1、BS EN 15647:2009ICS 71.100.40NO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAWBRITISH STANDARDSurface active agents Determination ofthe dispersing effect ofsurfactants on powderThis British Standardwas published under theauthority of the StandardsPolicy and StrategyCommittee on
2、28 February2009 BSI 2009ISBN 978 0 580 58331 5Amendments/corrigenda issued since publicationDate CommentsBS EN 15647:2009National forewordThis British Standard is the UK implementation of EN 15647:2009.The UK participation in its preparation was entrusted to TechnicalCommittee CII/34, Methods of tes
3、t 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 include all the necessary provisionsof a contract. Users are responsible for its correct application.Compliance with a British Standard ca
4、nnot confer immunityfrom legal obligations.BS EN 15647:2009EUROPEAN STANDARDNORME EUROPENNEEUROPISCHE NORMEN 15647January 2009ICS 71.100.40English VersionSurface active agents - Determination of the dispersing effect ofsurfactants on powderAgents de surface - Dtermination des forces de dispersiondes
5、 surfactants sur la poudreGrenzflchenaktive Stoffe - Bestimmung derDispersionswirkung von Tensiden auf PulverThis European Standard was approved by CEN on 29 November 2008.CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this Europea
6、nStandard 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 CEN Management Centre or to any CEN member.This European Standard exists in three official versions (English, Fr
7、ench, 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 Management Centre has the same status as theofficial versions.CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Cyprus,
8、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 STANDARDIZATIONCOMIT EURO
9、PEN DE NORMALISATIONEUROPISCHES KOMITEE FR NORMUNGManagement Centre: rue de Stassart, 36 B-1050 Brussels 2009 CEN All rights of exploitation in any form and by any means reservedworldwide for CEN national Members.Ref. No. EN 15647:2009: EBS EN 15647:2009EN 15647:2009 (E) 2 Contents Page Foreword 3 1
10、 Scope 4 2 Normative references 4 3 Terms and definitions .4 4 Principle 4 5 Reagents .4 6 Apparatus .5 7 Sampling and preparation of the test sample .5 8 Procedure .5 8.1 Preparation of the surfactant solution.5 8.2 Positioning of the cylinder 5 8.3 Adjustment of the stirrer velocity 6 8.4 Carrying
11、 out of the test .6 9 Calculation and expression of results .6 10 Precision .7 10.1 Repeatability limit 7 10.2 Reproducibility limit 7 11 Test report 8 Annex A (informative) Statistical and other data derived from the results of interlaboratory tests .9 Bibliography . 10 BS EN 15647:2009EN 15647:200
12、9 (E) 3 Foreword This document (EN 15647:2009) 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
13、, at the latest by July 2009, and conflicting national standards shall be withdrawn at the latest by July 2009. Attention is drawn to the possibility that some of the elements of this document may be the subject of patent rights. CEN and/or CENELEC shall not be held responsible for identifying any o
14、r all such patent rights. According to the CEN/CENELEC Internal Regulations, the national standards organizations of the following countries are bound to implement this European Standard: Austria, Belgium, Bulgaria, Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary,
15、 Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and the United Kingdom. BS EN 15647:2009EN 15647:2009 (E) 4 1 Scope This European Standard specifies a method for the determination of the ef
16、fectiveness of surface active agents to create and to stabilize a dispersion of pigment powder in water. It is applicable to all classes of surface active agents and formulations of surface active agents. The method can also be applied analogously to other powders. 2 Normative references The followi
17、ng 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 of sam
18、ple division 3 Terms and definitions For the purposes of this document, the following terms and definitions apply. 3.1 dispersing effect dispersing power of a surfactant on powder effectiveness of a surfactant to produce and to stabilize a solid-liquid dispersion 4 Principle The dispersing effect is
19、 determined by the “degree of dispersion”. The “degree of dispersion” is the amount of solid particles kept suspended by the surfactant at a defined distance from the bottom of a measuring cylinder after a defined time related to a homogeneous distribution. 10,00 g zinc oxide is added to a measuring
