1、April 2009DEUTSCHE NORM English price group 8No part of this standard 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 71.100.40!$W%_“1520260www
2、.din.deDDIN EN 15647Surface active agents Determination of the dispersing effect of surfactants on powderEnglish version of DIN EN 15647:2009-04Grenzflchenaktive Stoffe Bestimmung der Dispersionswirkung von Tensiden auf PulverEnglische Fassung DIN EN 15647:2009-04www.beuth.deDocument comprises 12 pa
3、gesDIN EN 15647:2009-04 2 National foreword This standard has been prepared by Technical Committee CEN/TC 276 “Surface active agents” (Secretariat: AFNOR, France). The responsible German body involved in its preparation was the Normenausschuss Materialprfung (Materials Testing Standards Committee),
4、Technical Committee NA 062-05-63 AA Anwendungstechnische Prfverfahren fr Tenside. The DIN Standards corresponding to the International Standards referred to in this document are as follows: EN ISO 3696 DIN ISO 3696 ISO 607 DIN ISO 607 ISO 5725-2 DIN ISO 5725-2 National Annex NA (informative) Bibliog
5、raphy DIN ISO 607, Surface active agents and detergents Methods of sample division DIN ISO 3696, Water for analytical laboratory use Specification and test methods DIN ISO 5725-2, Accuracy (trueness and precision) of measurement methods and results Part 2: Basic method for the determination of repea
6、tability and reproducibility of a standard measurement method EUROPEAN 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 dispersion
7、des 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 Euro
8、peanStandard 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,
9、 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 Management Centre has the same status as theofficial versions.CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Cypru
10、s, 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 E
11、UROPEN 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: EEN 15647:2009 (E) 2 Contents Page Foreword 3 1 Scope 4 2 No
12、rmative 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 out of the t
13、est .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 DIN EN 15647:2009-04 EN 15647:2009 (E) 3
14、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, at the
15、 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 or all su
16、ch 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, Iceland
17、, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and the United Kingdom. DIN EN 15647:2009-04 EN 15647:2009 (E) 4 1 Scope This European Standard specifies a method for the determination of the effec
18、tiveness 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 following
19、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 sample
20、 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 de
21、termined 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 cy
22、linder 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 hours,
23、 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 obtained
24、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 form
25、ed. 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 have
26、been checked in advance as to not interfere with the analytical results. 5.1 water of defined hardness and pH value DIN EN 15647:2009-04 EN 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 we
27、ighing 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 pi
28、pettes 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 T
29、he 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 liqu
30、id. 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
31、6 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. DIN EN
32、15647:2009-04 EN 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, wh
33、ich is 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
34、 of a second 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 stirr
35、ing speed 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 sti
36、rring is 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 c
37、ylinder. 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 a
38、s follows: 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 initi
39、al weight 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 v
40、alue. The 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.) DIN EN 15647:2009-04 EN 15647:2009 (E) 7 The degre
41、e of dispersion (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
42、 and the average 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
43、 average 10 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 repe
44、atability limit, 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 di
45、fferent operators 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. DIN EN 15647:2009-04 EN 15647:2009 (E) 8 11 Test report The test report shall include the following information: a
46、) all information 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 a
47、nd temperature d) 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 affecte
48、d the results. DIN EN 15647:2009-04 EN 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 Eu
49、ropen des agents de Surface 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 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% Rep
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