BS EN ISO 6571-2009 Spices condiments and herbs - Determination of volatile oil content (hydrodistillation method)《香料、调味品和香草 挥发油含量的测定(水蒸馏法)》.pdf

1、Licensed Copy: Wang Bin, ISO/EXCHANGE CHINA STANDARDS, 18/05/2010 08:10, Uncontrolled Copy, (c) BSIg49g50g3g38g50g51g60g44g49g42g3g58g44g55g43g50g56g55g3g37g54g44g3g51g40g53g48g44g54g54g44g50g49g3g40g59g38g40g51g55g3g36g54g3g51g40g53g48g44g55g55g40g39g3g37g60g3g38g50g51g60g53g44g42g43g55g3g47g36g58(

2、hydrodistillation method)ICS 67.220.10Spices, condiments and herbs Determination of volatile oil content BRITISH STANDARDBS EN ISO 6571:2009BS EN ISO 6571:2009Licensed Copy: Wang Bin, ISO/EXCHANGE CHINA STANDARDS, 18/05/2010 08:10, Uncontrolled Copy, (c) BSIThis British Standard was published under

3、the authority of the Standards Policy and Strategy Committee on 30 June 2008 BSI 2009ISBN 978 0 580 67277 4Amendments/corrigenda issued since publicationDate Comments 31 December 2009 This corrigendum renumbers BS ISO 6571:2008 as BS EN ISO 6571:2009request to its secretary. This publication does no

4、t purport to include all the necessary provisions of a contract. Users are responsible for its correct application. Compliance with a British Standard cannot confer immunity from legal obligations. National forewordThis British Standard is the UK implementation of EN ISO 6571:2009. It is identical w

5、ith ISO 6571:2008. It supersedes BS ISO 6571:2008 which is withdrawn.The UK participation in its preparation was entrusted to Technical Committee AW/7, Spices and condiments.A list of organizations represented on this committee can be obtained on EUROPEAN STANDARDNORME EUROPENNEEUROPISCHE NORMEN ISO

6、 6571July 2009ICS 67.220.10English VersionSpices, condiments and herbs - Determination of volatile oilcontent (hydrodistillation method) (ISO 6571:2008)pices, aromates et herbes - Dtermination de la teneur enhuiles essentielles (mthode par hydrodistillation) (ISO6571:2008)Gewrze, wrzende Zutaten und

7、 Kruter - Bestimmung destherischen lgehaltes(Wasserdampfdestillationsverfahren) (ISO 6571:2008)This European Standard was approved by CEN on 27 June 2009.CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this EuropeanStandard the stat

8、us of a national standard without any alteration. Up-to-date lists and bibliographical references concerning such nationalstandards may be obtained on application to the CEN Management Centre or to any CEN member.This European Standard exists in three official versions (English, French, German). A v

9、ersion in any other language made by translationunder the responsibility of a CEN member into its own language and notified to the CEN Management Centre has the same status as theofficial versions.CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Cyprus, Czech Republic, De

10、nmark, Estonia, Finland,France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal,Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom.EUROPEAN COMMITTEE FOR STANDARDIZATIONCOMIT EUROPEN DE NORMALISATI

11、ONEUROPISCHES KOMITEE FR NORMUNGManagement Centre: Avenue Marnix 17, B-1000 Brussels 2009 CEN All rights of exploitation in any form and by any means reservedworldwide for CEN national Members.Ref. No. EN ISO 6571:2009: ELicensed Copy: Wang Bin, ISO/EXCHANGE CHINA STANDARDS, 18/05/2010 08:10, Uncont

12、rolled Copy, (c) BSIii Foreword The text of ISO 6571:2008 has been prepared by Technical Committee ISO/TC 34 “Food products” of the International Organization for Standardization (ISO) and has been taken over as EN ISO 6571:2009 by Technical Committee CEN/SS C01 “Food Products” the secretariat of wh

13、ich 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 January 2010, and conflicting national standards shall be withdrawn at the latest by January 2010. Attention is drawn to the pos

14、sibility that some of the elements of this document may be the subject of patent rights. CEN and/or CENELEC shall not be held responsible for identifying any or all such patent rights. According to the CEN/CENELEC Internal Regulations, the national standards organizations of the following countries

15、are bound to implement this European Standard: Austria, Belgium, Bulgaria, Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sw

16、eden, Switzerland and the United Kingdom. Endorsement notice The text of ISO 6571:2008 has been approved by CEN as a EN ISO 6571:2009 without any modification. BS EN ISO 6571:2009EN ISO 6571:2009Licensed Copy: Wang Bin, ISO/EXCHANGE CHINA STANDARDS, 18/05/2010 08:10, Uncontrolled Copy, (c) BSI1Spice

17、s, condiments and herbs Determination of volatile oil content (hydrodistillation method) 1 Scope This International Standard specifies a method for the determination of the volatile oil content of spices, condiments and herbs. 2 Normative references The following referenced documents are indispensab

