1、 g49g50g3g38g50g51g60g44g49g42g3g58g44g55g43g50g56g55g3g37g54g44g3g51g40g53g48g44g54g54g44g50g49g3g40g59g38g40g51g55g3g36g54g3g51g40g53g48g44g55g55g40g39g3g37g60g3g38g50g51g60g53g44g42g43g55g3g47g36g58solvents in liquid detergents by GLCThe European Standard EN 14981:2006 has the status of a British
2、 StandardICS 71.100.40Surface active agents Determination of content of high boiling BRITISH STANDARDBS EN 14981:2006BS EN 14981:2006This British Standard was published under the authority of the Standards Policy and Strategy Committee on 30 November 2006 BSI 2006ISBN 0 580 49576 0Amendments issued
3、since publicationAmd. No. Date Commentscontract. Users are responsible for its correct application.Compliance with a British Standard cannot confer immunity from legal obligations.National forewordThis British Standard was published by BSI. It is the UK implementation of EN 14981:2006.The UK partici
4、pation in its preparation was entrusted to Technical Committee CII/34, Methods of test for surface active agents.A list of organizations represented on CII/34 can be obtained on request to its secretary.This publication does not purport to include all the necessary provisions of a EUROPEAN STANDARDN
5、ORME EUROPENNEEUROPISCHE NORMEN 14981October 2006ICS 71.100.40English VersionSurface active agents - Determination of content of high boilingsolvents in liquid detergents by GLCAgents de surface - Dtermination de la teneur en solvants point dbullition lev dans les dtergents liquides parchromatograph
6、ie en phase gazeuseGrenzflchenaktive Stoffe - Bestimmung des Gehaltes anhochsiedenden Lsemitteln in flssigen Reinigungsmittelndurch GLCThis European Standard was approved by CEN on 28 August 2006.CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions
7、 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 obtained on application to the Central Secretariat or to any CEN member.This European Standard exists in three official
8、 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 Central Secretariat has the same status as the officialversions.CEN members are the national standards bodies of Austria, Belgium
9、, 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 United Kingdom.EUROPEAN COMMITTEE FOR STANDARDIZATION
10、COMIT EUROPEN DE NORMALISATIONEUROPISCHES KOMITEE FR NORMUNGManagement Centre: rue de Stassart, 36 B-1050 Brussels 2006 CEN All rights of exploitation in any form and by any means reservedworldwide for CEN national Members.Ref. No. EN 14981:2006: EEN 14981:2006 (E) 2 Contents Page Foreword3 1 Scope
11、4 2 Normative references 4 3 Terms and Definitions .4 4 Principle4 5 Reagents.4 6 Apparatus .5 7 Sampling and preparation of the sample 5 8 Procedure .5 8.1 Gas chromatographic conditions 5 8.2 Preparation of solutions .5 8.2.1 Solvent reference solution 1.5 8.2.2 Solvent reference solution 2.5 8.2.
12、3 Stock solution for calibrations.6 8.2.4 Carvone internal standard solution .6 8.3 Calibration 6 8.4 Sample analysis.7 8.4.1 Solvent identification 7 8.4.2 Solvent quantification .7 9 Calculation and expression of results.7 10 Precision.8 10.1 Repeatability limit 8 10.2 Reproducibility limit 8 11 T
13、est report 8 Annex A (informative) Examples of chromatogram.9 A.1 Solvent identification 9 A.2 Solvent quantification .12 Annex B (informative) Statistical and other data derived from the results of inter-laboratory tests .13 Bibliography 14 EN 14981:2006 (E) 3 Foreword This document (EN 14981:2006)
14、 has been prepared by Technical Committee CEN/TC 276 “Surface active agents”, the secretariat of which is held by AFNOR. This European Standard shall be given the status of a national standard, either by publication of an identical text or by endorsement, at the latest by April 2007, and conflicting
15、 national standards shall be withdrawn at the latest by April 2007. According to the CEN/CENELEC Internal Regulations, the national standards organizations of the following countries are bound to implement this European Standard: Austria, Belgium, Cyprus, Czech Republic, Denmark, Estonia, Finland, F
16、rance, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom. EN 14981:2006 (E) 4 1 Scope This European Standard specifies a method for the identifying
17、 and quantifying of high boiling point solvents in finished liquid detergents and raw materials. 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
18、edition of the referenced document (including any amendments) applies. ISO 607, Surface active agents and detergents - Methods of sample division 3 Term and Definition For the purposes of this European Standard, the following term and definition applies. high boiling solvent solvent, mainly a glycol
