1、BRITISH STANDARD BS 4585-2: 1982 Methods of test for Spices and condiments Part 2: Determination of moisture content (entrainment method) UDC 633.82/.84:664.5:543.812BS4585-2:1982 This British Standard, having been prepared under the directionof the Food and Agriculture Standards Committee,was publi
2、shed underthe authority of the BoardofBSI and comes into effecton 26 February 1982 BSI 08-1999 First published March 1970 First revision February 1982 The following BSI references relate to the work on this standard: Committee reference FAC/7 Draft for comment 80/55145 DC ISBN 0 580 12466 5 Cooperat
3、ing organizations The Food and Agriculture Standards Committee, under whose direction this British Standard was prepared, consists of representatives from the following: Agricultural Co-operation and Marketing Services Agricultural Research Council (Meat Research Institute) British Food Manufacturin
4、g Industries Research Association British Industrial Biological Research Association Ltd. Campden Food Preservation Research Association Consumer Standards Advisory Committee of BSI Department of Agriculture and Fisheries for Scotland Department of Agriculture (Government of Northern Ireland) Depart
5、ment of Industry (Laboratory of the Government Chemist)* Flour Milling and Baking Research Association Food Manufacturers Federation Incorporated* Institute of Brewing Local Authorities Co-ordinating Body of Trading Standards Ministry of Agriculture, Fisheries and Food* National Farmers Union Nation
6、al Farmers Union of Scotland Tobacco Advisory Council The organizations marked with an asterisk in the above list, together with the following, were directly represented on the Technical Committee entrusted with the preparation of this British Standard: Association of Public Analysts British Essence
7、 Manufacturer Association Co-operative Union General Produce Brokers Association of London Overseas Development Administration (Tropical Products Institute) Amendments issued since publication Amd. No. Date of issue CommentsBS4585-2:1982 BSI 08-1999 i Contents Page Cooperating organizations Inside f
8、ront cover Foreword ii 0 Introduction 1 1 Scope and field of application 1 2 References 1 3 Definition 1 4 Principle 1 5 Reagent 1 6 Apparatus 1 7 Sampling 1 8 Procedure 1 9 Expression of results 2 10 Test report 2 Annex Example of entrainment distillation apparatus 3 Figure Distillation apparatus 4
9、 Publications referred to Inside back coverBS4585-2:1982 ii BSI 08-1999 Foreword This Part of BS4585, which has been prepared under the direction of the Food and Agriculture Standards Committee, supersedes BS4585-2:1970 which has therefore been withdrawn. It is identical with ISO 939 “Spices and con
10、diments Determination of moisture content Entrainment method” except for the following changes. In 8.1, detergent solution rather than potassium dichromate-sulphuric acid cleaning solution is required to clean the apparatus and in8.4 heat resisting material rather than asbestos cloth is required to
11、be wrapped round the flask and the tube leading to the receiver, in order to control refluxing. In addition, the references to international standards have been replaced by references to British Standards and wherever the words “International Standard” appeared they have been replaced by the words “
12、British Standard”. The text of the international standard has been used as the basis for this British Standard; therefore certain conventions are not identical with those normally used in British Standards; attention is especially drawn to the following. The comma has been used throughout as a decim
13、al marker. In British Standards it is current practice to use a full point on the baseline as the decimal marker. 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 with a Bri
14、tish 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, pages1 to 4, an inside back cover and a back cover. This standard has been updated (see copyright date) and may have had amendments
15、incorporated. This will be indicated in the amendment table on the inside front cover.BS4585-2:1982 BSI 08-1999 1 0 Introduction This British Standard 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
16、modify the method or even to choose a more suitable method. Such modifications or other methods will be indicated in the British Standards giving specifications for the spices and condiments in question. 1 Scope and field of application This British Standard specifies an entrainment method for the d
17、etermination of the moisture content of spices and condiments. 2 References The titles of the publications referred to in this standard are given on the inside back cover. 3 Definition moisture content the quantity of water, expressed as a percentage by mass, distilled and collected in accordance wi
18、th the method specified in this British Standard 4 Principle Determination of the amount of water entrained by azeotropic distillation, using an organic liquid immiscible with water, and collected in a graduated tube. 5 Reagent 5.1 Toluene Saturate the toluene by shaking with a small quantity of wat
19、er and distil. Use the distillate for the determination of the moisture. NOTEDifferent solvents are used for the determination of moisture. Unless otherwise specified in the British Standard giving specifications for the spice or condiment in question, toluene shall be the solvent used for the deter
20、mination. 6 Apparatus 6.1 Distillation apparatus (a suitable form of apparatus is described in the Annex and shown in the Figure), comprising the following components fitted together by means of ground glass joints: 6.1.1 Flask, short-necked, of capacity at least500ml. 6.1.2 Reflux condenser 6.1.3 R
21、eceiver, with a graduated tube, interposed between the flask and the condenser. 6.2 Analytical balance 7 Sampling Sample the material by the method specified in BS4540-1. 8 Procedure 8.1 Preparation of apparatus Clean the entire apparatus with a detergent solution to minimize the adherence of water
