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1、BS EN ISO 8799:2009 ICS 71.100.40 NO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAW BRITISH STANDARD Surface active agents Sulfated ethoxylated alcohols and alkylphenols Determination of content of unsulfated matter (ISO 8799:2009) Licensed CopyChinese University of Hong Kong, 1
2、3/06/2009 08:10, Uncontrolled Copy, (c) BSI This British Standard was published under the authority of the Standards Policy and Strategy Committee on 30 April 2009 BSI 2009 ISBN 978 0 580 65933 1 Amendments/corrigenda issued since publication DateComments BS EN ISO 8799:2009 National foreword This B
3、ritish Standard is the UK implementation of EN ISO 8799:2009. It is identical to ISO 8799:2009. It supersedes BS EN ISO 8799:1996 which is withdrawn. The UK participation in its preparation was entrusted to Technical Committee CII/34, Methods of test for surface active agents. A list of organization
4、s represented on this committee can be obtained on request to its secretary. This publication does not purport to include all the necessary provisions of a contract. Users are responsible for its correct application. Compliance with a British Standard cannot confer immunity from legal obligations. L
5、icensed CopyChinese University of Hong Kong, 13/06/2009 08:10, Uncontrolled Copy, (c) BSI EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN ISO 8799 March 2009 ICS 71.100.40Supersedes EN ISO 8799:1995 English Version Surface active agents - Sulfated ethoxylated alcohols and alkylphenols - Determi
6、nation of content of unsulfated matter (ISO 8799:2009) Agents de surface - Sulfates dalcools et dalkylphnols thoxyls - Dtermination de la teneur en matire insulfate (ISO 8799:2009) Grenzflchenaktive Stoffe - Sulfatierte ethoxylierte Alkohole und Alkylphenole - Bestimmung der unsulfatierten Anteile (
7、ISO 8799:2009) This European Standard was approved by CEN on 28 February 2009. CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this European Standard the status of a national standard without any alteration. Up-to-date lists and bib
8、liographical references concerning such national standards may be obtained on application to the CEN Management Centre or to any CEN member. This European Standard exists in three official versions (English, French, German). A version in any other language made by translation under the responsibilit
9、y of a CEN member into its own language and notified to the CEN Management Centre has the same status as the official versions. CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, I
10、reland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZATION COMIT EUROPEN DE NORMALISATION EUROPISCHES KOMITEE FR NORMUNG Management Centre: Avenue Marni
11、x 17, B-1000 Brussels 2009 CENAll rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN ISO 8799:2009: E Licensed CopyChinese University of Hong Kong, 13/06/2009 08:10, Uncontrolled Copy, (c) BSI BS EN ISO 8799:2009 ISO 8799:2009(E) ISO 2009 All
12、 rights reserved iii Contents Page Foreword iv 1 Scope . 1 2 Normative references. 1 3 Principle. 1 4 Reagents and materials . 1 5 Apparatus 2 6 Sampling 2 7 Procedure 2 7.1 Test portion. 2 7.2 Preparation of the ion-exchange resins. 2 7.2.1 Anion-exchange resin clean-up 2 7.2.2 Cation-exchange resi
13、n clean-up . 2 7.3 Final preparation of resins. 3 7.4 Arrangement of the mixed-bed exchange column 3 7.5 Separation of unsulfated matter 3 7.6 Check of the ion-exchange resin 3 8 Calculation and expression of results 3 9 Precision 4 9.1 Repeatability limit. 4 9.2 Reproducibility limit . 4 10 Test re
14、port . 4 Annex A (informative) Statistical and other data derived from the results of interlaboratory tests 5 Bibliography. 6 Licensed CopyChinese University of Hong Kong, 13/06/2009 08:10, Uncontrolled Copy, (c) BSI BS EN ISO 8799:2009 ISO 8799:2009(E) iv ISO 2009 All rights reserved Foreword ISO (
15、the International Organization for Standardization) is a worldwide federation of national standards bodies (ISO member bodies). The work of preparing International Standards is normally carried out through ISO technical committees. Each member body interested in a subject for which a technical commi
16、ttee has been established has the right to be represented on that committee. International organizations, governmental and non-governmental, in liaison with ISO, also take part in the work. ISO collaborates closely with the International Electrotechnical Commission (IEC) on all matters of electrotec
17、hnical standardization. International Standards are drafted in accordance with the rules given in the ISO/IEC Directives, Part 2. The main task of technical committees is to prepare International Standards. Draft International Standards adopted by the technical committees are circulated to the membe
