BS-2782-PART-7-METHOD-732D-1991 ISO-1628-4-1986.pdf

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1、BRITISH STANDARD BS 2782-7: Method 732D: 1991 ISO 1628-4: 1986 Methods of testing Plastics Part 7: Rheological properties Method 732D: Determination of viscosity number of polycarbonate moulding and extrusion materials IMPORTANT NOTE. Before reading this method it is essential to read BS 2782-0, Int

2、roduction, issued separately. Licensed Copy: London South Bank University, London South Bank University, Tue Dec 12 09:01:31 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS 2782-7:Method 732D:1991 This British Standard, having been prepared under the direction of the Plastics and Rubber Standards Poli

3、cy Committee, was published under the authority of the Standards Board and comes into effect on 28 June 1991 BSI 12-1999 The following BSI references relate to the work on this standard: Committee reference PRM/21 Draft announced in BSI News, July 1991 ISBN 0 580 19772 7 Committees responsible for t

4、his British Standard The preparation of this British Standard was entrusted by the Plastics and Rubber Standards Policy Committee (PRM/-) to Technical Committee PRM/21, upon which the following bodies were represented: British Plastics Federation British Steel Industry British Telecommunications plc

5、 British Textile Confederation Department of Trade and Industry (National Physical Laboratory) EEA (the Association of Electronics, Telecommunications and Business Equipment Industries) Electrical and Electronic Insulation Association (BEAMA Ltd.) Electrical Installation Equipment Manufacturers Asso

6、ciation (BEAMA Ltd.) GAMBICA (BEAMA Ltd.) Ministry of Defence Packaging and Industrial Films Association PIRA Plastic Industrial Containers Association Plastics and Rubber Institute RAPRA Technology Ltd. Standards Association of Australia Yarsley Technical Centre Ltd. Amendments issued since publica

7、tion Amd. No.DateComments Licensed Copy: London South Bank University, London South Bank University, Tue Dec 12 09:01:31 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS 2782-7:Method 732D:1991 BSI 12-1999i Contents Page Committees responsibleInside front cover National forewordii 1Scope and field of a

8、pplication1 2References1 3Definitions and units1 4Measurements1 5Apparatus1 6Solvent and solution2 7Temperature of measurement2 8Procedure2 9Expression of results2 10Test report3 Annex A Calibration procedures4 Figure 15 Figure 26 Publication(s) referred toInside back cover Licensed Copy: London Sou

9、th Bank University, London South Bank University, Tue Dec 12 09:01:31 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS 2782-7:Method 732D:1991 ii BSI 12-1999 National foreword This British Standard has been prepared under the direction of the Plastics and Rubber Standards Policy Committee and is identi

10、cal with ISO 1628-4:1986 “Plastics Determination of viscosity number and limiting viscosity number Part 4: Polycarbonate (PC) moulding and extrusion materials”, published by the International Organization for Standardization (ISO). The Technical Committee has reviewed the provisions of ISO 3105:1976

11、 and ISO 7391-1:1987, to which reference is made in the text, and has decided that they are acceptable for use in conjunction with this standard. WARNING NOTE. This British Standard, which is identical with ISO 1628-4, does not necessarily detail all the precautions necessary to meet the requirement

12、s of the Health and Safety at Work etc. Act 1974. Attention should be paid to any appropriate safety precautions and the method should be operated only by trained personnel. A British Standard does not purport to include all the necessary provisions of a contract. Users of British Standards are resp

13、onsible for their correct application. Compliance with a British Standard does not of itself confer immunity from legal obligations. Cross-references International StandardCorresponding British Standard ISO 1628-1:1984BS 2782 Methods of testing plastics Method 732A:1991 Determination of viscosity nu

14、mber: general conditions (Identical) ISO 4793:1980BS 1752:1983 Specification for laboratory sintered or fritted filters including porosity grading (Identical) Summary of pages This document comprises a front cover, an inside front cover, pages i and ii, pages 1 to 6, an inside back cover and a back

15、cover. This standard has been updated (see copyright date) and may have had amendments incorporated. This will be indicated in the amendment table on the inside front cover. Licensed Copy: London South Bank University, London South Bank University, Tue Dec 12 09:01:31 GMT+00:00 2006, Uncontrolled Co

16、py, (c) BSI BS 2782-7:Method 732D:1991 BSI 12-19991 1 Scope and field of application This part of ISO 1628 defines particular conditions for determination of the viscosity number of polycarbonate moulding and extrusion materials in dilute solution. It applies to polycarbonate homopolymers and copoly

17、mers and mixtures of the two, with and without filler, as defined in ISO 7391-1. 2 References ISO 1628-1, Plastics Guidelines for the standardization of methods for the determination of viscosity number and limiting viscosity number of polymers in dilute solution Part 1: General conditions. ISO 3105

