1、BRITISH STANDARD BS3762-2: 1989 Analysis of formulated detergents Part2: Qualitative test methods NOTEIt is recommended that this Part be read in conjunction with the information in the “General introduction”, published separately as BS3762-0. UDC 661.185.6:620.1BS3762-2:1989 This British Standard,
2、having been prepared under the directionof the Chemicals Standards Committee, was published under the authorityofthe Board of BSIandcomes into effect on 28February1989 BSI11-1999 The committees responsible forthis British Standard are shown inPart0. The following BSI references relate to the work on
3、 this standard: Committee reference CIC/34 Draft for comment87/51452DC ISBN 0 580 17071 3 Foreword This Part of BS3762 has been prepared under the direction of the Chemicals Standards Committee and supersedes Part2: Section A and method D7.A of BS3762:1964, which are being deleted by amendment. This
4、 standard describes methods of test only and should not be referred to as a specification defining limits of purity. Reference to the standard should indicate that the method of test used is in conformity with BS3762-2. A British Standard does not purport to include all the necessary provisions of a
5、 contract. Users of British 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, pagesi andii, pages1 and2, an inside back
6、cover and a back cover. 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 issue CommentsBS3762-2:1989 BSI 11-1999 i Contents Page
7、Foreword Inside front cover 1 Scope 1 2 Reagents 1 3 Procedure 1 4 Test report 2 Publications referred to Inside back coverii blankBS3762-2:1989 BSI 11-1999 1 1 Scope This Part of BS3762 describes qualitative tests which may be required as preliminary steps to the application of methods of analysis
8、described in other Parts and Sections of BS3762. The tests are for type of surface active agent, oxidizing agents, peroxy-compounds, urea and fluorescent whitening agents. NOTEThe titles of the publications referred to in this Part are listed on the inside back cover. 2 Reagents The reagents shall b
9、e of a recognized analytical grade. Water complying with grade3 of BS3978 shall be used throughout. 2.1 Chloroform 2.2 Ammonium hexathiocyanatocobaltate solution. Dissolve20g of ammonium thiocyanate and3g of cobalt nitrate in about70mL of water and dilute to100mL. 2.3 p-dimethylaminobenzaldehyde sol
10、ution. Dissolve1g of p-dimethylaminobenzaldehyde in100mL of ethanol 1)plus0.2mL of hydrochloric acid solution36%(m/m). 2.4 Mixed indicator 2.4.1 Dimidium bromide/acid blue1stock solution. This solution is prepared from acid blue1 (CI42045) (sodium!-4-(diethylamino) phenyl-!-4-(diethylimino) cyclohex
11、a-2,5-dienylidene toluene-2,4-disulphonate) and dimidium bromide(3,8-diamino-5-methyl-6- phenylphenanthridinium bromide). NOTEThis solution is available commercially under the name “dimidium bromide-disulphine blue indicator stock solution”. Weigh0.5 0.005g of dimidium bromide into a50mL beaker and0
12、.25 0.005g of acid blue1into a second50mL beaker. Add between20mL and30mL of hot10% (V/V) ethanol 1)to each beaker. Stir until dissolved and transfer the solutions to a250mL one-mark volumetric flask with the ethanol solution and dilute to the mark with10% (V/V) ethanol 1) . 2.4.2 Mixed acid indicat
13、or solution. Add200mL of water to20mL of the stock solution(2.4.1) in a500mL one-mark volumetric flask. Add20mL of the sulphuric acid solution(2.8), mix and dilute to the mark with water. Store out of direct sunlight. 2.5 Potassium iodide solution, c (KI)=0.5mol/L. 2.6 Potassium titanium oxalate sol
14、ution, 5g/L. 2.7 Sodium hydroxide solution, c (NaOH)=5mol/L. 2.8 Sulphuric acid solution, c (H 2 SO 4 )=2.5mol/L. 3 Procedure 3.1 Preparation of test solution Mix approximately5g of the sample with95mL of water until all soluble components appear to have been dissolved. Filter to remove any insolubl
15、e matter. NOTEIt is not necessary for the filtrate to be clear, as an emulsion, which will usually disappear, will not interfere with subsequent observations. 3.2 Test for type of surface active agent (acidmedium) Mix one drop of the test solution(3.1),5mL of the mixed acid indicator solution(2.4.2)
