1、March 2010 Translation by DIN-Sprachendienst.English price group 10No 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
2、87.060.10!$a.=“1621126www.din.deDDIN EN ISO 7579Dyestuffs Determination of solubility in organic solvents Gravimetric and photometric methods (ISO 7579:2009)English translation of DIN EN ISO 7579:2010-03Farbstoffe Bestimmung der Lslichkeit in organischen Lsemitteln Gravimetrisches und photometrische
3、s Verfahren (ISO 7579:2009)Englische bersetzung von DIN EN ISO 7579:2010-03Colorants Dtermination de la solubilit dans les solvants organiques Mthodes gravimtrique et photomtrique (ISO 7579:2009)Traduction anglaise de DIN EN ISO 7579:2010-03SupersedesDIN EN ISO 7579:1996-11www.beuth.deIn case of dou
4、bt, the German-language original shall be considered authoritative.Document comprises 17 pages03.10 DIN EN ISO 7579:2010-03 2 A comma is used as the decimal marker. National foreword This standard has been prepared by Technical Committee ISO/TC 35/SC 2 “Pigments and extenders” (Secre-tariat: DIN, Ge
5、rmany) in collaboration with Technical Committee CEN/TC 298 “Pigments and extenders” (Secretariat: DIN, Germany). The responsible German body involved in its preparation was the Normenausschuss Pigmente und Fllstoffe (Pigments and Extenders Standards Committee), Working Committee NA 078-00-21 AA Far
6、bmittel in Anstrichstoffen und Druckfarben, NA 078-00-21-3 AK Farbstoffe. The DIN Standards corresponding to the International Standards referred to in this document are as follows: ISO 787-2 DIN EN ISO 787-2 ISO 2811-1 DIN EN ISO 2811-1 ISO 15528 DIN EN ISO 15528 Amendments This standard differs fr
7、om DIN EN ISO 7579:1996-11 as follows: a) The dispersing time has been reduced from 24 h to 3 h while at the same time increasing the tempera-ture from 105 C to 150 C. b) Method B and Annex B have been deleted. c) The photometric method has been added. d) The normative references have been updated a
8、nd the content editorially revised. Previous editions DIN 5976: 1975-08 DIN EN ISO 7579:1996-11 National Annex NA (informative) Bibliography DIN EN ISO 787-2, General methods of test for pigments and extenders Part 2: Determination of matter volatile at 105 C DIN EN ISO 2811-1, Paints and varnishes
9、Determination of density Part 1: Pyknometer method DIN EN ISO 15528, Paints, varnishes and raw materials for paints and varnishes Sampling EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN ISO 7579 October 2009 ICS 87.060.10 Supersedes EN ISO 7579:1996English Version Dyestuffs - Determination of
10、solubility in organic solvents - Gravimetric and photometric methods (ISO 7579:2009) Colorants - Dtermination de la solubilit dans les solvants organiques - Mthodes gravimtrique et photomtrique (ISO 7579:2009) Farbstoffe - Bestimmung der Lslichkeit in organischen Lsemitteln - Gravimetrisches und pho
11、tometrisches Verfahren (ISO 7579:2009) This European Standard was approved by CEN on 5 October 2009. CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this European Standard the status of a national standard without any alteration. Up
12、-to-date lists and bibliographical references concerning such national standards 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 version in any other language made by translation u
13、nder the responsibility of a CEN member into its own language and notified to the CEN Management Centre has the same status as the official versions. CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greec
14、e, 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 COMIT EUROPEN DE NORMALISATION EUROPISCHES KOMITEE FR NORMUNG Managemen
15、t Centre: Avenue Marnix 17, B-1000 Brussels 2009 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN ISO 7579:2009: EContents DIN EN ISO 7579:2010-03 EN ISO 7579:2009 (E) 2 Page Foreword .3 Introduction.4 1 Scope5 2 Normative reference
16、s5 3 Terms and definitions .5 4 Principle .5 5 Solvent6 6 Apparatus.6 7 Sampling 6 8 Procedure.7 9 Test report12 Annex A (normative) Solubility calculations13 Foreword which is held by DIN. This European Standard shall be given the status of a national standard, either by publication of an identical
17、 text or by endorsement, at the latest by April 2010, and conflicting national standards shall be withdrawn at the latest by April 2010. 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 responsi
18、ble for identifying any or all such patent rights. This document supersedes EN ISO 7579:1996. 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 Re