18、le for the application of this document. For dated references, only the edition cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies. ISO 939, Spices and condiments Determination of moisture content Entrainment method ISO 2825, Spice

19、s and condiments Preparation of a ground sample for analysis 3 Terms and definitions For the purposes of this document, the following terms and definitions apply. 3.1 volatile oil content all the substances entrained by steam under the conditions specified in this International Standard NOTE The vol

20、atile oil content is expressed in millilitres per 100 g of dry product. 4 Principle An aqueous suspension of the product is distilled. The distillate is collected in a graduated tube containing a measured volume of xylene to fix the volatile oil. The organic and aqueous phases are then allowed to se

21、parate and the total volume of the organic phase read. The volatile oil content is calculated after deducting the volume of xylene. 5 Reagents Use only reagents of recognized analytical grade and only distilled water or water of at least equivalent purity. 5.1 Xylene. 5.2 Cleaning solutions. 5.2.1 A

22、cetone (for fatty residues). BS EN ISO 6571:2009EN ISO 6571:2009Licensed Copy: Wang Bin, ISO/EXCHANGE CHINA STANDARDS, 18/05/2010 08:10, Uncontrolled Copy, (c) BSI2 5.2.2 Liquid detergent (used at the concentration recommended by the manufacturer) or a solution of sulfuric acid and potassium dichrom

23、ate (see the warning) prepared by slowly adding, while stirring continuously, one volume of concentrated sulfuric acid to one volume of saturated potassium dichromate solution and by passing the mixture, after cooling, through a fritted glass filter. WARNING Avoid any contact of this solution with t

24、he skin and mucous membranes. 6 Apparatus Usual laboratory equipment, and in particular the following. 6.1 Distillation apparatus, made of strong glass having a low coefficient of thermal expansion1). The apparatus comprises the following components connected by ground glass joints. 6.1.1 Round-bott

25、om flask, with a ground neck, of capacity 500 ml or 1 000 ml, according to the product concerned (see Annex A). 6.1.2 Condenser system, comprising the following components joined together (see Figure 1): a) a vertical tube (AC), the base of which has a ground joint to fit the flask (6.1.1); b) a ben

26、t tube (CDE); c) a vertical bulb condenser (FG); d) an assembly consisting of a tube with a side-arm (K) provided with a ground stopper (K), a pear-shaped enlargement (J), a tube graduated in divisions of 0,05 ml (JL), a spherical enlargement (L) and a three-way tap (M) connected to the vertical tub

27、e (AC) by an inclined tube (O) provided with a safety tube (N), if necessary topped by the steam trap (6.1.3). 1)This apparatus corresponds to the type described in the European Pharmacopoeia (V 5.89), 2.8.12.BS EN ISO 6571:2009EN ISO 6571:2009Licensed Copy: Wang Bin, ISO/EXCHANGE CHINA STANDARDS, 1

28、8/05/2010 08:10, Uncontrolled Copy, (c) BSI3Dimensions in millimetres Key A, C, D, E, F, G, J, K, K, L, M, N, O see 6.1.2 B see Figure 2 a Capacity 5 ml. b Capacity 3 ml. 35 Figure 1 Condenser system BS EN ISO 6571:2009EN ISO 6571:2009Licensed Copy: Wang Bin, ISO/EXCHANGE CHINA STANDARDS, 18/05/2010

29、 08:10, Uncontrolled Copy, (c) BSI4 6.1.3 Steam trap (see Figure 2) which can be connected to the side-arm (K) or to the safety tube (N) (see 6.1.2). Figure 2 Steam trap 6.2 Filter paper, of diameter 110 mm. 6.3 Pipette, of capacity 1 ml. 6.4 Heating device. The method of heating should be such as t

30、o avoid overheating of the flask (6.1.1). A device for regulating the temperature is recommended. 6.5 Anti-bumping granules or glass beads. 6.6 Measuring cylinder, of capacity 500 ml. 6.7 Analytical balance. 7 Sampling A representative sample should have been sent to the laboratory. It should not ha

31、ve been damaged or changed during transport or storage. Sampling is not part of the method specified in this International Standard. A recommended sampling method is given in ISO 9481. 8 Procedure NOTE It is intended to specify the test parameters in the International Standard specifying requirement

32、s for each spice or condiment. In the meantime, these parameters are given in Annex A. 8.1 Preparation of the apparatus Carefully clean the condenser system (6.1.2). Tightly fix the glass stopper (K) on the side-arm (K) and the steam trap (6.1.3) on the safety tube (N). Turn the apparatus upside dow

33、n, fill it with the cleaning solution (5.2) and leave it in this position overnight. Rinse the apparatus very carefully with water after having cleaned it. 8.2 Preparation of the test sample If the test portion has to be ground (see Annex A), crush a sufficient quantity of the laboratory sample just

