1、STD-BSI BS EN IS0 31235-ENGL 1778 W Lb24bb7 0752373 752 1811 BS EN IS0 11215:1998 BRITISH STANDARD Incorporating Amendment No. 1 Modified starch - Determination of adipic acid content of acetylated di-starch adipates - Gas-chromatographic method The European Standard EN IS0 112151998 together with a
2、mendment no. 1 has the status of a British Standard ICs 67.180.20 NO COPYING WITHOUT ES1 PERMISSION EXCEPT AS PEI11IIITTED BY COPYRIGHT LAW BS EN IS0 11216:1998 Issue 2, Febnxary 1999 National foreword This British Standar is the Engiish language version of EN Is0 112161998, It is identicai with IS0
3、 112161998 and Amendment 11998. This British standard has been produced to fulnl BSls obiigation to publish all -ved European Standards but, because of the absence of interest in the UTK in the subject concerned, there has been no UK participalion in the preparation of EN 11215. Any queries relating
4、 to the EN are responsible for their correct appiication Compliance with a British Standard does not of itself confer immunity from legai obligations. I Amendments issued since publication AmdNo. Date I ISBN O 580 8- 6 STD-BSI BS EN IS0 LL2LS-ENGL 1798 1$1 lb24bb7 0752373 525 pl Issue 1, February 19
5、99 BS EN IS0 11215 : 1998 2 2 1 blank 2 I2 Summary of pages The following table identifies the current issue of each page. Issue 1 indicates that a page has been introduced for the first time by amendment. Subsequent issue numbers indicate an updated page. Vertical sidelining on replacement pages in
6、dicates the most recent changes (amendment, addition, deletion). Parte 1 issue II Page Front cover Inside front cover a b EN IS0 title page I EN IS0 foreword IS0 cover page IS0 Foreword 1 to 9 10 Inside back cover Back cover Issue Original original Original original O BSI 02-1999 a STD-BSI BS EN IS0
7、 11i-15-ENGL 1778 II Lb24bb7 0752374 qbl 0 EUROPEAN SIANDARD EN IS0 11215 NORME EUROPENNE EUROP ma is the mass, in micrograms, of adipic acid derived from the graph (9.1); I_ - = - rn is the mass, in grams, of the test portion; w, is the moisture content, in percentage by mass, of the test sample (s
8、ee 8.5). e - _. Round the result to the nearest 1 mg/kg. 9.3 Calculation of bound adipic acid content Calculate the bound adipic acid content by subtracting the free adipic acid content from the total adipic acid content. * rn * 10 Precision 10.1 Interlaboratory test Details of an interlaboratory te
9、st on the precision of the method are summarized in annex C. The values derived from this interlaboratory test may not be applicable to concentration ranges and matrices other than those given. 10.2 Repeatability The absolute difference between two independent single test results, obtained using the
10、 same method on identical test material in the same laboratory by the same operator using the same equipment within a short interval of time, will in not more than 5 % of cases exceed the value of r mentioned in or derived from table 1. 10.3 Reproducibility The absolute difference between two single
11、 test results, obtained using the same method on identical test material in different laboratories with different operators using different equipment, will in not more than 5 % of cases exceed the value of R mentioned in or derived from table 1. 5 I - - STD-BSI BS EN IS0 11215-ENGL 1798 W Lb24bbS U7
12、52383 47Li 6 EN IS0 1121k1998 Table 1 - Repeatability limit (0 and reproducibility limit (R) Mean total adipic acid content 405 430 659 7 22 36 11 Testreport The test report shall specify: - all information necessaiy for the complete identification of the sample; - the sampling method used, if known
13、; - the test method used; R mg/kg 33 91 114 1 42 175 . - the test result obtained; - if the repeatability has been checked, the final quoted result obtained; - all operating details not specified in this International Standard, or regarded as optional, together with details of any incidents that occ
14、urred when performing the method which may have influenced the test result(s). 6 STD-BSI BS EN IS0 LB2LS-ENGL 1798 IB ZL2LILb7 0752384 300 EN IS0 11215:1998 Annex A (informative) Typical conditions for chromatography A.1 Column WCOT fused silica, 0,32 mm internal diameter, 1 O m length, coating CP-S
15、IL 5C6, thickness 0,12 pm. A.2 Operating conditions Helium (4.1 l), carrier: 25 kPa (0,25 bar) Hydrogen (4.12) Air (4.13) : A.3 Chromatograph conditions Detector: 300 “C. - II e - e - A.4 Temperaturetime programme - - - Initial temperature: 50 kPa (0,5 bar) 100 kPa (1 ,O bar) 100 “C * * v1 Hold time
