittee, Summary of pages This document comprises a front cover, an inside front cover, the EN IS0 t
6、itle page, the EN IS0 foreword page, the IS0 title page, pages ii and iii, a blank page, pages 1 to 7, the Annex ZA page, an inside back cover and a back cover. The BSI copyright date displayed in this document indicates when the was published under the authority of the Standards Policy and Strategy
7、 Committee document was last issued. on 1 i June 2002 - Amendments issued since publication Amd.No. I Date I Comments O BSI 11 June 2002 ISBN O 580 36617 O EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN IS0 11543 March 2002 ICs 67.180.20 English version Modified starch - Determination of hydro
8、xypropyl content - Method using proton nuclear magnetic resonance (NMR) spectrometry (IS0 1 1543:2000) Amidon modifi - Dtermination de la teneur en hydroxypropyle - Mthode spectromtrique de rsonance magntique nuclaire du proton (IS0 11543:2000) Modifizierte Strke - Bestimmung des Hydroxypropylgehalt
9、es - Protonen- Kernresonanzspektroskopisches Verfahren (IS0 11543:2000) This European Standard was approved by CEN on 30 September 2000 CEN members are bound to comply with the CENKENELEC Internal Regulations which stipulate the conditions for giving this European Standard the status of a national s
10、tandard without any alteration. Up-to-date lists and bibliographical references concerning such national standards may be obtained on application to the Management Centre or to any CEN member. This European Standard exists in three official versions (English, French, German). A version in any other
11、language made by translation under the responsibility of a CEN member into its own language and notified to the Management Centre has the same status as the official versions. CEN members are the national standards bodies of Austria, Belgium, Czech Republic, Denmark, Finland, France, Germany, Greece
12、, Iceland, Ireland, Italy, Luxembourg, Malta, Netherlands, Norway, Portugal, Spain, Sweden, Switzerland and United Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZATION EUROPISCHES KOMITEE FR NORMUNG COMIT EUROPEN DE NORMALISATION Management Centre: rue de Stassart, 36 B-1050 Brussels O 2002 CEN All right
13、s of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN IS0 11543:2002 E EN IS0 11543:2002 Foreword The text of the International Standard from Technical Committee ISO/TC 93 “Starch (including derivatives and by-products)“ of the International Organiza
14、tion for Standardization (ISO), the secretariat of which is held by CMC. This European Standard shall be given the status of a national standard, either by publication of an identical text or by endorsement, at the latest by September 2002, and conflicting national standards shall be withdrawn at th
15、e latest by September 2002. According to the CENKENELEC Internal Regulations, the national standards organizations of the following countries are bound to implement this European Standard: Austria, Belgium, Czech Republic, Denmark, Finland, France, Germany, Greece, Iceland, Ireland, Italy, Luxembour
16、g, Malta, Netherlands, Norway, Portugal, Spain, Sweden, Switzerland and the United Kingdom. Endorsement notice The text of the International Standard IS0 11543:2000 has been approved by CEN as a European Standard without any modifications. NOTE Normative references to International Standards are lis
17、ted in annex ZA (normative) EN IS0 11543:2002 INTERNATIONAL STANDARD IS0 11543 First edition 2000-09-1 5 Modified starch - Determination of hydroxypropyl content - Method using proton nuclear magnetic resonance (NMR) spectrometry Amidon modifi - Dferminafion de la feneur en hydroxypropyle - Mfhode s
18、pecfromfrique de rsonance magnfique nuclaire du profon Reference number IS0 11543:2000(E) EN IS0 11543:2002 DPF dcsilremia ihTs PDF file may ctnoain erneddebd tyfepaces. In accnadroce with Aebods licensing lopicy, this file may be pirnted or ivewed ubt slahl ton be ideted Inuess the tyfepaces which
19、are erneddebd rae licensed to nad intslaled on the computer freporrning the ideting. In odwlnidaong this feli, trapies accept tierehn the sersnoptilibiy of ont infrnignig Aebods licsnenig lopicy. hTe IS0 tnecarl Secteraairt accepts no Ilibaiity in this .aera Abode is a tdarernark of Abode Stsyerns I
