《ISO-11025-1998.pdf》由会员分享，可在线阅读，更多相关《ISO-11025-1998.pdf（10页珍藏版）》请在三一文库上搜索。
1、A Reference number ISO 11025:1998(E) INTERNATIONAL STANDARD ISO 11025 First edition 1998-02-01 Oil of cassia, Chinese type Determination of trans-cinnamaldehyde content Gas chromatographic method on capillary columns Huile essentielle de cannelle type Chine Dtermination de la teneur en trans-cinnama
2、ldhyde Mthode par chromatographie en phase gazeuse sur colonne capillaire Copyright International Organization for Standardization Provided by IHS under license with ISO Licensee=NASA Technical Standards 1/9972545001 Not for Resale, 04/24/2007 22:22:20 MDTNo reproduction or networking permitted with
3、out license from IHS -,-,- ISO 11025:1998(E) ISO 1998 All rights reserved. Unless otherwise specified, no part of this publication may be reproduced or utilized in any form or by any means, electronic or mechanical, including photocopying and microfilm, without permission in writing from the publish
4、er. International Organization for Standardization Case postale 56 CH-1211 Genve 20 Switzerland Internetcentraliso.ch X.400c=ch; a=400net; p=iso; o=isocs; s=central Printed in Switzerland ii Foreword ISO (the International Organization for Standardization) is a worldwide federation of national stand
5、ards 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 has been established has the right to be represented on that committee. International orga
6、nizations, governmental and non- governmental, in liaison with ISO, also take part in the work. ISO collabo- rates closely with the International Electrotechnical Commission (IEC) on all matters of electrotechnical standardization. Draft International Standards adopted by the technical committees ar
7、e 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 11025 was prepared by Technical Committee ISO/TC 54, Essential oils. Annex A of this International Standard is for
8、 information only. Copyright International Organization for Standardization Provided by IHS under license with ISO Licensee=NASA Technical Standards 1/9972545001 Not for Resale, 04/24/2007 22:22:20 MDTNo reproduction or networking permitted without license from IHS -,-,- ISOISO 11025:1998(E) iii Int
9、roduction Since the description of methods of analysis by gas chromatography is very long, it is considered useful to establish general methods on the one hand, giving detailed information on all the recurrent parameters, appara- tus, products, methods, formulae, etc., and on the other hand standard
10、s with short details on the determination of specific constituents on the es- sential oils, giving only those operating conditions specific to the pertinent determination. This is the case with the present International Standard, which refers to the general standard ISO 7609 for the general paragrap
11、hs. Copyright International Organization for Standardization Provided by IHS under license with ISO Licensee=NASA Technical Standards 1/9972545001 Not for Resale, 04/24/2007 22:22:20 MDTNo reproduction or networking permitted without license from IHS -,-,- Copyright International Organization for St
12、andardization Provided by IHS under license with ISO Licensee=NASA Technical Standards 1/9972545001 Not for Resale, 04/24/2007 22:22:20 MDTNo reproduction or networking permitted without license from IHS -,-,- INTERNATIONAL STANDARD ISOISO 11025:1998(E) 1 Oil of cassia, Chinese type Determination of
13、 trans- cinnamaldehyde content Gas chromatographic method on capillary columns 1 Scope This International Standard specifies a method for the determination of the trans-cinnamaldehyde content of the essential oil of cassia, Chinese type (Cinna- momum aromaticum Nees, syn. Cinnamomum cassia Nees ex B
14、lume). 2 Normative references The following standards contain provisions which, through reference in this text, constitute provisions of this International Standard. As the time of publication, the editions indicated were valid. All standards are subject to revision, and parties to agreements based
15、on this International Standard are encouraged to in- vestigate the possibility of applying the most recent editions of the standards indicated below. Members of IEC and ISO maintain registers of currently valid Inter- national Standards. ISO 356:1996, Essential oils Preparation of test samples. ISO
16、7609:1985, Essential oils Analysis by gas chromatography on capillary columns General method. 3 Principle Analysis by gas chromatography on a capillary col- umn, under specified conditions, of oil of cassia, Chi- nese type. Determination of the trans-cinnamaldehyde content using the internal standar
17、d method. 4 Reagents and products During the analysis, unless otherwise specified, use only reagents of recognized analytical grade. 4.1 Reference substance trans-Cinnamaldehyde, of purity at least 99 %, deter- mined by chromatography under the test conditions. 4.2 Internal standard Tridecane, of pu
18、rity at least 99 %, determined by chromatography under the test conditions. 5 Apparatus 5.1 Chromatograph, recorder and electronic integrator See ISO 7609. 5.2 Column Length:25 m to 50 m Internal diameter: 0,2 mm to 0,3 mm Stationary phase: polydimethylsiloxane (OV 101) or polyethylene glycol 20 000
19、 (carbowax 20 M) 5.3 Detector Flame ionization type. 6 Preparation of test sample See ISO 356. 7 Operating conditions 7.1 Temperatures Oven temperature: For example, in the columns, linear temperature programming from 100 C to 200 C at a rate of 3 C/min, or 60 C to 200 C at a rate of 1,5 C/min, then
20、 kept constant at 200 C for 15 min. Copyright International Organization for Standardization Provided by IHS under license with ISO Licensee=NASA Technical Standards 1/9972545001 Not for Resale, 04/24/2007 22:22:20 MDTNo reproduction or networking permitted without license from IHS -,-,- ISO 11025:1
21、998(E) ISO 2 Injector temperature: For example, 230 C to 240 C. Detector temperature: For example, 230 C to 240 C. 7.2 Carrier gas flow rate and auxiliary gases flow rate See ISO 7609. 8 Column performance 8.1 Chemical inertness test Carry out the test as specified in ISO 7609. 8.2 Column efficiency
22、 Determine the column efficiency as specified in ISO 7609. 9 Determination of retention indexes See ISO 7609. 10 Determination 10.1 Determination of response factor Determine the response factor as specified in ISO 7609. 10.2 Internal standard method Carry out the determination of the trans-cinnam-
23、aldehyde content of the essential oil by the internal standard method specified in ISO 7609, using tride- cane (4.2) as internal standard. 11 Expression of results 11.1 Calculation See ISO 7609. NOTE Typical chromatograms are given, for information only, in annex A. 11.2 Repeatability See ISO 7609.