22、droplets to the sides of the condenser and the receiver. Rinse thoroughly with water and dry completely before use. 8.2 Preparation of test sample Prepare the test sample by the method specified in BS4540-2. 8.3 Test portion Weigh, to the nearest 0,01g, about40g of the test sample (8.2), such that t
23、he quantity of water collected will not exceed 4,5ml. 8.4 Determination Transfer quantitatively the test portion (8.3)to the distillation flask (6.1.1) with the toluene (5.1), add sufficient toluene (about75ml in all) to cover the sample completely and swirl to mix. Assemble the apparatus and fill t
24、he receiver (6.1.3) with the toluene by pouring it through the condenser (6.1.2) until it begins to overflow into the distillation flask. If necessary, insert a loose cotton plug in the top of the condenser or attach to it a small calcium chloride tube to prevent condensation of atmospheric moisture
25、 within the condenser tube. In order to control refluxing, wrap the flask and tube leading to the receiver with heat resisting material. Heat the flask so that the distillation rate is about100drops per minute. When the greater part of the water has distilled over, increase the distillation rate to
26、about200drops per minute and continue until no more water is collected. Purge the reflux condenser occasionally during the distillation with5ml portions of the toluene to wash down any moisture adhering to the walls of the condenser. The water in the receiver may be made to separate from the toluene
27、 by occasionally moving a spiral copper wire up and down in the condenser and receiver, thus causing the water to settle at the bottom of the receiver. Reflux until the water level in the receiver remains unchanged for30min and then shut off the source of heat. Flush the condenser with toluene as re
28、quired, making use of the spiral copper wire to discharge any moisture droplets.BS4585-2:1982 2 BSI 08-1999 Immerse the receiver in water at room temperature for at least 15min or until the toluene layer is clear; then read the volume of water. 9 Expression of results The moisture content, expressed
29、 as a percentage by mass, is equal to where It is assumed that the density of water is1g/ml exactly. 10 Test report The test report shall show the method used and the result obtained. It shall also mention all operating conditions not specified in this British Standard, or regarded as optional, as w
30、ell as any circumstances that may have influenced the result. The report shall include all details required for complete identification of the sample. V is the volume, in millilitres, of water collected; m is the mass, in grams, of the test portion. 100 V m -BS4585-2:1982 BSI 08-1999 3 Annex Example
31、 of entrainment distillation apparatus (This Annex does not form part of the standard.) The apparatus consists of a glass flask heated by a suitable means and provided with a reflux condenser discharging into a receiver connected to the flask. The connections between the receiver and the condenser a
32、nd the flask are interchangeable ground glass joints. The receiver serves to collect and measure the condensed water, and to return the solvent to the flask. The assembly of the apparatus is shown in the Figure and the various components are described below. a) Flask, of capacity 500ml, of the shape
33、 shown in the Figure and made of heat-resistant glass, well annealed and as free as possible from striae and similar defects. b) Reflux condenser, water cooled, made of glass, having a jacket approximately400mm long and an inner tube of diameter9,5to12,5mm. The tip of the condenser to be inserted in
34、 the receiver may be ground off at an angle of30from the vertical axis of the condenser. When inserted into the receiver, the tip of the condenser is6to7mm above the surface of the liquid in the receiver after distillation conditions have been established. c) Receiver, of capacity 5 ml, made of heat
35、-resistant glass, well annealed and as free as possible from striae and similar defects, provided with ground glass joints, with the shape, dimensions and tolerances given in the Figure, and consisting essentially of the upper chamber, together with the tube and ground joint leading to the flask, an
36、d the graduated tube. The graduated portion has a capacity of5ml when filled to the highest graduation mark. The scale covers the range of0 to5ml and is graduated at intervals of0,1ml. The graduation marks corresponding to each millilitre are numbered and carried completely round the tube. The gradu
37、ation marks midway between the numbered marks are carried three-quarter-way, and the remaining marks are carried half-way, around the tube. The error at any indicated capacity does not exceed0,05ml. d) Heat source, either an oil bath or an electric heater provided with a sliding rheostat or other me
38、ans of heat control. The temperature of the oil in the bath should not be very much higher than the boiling point of toluene. e) Copper wire, long enough to extend through the condenser and with one end twisted into a spiral. The diameter of the spiral is such that it fits snugly within the graduate
39、d portion of the receiver and yet can be moved up and down. NOTEA similar, suitable apparatus is specified in BS756.BS4585-2:1982 4 BSI 08-1999 Figure Distillation apparatusBS4585-2:1982 BSI 08-1999 Publications referred to BS 756, Dean and Stark apparatus. BS 4540, Sampling of spices and condiments
40、. BS 4540-1, Methods of sampling. BS 4540-2, Preparation of a ground sample for analysis. BS 4585-2: 1982 BSI 389 Chiswick High Road London W4 4AL BSIBritishStandardsInstitution BSI is the independent national body responsible for preparing BritishStandards. It presents the UK view on standards in E
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