19、public, 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 United Kingdom. Endorsement notice The text of ISO 7579:2009 has
20、been approved by CEN as a EN ISO 7579:2009 without any modification. varnishes” in collaboration with Technical Committee CEN/TC 298 “Pigments and extenders” the secretariat of This document (EN ISO 7579:2009) has been prepared by Technical Committee ISO/TC 35 “Paints and DIN EN ISO 7579:2010-03 EN
21、ISO 7579:2009 (E) 3 Introduction Many dyestuffs are soluble in a solvent to an extent which is independent of the amount of dyestuff present in the solvent, as long as excess dyestuff is present. This concentration is defined as the saturation concentration and represents the solubility of the dyest
22、uff in the solvent. In some cases, however, there is no fixed saturation concentration and the amount of dyestuff which dissolves increases with the amount of dyestuff added. A gravimetric and a photometric procedure to assess the solubility of these dyes are described in this International Standard
23、. DIN EN ISO 7579:2010-03 EN ISO 7579:2009 (E) 4 1 Scope This International Standard specifies two methods for determining the solubility of dyestuffs in organic solvents. They are applicable to dyestuffs that do not change chemically under the influence of the solvent and are stable and non-volatil
24、e under the specified drying conditions. For volatile solvents (boiling point 120 C), the photometric procedure is recommended. The choice of procedure should be made on a case-by-case basis. The methods are suitable for concentrations between 1 g and 1 000 g of dyestuff per litre of solvent. Higher
25、 concentrations can be used provided the viscosity of the solution is such that the procedure can be carried out readily. The methods are not suitable for the determination of insoluble matter in a dyestuff. 2 Normative references The following referenced documents are indispensable for the applicat
26、ion 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 787-2, General methods of test for pigments and extenders Part 2: Determination of matter volatile at 105 C ISO 28
27、11-1, Paints and varnishes Determination of density Part 1: Pyknometer method ISO 15528, Paints, varnishes and raw materials for paints and varnishes Sampling 3 Terms and definitions For the purposes of this document, the following terms and definitions apply. 3.1 solubility maximum mass of a dyestu
28、ff that is soluble in a given volume of a particular solvent under specified conditions NOTE Solubility is expressed in grams per litre of solvent (see Annex A). No distinction is made between “true” solubility and “colloidal” solubility. 4 Principle Different amounts of the dyestuff are each disper
29、sed in a defined volume of a solvent at 23 C. After mixing for 3 h, each dispersion is centrifuged and the solids content of the supernatant liquid is determined by either gravimetric or photometric measurements. DIN EN ISO 7579:2010-03 EN ISO 7579:2009 (E) 5 When using the gravimetric procedure, th
30、e amount of dyestuff which dissolves is assessed by determination of the non-volatile-matter content of the solution. When using the photometric procedure, the amount of dyestuff which dissolves is assessed by determination of the light absorbance compared to that of a standard solution. 5 Solvent W
31、hen using the gravimetric procedure, the organic solvent used shall be completely volatile at a temperature below the temperature of decomposition of the dyestuff. The density of the solvent at 23 C shall be known. The density of the solvent can be determined by the method described in ISO 2811-1 at
32、 23 C using a glass pyknometer. The dyestuff shall not react chemically with the solvent. As organic solvents are normally not chemically pure, the grade of purity (including the type and quantity of any major secondary constituents) shall be given in the test report. With solvents having a boiling
33、point above 120 C, the photometric method is recommended. 6 Apparatus Ordinary laboratory apparatus and glassware, together with the following: 6.1 Balance, accurate to 0,000 1 g. 6.2 Weighing bottles, squat form, with stoppers. 6.3 Containers, cylindrical, of capacity about 50 ml, of inert material
34、, with tightly fitting lids. 6.4 Pipette, capacity 20 ml (tolerance: 0,03 ml). 6.5 Volumetric flask, capacity 100 ml (tolerance: 0,5 ml). 6.6 Injection syringes, capacity 2 ml and 5 ml. 6.7 Mechanical shaker, with speed control and, preferably, a cooling unit. 6.8 Laboratory centrifuge, capable of i