16、: 1 min Rate of increase: 25 “C/min Final temperature: 290 “C Hold time: 5 min Cool temperature: 100 “C NOTE The conditions described have been successfully used for the analysis. A column of a different specification, using the same liquid phase, will also resolve the silylated acids, but probably
17、with conditions modified from those described. 7 Q EN IS0 11215:1998 Annex B (informative) Typical chromatogram Figure 6.1 shows a typical chromatogram of an acetylated adipyl cross-linked corn starch sample. The retention time of the adipic acid derivative is 3,2 min, and of pimelic acid 3,7 min. A
18、DP20025 RAW 60 - 50 - 40 - 30 - 20 - 10 - 0- icc L O 1 2 3 4 5 6 7 min Figure B.l -Typical chromatogram of an acetylated adipyl cross-linked corn starch sample EN IS0 11215:1998 Number of outliers (laboratories) Number of acceoted results Annex C (informative) O O O O 1 18 18 18 18 16 Results of an
19、interlaboratory trial Repeatability standard deviation (sr), mgkg Repeatability relative standard deviation, % Reproducibility standard deviation (SR), mgikg Reproducibility relative standard deviation, % Reproducibility limit (R) R = 2,8 x sR, mgikg Repeatability limit (I) r= 2,8 x SA, mgkg An inte
20、rnational collaborative test involving nine laboratories was carried out on five different samples of acetylated di-starch adipates with waxy maize starch as the base material. 394 61 28 23 23 10.3 535 11 13 16,l 2,s 9,6 17,l 57 63 7,o 11,4 29,3 6,O 6,O 31,2 35,O 26,7 33,7 41 31,2 32,4 82,8 17,O 17,
21、O 88,3 The results obtained were subjected to statistical analysis in accordance with IS0 5725 l to give the precision data shown in tables C.l and C.2. Table C.l - Statistical results for total adipic acid content Repeatability relative standard deviation, % 5,1 593 5,5 5,4 1,7 Repeatability limit
22、(I) r= 2,8 x SA, mgikg 61 58 102 14 19 Reproducibility standard deviation (sR), mgikg 50 32 62 12 40 Reproducibility relative standard deviation, % 11,7 8,4 9,4 13,O 10,o - I ReproducibilioROP&CEE NOFN May 1998 ICs 67.180.20 Descriptors: see IS0 document Incorporates corrigendum October 1998 Engush
23、version Modified starch - Determination of adipic acid content of acetylated di-starch adipates - Gas-chomafrgmphic method (IS0 11215: 1998) (Incorporates corrigendum October 1998) Amidons et fcules modifis - Dtermination de la teneur en acide adipique dans les adipates de diamidon actyles - Mthode
24、par chromatographie en phase gazeuse Verfahren (IS0 11215:1998) (IS0 112151998) (Inclut le corrigendum octobre 1998) Modifizierte Strke - Bestimmung des Gehalts an Adipinsure in acetylierten Di-Strke-Adipaten - Gaschromatographisches (Eingearbeitet corrigendum Oktober 1998) This European Standard wa
25、s approved by CEN on 24 May 1998 and corrigendum October 1998. CEN members are bound to comply with the CENKENELEC Internal Regulations which stipulate the conditions for giving this Earopean Standard the status of a national standard without any alteration. Uptodate lists and bibliographical refere
26、nces concerning such national standards may be obtained on application to the Central Secretariat or to any CEN member. This European Standard exists in three official versions (English, French, German). A version in any other language made by translation under the responsibility of a CEN member int
27、o its own language and nosied to the Central Secretariat has the same status as the official versions. CEN members are the national standards bodies of Austria, Belgium, Denmark, Finland, France, Germany, Greece, Iceland, Ireland, Italy, Luxembourg, Netherlans, Norway, Portugal, Spain, Sweden, Switz
28、erland and United Kingdom. CEN European Committee for Standardization Comit Europen de Normalisation Europisches Komitee fur Normung Central Secretariat: rue de Stassart 36, B-1060 Brussels O 1998 CEN AU rights of exploitation in any form and by any means reserved worldwide for CEN national Members
29、Ref. No. EN IS0 112151998 E Issue 2, February 1999 EN IS0 11215:1998 Foreword The text of the International Standard IS0 112151998 has been prepared by Technical Committee ISORC 93, Starch (including derivatives and by-products), in collaboration with CEN/CS. This European standard shall be given th
30、e status of a national standard, either by publication of an identical text or by endorsement, at the latest by November 1998, and conflicting national standards shall be withdrawn at the latest by November 1998. According to the CENKENELEC Internal Regulations, the national standards organizations