18、r bodies for voting. Publication as an International Standard requires approval by at least 75 % of the member bodies casting a vote. Attention is drawn to the possibility that some of the elements of this document may be the subject of patent rights. ISO shall not be held responsible for identifyin
19、g any or all such patent rights. ISO 8799 was prepared by the European Committee for Standardization (CEN) Technical Committee CEN/TC 276, Surface active agents, in collaboration with ISO Technical Committee ISO/TC 91, Surface active agents, in accordance with the Agreement on technical cooperation
20、between ISO and CEN (Vienna Agreement). This second edition cancels and replaces the first edition (ISO 8799:1988), which has been technically revised. Licensed CopyChinese University of Hong Kong, 13/06/2009 08:10, Uncontrolled Copy, (c) BSI BS EN ISO 8799:2009 INTERNATIONAL STANDARD ISO 8799:2009(
21、E) ISO 2009 All rights reserved 1 Surface active agents Sulfated ethoxylated alcohols and alkylphenols Determination of content of unsulfated matter 1 Scope This International Standard specifies a method for the determination of the content of unsulfated matter present in ordinary commercial neutral
22、ized products of sulfation of ethoxylated alcohols or alkylphenols alkyl oxyethylene sulfates (ethoxylated alcohol sulfates) or alkylphenol oxyethylene sulfates (ethoxylated alkylphenol sulfates) containing an average of not more than 20 oxyethylene groups per molecule. 2 Normative references The fo
23、llowing referenced documents are indispensable for the application of this document. For dated references, only the edition cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies. ISO 607, Surface active agents and detergents Methods o
24、f sample division ISO 2271, Surface active agents Detergents Determination of anionic-active matter by manual or mechanical direct two-phase titration procedure ISO 3696, Water for analytical laboratory use Specification and test methods EN 14480, Surface active agents Determination of anionic surfa
25、ce active agents Potentiometric two-phase titration method 3 Principle From a methanolic solution of the test portion, the unsulfated matter is separated on an ion-exchange column (filled with a mixture of cation-exchange resins and anion-exchange resins). The unsulfated matter is recovered from the
26、 eluate by evaporation and weighing of the residue. 4 Reagents and materials 4.1 General. WARNING The procedures described in this International Standard involve the use of hazardous substances. The necessary precautions, as described in regulations covering the handling of hazardous substances, sho
27、uld be taken. Technical, organizational and personal protection measures should be observed. During the analysis, unless otherwise specified, use only reagents of recognized analytical grade that have been checked in advance so as to not interfere with the analytical results, and water of grade 1 as
28、 defined in ISO 3696. Licensed CopyChinese University of Hong Kong, 13/06/2009 08:10, Uncontrolled Copy, (c) BSI BS EN ISO 8799:2009 ISO 8799:2009(E) 2 ISO 2009 All rights reserved 4.2 Methanol, CH3OH, (CAS number: 67-56-1). 4.3 Hydrochloric acid solution, c(HCl), about 1 mol/l, (CAS number: 7647-01
29、-0). 4.4 Sodium hydroxide solution, c(NaOH), about 2 mol/l, (CAS number 1310-73-2). 4.5 Cation-exchange resin, polystyrene sulfonic acid type, 2 % to 3 % crosslinked, 150 m to 330 m, hydrogen form. 4.6 Anion-exchange resin, polystyrene quaternary ammonium type, 2 % to 3 % crosslinked, 150 m to 330 m
30、, chloride form. 5 Apparatus Ordinary apparatus and the following: 5.1 Rotary evaporator, with round-bottom flasks of capacity 250 ml. 5.2 Ion-exchange column: open glass column of internal diameter 25 mm and length 200 mm, provided with a 10 mm to 20 mm layer of glass wool or sintered glass filter
31、and with a stopcock. 5.3 Water bath, the temperature of which can be adjusted between 25 C to 40 C. 6 Sampling The test sample shall be prepared and stored in accordance with ISO 607. 7 Procedure 7.1 Test portion From the laboratory sample, if necessary homogenized by introducing an appropriate and
32、known quantity of water, weigh, to the nearest 1 mg, into a 100 ml beaker, a quantity of the homogeneous laboratory sample corresponding to 5 mmol of anionic-active matter. 7.2 Preparation of the ion-exchange resins 7.2.1 Anion-exchange resin clean-up Take 100 g of the anion-exchange resin (4.6) and
33、 allow to swell in water for 24 h. Transfer the resin to a suitable column and pass 500 ml of the sodium hydroxide solution (4.4) through the column, followed by about 1 000 ml of water. Then pass 400 ml of the hydrochloric acid solution (4.3) through the column and again wash with enough water unti
34、l the washings have a pH between 5 and 7. The treated resin may be stored in water. 7.2.2 Cation-exchange resin clean-up Take 100 g of the cation-exchange resin (4.5) and allow it to swell in water for 24 h. Transfer the resin to a suitable column, pass 500 ml of the hydrochloric acid solution (4.3)