18、, Glass capillary kinematic viscosimeters Specification and operating instructions. ISO 4793, Laboratory sintered (fritted) filters Porosity grading, classification and designation. ISO 7391, Plastics Polycarbonate (PC) moulding and extrusion materials Part 1: Designation Part 2: Preparation of test

19、 specimens and determination of properties. 3 Definitions and units (see ISO 1628-1, clause 3) viscosity number, V.N. expressed in millilitres per gram, where is the dynamic viscosity, in pascal seconds, of the solution; 0is the dynamic viscosity, in pascal seconds, of the solvent; is the density, i

20、n kilograms per cubic metre, of the solution; 0is the density, in kilograms per cubic metre, of the solvent; is the kinematic viscosity, in metres squared per second, of the solution; is the kinematic viscosity, in metres squared per second, of the solvent; cis the concentration, in grams per millil

21、itre, of polycarbonate in the solution. NOTEBecause of the small differences between the densities of the solution and solvent, may be replaced by in the formula for V.N. 4 Measurements (see ISO 1628-1, clause 4) where kis a constant of the viscometer, in millimetres squared per second squared; tis

22、the efflux time, in seconds; is the kinetic energy correction time, in seconds; is the density, in grams per cubic millimetre. NOTEContrary to the instruction in ISO 1628-1, clause 4, the kinetic energy correction time t may be neglected only if it is less than 0,2 % of t. 5 Apparatus (see ISO 1628-

23、1, clause 5) 5.1 Capillary viscometer, suspended-level Ubbelohde type OC, with capillary diameter of 0,36 mm and measuring bulb volume of 2 ml, according to ISO 3105. Any other viscometer listed in ISO 3105 may be used, provided that it gives equivalent results to the specified viscometer, which sha

24、ll be used for reference in case of dispute. The calibration of the viscometer used shall be checked according to the method given in the annex, clause A.1. 5.2 Timing-device, which can be read to the nearest 0,1 s and has a rate constant to 0,1 % over 15 min. 5.3 Thermostatic bath, capable of being

25、 maintained at 25 0,05 C. 5.4 One-mark volumetric flask, of capacity 100 ml, provided with a ground glass stopper. 5.5 Balance, accurate to 0,1 mg. 5.6 Drying cabinet, capable of being maintained at 110 C. 5.7 Petri dishes 5.8 Glass filter crucibles, grade P 1,6 (see ISO 4793). 5.9 Glass filter cruc

26、ibles, grade P 4 (see ISO 4793). 5.10 Diatomaceous filter aid material 5.11 Shaking machine 5.12 Centrifuge -= 0 0 0 -= t A kt - -= Licensed Copy: London South Bank University, London South Bank University, Tue Dec 12 09:01:31 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS 2782-7:Method 732D:1991 2 B

27、SI 12-1999 6 Solvent and solution (see also ISO 1628-1, clause 6) 6.1 Solvent Dichloromethane, redistilled, boiling range 39 to 41 C, refractive index within the range of 1,423 to 1,425. 6.2 Sampling The sample shall be representative of the material under test. 6.3 Solution concentration The concen

28、tration shall be 5 g of resin per litre of solution. 6.4 Preparation of solution 6.4.1 PC material without fillers Weigh, to the nearest 0,1 mg, 0,5 0,01 g of the sample, into the one-mark volumetric flask (5.4). Add 70 ml of the dichloromethane (6.1) and dissolve the sample with agitation. Then dil

29、ute to the mark with dichloromethane at 20 1 C or weigh in as much solvent as is necessary to reach the concentration of 0,5 g/100 ml, and briefly agitate again. For pigmented materials and/or materials containing special additives, the quantity weighed into the one-mark volumetric flask shall be in

30、creased so that the solution will contain 0,5 g PC per 100 ml (see the notes). NOTE 1This correction is necessary for a pigment or additive content greater than 0,5 % (m/m) in most cases the pigment content is below 0,5 % (m/m). Dissolved dyestuffs and pigments under 0,5 % (m/m) will not interfere w

31、ith the measurement. NOTE 2To prevent contamination of the capillary in the case of solutions with higher pigment contents, it may be advisable to handle those materials as given under 6.4.2. To remove the additives, the diatomaceous filter aid material (5.10) or the centrifuge (5.12) may be used. 6

32、.4.2 PC materials with fillers Dissolve approximately 5 g of the sample in approximately 70 ml of the dichloromethane (6.1) in a round-bottomed flask with continuous stirring. To ensure complete dissolution, the material may be ground into fine particles. When the filler, for example glass fibre, ha

33、s settled, filter the solution through a grade P 4 glass filter crucible (5.9) into Petri dishes (5.7). Evaporate the dichloromethane under a fume hood and dry the resulting films in the drying cabinet (5.6) at 110 C to constant mass (1 to 10 h, depending on film thickness). Prepare a solution of th

