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SOLVAY DSC GELATION MEASUREMENT : INFLUENCE OF PIPE FORMULATION ON RESULT Joël Fumire Research & Technology SBU Vinyls São Paulo, 2005.

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Presentation on theme: "SOLVAY DSC GELATION MEASUREMENT : INFLUENCE OF PIPE FORMULATION ON RESULT Joël Fumire Research & Technology SBU Vinyls São Paulo, 2005."— Presentation transcript:

1 SOLVAY DSC GELATION MEASUREMENT : INFLUENCE OF PIPE FORMULATION ON RESULT Joël Fumire Research & Technology SBU Vinyls São Paulo, 2005

2 SOLVAY Introduction Considering the fact that … The level of gelation of PVC determines the mechanical properties of the finished item The level of gelation has a significant influence on subsequent processing (biorientation or corrugation)  A few methods exist since a long time : MCT, SEM homogeneity, short die melt rheology, etc… none of them was considered as totally satisfactory.

3 SOLVAY Introduction Considering the fact that … The measurement by DSC method seems to realise a good compromise between accuracy, universal application and cost  But : some authors found limitations to the application of the method related to the composition of the item THIS IS THE REASON FOR OUR INVESTIGATION

4 SOLVAY DSC measurement Apparatus : DSC TA 2920 from TA Instruments Operating instruction : 20 mg of sample in Al capsule, Heating speed : 20°K/min measurement range : 50 to 220 °C (conventionnally)

5 SOLVAY DSC measurement Endotherm A is the endotherm after Tg and up to the minimum at Tm (processing temperature) Endotherm B is taken from this Tm up to 220 °C (conventionnaly) Gelation level is calculated as : G = A / (A + B) A DSC Temperature mW Heat Flow A-onset B-onset Tg B

6 SOLVAY DSC measurement This method is not yet an international standard Standardisation group ISO TC138/SC5/WG2 is working on this topic with designation : ISO The operation instruction adopted in this work is close to the existing draft

7 SOLVAY Parameters The main parameters investigated are : Type of stabilisation (Pb, Ca-Zn, Sn) Amount of filler Presence of impact modifier Level of lubricant

8 SOLVAY Parameters The main target is not : to assess the effect of additives to promote gelation The main target is : To check if some additives affect the DSC thermogram (shape or amplitute of endotherm)

9 SOLVAY Evolution of gelation Gelation as measured by the DSC method (transformation of crystallites) appears rather late compared to a standard plastograph gelation test.

10 SOLVAY Sample preparation The formulation is of the pipe-type, i.e. low level of additives but highly lubricated and the samples are gelified on a 2-roll mill Table PVC K66100 Solid tin one-pack 2 Lead one-pack 2.4 Ca-Zn one-pack 2.8 Liquid tin stab. 0.8 Internal lubricant Lubricant CC filler Acryl Impact modif. 4 TiO2 pigment0.25 C pigment0.025 CharacteristicLeadAcryl.Ca-Zn réf.lubricantfiller 15filler 30Liqu-TinTin-O.P.

11 SOLVAY Parameters (1 st serie) DSC -Tm LeadAcryl.Ca-Zn réf. lubricantfiller 15filler 30Liqu-TinTin-O.P. Was milled at 180°C

12 SOLVAY Sample preparation Characteristic Table 2 PVC Solid Tin O.P. Lead stab. Ca-Zn stab. Liqu. Tin Int. Lubr. Lubric. CC filler CC coarse filler Precip. Filler pigment Leadfiller 6 intern. Lubric. coarse filler Precip.CCTin OP. tin+ coarse f.

13 SOLVAY Parameters (2 nd serie) Tm PbFiller 6Intern. Lubric Coarse filler PCCTintin+c.f. All milled at 180°C 40% 50% 60% 70% 80% 90% Gelation PbFiller 6Intern. Lubric Coarse filler PCCTintin+c.f.

14 SOLVAY Parameters The variants of additives did generally not introduce a different shape of endotherm Only the ox-PE wax (lubricant) introduced an additional peak at 130 °C

15 SOLVAY Parameters Relation between B onset and gelation 2nd series R² = % 50% 60% 70% 80% 90% 100% B onset (°C) Gelation

16 SOLVAY Parameters The processing temperaure can be checked with good accuracy but on these small machines this value is not totally correlated with the gelation level The shape of the endotherm was generally not affected by the composition (except by PE-wax) The sample with Pb stabilisation shows higher endotherms than the average For the sample with modifier and highly lubricated the energy/g of the endotherm was lower than the average

17 SOLVAY Alternative method Another method was extensively used within our company to assess the level of gelation of window profiles : Elongation at rupture measured at 100°C in a tensile test Elongations measured are in the range 200% (bad gelation) to 300% (good gelation) or higher (too strong gelation)

18 SOLVAY Alternative method Correlation is rather satisfactory DSC could lead to a lack of precision in high gelations Elongation at 100°C is also a precise method but the measurement is more labor intensive and equipment is more expensive. y = e x R² =

19 SOLVAY Conclusions Normal levels of additives have no adverse affects on the measurement with this standard procedure (even with high levels of fillers) In some cases, the processing temperature is not a reliable way of expressing the gelation level The method is correctly correlated with other methods of assessing the gelation level The method appears to be enough robust to be used as quality control of extrusion

20 Thank you for your attention !


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