20、 cylinder and mixed with 50 ml of an aqueous solution of the surface active agent (6 g/l). The mixture is stirred with a defined stirring speed for 30 minutes. The dispersion is then diluted by adding 150 ml water and stirred again with the same speed for another 30 minutes. After standing for 3 hou
21、rs, during which the zinc oxide particles are allowed to sediment, a 5 ml sample is taken at the 150 ml marking of the measuring cylinder and the oven-dry mass is determined. The degree of dispersion is the amount of the oven-dry mass in percentage of the maximum amount. The maximum amount is obtain
22、ed if a homogeneous dispersion is formed and no sedimentation occurs. An important aspect of the method is to use reproducible stirring conditions. This is achieved by using defined stirrer and vessel dimensions together with a stirring speed that is adjusted using the length of the conical vortex f
23、ormed. 5 Reagents WARNING Your attention is drawn to the regulations covering the handling of hazardous substances. Technical, organisational and personal protection measures should be observed. During the analysis, unless otherwise specified, use only reagents of recognized analytical grade that ha
24、ve been checked in advance as to not interfere with the analytical results. 5.1 water of defined hardness and pH value BS EN 15647:2009EN 15647:2009 (E) 5 5.2 zinc oxide of defined quality, CAS number : 1314-13-2 (or an other pigment powder) 6 Apparatus Ordinary apparatus and the following: 6.1 weig
25、hing papers 6.2 250 ml graduated flask for the preparation of the surfactant solution 6.3 measuring cylinder to measure 150 ml of water 6.4 50 ml transfer pipette 6.5 250 ml measuring cylinders with an inner diameter of 3,5 cm 6.6 5 ml transfer pipettes with a good closing peleus ball or piston pipe
26、ttes 6.7 magnetic stirrers 6.8 stirring bars in cross form, length 25 mm, volume 1,5 ml 6.9 drying oven or automatic moisture analyzer 6.10 Petri pan or pan of the automatic moisture analyzer 6.11 analytical balance, accurate to 0,001 g 6.12 pH meter 7 Sampling and preparation of the test sample The
27、 test sample shall be prepared and stored in accordance with ISO 607. 8 Procedure 8.1 Preparation of the surfactant solution (1,500 0,002) g of the surfactant to be tested is weighed into a 250 ml graduated flask. About 100 ml of water are added and the surfactant is dissolved by swirling the liquid
28、. NOTE For surfactants which are hard to dissolve sonification may be used. After the surfactant is completely dissolved the graduated flask is filled up with water to 250 ml. The pH value is determined. The standard cannot be applied, if the pH of the surfactant solution is out of the range from 6
29、to 9. 8.2 Positioning of the cylinder The stirring bar in cross form is put in the 250 ml measuring cylinder. The measuring cylinder is placed on the magnetic stirrer in a way that the stirring bar can rotate freely. The position of the measuring cylinder on the magnetic stirrer is marked. BS EN 156
30、47:2009EN 15647:2009 (E) 6 8.3 Adjustment of the stirrer velocity The stirring speed is determined as follows: 50 ml of the surfactant solution is pipetted into the 250 ml measuring cylinder. The stirring speed of the magnetic stirrer is now adjusted, so that the tip of the conical vortex, which is
31、formed when the stirring speed is increased, just touches the magnetic bar. This stirring speed is never changed during the test. 8.4 Carrying out of the test 8.4.1 (10,00 0,01) g zinc oxide are weighed with a weighing paper and put carefully into a dry 250 ml measuring cylinder. NOTE The use of a s
32、econd weighing paper as a funnel for the cylinder is recommended. 8.4.2 50 ml of the surfactant solution are pipetted into the measuring cylinder. NOTE The flow time of the pipette has to be followed. 8.4.3 The dispersion is stirred for 30 minutes on a magnetic stirrer with the adjusted stirring spe
33、ed accordingly to 8.3. 8.4.4 In a separate measuring cylinder 150 ml of water are measured and added after these 30 minutes of stirring to the zinc oxide dispersion. 8.4.5 The dispersion is stirred for a further 30 minutes with the stirring speed adjusted. 8.4.6 After these 30 minutes the stirring i
34、s stopped and the dispersion is allowed to stand without any disturbance for 3 hours. 8.4.7 After the 3 hours of standing, a 5 ml sample is taken out with a transfer pipette with a hard-closing peleus ball or with a piston pipette exactly at the height of the 150 ml marking of the measuring cylinder
