1、BRITISH STANDARD BS EN ISO 11543:2002 Modified starch Determination of hydroxypropyl content Method using proton nuclear magnetic resonance (NMR) spectrometry The European Standard EN ISO 11543:2002 has the status of a British Standard ICS 67.180.20 NO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMIT
2、TED BY COPYRIGHT LAWBS EN ISO 11543:2002 This British Standard, having been prepared under the direction of the Consumer Products and Services Sector Policy and Strategy Committee, was published under the authority of the Standards Policy and Strategy Committee on 11 June 2002 BSI 11 June 2002 ISBN
3、0 580 36617 0 National foreword This British Standard is the official English language version of EN ISO 11543:2002. It is identical with ISO 11543:2000. The UK participation in its preparation was entrusted to Technical Committee AW/100, Miscellaneous agriculture and food, which has the responsibil
4、ity to: A list of organizations represented on this committee can be obtained on request to its secretary. Cross-references 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
5、 “International 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
6、with a British Standard does not of itself confer immunity from legal obligations. aid enquirers to understand the text; present to the responsible international/European committee any enquiries on the interpretation, or proposals for change, and keep the UK interests informed; monitor related inter
7、national and European developments and promulgate them in the UK. Summary of pages This document comprises a front cover, an inside front cover, the EN ISO title page, the EN ISO foreword page, the ISO title page, pages ii and iii, a blank page, pages 1 to 7, the Annex ZA page, an inside back cover
8、and a back cover. The BSI copyright date displayed in this document indicates when the document was last issued. Amendments issued since publication Amd. No. Date CommentsEUROPEANSTANDARD NORMEEUROPENNE EUROPISCHENORM ENISO11543 March2002 ICS67.180.20 Englishversion ModifiedstarchDeterminationofhydr
9、oxypropylcontent Methodusingprotonnuclearmagneticresonance(NMR) spectrometry(ISO11543:2000) AmidonmodifiDterminationdelateneuren hydroxypropyleMthodespectromtriquedersonance magntiquenuclaireduproton(ISO11543:2000) ModifizierteStrkeBestimmungdes HydroxypropylgehaltesProtonen Kernresonanzspektroskopi
10、schesVerfahren(ISO 11543:2000) ThisEuropeanStandardwasapprovedbyCENon30September2000. CENmembersareboundtocomplywiththeCEN/CENELECInternalRegulationswhichstipulatetheconditionsforgivingthisEurope an Standardthestatusofanationalstandardwithoutanyalteration.Uptodatelistsandbibliographicalreferencescon
11、cernings uchnational standardsmaybeobtainedonapplicationtotheManagementCentreortoanyCENmember. ThisEuropeanStandardexistsinthreeofficialversions(English,French,German).Aversioninanyotherlanguagemadebytra nslation undertheresponsibilityofaCENmemberintoitsownlanguageandnotifiedtotheManagementCentrehas
12、thesamestatusasthe official versions. CENmembersarethenationalstandardsbodiesofAustria,Belgium,CzechRepublic,Denmark,Finland,France,Germany,Greece, Iceland,Ireland,Italy,Luxembourg,Malta,Netherlands,Norway,Portugal,Spain,Sweden,SwitzerlandandUnitedKingdom. EUROPEANCOMMITTEEFORSTANDARDIZATION COMITEU
13、ROPENDENORMALISATION EUROPISCHESKOMITEEFRNORMUNG ManagementCentre:ruedeStassart,36B1050Brussels 2002CEN Allrightsofexploitationinanyformandbyanymeansreserved worldwideforCENnationalMembers. Ref.No.ENISO11543:2002EINESO11:3452002(E) 2 Foreword ThetextoftheInternationalStandardfromTechnicalCommitteeIS
14、O/TC93“Starch(including derivativesandbyproducts)“oftheInternationalOrganizationforStandardization(ISO),the secretariatofwhichisheldbyCMC. ThisEuropeanStandardshallbegiventhestatusofanationalstandard,eitherbypublicationof anidenticaltextorbyendorsement,atthelatestbySeptember2002,andconflictingnation
15、al standardsshallbewithdrawnatthelatestbySeptember2002. AccordingtotheCEN/CENELECInternalRegulations,thenationalstandardsorganizationsof thefollowingcountriesareboundtoimplementthisEuropeanStandard:Austria,Belgium,Czech Republic,Denmark,Finland,France,Germany,Greece,Iceland,Ireland,Italy,Luxembourg,