16、 and5mL of the chloroform(2.1). Allow the layers to separate. If the chloroform layer is not distinctly blue or pink, add a few more drops of the test solution, shake and allow to separate. Repeat if necessary until about1mL of the test solution has been added. A pink colour in the chloroform layer
17、denotes the presence of a synthetic anionic-active surface-active agent. A blue colour in the chloroform layer denotes the presence of a long chain amine, long chain amine oxide, or cationicactive or ampholytic surface-active agent. In the case of a blue colour or no colour, proceed in accordance wi
18、th3.3. 3.3 Test for type of surface active agent (alkaline medium) Mix one drop of the test solution(3.1),5mL of the mixed acid indicator solution(2.4.2),1mL of the sodium hydroxide solution(2.7) and5mL of the chloroform(2.1). Allow the layers to separate. If the chloroform layer is not distinctly b
19、lue or pink, add a few more drops of the test solution, shake and allow to separate. Repeat if necessary until about1mL of the test solution has been added. A pink colour in the chloroform layer denotes the presence of a soap or synthetic anionic-active or ampholytic surface-active agent. Use the re
20、sults from3.2 to distinguish these agents. A blue colour in the chloroform layer denotes the presence of a cationic-active surface-active agent. 1) The ethanol may be replaced by industrial methylated spirits complying with BS3591, or such spirits diluted as required. Theuse of industrial methylated
21、 spirits is governed by the Methylated Spirits Regulations,1983 (SI1983 No.252). It is not permissible to use duty-free ethanol, received under the provisions of the Alcoholic Liquors Duties Act1972, Section10, for purposes for which industrial methylated spirits is an acceptable alternative.BS3762-
22、2:1989 2 BSI 11-1999 3.4 Test for non-ionic surface-active agents Mix1mL of the test solution(3.1),10mL of the ammonium hexathiocyanatocobaltate solution(2.2) and5mL of the chloroform(2.1). Allow the layers to separate. A blue colour in the chloroform layer (in case of doubt, compare with a blank te
23、st, i.e.omitting the test solution) denotes the presence of a non-ionic surface-active agent. NOTENon-ionic surface active agents that contain less than three ethylene oxide units per molecule, including those not based on ethylene oxide, will not be detected by this test. 3.5 Test for oxidizing age
24、nts Mix5mL of the test solution(3.1) with a few drops of the sulphuric acid solution(2.8) and add1mL of the potassium iodide solution(2.5). A yellow or yellow-brown colour indicates the presence of an oxidizing agent. 3.6 Test for peroxy-compounds Mix5mL of the test solution(3.1) with1mL of the sulp
25、huric acid solution(2.8) and add1mL of the potassium titanium oxalate solution(2.6). A yellow or orange colour indicates the presence of a peroxy-compound. A negative reaction in conjunction with a positive reaction in3.4 suggests the presence of a chlorine bleach. 3.7 Test for urea Place a drop of
26、the test solution(3.1) on to a filter paper and add a drop of the p-dimethylaminobenzaldehyde solution(2.3). Hang the paper up to dry. A bright yellow spot indicates the presence of urea or certain amines or other amides; absence of a yellow spot indicates the absence of urea. 3.8 Test for fluoresce
27、nt whitening agents Dissolve or disperse2g of the sample in100mL of water. Take two strips of filter paper of size approximately5cm 2cm and dip one to a depth of2cm to3cm in the solution and dip the other into distilled water. Remove the strips and compare them under a source of ultraviolet light, p
28、referably in a darkened room. Note whether the test strip shines more brightly than the control, indicating the presence of a fluorescent agent. 4 Test report The test report shall include the following information: a) a reference to this British Standard, i.e.BS3762-2:1989; b) a reference to the te
29、st method(s) used; c) the result(s); d) a complete identification of the sample.BS3762-2:1989 BSI 11-1999 Publications referred to BS3591, Specification for industrial methylated spirits. BS3978, Specification for water for laboratory use. BS3762-2: 1989 BSI 389 Chiswick High Road London W4 4AL BSIB
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