35、mparting a relative centrifugal acceleration of about 10 km/s2. A centrifuge with a rotational frequency of 2 000 min1to 3 000 min1is suitable. 6.9 Centrifuge tubes, of transparent and inert material, with tightly fitting lids. 6.10 Drying oven, with air circulation and temperature control up to 150
36、 C (tolerance 2 C). 6.11 Spectrophotometer. 6.12 Ultrasonic bath. 7 Sampling Take a representative sample of the product to be tested, as described in ISO 15528. DIN EN ISO 7579:2010-03 EN ISO 7579:2009 (E) 6 8 Procedure 8.1 Preliminary determination If the approximate solubility of the dyestuff in
37、the solvent is not known, carry out a preliminary determination, using the procedure described in 8.2.2 and 8.2.3, with one of the following series of test portions of the dyestuff: dyestuff of low solubility: 1 g, 10 g and 50 g of dyestuff per litre of solvent; dyestuff of high solubility: 100 g, 5
38、00 g and 1 000 g of dyestuff per litre of solvent. Take as the approximate solubility of the dyestuff the concentration of the dispersion in which the undissolved matter after centrifuging is greater than about one-quarter of the total quantity of dyestuff dispersed. 8.2 Preparation of test solution
39、s 8.2.1 When the approximate solubility of the dyestuff is known or has been determined in the preliminary determination, carry out the following procedure. Prepare six suspensions by taking test portions of the dyestuff to give concentrations of about 40 %, 60 %, 80 %, 100 %, 120 % and 140 % (by ma
40、ss) of the approximate solubility, using the procedure described in 8.2.2 and 8.2.3. If, at the lowest concentration employed, 10 % or more of the dyestuff remains undissolved, reduce the concentration until more than 90 % of the dyestuff is dissolved. If, at the highest concentration, the residue i
41、s less than 25 % of the test portion, then increase the mass of the test portion. If the solubility limit cannot be obtained because of a large increase in viscosity with increasing amount of the test portion, the last value obtained shall be recorded (see Clause A.4.) 8.2.2 Place the required amoun
42、t of dyestuff in a container (6.3) and add exactly 20 ml of the solvent, using the pipette (6.4). Close the container immediately to prevent loss of solvent. Shake the container using a mechanical shaker (6.7) at (23 2) C for 3 h. Check that no significant agglomerates are visible. If an orbital sha
43、ker is used, this shall be stated in the test report. 8.2.3 After shaking the dyestuff and solvent for 3 h, place portions of the suspension in centrifuge tubes (6.9) and cap each tube. Centrifuge the tubes at (23 2) C for 10 min. Check whether the supernatant liquid is clear, for instance by observ
44、ing whether the supernatant liquid flows smoothly from a pipette tube dipped into it; if not, or if in doubt, centrifuge for another 10 min. Decant the supernatant liquid from each tube into a clean, dry container (6.3) and close securely. 8.3 Gravimetric determination of the concentration of the di
45、ssolved dyestuff 8.3.1 General Take a known amount of the supernatant liquid prepared in 8.2.3 and determine the concentration of the dyestuff using the method described in 8.3.2. Carry out the weighings to the nearest 0,2 mg. For each determination, the amount of supernatant liquid taken shall cont
46、ain at least 30 mg of the dyestuff. Two determinations on each supernatant liquid shall be carried out. The mean values shall be recorded and used for the calculation as given in 8.3.4. 8.3.2 Procedure Place a portion (about 3 g) of the clear supernatant liquid into a previously tared weighing bottl
47、e (6.2), insert the stopper and weigh (m0). Remove the stopper, place the weighing bottle in the oven (6.10) maintained at a DIN EN ISO 7579:2010-03 EN ISO 7579:2009 (E) 7 temperature about 10 C below the boiling point of the solvent and leave in the oven until most of the solvent has evaporated (th
48、is will normally take about 1 h). Increase the drying temperature to about 30 C below the decomposition temperature of the dyestuff and continue drying for a further 3 h. NOTE Most metal-complex dyestuffs can be dried at a temperature of 150 C. If the drying temperature is not at least 50 C above the boiling point of the solvent, either extend the drying time or remove the last traces of solvent in a vacuum oven. In such cases, there shall, however, be no loss of dyestuff by sublimation. On c
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