BS EN ISO 7579-2009 Dyestuffs - Determination of solubility in organic solvents - Gravimetric and photometric methods《颜料 在有机溶剂中溶解度的测定 重量法和光度测定法》.pdf

1、BS EN ISO7579:2009ICS 87.060.10NO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAWBRITISH STANDARDDyestuffs Determinationof solubility inorganic solvents Gravimetric andphotometric methods(ISO 7579:2009)This British Standard was published under the authority of the Standards Polic

2、y and Strategy Committee on 30 November 2009. BSI 2009ISBN 978 0 580 62859 7Amendments/corrigenda issued since publicationDate CommentsBS EN ISO 7579:2009National forewordThis British Standard is the UK implementation of EN ISO 7579:2009. It supersedes BS EN ISO 7579:1997 which is withdrawn.The UK p

3、articipation in its preparation was entrusted to TechnicalCommittee STI/1, Pigments.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 c

4、orrect application. Compliance with a British Standard cannot confer immunityfrom legal obligations.EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN ISO 7579 October 2009 ICS 87.060.10 Supersedes EN ISO 7579:1996English Version Dyestuffs - Determination of solubility in organic solvents - Gravim

5、etric 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 photometrisches Verfahren (ISO 7579:2009)

6、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-to-date lists and bibliographical refe

7、rences 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 under the responsibility of a CEN member

8、 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, Greece, Hungary, Iceland, Ireland, Italy, La

9、tvia, 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 Management Centre: Avenue Marnix 17, B-1000 Brus

10、sels 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: EBS EN ISO 7579:2009EN ISO 7579:2009 (E) 3 Foreword This document (EN ISO 7579:2009) has been prepared by Technical Committee ISO/TC 35 “Paints and varnishes“

11、 in collaboration with Technical Committee CEN/TC 298 “Pigments and extenders” the secretariat of which is held by DIN. 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 2010, and conflicting

12、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 responsible for identifying any or all such patent rights. This document super

13、sedes 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 Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, I

14、celand, 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 been approved by CEN as a EN ISO 7579:2009 without any modification. B

15、S EN ISO 7579:2009ISO 7579:2009(E) ISO 2009 All rights reserved iiiContents Page Foreword iv Introduction.v 1 Scope1 2 Normative references1 3 Terms and definitions .1 4 Principle .1 5 Solvent2 6 Apparatus.2 7 Sampling 2 8 Procedure.3 9 Test report8 Annex A (normative) Solubility calculations9 BS EN

16、 ISO 7579:2009ISO 7579:2009(E) iv ISO 2009 All rights reservedForeword ISO (the International Organization for Standardization) is a worldwide federation of national standards bodies (ISO member bodies). The work of preparing International Standards is normally carried out through ISO technical comm

17、ittees. Each member body interested in a subject for which a technical committee has been established has the right to be represented on that committee. International organizations, governmental and non-governmental, in liaison with ISO, also take part in the work. ISO collaborates closely with the

18、International Electrotechnical Commission (IEC) on all matters of electrotechnical standardization. International Standards are drafted in accordance with the rules given in the ISO/IEC Directives, Part 2. The main task of technical committees is to prepare International Standards. Draft Internation

19、al Standards adopted by the technical committees are circulated to the member bodies for voting. Publication as an International Standard requires approval by at least 75 % of the member bodies casting a vote. Attention is drawn to the possibility that some of the elements of this document may be th

20、e subject of patent rights. ISO shall not be held responsible for identifying any or all such patent rights. ISO 7579 was prepared by Technical Committee ISO/TC 35, Paints and varnishes, Subcommittee SC 2, Pigments and extenders. This second edition cancels and replaces the first edition (ISO 7579:1

21、990), in which the mixing time has been reduced from 24 h to 3 h but the temperature has been increased from 105 C to 150 C, Method B and Annex B have been deleted and a photometric test method has been added. BS EN ISO 7579:2009ISO 7579:2009(E) ISO 2009 All rights reserved vIntroduction Many dyestu

22、ffs 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 dyestuff in the solvent. In some cases, however,

23、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. BS EN ISO 7579:2009BS EN ISO 7579:2009INTE

24、RNATIONAL STANDARD ISO 7579:2009(E) ISO 2009 All rights reserved 1Dyestuffs Determination of solubility in organic solvents Gravimetric and photometric methods 1 Scope This International Standard specifies two methods for determining the solubility of dyestuffs in organic solvents. They are applicab

25、le to dyestuffs that do not change chemically under the influence of the solvent and are stable and non-volatile 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 basi

26、s. The methods are suitable for concentrations between 1 g and 1 000 g of dyestuff per litre of solvent. Higher 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 mat

27、ter in a dyestuff. 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 of the referenced document (including any amendments) applies. ISO 787

28、-2, General methods of test for pigments and extenders Part 2: Determination of matter volatile at 105 C ISO 2811-1, 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 th

29、e purposes of this document, the following terms and definitions apply. 3.1 solubility maximum mass of a dyestuff 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 betw

30、een “true” solubility and “colloidal” solubility. 4 Principle Different amounts of the dyestuff are each dispersed 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 ph

31、otometric measurements. BS EN ISO 7579:2009ISO 7579:2009(E) 2 ISO 2009 All rights reservedWhen using the gravimetric procedure, the 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

32、dyestuff which dissolves is assessed by determination of the light absorbance compared to that of a standard solution. 5 Solvent When using the gravimetric procedure, the organic solvent used shall be completely volatile at a temperature below the temperature of decomposition of the dyestuff. The de

33、nsity 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 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 (inclu

34、ding the type and quantity of any major secondary constituents) shall be given in the test report. With solvents having a boiling 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

35、,000 1 g. 6.2 Weighing bottles, squat form, with stoppers. 6.3 Containers, cylindrical, of capacity about 50 ml, of inert material, 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

36、 2 ml and 5 ml. 6.7 Mechanical shaker, with speed control and, preferably, a cooling unit. 6.8 Laboratory centrifuge, capable of imparting 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 t

37、ransparent and inert material, with tightly fitting lids. 6.10 Drying oven, with air circulation and temperature control up to 150 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. BS EN IS

38、O 7579:2009ISO 7579:2009(E) ISO 2009 All rights reserved 38 Procedure 8.1 Preliminary determination If the approximate solubility of the dyestuff in 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

39、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, 500 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

40、undissolved matter after centrifuging is greater than about one-quarter of the total quantity of dyestuff dispersed. 8.2 Preparation of test solutions 8.2.1 When the approximate solubility of the dyestuff is known or has been determined in the preliminary determination, carry out the following proce

41、dure. Prepare six suspensions by taking test portions of the dyestuff to give concentrations of about 40 %, 60 %, 80 %, 100 %, 120 % and 140 % (by mass) 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 dyes

42、tuff remains undissolved, reduce the concentration until more than 90 % of the dyestuff is dissolved. If, at the highest concentration, the residue is 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 increas

43、e 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 amount 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 so

44、lvent. 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 shaker 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 centrif

45、uge 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 observing 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

46、 supernatant liquid from each tube into a clean, dry container (6.3) and close securely. 8.3 Gravimetric determination of the concentration of the dissolved 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 th

47、e 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 contain 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

48、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 bottle (6.2), insert the stopper and weigh (m0). Remove the stopper, place the weighing bottle in the oven (6.10) maintained at a BS EN ISO 7579:2009ISO 757

49、9:2009(E) 4 ISO 2009 All rights reservedtemperature about 10 C below the boiling point of the solvent and leave in the oven until most of the solvent has evaporated (this 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 ex