31、of the following counties are bound to implement this European Standard: Austria, Belgium, Czech Republic, Denmark, Finland, France, Ge-, Greece, Iceland, Ireland, Italy, Luxembourg, Netherlands, Norwax Portugal, Spain, Sweden, Switzerland and the United Kingdom. NOTE FROM CENKS The foreword is susc
32、eptible to be amended on receipt of the Gem language version. The confirmed or amended foreword, and when appropriate, the nonnative annex ZA for the references to international publications with their relevant European publications will be circulated with the Gem version. Endorsement notice The tex
33、t of the Internatonal Standard IS0 11215:1998 was approved by CEN as a European Standard without any modification. Foreword to corrigendum The text of the International standard IS0 112151998 has been prepared by Technicd Committee ISO/Tc 93, Starch (including derivatives and by-products), in collab
34、oraiion with CEN/CS. This European standard shall be given the status of a national standard, either by publication of an identicai text or by endorsement, at e latest by November 1998, and conflicting national standards shall be withdrawn at the latest by November 1998. Endorsement notice The text
35、of the International Standard IS0 112151998 was approved by CEN as a European Standard without any modication. NOTE Normative references to International Standards are listed in annex ZA (normative). According to CENKENELEC Internal Regulations, the foiowing counties are bound to implement this Euro
36、pean Standard: Austria, Belgium, Czech Republic, Denmark, Finiand, Fhnce, Germany, Greece, Iceland, Ireland, Italy, Luxembourg, Netherlands, Norway, Portugal, Spain, Sweden, Switzerland and the United Kingdom. O BSI 02-1999 EN IS0 11215:1998 Repeatability relative standard deviation, YO Repeatabilit
37、y limit (0 r= 2,8 x SA, mg/kg Reproducibility relative standard deviation, % Reproducibility standard deviation mg/kg Reproducibility limit (R) IR = 2,8 x sal, mdka Annex C (informat ive) 591 513 585 5,4 1,7 61 58 102 14 19 50 32 62 12 40 11,7 8,4 9,4 13,O 10,o 142 91 175 33 114 Results of an interl
38、aboratory trial An international collaborative test involving nine laboratories was carried out on five different samples of acetylated di-starch adipates with waxy maize starch as the base material. The results obtained were subjected to statistical analysis in accordance with IS0 5725 l to give th
39、e precision data shown in tables C.1 and C.2. 1) All samples were acetylated di-starch adipates with waxy maize starch as the base material. NOTE Reference 121 shows that better orecision can be obtained with the method in certain cases. Table C.2 - Statistical results for free adipic acid content P
40、arameter i I 1 I 2 I 3 I 4 1 5 I I Number of laboratories retained aiter eliminating I outliers I Number of outliers (laboratories) lololool I Number of accepted results I 18 I 18 I 18 I 18 I 16 I 1) All samples were acetylated di-starch adipates with waxy maize starch as the base material. I 9 EN I
41、S0 11215:1998 Issue 2, February 19% Annex D (informative) Bibliography l IS0 !S25:1986, Pmision of test methods - Detemination of repeatabi/iy and reproducibi/ity for a siandard testmethodbyinter-boto tests (now withdrawn) was used to obtain the precision data. 2 Sanders, P. and Brunt, K., Improved
42、method for the determination of the total adipyl content in acetylated adipyl cross-linked starches, StacWWrke, 46 (1 994) No. 7, pp. 255-259. 3 Sanders, P. and Brunt, K., Gas chromatographic determination of free adipic acid and adipyl cross-linked starches, StatWStdrke, 48 (1996) No. 11/12, pp. 44
43、8-452. Annex 24 (nonnative) Normative references to international publications with their relevant European publications This European Standard incorporates by dated or undated reference, provisions from other pubiications. These normative references are cited at the appropriate places in the text a
44、nd the publications are listed hereafter. For dated references, subsequent amendments to or revisions of any of these publications apply to this European Standard only when incotpomted in it by amendment or revision. For undated references the latest &ion of the publication referred to applies. Is0 1666 1996 stareh - Detemnatim of moisture EN IS0 1666 content - Ovendrying methods YmI 1997 IS0 3696 1987 Water for anaiytii laboratoty use - Specification and test methods EN IS0 3696 1995 10 Q BSI 02-1999