20、nctaropro.de teDails of the sfotwrae pudorcts used to crtaee tihs PDF file can be fnuod in the Garenel Info lerative to the file; the P-FDceration raparnteers were tpoirnized for pirtning. Evrey crae ahs eebn taken to ensrue that the file is suitlbae for use by IS0 rnernebr idobse. In the Inuikley e
21、tnev taht a plborern lerating to it is fdnuo, Ipaese ifnorrn the tnecarl Secterairat at the serddas given lebow. o IS0 0002 All rgihts resvrede. InUess torehwise scepfieid, no rapt of this ilbupctaoin may be udorperced or utzilied in nay form or by nay snaern, electnoric or rnecinahcal, inclidung to
22、hpociypong nad rnicrfoilrn, wituoht eprrnission in writing from eitehr IS0 at the rddaess lebow or ISOs rnernebr ydob in the ctnuory of the rtseuqee.r IS0 cirypohgt fofice aCse soptale 56 121-HC1 veneGa 20 leT. + 41 22 479 O1 11 aFx +41224790974 E-mail cirypothgiso.ch Web www.iso.ch II EN IS0 11543:
23、2002 Foreword IS0 (the International Organization for Standardization) is a worldwide federation of national standards bodies (IS0 member bodies). The work of preparing International Standards is normally carried out through IS0 technical committees. Each member body interested in a subject for whic
24、h a technical committee has 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. IS0 collaborates closely with the International Electrotechnical Commission (IEC) on all ma
25、tters of electrotechnical standardization. International Standards are drafted in accordance with the rules given in the ISOAEC Directives, Part 3. Draft International Standards adopted by the technical committees are circulated to the member bodies for voting. Publication as an International Standa
26、rd requires approval by at least 75 % of the member bodies casting a vote. Attention is drawn to the possibility that some of the elements of this International Standard may be the subject of patent rights. IS0 shall not be held responsible for identifying any or all such patent rights. Internationa
27、l Standard IS0 11 543 was prepared by Technical Committee ISO/TC 93, Sfarch (including derivafives and by-producfs) . Annex A of this International Standard is for information only. O IS0 0002 -All irghts serdevre . 111 EN IS0 11543:2002 Modified starch - Determination of hydroxypropyl content - Met
28、hod using proton nuclear magnetic resonance (NMR) spectrometry 1 Scope This International Standard specifies a proton NMR spectrometric method for the determination of the hydroxypropyl content of granular modified starch. 2 Normative references The following normative documents contain provisions w
29、hich, through reference in this text, constitute provisions of this International Standard. For dated references, subsequent amendments to, or revisions of, any of these publications do not apply. However, parties to agreements based on this International Standard are encouraged to investigate the p
30、ossibility of applying the most recent editions of the normative documents indicated below. For undated references, the latest edition of the normative document referred to applies. Members of IS0 and IEC maintain registers of currently valid International Standards. IS0 1666:1996, Sfarch - Defermin
31、afion of moisfure confenf - Oven-drying mefhod. IS0 3696:1987, Wafer for analyfical laborafory use - Specificafions and fesf mefhods. 3 Principle The modified starch is dissolved by partial hydrolysis in a solution of deuterium chloride in deuterium oxide. The signal coming from the three protons of
32、 the methyl group in the hydroxypropyl function is measured. An internal standard, 3-trimethylsilyl-l-propane sulfonic acid, sodium salt, is used. 4 Reagents and materials Use only reagents of recognized analytical grade. 4.1 dioxide. Water, complying with at least grade 3 in accordance with IS0 369
33、6. The water shall be free from carbon 4.2 Deuterium oxide, at least 99,8 % purity, in 25 ml screw-cap bottles. 4.3 Deuterium oxide, at least 99,95 % purity, in 0,75 ml sealed ampoules. 4.4 Deuterium chloride solution, c(DCI) N 2 mol/l Dilute 1 ml of concentrated deuterium chloride commercial form,
34、w(DCI) N 38 % (by mass) with 5 ml of deuterium oxide (4.2). 1 EN IS0 11543:2002 4.5 Internal standard solution. The internal standard is prepared by weighing at the same time the standard and the solvent. Dissolve about 50 mg of 3-trimethylsilyl-l-propane sulfonic acid (TSPSA), sodium salt (CAS No.