24、12 Test report See ISO 7609. Copyright International Organization for Standardization Provided by IHS under license with ISO Licensee=NASA Technical Standards 1/9972545001 Not for Resale, 04/24/2007 22:22:20 MDTNo reproduction or networking permitted without license from IHS -,-,- ISO ISO 11025:1998
25、(E) 3 Annex A (informative) Typical chromatograms for determination of the trans-cinnamaldehyde content in oil of cassia, Chinese type Peak identification 1 Styrene 2 Benzaldehyde 3 Salicylic aldehyde 4 Acetophenone 5 Phenethyl alcohol 6 Dihydrocinnamaldehyde 7 cis-Cinnamaldehyde 8 trans-Cinnamaldeh
26、yde 9 trans-Cinnamyl alcohol 10 Tridecane (Internal standard) 11 Eugenol 12 Coumarin 13 Cinnamyl acetate 14 cis-o-Methoxycinnamaldehyde 15 trans-o-Methoxycinnamaldehyde 16 o-Methoxycinnamyl acetate Operating conditions Column: fused silica capillary, length 50 m, internal diameter 0,20 mm Stationary
27、 phase: polydimethylsiloxane (OV 101) Oven temperature: from 100 C to 200 C, at rate of 3 C/min Injector temperature: 230 C Detector temperature: 230 C Volume injected: 0,2 ml Detector: flame ionization Carrier gas: nitrogen Carrier gas pressure: 0,4 bar Split ratio: 1/100 NOTE The trans-cinnamaldeh
28、yde peak should not hide any other peak greater than 0,25 % Figure A.1 Typical chromatogram taken on an apolar column Copyright International Organization for Standardization Provided by IHS under license with ISO Licensee=NASA Technical Standards 1/9972545001 Not for Resale, 04/24/2007 22:22:20 MDT
29、No reproduction or networking permitted without license from IHS -,-,- ISO 11025:1998(E) ISO 4 Peak identification 1 Tridecane (internal standard) 2 trans-Cinnamaldehyde Operating conditions Column: fused silica capillary, length 60 m, internal diameter 0,25 mm Stationary phase: polyethylene glycol
30、20 000 (carbowax 20 M) Oven temperature: from 60 C to 200 C at a rate of 1,5 C/min, then constant at Oven temperature: 200 C for 15 min Injector temperature: 240 C Detector temperature: 240 C Volume injected: 0,3 ml Detector: flame ionization Carrier gas: hydrogen Carrier gas pressure: 0,4 bar Split
31、 ratio: 1/100 Figure A.2 Typical chromatogram taken on a polar column Copyright International Organization for Standardization Provided by IHS under license with ISO Licensee=NASA Technical Standards 1/9972545001 Not for Resale, 04/24/2007 22:22:20 MDTNo reproduction or networking permitted without
32、license from IHS -,-,- Copyright International Organization for Standardization Provided by IHS under license with ISO Licensee=NASA Technical Standards 1/9972545001 Not for Resale, 04/24/2007 22:22:20 MDTNo reproduction or networking permitted without license from IHS -,-,- ISO 11025:1998(E) ISO IC
33、S 71.100.60 Descriptors: fruit and vegetable products, essential oils, cassia, chemical analysis, determination of content, gas phase chromatography, chromatograms. Price based on 4 pages Copyright International Organization for Standardization Provided by IHS under license with ISO Licensee=NASA Technical Standards 1/9972545001 Not for Resale, 04/24/2007 22:22:20 MDTNo reproduction or networking permitted without license from IHS -,-,-