1、BRITISH STANDARD CONFIRMED MAY1996 BS3762-3.7: 1986 Analysis of formulated detergents Part3: Quantitative test methods Section3.7 Method for determination of total non-ionic matter content NOTEIt is recommended that this Section be read in conjunction with the information in the “General Introductio
2、n”, published separately as BS3762-0. UDC 661.185:543BS3762-3.7:1986 This British Standard, having been prepared under the directionof the Chemicals Standards Committee, was published under the authority ofthe Board of BSI and comes intoeffect on 30 September1986 BSI 10-1999 The committees responsib
3、le for this British Standard are shown inPart0 The following BSI references relate to the work on this standard: Committee reference CIC/34 Draft for comment 85/52541 DC ISBN 0 580 15326 6 Foreword This Section of BS3762 has been prepared under the direction of the Chemicals Standards Committee and
4、supersedes method C1 of BS3762:1964 in so far as it applies to formulated detergents, but that method will continue to exist until a British Standard for the determination in surface active agents(raw materials) has been published. This standard describes a method of test only and should not be refe
5、rred to as a specification defining limits of purity. Reference to the standard should indicate that the method of test used is in conformity with BS3762-3.7. A British Standard does not purport to include all the necessary provisions of a contract. Users of British Standards are responsible for the
6、ir 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 cover and a back cover. This standard has been updated (see c
7、opyright 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 CommentsBS3762-3.7:1986 BSI 10-1999 i Contents Page Foreword Inside front cover 1 Scope 1 2 Principle 1 3 Reage
8、nts 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 blankBS3762-3.7:1986 BSI 10-1999 1 1 Scope This Section of BS3762 describes a gravimetric method for the determination of the total non-ionic matter content of deter
9、gent products. NOTEThe titles of the publications referred to in this Section are listed on the inside back cover. 2 Principle A suitable aliquot portion is taken from the ethanol soluble portion(seeBS3762-3.5). The solution is stirred with a mixed bed of cation and anion exchange resins to remove i
10、onic active matter. The solution is then filtered and evaporated, and the non-ionic matter is determined gravimetrically. This extract will include non-detergent organic matter and also any alkanolamide-type lather improver if present. 3 Reagents The reagents shall be of a recognized analytical reag
11、ent grade. Water complying with BS3978 shall be used throughout. 3.1 Ethanol NOTEFor the purposes of3.1, 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 industrial methylated spirits is govern
12、ed by The Methylated Spirits Regulations,1983 (S.I.1983 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. 3.2 Acetone 3.3 A mixt
13、ure of ion-exchange resins, produced from a strongly acidic(H form) cation exchanger mixed with a strongly basic(OH form) anion exchanger in inverse proportion by mass approximating to their respective ion exchange capacities. Use10g of this mixed resin for products containing up to4%ethanol soluble
14、 ionic matter, and use an additional5g resin for each additional4%ethanol soluble ionic matter. Immediately before use wash the mixed bed resin, contained in a250mL conical flask, three times by swirling and decanting with twice its volume of ethanol(3.1) to remove water and any trace of ethanol-sol
15、uble contamination. NOTEReady prepared mixed bed resins are available commercially. 3.4 Methylene blue solution, 0.03g/L. Dissolve0.15g of methylene blue (CI52015) in100mL of water, then dilute2mL of this solution to100mL. 3.5 Chloroform 4 Apparatus Ordinary laboratory apparatus and the following ar
16、e required. 4.1 One-mark volumetric flask, 250mL, complying with BS1792. 4.2 Wide-mouthed, flat-bottomed flask, 250mL. 5 Procedure 5.1 Test portion Carry out an ethanol extraction in accordance with BS3762-3.5, by method1 or method2. Pipette100mL of the solution from the one-mark volumetric flask(4.
17、1) into the250mL conical flask containing the washed ion-exchange resin(3.3). 5.2 Determination Insert a magnetic follower, cover the flask with a watch glass, and begin to stir, avoiding any splashing. Continue stirring for20min. Decant the solution into the250mL one-mark volumetric flask(4.1) thro
18、ugh a12.5cm diameter filter paper(fast speed). Allow the solvent to drain thoroughly. Add20mL of the ethanol(3.1) to the conical flask and swirl. Filter, allowing the solvent to drain completely. Repeat with three more20mL portions of ethanol. Wash the filter paper with ethanol. Dilute to the mark w
19、ith ethanol. Check the resin as follows. Remove exactly5mL of the solution from the volumetric flask using a clean, dry pipette and without rinsing the pipette with the solution. Transfer approximately2mL of this aliquot portion to a test tube and discard the rest. Add10mL of water,1mL of the methyl
20、ene blue solution(3.4) and1mL of the chloroform(3.5) to the test tube, cover and shake. Allow the layers to separate. If the blue colour of the lower layer is more intense than that of the upper layer, the ion exchange was incomplete and the determination should be restarted using a fresh supply of
21、ion-exchange resins; otherwise, continue with the determination. NOTE 1Ion-exchange resins have a finite exchange capacity and it is essential that they are not overloaded in terms of alcohol-soluble ionic constituents. It can arise that the exchange of anions is not complete. Weigh, to the nearest0
22、.0005g, a250mL wide-mouthed, flat-bottomed flask (4.2) containing a few anti-bumping granules. Transfer the solution quantitatively from the volumetric flask to this weighed flask.BS3762-3.7:1986 2 BSI 10-1999 Evaporate off the solvent on a steam bath to approximately2mL to3mL. Add5mL of the acetone
23、(3.2) and evaporate to dryness while blowing with a gentle stream of air. Repeat with a further three portions of the acetone. Blow with a gentle stream of air until the last traces of acetone are removed. Wipe the outside of the flask dry. Cool in a desiccator for30min and weigh to the nearest0.000
24、5g. Repeat the acetone drying procedure until two consecutive weighings agree within0.002g. NOTE 2The weighed residue may be used for the determination of alkanolamides content(seeBS3762-3.8). 6 Expression of results The total non-ionic matter, expressed as a percentage by mass, is given by the foll
25、owing expression: where NOTEThe factor250/245 is to correct for the5mL of solution removed in the check of the ion-exchange resin. 7 Precision The precision is expected to depend markedly upon the content and the nature of the non-ionic matter. Some typical values are given below. The precision data
26、 were determined in an experiment conducted in1985 involving seven laboratories. NOTEFor the meaning of the precision terms seeBS5497-1. 8 Test report The test report shall include the following information: a) a reference to this British Standard, i.e.BS3762-3.7:1986; b) the results expressed in ac
27、cordance with clause6; c) a complete identification of the sample. m 0 is the mass of the sample taken in accordance with BS3762-3.5(ing); m 1 is the mass of the evaporation flask(ing); m 2 is the mass of the flask plus evaporated residue(ing). m 2 m 1 m 0 - 250 245 - 250 100 - 100 Mean result Repea
28、tability Reproducibility Detergent powder % 1.5 % 0.27 % 0.43 Dishwashing liquid 8 0.44 1.2BS3762-3.7:1986 BSI 10-1999 Publications referred to BS1792, Specification for one-mark volumetric flasks. BS3591, Specification for industrial methylated spirits. BS3762, Analysis of formulated detergents. BS
29、3762-3.5, Methods for determination of total organic matter content. BS3762-3.8, Method for determination of alkanolamides content. BS3978, Water for laboratory use. BS5497, Precision of test methods. BS5497-1, Guide for the determination of repeatability and reproducibility for a standard test meth
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