DIN EN ISO 8799-2010 Surface active agents - Sulfated ethoxylated alcohols and alkylphenols - Determination of content of unsulfated matter (ISO 8799 2009) German version EN ISO 87.pdf

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1、April 2010 Translation by DIN-Sprachendienst.English price group 8No part of this translation may be reproduced without prior permission ofDIN Deutsches Institut fr Normung e. V., Berlin. Beuth Verlag GmbH, 10772 Berlin, Germany,has the exclusive right of sale for German Standards (DIN-Normen).ICS 7

2、1.100.40!$aU1“1625014www.din.deDDIN EN ISO 8799Surface active agents Sulfated ethoxylated alcohols and alkylphenols Determination of content of unsulfated matter (ISO 8799:2009)English translation of DIN EN ISO 8799:2010-04Grenzflchenaktive Stoffe Sulfatierte ethoxylierte Alkohole und Alkylphenole B

3、estimmung der unsulfatierten Anteile (ISO 8799:2009)Englische bersetzung von DIN EN ISO 8799:2010-04Agents de surface Sulfates dalcools et dalkylphnols thoxyls Dtermination de la teneur en matire insulfate (ISO 8799:2009)Traduction anglaise de DIN EN ISO 8799:2010-04SupersedesDIN EN ISO 8799:1995-09

4、www.beuth.deIn case of doubt, the German-language original shall be considered authoritative.Document comprises 11 pages04.10 DIN EN ISO 8799:2010-04 2 A comma is used as the decimal marker. National foreword This standard has been prepared by Technical Committee CEN/TC 276 “Surface active agents” (

5、Secretariat: AFNOR, France) in collaboration with Technical Committee ISO/TC 91 “Surface active agents”. The responsible German body involved in its preparation was the Normenausschuss Materialprfung (Materials Testing Standards Committee), Technical Committee NA 062-05-62 AA Analytik von Tensiden.

6、The DIN Standards corresponding to the International Standards referred to in this document are as follows: ISO 607 DIN ISO 607 ISO 2271 DIN ISO 2271 ISO 3696 DIN ISO 3696 Amendments This standard differs from DIN EN ISO 8799:1995-09 as follows: a) Further specifications on reagents have been includ

7、ed. b) The amounts of reagents to be used for the anion-exchange resin and cation-exchange resin clean-up have been reduced and a pH between 5 and 7 has been specified for the washings. c) In addition to the procedure described in DIN ISO 2271, the potentiometric two-phase titration method according

8、 to DIN EN 14480 may also be used for the check of the ion-exchange resin. d) The symbol of the unsulfated matter content, expressed as a percentage by mass, has been changed from NS to w. e) A Bibliography has been added. f) The standard has been editorially revised. Previous editions DIN EN ISO 87

9、99: 1995-09 National Annex NA (informative) Bibliography DIN ISO 607, Surface active agents and detergents Methods of sample division DIN ISO 2271, Surface active agents Detergents Determination of anionic-active matter (direct two-phase titration procedure) DIN ISO 3696, Water for analytical labora

10、tory use Specification and test methods EUROPEAN STANDARDNORME EUROPENNEEUROPISCHE NORMEN ISO 8799March 2009ICS 71.100.40 Supersedes EN ISO 8799:1995 English VersionSurface active agents - Sulfated ethoxylated alcohols andalkylphenols - Determination of content of unsulfated matter(ISO 8799:2009)Age

11、nts de surface - Sulfates dalcools et dalkylphnolsthoxyls - Dtermination de la teneur en matire insulfate(ISO 8799:2009)Grenzflchenaktive Stoffe - Sulfatierte ethoxylierte Alkoholeund Alkylphenole - Bestimmung der unsulfatierten Anteile(ISO 8799:2009)This European Standard was approved by CEN on 28

12、February 2009.CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this EuropeanStandard the status of a national standard without any alteration. Up-to-date lists and bibliographical references concerning such nationalstandards may be o

13、btained 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 translationunder the responsibility of a CEN member into its own language and notified to the CEN Manag

14、ement Centre has the same status as theofficial versions.CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Cyprus, Czech Republic, Denmark, Estonia, Finland,France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway

15、, Poland, Portugal,Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom.EUROPEAN COMMITTEE FOR STANDARDIZATIONCOMIT EUROPEN DE NORMALISATIONEUROPISCHES KOMITEE FR NORMUNGManagement Centre: Avenue Marnix 17, B-1000 Brussels 2009 CEN All rights of exploitation in any form and by

16、any means reservedworldwide for CEN national Members.Ref. No. EN ISO 8799:2009: EContents DIN EN ISO 8799:2010-04 EN ISO 8799:2009 (E) 2 Page Foreword .3 1 Scope4 2 Normative references4 3 Principle .4 4 Reagents and materials 4 5 Apparatus.5 6 Sampling 5 7 Procedure.5 7.1 Test portion5 7.2 Preparat

17、ion of the ion-exchange resins5 7.2.1 Anion-exchange resin clean-up .5 7.2.2 Cation-exchange resin clean-up 5 7.3 Final preparation of resins .6 7.4 Arrangement of the mixed-bed exchange column.6 7.5 Separation of unsulfated matter 6 7.6 Check of the ion-exchange resin .6 8 Calculation and expressio

18、n of results 6 9 Precision 7 9.1 Repeatability limit7 9.2 Reproducibility limit7 10 Test report7 Annex A (informative) Statistical and other data derived from the results of interlaboratory tests 8 Bibliography9 Foreword which is held by AFNOR. This European Standard shall be given the status of a n

19、ational standard, either by publication of an identical text or by endorsement, at the latest by September 2009, and conflicting national standards shall be withdrawn at the latest by September 2009. Attention is drawn to the possibility that some of the elements of this document may be the subject

20、of patent rights. CEN and/or CENELEC shall not be held responsible for identifying any or all such patent rights. This document supersedes EN ISO 8799:1995. According to the CEN/CENELEC Internal Regulations, the national standards organizations of the following countries are bound to implement this

21、European Standard: Austria, Belgium, Bulgaria, Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and the Un

22、ited Kingdom. This document (EN ISO 8799:2009) has been prepared by Technical Committee ISO/TC 91 “Surface active agents” in collaboration with Technical Committee CEN/TC 276 “Surface active agents”, the secretariat of DIN EN ISO 8799:2010-04 EN ISO 8799:2009 (E) 3 1 Scope This International Standar

23、d specifies a method for the determination 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 alkylphen

24、ol sulfates) containing an average 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 o

25、f the referenced document (including 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 an

26、alytical laboratory use Specification 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 (fi

27、lled with a mixture of cation-exchange resins and anion-exchange resins). The unsulfated matter is recovered from the eluate by evaporation and weighing of the residue. 4 Reagents and materials WARNING The procedures described in this International Standard involve the use of hazardous substances. T

28、he necessary precautions, 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

29、have been checked in advance so as to not interfere with the analytical results, and water of grade 1 as defined in ISO 3696. DIN EN ISO 8799:2010-04 EN ISO 8799:2009 (E) 4 4.1 General 4.2 Methanol, CH3OH, (CAS number: 67-56-1). 4.3 Hydrochloric acid solution, c(HCl), about 1 mol/l, (CAS number: 764

30、7-01-0). 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 3

31、30 m, 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 fil

32、ter 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

33、and 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)

34、 and 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

35、until 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 (

36、4.3) 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. DIN EN ISO 8799:2010-04 EN ISO 8799:2009 (E) 5 7.3 Final preparation of resins Take the required amount of anion-exchange resin, prepared as specified in 7.2.1, namely

37、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, prepared as spe

38、cified 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 beaker. F

39、ill 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 through

40、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 a tared

41、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 from met

42、hanol, 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 ethoxylated

43、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 mmol, r

44、eject 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 percentage

45、 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. DIN EN ISO 8799:2010-04 EN ISO 8799:2009 (E) 6 9 Precision 9.1 Repeatability limit The absolute difference between two independent

46、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 limit The absolute differenc

47、e 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 test report shall include t

48、he 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 to which reference is made,

49、and any operations regarded as optional, as well as any incidents likely to have affected the results. DIN EN ISO 8799:2010-04 EN ISO 8799:2009 (E) 7 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; standard deviation of reproducibility, R: 0,39