1、BS EN ISO8799:2009ICS 71.100.40NO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAWBRITISH STANDARDSurface activeagents Sulfatedethoxylated alcoholsand alkylphenols Determination ofcontent of unsulfatedmatter (ISO 8799:2009) This British Standardwas published under theauthority of
2、the StandardsPolicy and StrategyCommittee on 30 April2009 BSI 2009ISBN 978 0 580 65933 1Amendments/corrigenda issued since publicationDate CommentsBS EN ISO 8799:2009National forewordThis British Standard is the UK implementation of EN ISO 8799:2009. It is identical to ISO 8799:2009. It supersedes B
3、S EN ISO 8799:1996 which is withdrawn.The UK participation in its preparation was entrusted to TechnicalCommittee CII/34, Methods of test for surface active agents.A list of organizations represented on this committee can be obtained onrequest to its secretary.This publication does not purport to in
4、clude all the necessary provisionsof a contract. Users are responsible for its correct application.Compliance with a British Standard cannot confer immunityfrom legal obligations.EUROPEAN STANDARDNORME EUROPENNEEUROPISCHE NORMEN ISO 8799March 2009ICS 71.100.40 Supersedes EN ISO 8799:1995 English Ver
5、sionSurface active agents - Sulfated ethoxylated alcohols andalkylphenols - Determination of content of unsulfated matter(ISO 8799:2009)Agents de surface - Sulfates dalcools et dalkylphnolsthoxyls - Dtermination de la teneur en matire insulfate(ISO 8799:2009)Grenzflchenaktive Stoffe - Sulfatierte et
6、hoxylierte Alkoholeund Alkylphenole - Bestimmung der unsulfatierten Anteile(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 EuropeanStandard the statu
7、s of a national standard without any alteration. Up-to-date lists and bibliographical references concerning such nationalstandards 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 ve
8、rsion in any other language made by translationunder the responsibility of a CEN member into its own language and notified to the CEN Management Centre has the same status as theofficial versions.CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Cyprus, Czech Republic, Den
9、mark, Estonia, Finland,France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal,Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom.EUROPEAN COMMITTEE FOR STANDARDIZATIONCOMIT EUROPEN DE NORMALISATIO
10、NEUROPISCHES KOMITEE FR NORMUNGManagement Centre: Avenue Marnix 17, B-1000 Brussels 2009 CEN All rights of exploitation in any form and by any means reservedworldwide for CEN national Members.Ref. No. EN ISO 8799:2009: EBS EN ISO 8799:2009ISO 8799:2009(E) ISO 2009 All rights reserved iiiContents Pag
11、e 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 resin clean-up . 2 7.3 Final prepa
12、ration 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 report . 4 Annex A (informative
13、) Statistical and other data derived from the results of interlaboratory tests 5 Bibliography . 6 BS EN ISO 8799:2009ISO 8799:2009(E) iv ISO 2009 All rights reservedForeword ISO (the International Organization for Standardization) is a worldwide federation of national standards bodies (ISO member bo
14、dies). 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 committee has been established has the right to be represented on that committee. International organizations, governmental an
15、d 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 electrotechnical standardization. International Standards are drafted in accordance with the rules given in the ISO/IEC Directives,
16、 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 member bodies for voting. Publication as an International Standard requires approval by at least 75 % of the member bodies cas
17、ting 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 identifying any or all such patent rights. ISO 8799 was prepared by the European Committee for Standardization (CEN) Technical Comm
18、ittee 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 between ISO and CEN (Vienna Agreement). This second edition cancels and replaces the first edition (ISO 8799:1988), which
19、 has been technically revised. BS EN ISO 8799:2009INTERNATIONAL STANDARD ISO 8799:2009(E) ISO 2009 All rights reserved 1Surface active agents Sulfated ethoxylated alcohols and alkylphenols Determination of content of unsulfated matter 1 Scope This International Standard specifies a method for the de
20、termination of the content of unsulfated matter present in ordinary commercial neutralized products of sulfation of ethoxylated alcohols or alkylphenols alkyl oxyethylene sulfates (ethoxylated alcohol sulfates) or alkylphenol oxyethylene sulfates (ethoxylated alkylphenol sulfates) containing an aver
21、age of not more than 20 oxyethylene groups per molecule. 2 Normative references The following 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 (incl
22、uding any amendments) applies. ISO 607, Surface active agents and detergents Methods of 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 Specifi
23、cation and test methods EN 14480, Surface active agents Determination of anionic surface 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-e
24、xchange resins and anion-exchange resins). The unsulfated matter is recovered from the 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 preca
25、utions, as described in regulations covering the handling of hazardous substances, should 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
26、in advance so as to not interfere with the analytical results, and water of grade 1 as defined in ISO 3696. BS EN ISO 8799:2009ISO 8799:2009(E) 2 ISO 2009 All rights reserved4.2 Methanol, CH3OH, (CAS number: 67-56-1). 4.3 Hydrochloric acid solution, c(HCl), about 1 mol/l, (CAS number: 7647-01-0). 4.