34、 before adding to the round-bottom flask to a suitable degree of fineness according to the product concerned (see ISO 2825). During the crushing procedure, ensure that the temperature of the test portion does not rise. The mesh size of the sample shall be stated in each International Standard relati

35、ng to a given spice. BS EN ISO 6571:2009EN ISO 6571:2009Licensed Copy: Wang Bin, ISO/EXCHANGE CHINA STANDARDS, 18/05/2010 08:10, Uncontrolled Copy, (c) BSI58.3 Test portion Weigh, to the nearest 0,01 g, on the filter paper (6.2), the specified quantity of test sample (see Annex A). 8.4 Determination

36、 8.4.1 Determination of the volume of xylene Using the measuring cylinder (6.6), transfer the specified quantity of water (see Annex A) to the flask (6.1.1) and add the anti-bumping granules or glass beads (6.5). Connect the flask to the condenser system (6.1.2) and fill the tube graduated in divisi

37、ons of 0,05 ml (JL), the collector bulb (L) and the inclined tube (O) with water through the side-arm (K). Using the pipette (6.3), add 1 ml of the xylene (5.1) through the side-arm. Half fill the steam trap (6.1.3) with water and connect it to the condenser system. Heat the flask and regulate the r

38、ate of distillation to 2 ml/min or 3 ml/min unless otherwise specified. Distil for about 30 min and then remove the source of heat (6.4). By means of the three-way tap (M), allow the xylene to flow into the tube (JL) in such a way that the upper level coincides with the zero mark. Allow to cool for

39、at least 10 min and measure the volume of xylene. 8.4.2 Determination of volume of organic phase (volatile oil and xylene) Transfer the filter paper (6.2) with the test portion (8.3) to the flask (6.1.1), and again connect the flask to the condenser system. Heat the flask and regulate the rate of di

40、stillation to 2 ml/min or 3 ml/min unless otherwise specified. Allow the distillation to continue for the specified time (see Annex A). (Record the distillation time for inclusion in the test report.) Remove the source of heat (6.4) and allow to cool. After 10 min, read the volume of the organic pha

41、se (mixture of volatile oil and xylene) collected in the measurement tube. 8.4.3 Determination of moisture content Determine the moisture content by the method specified in ISO 939. 9 Expression of results The volatile oil content, wVO, expressed in millilitres per 100 g of dry product, is given by

42、the following equation: 210VOHO100100100VVwmw= where V0is the volume, in millilitres, of xylene measured in 8.4.1; V1is the total volume, in millilitres, of volatile oil and xylene measured in 8.4.2; m is the mass, in grams, of the test portion; wH2Ois the moisture content, expressed as a percentage

43、 mass fraction, determined in 8.4.3. 10 Precision Details of an interlaboratory trial on the precision of the method are summarized in Annex B. The values derived from this interlaboratory test may not be applicable to concentration ranges and matrices other than those given. BS EN ISO 6571:2009EN I

44、SO 6571:2009Licensed Copy: Wang Bin, ISO/EXCHANGE CHINA STANDARDS, 18/05/2010 08:10, Uncontrolled Copy, (c) BSI6 10.1 Repeatability The absolute difference between two independent single test results, obtained with the same method on identical test material in the same laboratory by the same operato

45、r using the same equipment within a short interval of time, shall in not more than 5 % of the cases exceed the repeatability limits, r, given in Table 1. Table 1 Repeatability Sample Mean volatile oil contentx ml/100 g Repeatability limit r ml/100 g Oregano, rubbed 1,907 0,176 Cloves, ground 13,956

46、1,960 Black pepper, ground 2,624 0,331 10.2 Reproducibility The absolute difference between two single test results, obtained with the same method on identical test material in different laboratories by different operators using different equipment, shall in not more than 5 % of the cases exceed the

47、 reproducibility limits, R, given in Table 2. Table 2 Reproducibility Sample Mean volatile oil contentx ml/100 g Reproducibility limit R ml/100 g Oregano, whole/leaf 1,907 0,536 Cloves, ground 13,956 3,662 Black pepper, ground 2,624 0,796 11 Test report The test report shall contain at least the fol

48、lowing information: a) all information necessary for the complete identification of the sample; b) the test method used, with reference to this International Standard; c) the distillation time, in hours; d) the test results obtained and the units in which they are specified; e) date when the analysi

49、s was finished; f) whether the repeatability limit requirement has been fulfilled; g) all operating details not specified in this International Standard, or regarded as optional, together with details of any incidents occurred when performing the method which may have influenced the test results. BS EN ISO 6571:2009EN ISO 6571:2009Licensed Copy: Wang Bin, ISO/EXCHANGE CHINA STANDARDS, 18/05/2010 08:10, Uncontrolled Copy, (c) BSI7Annex A (normative) Test parameters for different spices, condiments and herbs Mass of test portion Form for distilla