19、 and glycol ether product, with a boiling point significantly higher than water (100 C) 4 Principle The organic solvents are determined by gas chromatography. The sample is dissolved in ethanol and injected into a polar phase capillary column and the unknown solvent is identified by its retention ti
20、me. After qualitative determination, the solvent is quantified using (-) Carvone (2-Methyl-5-(1-methylethenyl)-2-cyclohexene-1-one) as internal standard. 5 Reagents During the analysis, unless otherwise specified, use only reagents of recognized analytical grade that have been checked in advance so
21、as not to interfere with the analytical results. WARNING Some reagents used throughout this procedure are toxic. Care should be taken not to inhale the vapours. Contact with the skin should also be avoided. Safety glasses and gloves should be worn when handling the reagents. Waste solvent disposal s
22、hould be carried out in accordance with safety and environmental regulations. 5.1 Ethanol (CAS number: 64-17-5). 5.2 (-) Carvone (2-Methyl-5-(1-methylethenyl)-2-cyclohexene-1-one), minimum purity 99,5 % (CAS number : 6485-40-1) 5.3 Solvents to be determined (see example in Annex A) WARNING Some solv
23、ents may exist as different isomers. 5.4 Carrier gas for gas chromatography 5.5 Auxiliary gas for gas chromatography EN 14981:2006 (E) 5 6 Apparatus Ordinary laboratory apparatus and the following: 6.1 Gas chromatograph equipped with split/splitless injection port and flame ionization detector (FID)
24、. 6.2 Electronic integrator or, preferably, a suitable data acquisition system. 6.3 Capillary column, capable of the separation characteristics shown in Figures A.1 and A.2. 6.4 Glass tube, with a capacity of at least 40 ml. NOTE A 30 m x 0,25 mm internal diameter, fused silica capillary column (fil
25、m thickness 0,25 m) with 100 % polyethylene glycol stationary phase is advisable. 7 Sampling and preparation of the sample The laboratory sample shall be prepared and stored in accordance with ISO 607. 8 Procedure 8.1 Gas chromatographic conditions The following GC conditions have been found to be s
26、uitable. At least the quality of separation shown in Figures A.1 and A.2 shall be achieved. Oven temperature programs: qualitative analysis: 60C (5 min) to 240C (5 min) at 5C/min; quantitative analysis: 60C to 240C (5 min) at 20C/min; Injection: split ratio at 100:1 and temperature at 225C; Detectio
27、n : flame ionization detector (FID) at 275C with nitrogen as make up gas at 25 ml/min; Carrier gas: hydrogen at 50 kPa head pressure. 8.2 Preparation of solutions 8.2.1 Solvent reference solution 1 Into a glass tube (6.4), weigh approximately 20 mg of each solvent as listed on chromatogram 1. Add 30
28、 ml of ethanol and mix well. 8.2.2 Solvent reference solution 2 Into a glass tube (6.4), weigh approximately 20 mg of each solvent as listed on chromatogram 2. Add 30 ml of ethanol and mix well. Inject 1 l of the solvent reference solutions 1 and 2 into the gas chromatograph. Refer to the annexed ch
29、romatograms 1 and 2 for peak identities. EN 14981:2006 (E) 6 8.2.3 Stock solution for calibrations Weigh to the nearest 0,1 mg, approximately 250 mg of each of the solvent(s) of interest into a 100 ml volumetric flask. Dilute to volume with ethanol, and mix well. 8.2.4 Carvone internal standard solu
30、tion Weigh to the nearest 0,1 mg, approximately 500 mg of carvone into a 100 ml volumetric flask. Dilute to volume with ethanol and mix thoroughly (5,0 mg/ml of carvone). 8.3 Calibration Using precision glass pipettes, transfer 5,0 ml, 7,0 ml, 10,0 ml, 12,0 ml, and respectively 15,0 ml of the stock
31、solution for calibrations into a series of glass tubes (6.4). Using a volumetric glass pipette, add 5,0 ml of the carvone internal standard solution, make up to 30 ml with ethanol and mix well. Inject 1 l of each solution into the gas chromatograph. Record the peak areas of the peaks of interest and
32、 carry out a regression analysis of (Area of solvent/Area of internal standard) versus (mass of solvent/mass of internal standard), for each solvent(s). The response factor, Ki, for each solvent i, is the slope of the calculated regression curve. If a correlation factor of less than 0,98 is obtained
33、 prepare new calibration solution and re-inject. If a data acquisition system is not available, calculate the response factor for all the standard solutions according to the following formula: siisiAfmAfmKis= (1) where ms is the mass, in milligrams, of the internal standard ; fsis the purity of the
34、internal standard, in % (m/m); fi is the purity of the solvent i, in % (m/m); Ai is the peak area of the solvent i; miis the mass, in milligrams, of the solvent i; As peak area of the internal standard. Calculate the mean response factor of all Kifor each solvent and the relative standard deviation.