27、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, chlor
28、ide 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 and wit
29、h 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 known q
30、uantity 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 allow
31、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 until the w
32、ashings 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) throug
33、h the column and wash with water until the washings have a pH between 5 and 7. The treated resin may be stored in water. BS EN ISO 8799:2009ISO 8799:2009(E) ISO 2009 All rights reserved 37.3 Final preparation of resins Take the required amount of anion-exchange resin, prepared as specified in 7.2.1,
34、 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 1 to 2 volumes of methanol (4.2). Take the required amount (25 ml) of cation-exchange resin, prepare
35、d 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 the cation-exchange resin and 25 ml of the anion-exchange resin, prepared as specified in 7.3, in a b
36、eaker. 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 matter Dissolve the test portion (7.1) in 50 ml of methanol (4.2). Filter off the insoluble matter
37、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 ml/min and wash with about 450 ml of methanol. Transfer the eluate and the washings in portions to
38、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 about 40 ml to 50 ml of methanol and allow the methanol to evaporate. When the flask appears to be free
39、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 weighing until a mass constant to 3 mg is obtained. 7.6 Check of the ion-exchange resin In the case of etho
40、xylated 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 titration in accordance with ISO 2271 or EN 14480. If the anion-active matter content exceeds 0,005
41、 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 columns. 8 Calculation and expression of results The unsulfated matter content, w, expressed as a pe
42、rcentage by mass, is given by Equation (1): 10100mwm= (1) where m0is the mass, in grams, of the test portion (see 7.1); m1is the mass, in grams, of the residue obtained in 7.5. BS EN ISO 8799:2009ISO 8799:2009(E) 4 ISO 2009 All rights reserved9 Precision 9.1 Repeatability limit The absolute differen
43、ce between two independent single test results, obtained using the same method on identical test material 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 l
44、imit The absolute difference between two independent single test results, obtained using the same method 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
45、test report shall include the following information: a) all information necessary for the identification 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 t
46、o which reference is made, and any operations regarded as optional, as well as any incidents likely to have affected the results. BS EN ISO 8799:2009ISO 8799:2009(E) ISO 2009 All rights reserved 5Annex A (informative) Statistical and other data derived from the results of interlaboratory tests Compa
47、rative 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; standard deviation of reproducibility, R: 0,39. BS EN ISO 8799:2009ISO 8799:2009
48、(E) 6 ISO 2009 All rights reservedBibliography 1 ISO 6842, Surface active agents Sulfated ethoxylated alcohols and alkylphenols Determination of total active matter content BS EN ISO8799:2009BSI GroupHeadquarters 389Chiswick High Road,London, W4 4AL, UKTel +44 (0)20 8996 9001Fax +44 (0)20 8996 - Br
49、itish Standards InstitutionBSI is the independent national body responsible for preparing BritishStandards. It presents the UK view on standards in Europe and at theinternational level. It is incorporated by Royal Charter.RevisionsBritish Standards are updated by amendment or revision. Users of BritishStandards should make sure that they possess the latest amendments oreditions.It is the constant aim of BSI to improve the quality of our products and services.We would
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