1、BRITISH STANDARD BS 4585-9: 1998 ISO 930:1997 Methods of test for spices and condiments Part 9: Determination of acid-insoluble ash ICS 67.220.10BS4585-9:1998 This British Standard, having been prepared under the direction of the Consumer Products and Services Sector Board, was published under theau
2、thority of the StandardsBoard and comes intoeffect on 15 February 1998 BSI 04-1999 ISBN 0 580 29129 4 National foreword This British Standard reproduces verbatim ISO930:1997 and implements it as the UK national standard. It supersedes BS4585-9:1981 which is withdrawn. The UK participation in its pre
3、paration was entrusted to Technical Committee AW/7, Spices and condiments, which has the responsibility to: 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 inform
4、ed; monitor related international and European developments and promulgate them in the UK. A list of organizations represented on this committee can be obtained on request. Cross-references The British Standards which implement international or European publications referred to in this document may
5、be found in the BSI Standards Catalogue under the section entitled “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 St
6、andards are responsible for their correct application. Compliance with a British Standard does not of itself confer immunity from legal obligations. Summary of pages This document comprises a front cover, an inside front cover, pages i and ii, theISO title page, page ii, pages 1 to 3 and abackcover.
7、 This standard has been updated (see copyright date) and may have had amendments incorporated. This will be indicated in the amendment table on the inside front cover. Amendments issued since publication Amd. No. Date CommentsBS4585-9:1998 BSI 04-1999 i Contents Page National foreword Inside front c
8、over Foreword ii Introduction 1 1 Scope 1 2 Normative references 1 3 Definition 1 4 Principle 1 5 Reagents 1 6 Apparatus 1 7 Procedure 1 8 Expression of results 2 9 Precision 2 10 Test report 2 Annex A (informative) Results of interlaboratory test 3 Table A.1 Interlaboratory test for the determinati
9、on of acid-insoluble ash 3ii blankBS4585-9:1998 ii BSI 04-1999 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 com
10、mittees. 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
11、 International Electrotechnical Commission (IEC) on all matters of electrotechnical standardization. Draft International Standards adopted by the technical committees are circulated to the member bodies for voting. Publication as an International Standard requires approval by at least75% of the memb
12、er bodies casting a vote. International Standard ISO 930 was prepared by Technical Committee ISO/TC 34, Agricultural food products, Subcommittee SC 7, Spices and condiments. This second edition cancels and replaces the first edition (ISO930:1980), which has been technically revised. Annex A of this
13、International Standard is for information only. Descriptors: Agricultural products, food products, seasonings, aromatic plants, spices, herbs, tests, determination of content, ash determination, insoluble matter, incineration analysis.BS4585-9:1998 BSI 04-1999 1 Introduction This International Stand
14、ard is applicable to most spices and condiments. In view of the number and variety of such products, however, it may be necessary in particular cases to modify the method or even to choose a more suitable method. Such modifications and other methods will be indicated in the International Standards g
15、iving specifications for the spices and condiments in question. 1 Scope This International Standard specifies a method for the determination of acid-insoluble ash from spices and condiments. 2 Normative references The following standards contain provisions which, through reference in this text, cons
16、titute provisions of this International Standard. At the time of publication, the editions indicated were valid. All standards are subject to revision, and parties to agreements based on this International Standard are encouraged to investigate the possibility of applying the most recent editions of
17、 the standards indicated below. Members of IEC and ISO maintain registers of currently valid International Standards. ISO 928:1997, Spices and condiments Determination of total ash. ISO 3696:1987, Water for analytical laboratory use Specification and test methods. 3 Definition For the purposes of th
18、is International Standard, the following definition applies. 3.1 acid-insoluble ash of spices and condiments that part of the total ash remaining after treatment with hydrochloric acid under the conditions specified in this International Standard, expressed as a percentage by mass 4 Principle Treatm
19、ent of the total ash, obtained as described in ISO928, with hydrochloric acid, filtration, incineration and weighing of the residue. 5 Reagents All reagents shall be of a recognized analytical quality. Use water in accordance with grade 3 of ISO3696. 5.1 Dilute hydrochloric acid ( 20= 1,045 g/ml to
20、1,050 g/ml), percentage by mass about10%. 5.2 Silver nitrate solution Dissolve10g of silver nitrate in water to a total volume of100ml. 6 Apparatus Usual laboratory apparatus and, in particular, the following. 6.1 Electrical muffle furnace, capable of being maintained at (550 25) C. 6.2 Desiccator,
21、provided with an efficient desiccant. 6.3 Filter paper, ashless. 6.4 Analytical balance, capable of weighing to the nearest0,0001g. 6.5 Water bath. 7 Procedure Carry out two determinations. 7.1 Test portion 7.1.1 The test portion may be the total ash retained after determination of the total ash in
22、accordance with ISO928. 7.1.2 Alternatively, take a new test portion and prepare the total ash by the procedure specified in ISO928. It is not necessary, in this case, to cool and weigh the total ash. 7.2 Determination Add to the total ash, in the same dish in which it was prepared as specified in I
23、SO928,15ml of the hydrochloric acid (5.1). Heat the solution for about10min in the boiling water bath (6.5) and filter the contents of the dish through the filter paper (6.3). Wash the dish and the filter paper with hot water until the washings are free from hydrochloric acid (about6 to 8 times). Te
24、st for the absence of hydrochloric acid with silver nitrate solution (5.2). NOTELack of turbidity when a portion of silver nitrate solution is added to the filtrate indicates absence of hydrochloric acid. Return the filter paper with the residue to the dish and ignite it in the muffle furnace (6.1)
25、set at550C. Cool the dish in the desiccator (6.2) and weigh to the nearest0,0001g. Repeat the operations of igniting, cooling and weighing until the difference between successive weighings does not exceed0,0005 g (m 3 ).BS4585-9:1998 2 BSI 04-1999 8 Expression of results 8.1 Calculate the acid-insol
26、uble ash (w A ), expressed as a percentage by mass, using the following equation: where 8.2 Calculate the mean of two determinations and express the result to one decimal place. 8.3 For determination on a moisture-free basis, the value should be multiplied by where c is the moisture content, express
27、ed as a percentage. 9 Precision Details of an interlaboratory test on the precision of the method are summarized in Annex A. The values derived from this interlaboratory test may not be applicable to concentration ranges and matrices other than those given. 10 Test report The test report shall show
28、the method used and the result obtained. It shall mention all operating conditions not specified in this International Standard, or regarded as optional, and any circumstances that may have influenced the result. The report shall include all details required for complete identification of the sample
29、. m 1 is the mass, in grams, of the empty dish; m 2 is the mass, in grams, of the dish and the test portion; m 3 is the mass, in grams, of the dish and the residue retained from the determination specified in 7.2. w A m 3 m 1 m 2 m 1 -100% = 100 % 100 %c -BS4585-9:1998 BSI 04-1999 3 Annex A (informa
30、tive) Results of interlaboratory test An interlaboratory test, carried out in 1994 with the participation of15 laboratories in Germany, in accordance with this method gave the statistical results shown in Table A.1 Table A.1 Interlaboratory test for the determination of acid-insoluble ash Sample w A
31、 % Repeatability limit r Reproducibility limit R No. of laboratories remaining after elimination of outliers Pepper, black, ground 0,079 0,058 0,105 12 Oregano, minced 0,987 0,435 0,566 14 Cloves, ground 0,041 0,069 0,136 14BS 4585-9: 1998 ISO 930:1997 BSI 389 Chiswick High Road London W4 4AL BSIBri
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