BS-5711-17-1983.pdf
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1、BRITISH STANDARD CONFIRMED AUGUST 1994 BS 5711-17: 1983 Methods of Sampling and test for glycerol Part 17: Limit test for lead NOTEIt is recommended that this Part of BS 5711 be read in conjunction with the general information given in BS 5711-0 “General introduction”, issued separately. UDC 661.188
2、.1:547.426.1:546.815 Licensed Copy: sheffieldun sheffieldun, na, Mon Dec 04 15:12:27 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS 5711-17:1983 This British Standard, having been prepared under the direction of the Chemicals Standards Committee, was published under the authority of the Board of BSI
3、and comes into effect on 31 January 1983 BSI 12-1999 The following BSI references relate to the work on this standard: Committee reference CIC/6 Draft for comment 75/53579 DC ISBN 0 580 13146 7 A British Standard does not purport to include all the necessary provisions of a contract. Users of Britis
4、h Standards 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, pages 1 and 2, an inside back cover and a back cover
5、. 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 of issueComments Licensed Copy: sheffieldun sheffieldun, na, Mon Dec 04 15:12:27 G
6、MT+00:00 2006, Uncontrolled Copy, (c) BSI BS 5711-17:1983 BSI 12-1999i Contents Page 1Scope and field of application1 2Principle1 3Reagents1 4Apparatus1 5Sampling1 6Procedure1 7Test report1 Publications referred toInside back cover Licensed Copy: sheffieldun sheffieldun, na, Mon Dec 04 15:12:27 GMT+
7、00:00 2006, Uncontrolled Copy, (c) BSI ii blank Licensed Copy: sheffieldun sheffieldun, na, Mon Dec 04 15:12:27 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS 5711-17:1983 BSI 12-19991 1 Scope and field of application This British Standard describes a colorimetric limit test for lead in chemically pu
8、re glycerol. NOTEThe titles of the publications referred to in this standard are listed on the inside back cover. 2 Principle Dissolution of a test portion in acetic acid, neutralization with ammonia solution and the development of colour with potassium cyanide and sodium sulphide solutions. 3 Reage
9、nts The reagents used shall be of a recognized analytical grade and shall be free from lead. Distilled water complying with BS 3978 or water of at least equal purity shall be used. 3.1 Lead nitrate, standard solutions. 3.1.1 Stock solution. Dissolve 0.16 g of lead nitrate in 5 mL of concentrated nit
10、ric acid, 70 % (m/m), transfer the solution to a 100 mL one-mark volumetric flask and dilute to the mark. 1 mL N 1 mg Pb 3.1.2 Working solution. Transfer 10 mL of the stock lead nitrate solution (3.1.1) to a 1 000 mL one-mark volumetric flask and dilute to the mark. Prepare immediately before use. 1
11、 mL N 0.01 mg Pb 3.2 Potassium cyanide, 100 g/L solution. Dissolve 10 g of potassium cyanide in 90 mL of water, add 2 mL of hydrogen peroxide, 6 g/L solution, allow to stand for 24 h and dilute to 100 mL with water. NOTE 1WARNING. Potassium cyanide is extremely toxic. The appropriate first aid and m
12、edical facilities should be available BEFORE using cyanide and appropriate protective clothing should be worn. Do not measure solutions containing cyanide by means of a pipette filled by suction with the mouth: use a burette or an automatic dispensing device. NOTE 2Information on the safe disposal o
13、f waste cyanide solutions is given in the Laboratory Waste Disposal Manual published by the Manufacturing Chemists Association, 1825 Connecticut Avenue NW, Washington DC, USA. 3.3 Sodium sulphide, 100 g/L solution. Dissolve 10 g of sodium sulphide in water, dilute to 100 mL and filter. 3.4 Ammonia s
14、olution, 100 g/L solution. Dilute concentrated ammonia solution, 35 % (m/m) 1 + 2. 3.5 Acetic acid, 336 g/L solution. Dilute glacial acetic acid 1 + 2. 4 Apparatus All glass apparatus used shall be free from soluble lead compounds. 4.1 Nessler cylinders, matched pair, capacity 50 mL, complying with
15、BS 612. 5 Sampling Prepare the laboratory sample as described in Part 2 of this British Standard. 6 Procedure Prepare a primary test solution by dissolving 12.0 g of the sample in hot water containing 5 mL of the acetic acid (3.5) and a secondary test solution by dissolving 2.0 g of the sample in th
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