34、e dried film in accordance with 6.4.1. 7 Temperature of measurement The temperature shall be 25 0,05 C. 8 Procedure (see clause 3 and ISO 1628-1, clause 8) Introduce the dichloromethane solvent into the viscometer (5.1) using the glass filter crucible grade P 1,6 (5.8). Determine the efflux times of

35、 the solvent at 25 0,05 C in three to five passes through the same viscometer. The range of efflux times shall not exceed 0,01 %. Repeat the procedure with the test solution. 9 Expression of results (see ISO 1628-1, clause 9) Calculate the viscosity number, expressed in millilitres per gram, a) by t

36、he method given in the annex, clause A.3, or b) by means of the following equation: where is the kinematic viscosity of the solution, in metres squared per second; 0is the kinematic viscosity of the solvent, in metres squared per second; tis the arithmetic mean of the readings obtained for the efflu

37、x time, in seconds, of the solution; t0is the arithmetic mean of the readings obtained for the efflux time, in seconds, of the solvent; cis the concentration, in grams per millilitre, of the solution; tis the kinetic energy correction time for t as given by the manufacturer of the viscometer, in sec

38、onds; t0is the kinetic energy correction time for t0 as given by the manufacturer of the viscometer, in seconds. NOTEThis equation is in accordance with ISO 1628-1, but introduces the kinetic energy correction time. This is necessary in order to obtain accurate results with the viscometer size speci

39、fied. Licensed Copy: London South Bank University, London South Bank University, Tue Dec 12 09:01:31 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS 2782-7:Method 732D:1991 BSI 12-19993 Equation (10) for the viscosity number given in ISO 1628-1 can be used to give results of similar accuracy if a visc

40、ometer with a suitable smaller capillary diameter is used so that the kinetic energy correction time is less than 0,2 % of the efflux time. To verify the kinetic energy correction times t and t0, see the annex, clauses A.1 and A.2, respectively. 10 Test report See ISO 1628-1, clause 10. Licensed Cop

41、y: London South Bank University, London South Bank University, Tue Dec 12 09:01:31 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS 2782-7:Method 732D:1991 4 BSI 12-1999 Annex A Calibration procedures (This annex forms an integral part of the Standard.) A.1 Verification of the accuracy of the viscomete

42、r Experience has shown that the required high accuracy of viscosity number determination of PC solutions cannot always be achieved with commercially available Ubbelohde viscometers because of small irregularities of the capillary. It is therefore advisable to check the accuracy of measurement with t

43、he help of calibrating liquids of known kinematic viscosity. The following liquids are recommended1): Determine the kinetic energy corrected efflux time of these liquids at 25 0,05 C in three to five passes through the viscometer to be used. The range of efflux times shall not exceed 0,1 %. Calculat

44、e the viscosity ratios according to clause 9 as and Comparing these values with the “true” values and the deviation should be less than 0,4 %. A.2 Determination of effective capillary constant keff and kinetic energy correction teff If the deviation between the expected and the measured viscosity ra

45、tio of the calibrating liquids is more than 0,4 %, the effective capillary constant keff and the kinetic energy correction time ti,eff may be determined by the following method. Calculate keff of the viscometer used as the arithmetic mean of three equations 0 Dichloromethane (analytical purity) 0, 2

46、5,00 C = 0,314 2 mm2/s 0, 25,00 C = 1,316 3 g/ml 1 Trichloroethylene (analytical purity) 1, 25,00 C = 0,369 3 mm2/s 1, 25,00 C = 1,455 5 g/ml 2 Tetrachloroethylene (analytical purity) 2, 25,00 C = 0,525 7 mm2/s 2, 25,00 C = 1,614 4 g/ml 1) BAUER, H. and MEERLENDER, G. Newtonian reference materials w

47、ith 1 mm2/s and their application in extending the range of capillary viscometers, Rheol. Acta 21 (1982), pp. 499501. Licensed Copy: London South Bank University, London South Bank University, Tue Dec 12 09:01:31 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS 2782-7:Method 732D:1991 BSI 12-19995 wher

48、e iis the kinematic viscosity of the calibrating liquids (0, 1 or 2 respectively) mentioned in clause A.1; tiis the corresponding efflux time; tiis the kinetic energy correction time for ti as given by the manufacturer of the viscometer. Calculate and plot the resulting ti,eff values against the cor

49、responding efflux times, as in Figure 1. The appropriate ti corresponding to a certain ti can be determined by interpolation from this plot. A.3 Simplified calibration method The correlation of efflux time versus viscosity ratio of viscometers not meeting the requirement of clause A.1 may be directly determined with the help of the calibrating liquids. This calibration is independent of a knowledge of capillary constant and kinetic energy correction. For the particular