35、. NOTE It is very important that no liquid is soaked up when the pipette crosses the surface of the liquid. A soaking up is avoided by closing the pipette at the top with a good working peleus ball or by the use of a piston pipette. 8.4.8 The weight of the oven-dry 5 ml sample is determined as follo
36、ws: a) by drying the sample on a Petri pan in an oven at 80 C until the weight is constant (deviation 1 mg after 50 seconds) or b) by drying the sample with an automatic moister analyser at a drying temperature of 80 C until the weight difference is less than 1 mg for 50 seconds. If the initial weig
37、ht of the 5 ml sample differs from 5,00 g, the oven-dry mass has to be corrected to correspond to a sample weight of 5,00 g. 9 Calculation and expression of results The degree of dispersion is the value of the oven-dry mass of the 5 ml sample of the dispersion as a percentage of the maximum value. T
38、he maximum value is 0,25 g (10,00 g, divided by the factor 200 ml/5 ml) and is obtained theoretically for a homogeneous dispersion of the zinc oxide. (For the calculation of the maximum value the oven-dry mass of the surfactant is neglected.) BS EN 15647:2009EN 15647:2009 (E) 7 The degree of dispers
39、ion (D), expressed in %, is calculated by the equation (1) : 25,0100D=m(1) where m is the oven-dry mass of the dispersion sample, in grams. At least 3 tests with zinc oxide and a blank test with the surfactant alone shall be done. The resulting values shall be compiled as shown in Table1 and the ave
40、rage calculated: Table 1 Example of Table of results Name of the Surfactant: Test no. Initial weight of the 5 ml sample g oven-dry mass g corrected to a sample weight of 5,00 g oven-dry mass of the dispersion sample minus the oven-dry mass of the blank sample degree of dispersion % 1 2 3 average 10
41、Precision 10.1 Repeatability limit The absolute difference 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 li
42、mit, r, in more than 5 % of cases. Typical precision data obtained in ring tests are given in Annex A. 10.2 Reproducibility limit The absolute difference between two independent single test results, obtained using the same method on identical test material in different laboratories by different oper
43、ators using different equipment, will not exceed the reproducibility limit, R, in more than 5 % of cases. Typical precision data obtained in ring tests are given in Annex A. BS EN 15647:2009EN 15647:2009 (E) 8 11 Test report The test report shall include the following information: a) all information
44、 necessary for the identification of the surfactant tested; b) all information necessary for the complete identification of the zinc oxide (or another pigment powder), like the specific density and the particle size distribution c) the quality of the water used: water hardness, pH and temperature d)
45、 a reference to this European Standard (EN 15647) e) the test results ; f) details of any operation not specified in this European Standard or in the European Standards to which reference is made, and any operations regarded as optional, as well as any incidents like to have affected the results. BS
46、 EN 15647:2009EN 15647:2009 (E) 9 Annex A (informative) Statistical and other data derived from the results of interlaboratory tests The data for the repeatability and reproducibility limits of this method are the results of inter laboratory tests carried out by CESIO (Comit Europen des agents de Su
47、rface et de leurs Intermdiaires Organiques) in 2005 and 2006. The evaluation of the laboratory test was performed in accordance with ISO 5725-2. The tested samples were the following : sample A : Tamol NH 7519; sample B : Baykanol SL. Table A.1 - Interlaboratory test of samples Designation Sample A
48、Sample B Number of participating laboratories 7 8 Number of accepted test results 21 24 Mean value (w) (g/100 g) 80,4 77,5 Repeatability standard deviation (sr) 1,95 1,39 Repeatability coefficient of variation 2,4 % 1,8% Repeatability limit (r) (2,8 x sr) 5,5 3,9 Reproducibility standard deviation (
49、sR) 4,29 2,45 Reproducibility coefficient of variation 5,3 % 3,2% Reproducibility limit, (R) (2,8 x sR) 12,1 6,9 BS EN 15647:2009EN 15647:2009 (E) 10 Bibliography 1 ISO 5725-2, Accuracy (trueness and precision) of measurement methods and results. Part 2: Basic method for the determination of repeatability and reproducibility of a standard measurement method 2 EN ISO 3696, Water for analytical laboratory use Specification and test methods (ISO 3696:1987) BS EN 15647:2009This page has been intentionally left blank