16、 Malta,Netherlands,Norway,Portugal,Spain,Sweden,SwitzerlandandtheUnitedKingdom. Endorsementnotice ThetextoftheInternationalStandardISO11543:2000hasbeenapprovedbyCENasa EuropeanStandardwithoutanymodifications. NOTENormativereferencestoInternationalStandardsarelistedinannexZA(normative). ENISO11543:20
17、02 Reference number ISO 11543:2000(E) INTERNATIONAL STANDARD ISO 11543 First edition 2000-09-15 Modified starch Determination of hydroxypropyl content Method using proton nuclear magnetic resonance (NMR) spectrometry Amidon modifi Dtermination de la teneur en hydroxypropyle Mthode spectromtrique de
18、rsonance magntique nuclaire du proton ENISO11543:2002 DPFdcsilremia ihTsPDFfilemayctnoainemeddebdtyfepaces.InaccnadrocewithAebodslicensinglopicy,thisfilemaybepirntedorivewedubtslahlton beidetedlnuessthetyfepaceswhichareemeddebdraelicensedtonadintslaledonthecomputerfrepormingtheideting.Inodwlnidaongt
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21、orutziliedinnayformorbynaysnaem,electnoric ormecinahcal,inclidungtohpociypongnadmicrfoilm,wituohteprmissioninwritingfromeitehrISOattherddaessleboworISOsmemebrydob inthectnuoryofthertseuqee.r ISOcirypohgtfofice aCsesoptale56 121-HC1veneGa20 leT.+41224790111 aFx+41224790974 E-mailcirypothgiso.ch Webww
22、w.iso.ch ii ENISO11543:2002 ISO 0002 All irghts serdevre iii Foreword ISO (the International 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 commi
23、ttees. Each member body interested in a subject for which 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. ISO collaborates closely with the I
24、nternational Electrotechnical Commission (IEC) on all matters of electrotechnical standardization. International Standards are drafted in accordance with the rules given in the ISO/IEC Directives, Part 3. Draft International Standards adopted by the technical committees are circulated to the member
25、bodies for voting. Publication as an International Standard 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. ISO shall not be held responsible fo
26、r identifying any or all such patent rights. International Standard ISO 11543 was prepared by Technical Committee ISO/TC 93, Starch (including derivatives and by-products). Annex A of this International Standard is for information only. ENISO11543:2002 INTENRATIONAL TSANDADR ISO 34511:(0002)E ISO 00
27、02 All rights rsedevre 1 Modified starch Determination of hydroxypropyl content Method 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 st
28、arch. 2 Normative references The following normative documents contain provisions which, 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
29、agreements based on this International Standard are encouraged to investigate the possibility 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 ISO and IEC maintain reg
30、isters of currently valid International Standards. ISO 1666:1996, Starch Determination of moisture content Oven-drying method. ISO 3696:1987, Water for analytical laboratory use Specifications and test methods. 3P r i n c i p l e The modified starch is dissolved by partial hydrolysis in a solution o
31、f deuterium chloride in deuterium oxide. The signal coming from the three protons of the methyl group in the hydroxypropyl function is measured. An internal standard, 3-trimethylsilyl-1-propane sulfonic acid, sodium salt, is used. 4 Reagents and materials Use only reagents of recognized analytical g
32、rade. 4.1 Water, complying with at least grade 3 in accordance with ISO 3696. The water shall be free from carbon dioxide. 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 solutio
33、n, c(DCl) 2mol /l. Dilute 1 ml of concentrated deuterium chloride commercial form, w(DCl) 38 % (by mass) with 5 ml of deuterium oxide (4.2). ENISO11543:20021ISO 34511:(0002)E 2 ISO 0002 All rights rsedevre 4.5 Internal standard solution. The internal standard is prepared by weighing at the same time
34、 the standard and the solvent. Dissolve about 50 mg of 3-trimethylsilyl-1-propane sulfonic acid (TSPSA), sodium salt (CAS No. 2039-96-51), weighed to the nearest 0,1 mg, in about 5 g of deuterium oxide (4.2), weighed to the nearest 0,1 mg. Store in a sealed bottle. 5 Apparatus Usual laboratory appar