35、 through the column and wash with water until the washings have a pH between 5 and 7. The treated resin may be stored in water. Licensed CopyChinese University of Hong Kong, 13/06/2009 08:10, Uncontrolled Copy, (c) BSI BS EN ISO 8799:2009 ISO 8799:2009(E) ISO 2009 All rights reserved 3 7.3 Final pre
36、paration of resins Take the required amount of anion-exchange resin, prepared as specified in 7.2.1, namely 25 ml per determination, and transfer to a suitable column. Pass five times the volume of the sodium hydroxide solution (4.4) through the column, wash with water until neutral, then wash with
37、1 to 2 volumes of methanol (4.2). Take the required amount (25 ml) of cation-exchange resin, prepared as specified in 7.2.2, place it in a suitable column and wash it with twice its volume of methanol (4.2). 7.4 Arrangement of the mixed-bed exchange column Mix with the help of a glass rod 25 ml of t
38、he cation-exchange resin and 25 ml of the anion-exchange resin, prepared as specified in 7.3, in a beaker. Fill the column (5.2) with the mixed resin in small portions, let the mixed resin settle to a volume between 50 ml and 60 ml and wash with 500 ml of methanol (4.2). 7.5 Separation of unsulfated
39、 matter Dissolve the test portion (7.1) in 50 ml of methanol (4.2). Filter off the insoluble matter through a fast-running filter paper above the prepared column (see 7.4). Pass the filtrate through the column at a flow rate of 2 ml/min and collect the eluate in a 500 ml beaker. Adjust the flow to 3
40、 ml/min and wash with about 450 ml of methanol. Transfer the eluate and the washings in portions to a tared 250 ml round-bottom flask (see 5.1) and evaporate by means of the rotary evaporator (5.1) on the water bath (5.3) at not more than 40 C, under vacuum. Rinse the beaker and evaporator with abou
41、t 40 ml to 50 ml of methanol and allow the methanol to evaporate. When the flask appears to be free from methanol, leave it on the evaporator for about 15 min. Weigh the flask plus residue, then dry again in the vacuum desiccator for 15 min. Weigh again and repeat the procedure of drying and weighin
42、g until a mass constant to 3 mg is obtained. 7.6 Check of the ion-exchange resin In the case of ethoxylated alcohols, it may happen that the exchange of anions is not complete. Dissolve the residue obtained in 7.5 in 20 ml of water and determine the content of total active matter by direct two-phase
43、 titration in accordance with ISO 2271 or EN 14480. If the anion-active matter content exceeds 0,005 mmol, reject the result and repeat the determination with a fresh sample, using a flow rate of less than 2 ml/min and washing with 250 ml of methanol instead of 450 ml or using separate ion-exchange
44、columns. 8 Calculation and expression of results The unsulfated matter content, w, expressed as a percentage by mass, is given by Equation (1): 1 0 100m w m = (1) where m0 is the mass, in grams, of the test portion (see 7.1); m1 is the mass, in grams, of the residue obtained in 7.5. Licensed CopyChi
45、nese University of Hong Kong, 13/06/2009 08:10, Uncontrolled Copy, (c) BSI BS EN ISO 8799:2009 ISO 8799:2009(E) 4 ISO 2009 All rights reserved 9 Precision 9.1 Repeatability limit The absolute difference between two independent single test results, obtained using the same method on identical test mat
46、erial in the same laboratory by the same operator using the same equipment within a short interval of time, will not exceed the repeatability limit, r, in more than 5 % of cases. 9.2 Reproducibility limit The absolute difference between two independent single test results, obtained using the same me
47、thod on identical test material in different laboratories by different operators using different equipment, will not exceed the reproducibility limit, R, in more than 5 % of cases. 10 Test report The test report shall include the following information: a) all information necessary for the identifica
48、tion of the sample tested; b) a reference to this International Standard (ISO 8799); c) the test results; d) details of any operation not specified in this International Standard or in the standards to which reference is made, and any operations regarded as optional, as well as any incidents likely
49、to have affected the results. Licensed CopyChinese University of Hong Kong, 13/06/2009 08:10, Uncontrolled Copy, (c) BSI BS EN ISO 8799:2009 ISO 8799:2009(E) ISO 2009 All rights reserved 5 Annex A (informative) Statistical and other data derived from the results of interlaboratory tests Comparative analyses of two samples with unsulfated mass fractions of 0,6 % and 2,3 %, respectively, carried out in 15 laboratories, have given the following statistical results: standard deviation of repeatability, r: 0,18;
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