35、 If the relative standard deviation (RSD) of Kiis 3 %, repeat the calibration procedure. EN 14981:2006 (E) 7 8.4 Sample analysis 8.4.1 Solvent identification Into a glass tube (6.4), weigh 1g to 2 g of sample. Add 30 ml of ethanol and mix thoroughly. Inject 1 l of the obtained solution into the GC a
36、nd allow the chromatogram to develop. Identify the solvent(s) present in the sample by comparing the retention time(s) with the reference chromatogram. Spike the sample with 20 mg of each of the identified solvent(s). Mix the solution thoroughly and inject 1 l of this new solution into the GC. Allow
37、 the chromatogram to develop. Confirm the identification of the solvent(s). 8.4.2 Solvent quantification Into a glass tube (6.4) accurately weigh sufficient sample to contain approximately 25 mg of solvent. Using a volumetric glass pipette, add 5,0 ml of the carvone internal standard solution follow
38、ed by 25 ml of ethanol and mix well. Inject 1 l of the ethanolic solution into the gas chromatograph. Record the peak areas of the peaks of interest and calculate the results according to clause 9. 9 Calculation and expression of results The content of solvent i, wi, expressed in grams per 100 grams
39、 is calculated according to the following equation: i0i0iKAmAfmwo= (2) where m0 is the mass, in milligrams, of the internal standard; f0 is the purity of the internal standard, expressed in % (m/m); Ai is the peak area of the solvent i in the sample analysis; m is the mass, in milligrams, of the sam
40、ple; A0 is the peak area of the internal standard in the sample analysis; Ki is the response factor for solvent i, calculated in 8.3. EN 14981:2006 (E) 8 10 Precision 10.1 Repeatability limit The absolute difference between two independent single test results, obtained using the same method on ident
41、ical 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. Precision data are given in Annex B. 10.2 Reproducibility limit The absolute difference between two independ
42、ent 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. Precision data are given in Annex B. 11 Test report The test report
43、shall include the following information: a) all information necessary for the identification of the sample tested; b) reference to this European Standard (EN 14981); c) method used; d) test results; e) details of any operation not specified in this European Standard or in the European Standards to w
44、hich reference is made, and any operations regarded as optional, as well as any incidents likely to have affected the results. EN 14981:2006 (E) 9 Annex A (informative) Examples of chromatogram A.1 Solvent identification EN 14981:2006 (E) 10 Key Peak Identification 1 Ethylene glycol diethyl ether (C
45、AS Number:629-14-1) 14 Diethylene glycol monoethyl ether (CAS Number:111-90-0) 2 Propylene glycol monomethyl ether (CAS Number: 107-98-2) 15 Ethylene glycol (CAS Number:107-21-1) 3 Ethylene glycol monomethyl ether (CAS Number:109-86-4) 16 Hexylene glycol (2-methyl-2,4-pentanediol) (CAS Number:107-41
46、-5) 4 Limonene (CAS number:5989-27-5) 17 (-)Carvone (CAS Number:6485-40-1) 5 Propylene glycol tert-butyl ether (CAS Number:57018-52-7) 18 Diethylene glycol monobutyl ether (CAS Number:112-34-5) 6 Ethylene glycol monoethyl ether (CAS Number:110-80-5) 19 Benzyl alcohol (CAS Number:100-51-6) 7 Ethylene
47、 glycol monoisopropyl ether (CAS Number:109-59-1) 20 Diethylene glycol (CAS Number:111-46-6) 8 Propylene glycol monoisobutyl ether (CAS Number:80783-53-5) 21 Diethylene glycol monohexyl ether (CAS Number:112-59-4) 9 Propylene glycol monobutyl ether (CAS Number:5131-66-8) 22 Propylene glycol monophen
48、yl ether (CAS Number:770-35-4) 10 Ethylene glycol monobutyl ether (CAS Number:111-76-2) 23 Ethylene glycol monophenyl ether (CAS Number:122-99-6) 11 Diethylene glycol monomethyl ether (CAS Number:111-77-3) 24 Triethylene glycol monobutyl ether (CAS Number:143-22-6) 12 1,2- Propanediol (CAS Number:57
49、-55-6) 25 Glycerol (CAS Number:56-81-5) 13 Ethylene glycol monohexyl ether (CAS Number:112-25-4) 26 Diethyl phthalate (CAS Number:84-66-2) X Time (min) NOTE Chromatography Column: 30 m x 250 m internal diameter. x 0,25 m of 100% polyethylene glycol (i.e., Zebron ZB-WAX column from Phenomenex).1)Oven: 60C (5 min) then to 240C (5 min) at 5C/min. Injection: 225C split ratio at 100:1 Detection: FID at 275C. Carrier gas: hydrogen at 50 kPa head pressure (or helium at 94 kPa). Figure A.1 - Chromat
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