1、BRITISH STANDARD BS3762-3.6: 1986 Analysis of formulated detergents Part3: Quantitative test methods Section3.6 Method for determination of matter soluble in light petroleum NOTEIt is recommended that this Section be read in conjunction with the information in the “General Introduction”, published s
2、eparately as BS3762-0. UDC 661.185:543.832.062:547.215/.217.2BS3762-3.6:1986 This BritishStandard, having been prepared under the directionof the Chemicals Standards Committee, was published under the authority ofthe Board of BSI and comesintoeffect on 28November1986 BSI12-1999 The committees respon
3、sible for this BritishStandard are shown inPart0. The following BSI references relate to the work on this standard: Committee reference CIC/34 Draft for comment85/55067 DC ISBN 0 580 15505 6 Foreword This Section of BS3762 has been prepared under the direction of the Chemicals Standards Committee an
4、d supersedes method B2of BS3762:1964, which is being deleted by amendment. This standard describes a method 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 BS3762-3.6
5、. 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 British Standard does not of itself confer immunity from legal obligations. Summary of pages This document comprise
6、s a front cover, an inside front cover, pagesi andii, pages1and2, an inside back 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 publ
7、ication Amd. No. Date of issue CommentsBS3762-3.6:1986 BSI 12-1999 i Contents Page Foreword Inside front cover 1 Scope 1 2 Principle 1 3 Reagents 1 4 Apparatus 1 5 Procedure 1 6 Expression of results 2 7 Precision 2 8 Test report 2 Publications referred to Inside back coverii blankBS3762-3.6:1986 BS
8、I 12-1999 1 1 Scope This Section of BS3762 describes a method for the determination, in formulated detergents, of the matter soluble in light petroleum. The matter soluble in light petroleum usually consists of unreacted fatty alcohols or hydrocarbons, but it may also contain added fatty matter and
9、perfume. Unreacted fatty matter from ingredients such as mono-glyceride sulphate or alkanolamide sulphate is not extracted with light petroleum, and ethoxylated alcohols, either added deliberately or present as unsulphated matter, are only partially extracted. These compounds can be determined, if d
10、esired, using the method described in BS3762-3.7. NOTEThe titles of the publications referred to in this Section are listed on the inside back cover. 2 Principle An aqueous alcoholic solution of the sample is extracted with light petroleum which is subsequently evaporated and the residue weighed. If
11、 the presence of soap is known or suspected, the solution is acidified before the extractions and the liberated fatty acids are subsequently washed out of the light petroleum extract by treatment with alkali and reserved for further examination if required. 3 Reagents The reagents shall be of a reco
12、gnized analytical grade. Water complying with BS3978 shall be used throughout. 3.1 Ethanol NOTEFor the purposes of3.1, 3.2, 3.3, 3.4 and3.5 the ethanol may be replaced by industrial methylated spirits complying with BS3591, or such spirits diluted as required. It should be noted that the use of indu
13、strial methylated spirits is governed by The Methylated Spirits Regulations,1983 (S.I.1983No.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 a
14、lternative. 3.2 Ethanol solution, 70% (V/V). 3.3 Ethanol solution, 50% (V/V). 3.4 Ethanol solution, 40% (V/V). 3.5 Ethanol solution, 25% (V/V). 3.6 Light petroleum, boiling range30 C to40 C. 3.7 Acetone 3.8 Sodium hydroxide solution, c (NaOH)=0.10mol/L. 3.9 Hydrochloric acid solution, c (HCl)=1.0mol
15、/L. 3.10 Phenolphthalein indicator solution, 5g/L in50% ethanol solution. 4 Apparatus Ordinary laboratory apparatus and the following are required. 4.1 Separating funnels, of1000mL capacity. 4.2 Flat-bottom flask, of capacity not exceeding250mL. 4.3 Steam bath 5 Procedure 5.1 Test portion If the sam
16、ple is completely soluble in50% ethanol, weigh, to the nearest0.01g, sufficient sample to contain1.6g to2.0g of active matter, dissolve in the50% ethanol solution(3.3), transfer to one of the separating funnels(4.1) and dilute to300mL with the50% ethanol solution. In other cases extract the organic
17、matter, as described in BS3762-3.5, up to the stage of diluting to250mL. If the ethanol soluble matter has been determined by method1of Section3.5, transfer50mL of the ethanol solution thus obtained to a separating funnel(4.1) and add250mL of the40% ethanol solution(3.4). If method2 of Section3.5 ha
18、s been used, transfer100mL of the ethanol solution thus obtained to a separating funnel and add200mL of the25% ethanol solution(3.5). 5.2 Determination If the presence of soap is known or suspected, add the hydrochloric acid solution(3.9) until the pH is just below3.5 (for example, as shown by indic
19、ator papers). Add100mL of the light petroleum(3.6), swirl gently but thoroughly to give adequate extraction and allow the two phases to separate, adding a few millilitres of the ethanol(3.1) when necessary to break tenacious emulsions. Run off the aqueous ethanolic phase into a second separating fun
20、nel(4.1) and extract with a further100mL of the light petroleum. Repeat the extraction of the aqueous ethanolic phase in a third separating funnel(4.1) with a further100mL of the light petroleum. Combine the three extracts in the first separating funnel and wash six times with fresh50mL quantities o
21、f the70% ethanol solution(3.2). NOTE 1If auxiliary surface active agents (alkanolamide foam stabilizers) and sarcosinates are known to be absent, the washing procedure may be simplified. Give four washes with50% ethanol solution(3.3) instead of six washes with70% ethanol solution. Discard the aqueou
22、s ethanolic phase and washings.BS3762-3.6:1986 2 BSI 12-1999 Wash the light petroleum extract alternately three times each with25mL of the sodium hydroxide solution(3.8) and water, and finally with water until the wash liquor is no longer alkaline to the phenolphthalein indicator solution(3.10). NOT
23、E 2If soap and sarcosinates are known to be absent, the alkali washes can be omitted. Free fatty acids when present will be included in this fraction. Transfer the washed light petroleum extract in stages to the flask(4.2), previously weighed to the nearest0.001g, and evaporate off the solvent. WARN
24、ING. Appropriate precautions should be taken when evaporating the solvent as it is highly flammable. Add10mL of the acetone(3.7) and again evaporate off the solvent, rotating the flask on the steam bath(4.3) during this operation to remove as much of the solvent as possible. Cool the flask to about4
25、0 C, gently blow off the last traces of the solvent with a current of dry air, cool and weigh to the nearest0.001g. 6 Expression of results The matter soluble in light petroleum, expressed as a percentage by mass, is given by the following expression: 7 Precision No precision data are available. 8 T
26、est report The test report shall include the following information: a) a reference to this BritishStandard, i.e.BS3762-3.6:1986; b) the results expressed in accordance with clause6; c) a complete identification of the sample; d) any operational details regarded as optional. where m 1 is the mass of
27、extract (ing); m 2 is the mass of sample taken or of sample represented by the volume of ethanol extract taken (ing). 100m 1 m 2 -BS3762-3.6:1986 BSI 12-1999 Publications referred to BS3591, Specification for industrial methylated spirits. BS3762, Analysis of formulated detergents. BS3762-3.5, Metho
28、ds for determination of total organic matter content. BS3762-3.7, Method for determination of total non-ionic matter content. BS3978, Specification for water for laboratory use. BS3762-3.6: 1986 BSI 389 Chiswick High Road London W4 4AL BSIBritishStandardsInstitution BSI is the independent national b
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