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Metrohm 763 PVC Thermomat Manual User Manual

Page 73

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4 Operation

763 PVC Thermomat

66

4.6.2

Sample preparation

PVC or other plastics which decompose through the action of heat with

cleavage of hydrogen halides are prepared in accordance with DIN

53'381 as follows:

1 Powdery samples

Polymers, dry blends and coating powders need no special

sample pretreatment.

2 Pastes

Pastes are fused on a glass plate in a drying oven to a sheet

with a thickness of about 0.5 mm. After cooling, the sheet is

cut into pieces of edge length about 2 mm.

3 Solid samples

Molding compounds in granular form, molded and finished

parts, semi-finished products as well as coatings separated

from the substrate are pulverized in accordance with DIN

53'733 and screened to separate the screening fraction be-

tween the analytical screens with wire mesh screen DIN 4188-

1.4 (wire mesh of stainless steel with 1.4 mm inside diameter

mesh size) and wire mesh screen DIN 4188-2 (wire mesh of

stainless steel with 2 mm inside diameter mesh size) for the

experiments.

4 Sheets

Sheets are cut into pieces with an edge length of about 2

mm.

According to DIN 53'581, the samples are to be added directly into

the prewarmed reaction vessels inserted in the heating block. Never-

theless, comparative measurements have shown identical results for

sample addition to cold or hot reaction vessels.

4.6.3

Prepare instruments and accessories

Clean instruments and accessories

The cleanness of instruments and accessories is an absolute neces-

sity for achieving reliable, reproducible and correct analytical results.

Even minute contamination can catalytically accelerate the thermal de-

composition and lead to completely false results. Make sure that the

following checks and cleaning procedures are carried out before the

start of a determination:

1 Openings for reaction vessels

Check whether the openings for the reaction vessels are

clean and empty. Blow out any dust in the openings with ni-

trogen.