35、atus and, in particular, the following. 5.1 Analytical balance, capable of weighing to the nearest 0,1 mg. 5.2 Beaker, of 400 ml capacity. 5.3 Bchner flask and funnel. 5.4 Vacuum oven, equipped with a pump that can maintain a pressure not in excess of 10 kPa. 5.5 Tube, 5 mm, for NMR, equipped with a
36、 spinner in order to record the spectrum in rotation. 5.6 Micropipettes, of 5 ml capacity accurate to 0,05 ml, and micropipettes of capacities 0,1 ml and 0,05 ml accurate to 0,001 ml. 5.7 Boiling water bath. 5.8 Nuclear magnetic resonance spectrometer, of minimum power 60 MHz, capable of performing
37、a proton spectrum, and of carrying out quantitative analyses. 5.9 Sieve, 800 m. 5.10 Blade mill. 6 Sampling It is important that 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
38、 in this International Standard. 7 Preparation of test sample Sieve the laboratory sample through the 800 m sieve (5.9). If the material does not pass through the sieve, then grind the sample with a blade mill (5.10) untill it passes completely through the 800 m sieve. Homogenize the sample. 8 Proce
39、dure 8.1 Sample washing 8.1.1 Weigh about 20 g of the prepared test sample into the beaker (5.2). Add 200 ml of water (4.1) at room temperature and agitate for 15 min. If problems of poor dispersibility or slow filtration are encountered, then repeat 8.1.1 with refrigerated water (4.1). ENISO11543:2
40、0022ISO 34511:(0002)E ISO 0002 All rights rsedevre 3 8.1.2 Fi l te rth esta rcho nth eB chner flask (5.3) under vacuum. 8.1.3 Repeat steps 8.1.1 and 8.1.2 twice. 8.1.4 Dry the washed starch for at least 4 h in the vacuum oven (5.4) at a temperature of (30 5) C. 8.2 Moisture content Using a test port
41、ion of 5 g, determine the moisture content of the washed and dried test sample (8.1.4) in accordance with ISO 1666. 8.3 Preparation of test solution 8.3.1 Weigh, to the nearest 0,1 mg, about 12 mg (dry basis) of the washed and dried test sample (8.1.4) in the tube (5.5). 8.3.2 Add the contents of an
42、 ampoule of deuterium oxide (4.3) to the tube (5.5) and 0,1 ml of deuterium chloride solution (4.4) using a micropipette (5.6). 8.3.3 Cap the tube, mix, and then place it in a boiling water bath (5.7). 8.3.4 After 3 min, if a clear solution is obtained, remove and allow it to cool to room temperatur
43、e. If not clear, continue the treatment in the water bath (5.7) for up to a maximum of 1 h to achieve a clear solution. 8.3.5 Dry the exterior of the tube (5.5) and weigh it to the nearest 0,1 mg. Using a micropipette (5.6), add 0,05 ml of internal standard solution (4.5) to the tube. Weigh, to the
44、nearest 0,1 mg, to determine the mass of the internal standard solution (4.5) introduced into the tube (5.5). 8.3.6 Mix thoroughly, adjust the spinner and place the tube (5.5) in the instrument (5.8). Start the rotation of the tube (5.5). 8.4 Recording of spectrum 8.4.1 Make the appropriate instrume
45、nt settings so as to obtain a suitable spectrum. A relaxation delay of at least 15 s is recommended for a Fourier Transform (FT) instrument. 8.4.2 Use a spectral window of between 0,5 ppm and 6 ppm, referring to the methyl signal of TSPSA at 0 ppm. 8.4.3 For FT-NMR, transform the FID (Free Induction
46、 Decay) to a spectrum and start the integration sub-routine after phase corrections. 8.4.4 Measure the peak areas of the doublet coming from the methyl group of the hydroxypropyl function, at 1,2 ppm, and of the methyl groups of TSPSA at 0 ppm, after baseline correction. 9 Calculation and expression
47、 of results Calculate the hydroxypropyl content, w h , of the dry test sample by the equation: is is h hh is is m 3 100 % 100 % 100 % wm A wM AMmw where w h is the hydroxypropyl content, as a percentage by mass, of the dry test sample; ENISO11543:20023ISO 34511:(0002)E 4 ISO 0002 All rights rsedevre
48、 A h is the area, in units of area, of the methyl group of hydroxypropyl; A is is the area, in units of area, of the methyl groups in the internal standard (TSPSA); 3 is a numerical value representing the three methyl groups in TSPSA; w is is the mass fraction, in milligrams per gram, of TSPSA in the internal standard solution (4.5); m is is the mass, in grams, of the internal standard solution (4.5) in the