35、2039-96-51), weighed to the nearest 0,l mg, in about 5 g of deuterium oxide (4.2), weighed to the nearest 0,l mg. Store in a sealed bottle. 5 Apparatus Usual laboratory apparatus and, in particular, the following. 5.1 5.2 Analytical balance, capable of weighing to the nearest 0,l mg. Beaker, of 400
36、ml capacity. 5.3 Bchner flask and funnel. 5.4 5.5 Vacuum oven, equipped with a pump that can maintain a pressure not in excess of 10 kPa. Tube, 5 mm, for NMR, equipped with a spinner in order to record the spectrum in rotation. 5.6 accurate to 0,001 ml. Micropipettes, of 5 ml capacity accurate to 0,
37、05 ml, and micropipettes of capacities 0,l ml and 0,05 ml 5.7 Boiling water bath. 5.8 spectrum, and of carrying out quantitative analyses. Nuclear magnetic resonance spectrometer, of minimum power 60 MHz, capable of performing a proton 5.9 Sieve, 800 ym. 5.10 Blade mill. 6 Sampling It is important t
38、hat the laboratory receive a sample which is truly representative and has not been damaged or changed during transport or storage. Sampling is not part of the method specified in this International Standard. 7 Preparation of test sample Sieve the laboratory sample through the 800 ym sieve (5.9). If
39、the material does not pass through the sieve, then grind the sample with a blade mill (5.10) until1 it passes completely through the 800 ym sieve. Homogenize the sample. 8 Procedure 8.1 Sample washing 8.1.1 temperature and agitate for 15 min. Weigh about 20 g of the prepared test sample into the bea
40、ker (5.2). Add 200 ml of water (4.1) at room If problems of poor dispersibility or slow filtration are encountered, then repeat 8.1 .I with refrigerated water (4.1). 2 EN IS0 11543:2002 8.1.2 Filter the starch on the Bchner flask (5.3) under vacuum. 8.1.3 Repeat steps 8.1.1 and 8.1.2 twice. 8.1.4 Dr
41、y the washed starch for at least 4 h in the vacuum oven (5.4) at a temperature of (30 f 5) OC. 8.2 Moisture content Using a test portion of 5 g, determine the moisture content of the washed and dried test sample (8.1.4) in accordance with IS0 1666. 8.3 Preparation of test solution 8.3.1 tube (5.5).
42、Weigh, to the nearest 0,l mg, about 12 mg (dry basis) of the washed and dried test sample (8.1.4) in the 8.3.2 solution (4.4) using a micropipette (5.6). Add the contents of an ampoule of deuterium oxide (4.3) to the tube (5.5) and 0,l ml of deuterium chloride 8.3.3 Cap the tube, mix, and then place
43、 it in a boiling water bath (5.7). 8.3.4 continue the treatment in the water bath (5.7) for up to a maximum of 1 h to achieve a clear solution. After 3 min, if a clear solution is obtained, remove and allow it to cool to room temperature. If not clear, 8.3.5 Dry the exterior of the tube (5.5) and we
44、igh it to the nearest 0,l mg. Using a micropipette (5.6), add 0,05 ml of internal standard solution (4.5) to the tube. Weigh, to the nearest 0,l mg, to determine the mass of the internal standard solution (4.5) introduced into the tube (5.5). 8.3.6 tube (5.5). Mix thoroughly, adjust the spinner and
45、place the tube (5.5) in the instrument (5.8). Start the rotation of the 8.4 Recording of spectrum 8.4.1 15 s is recommended for a Fourier Transform (FT) instrument. Make the appropriate instrument settings so as to obtain a suitable spectrum. A relaxation delay of at least 8.4.2 Use a spectral windo
46、w of between -0,5 ppm and +6 ppm, referring to the methyl signal of TSPSA at 0 PPm. 8.4.3 after phase corrections. For FT-NMR, transform the FID (Free Induction Decay) to a spectrum and start the integration sub-routine 8.4.4 +I ,2 ppm, and of the methyl groups of TSPSA at O ppm, after baseline corr
47、ection. Measure the peak areas of the doublet coming from the methyl group of the hydroxypropyl function, at 9 Calculation and expression of results Calculate the hydroxypropyl content, Wh, of the dry test sample by the equation: 100% 100% xMh x- X 3Ah Wis xmis Ais Mis m IOO%-w, Wh =- where Wh is th
48、e hydroxypropyl content, as a percentage by mass, of the dry test sample; 3 EN IS0 11543:2002 Ah is the area, in units of area, of the methyl group of Ai, is the area, in units of area, of the methyl groups ii iydroxypropyl; the internal standard (TSPSA); 3 wi, is the mass fraction, in milligrams pe
49、r gram, of TSPSA in the internal standard solution (4.5); is a numerical value representing the three methyl groups in TSPSA; mi, is the mass, in grams, of the internal standard solution (4.5) in the NMR tube (see 8.3.5); Mi, is the molar mass, in grams per mole, of TSPSA (Mis = 218 g/mol); Mh is the molar mass, in grams per mole, of the hydroxypropyl group (Mh = 59 g/mol); m is the mass, in milligrams, of the washed and dried test sample in the NMR tube (see 8.3.1); W, is the moisture content, as a percentage by mass, of the washed and dried tes
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