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PER CONTENT

20-Aug, 2020
Overview
Scope
• The method covers the determination of polypropylene ethylene rubber content of
polypropylene block copolymer.

Meaning of polypropylene ethylene rubber

• It improves the impact strength at low temperature. 145 oC 200 mL


1hr Stirring n-decane
Principle of method

• Both CPP and PER are dissolved in n-decane at 145 oC.


Room
• At room temperature, only PER is dissolved in n-decane. temperature
• PER will precipitate in the mixture of n-decane and acetone.

Filtration
PER & Dry N-decane Filtration
Acetone

n-decane & PER


PER PP
Apparatus
Dissolving apparatus
1. Oil bath able to maintain at 145 ± 5 oC with magnetic stirrer.
2. Erlenmeyer flask, 300 ml.
3. Magnetic stirrer
4. Condenser
5. Thermometer : 0-200 oC.
6. Electric agitator - equipped with a speed controller

Separating & filtering apparatus


1. Filter Funnel (glass)
2. Filter - stainless steel, 100 Ømm , 325 mesh (44µm)
3. Glass rod with silicone rubber, 10 Ømm, 25mm in length and silicone rubber ~20 Ømm at one end.
4. Suction bottle, 1L.
5. Beaker, 2L,
6. Funnel – glass, 100 Ømm
7. Stirring rod (50 mm) coated with Teflon
8. Filter (stainless steel ,100 Ømm, 325 mesh)

Vacuum oven
105oC @ 10 mmHg
Balance @ 0.1mg

Oil
bat
h
Chemicals
Chemicals
1. N-Decane (98% grade or higher)
2. Acetone.
3. Dry ice (solid carbon dioxide).
4. Heat resistant stabilizer (BHT)
5. Polyethylene glycol – No. 400 (used for oil bath)

Safety Check
Chemicals
1. Heat resistant gloves (for handling samples in oil bath and dry ice).
2. Chemical gloves.
3. Use mask when handling powder samples.
Procedure
Polymer Dissolution 5 ± 0.1 g

1. Set up the apparatus as in Fig. 1.


2. Set the oil bath to stabilize at 145 ± 5 oC.
3. Weigh precisely 5 ± 0.1 g sample to 0.1 mg. Record the weight as “a”.
4. Transfer the sample to the Erlenmeyer flask, which contains 200 ml n-
decane.
5. Immerse the flask to the oil bath with a magnetic stirrer.
6. Stir the sample for 1 hour until the sample is completely dissolved.
7. Take out the flask, clean the oil remaining on the outside of the flask. 145 oC
8. Stir the flask on a magnetic stirrer for 2 hours until the solution is cool. Stirring 1 hour

 2 phases slurry.
9. During waiting time, assemble the filtering apparatus as in Fig. 2.

Polymer Filtration

10. Transfer the slurry to the filter funnel and filter the slurry using 325 mesh filter.
11. Rub off the polymer sticking to the inner wall of the flask with the silicon-
coated glass rod.
12. Wash the inner wall of the flask with n-decane to remove all the remaining
polymer.
13. Press slightly the cake-like polymer remaining on the wire mesh with glass rod.
Procedure
PER Separation and Filtration

14. Transfer the filtrate to the 2-1 beaker as in Fig. 3.


15. Add acetone 2 to 4 times the quantity of the filtrate and place a magnetic
stirrer bar in it.
16. Stir for 1 hour to separate the PER content.
17. If the supernatant is still not transparent, continue to add acetone and stir.
18. Place 4-folded, 325 wire mesh on the glass funnel to filter out the PER content
and transfer it to the sample–drying vat.
Supernatant
PER Drying and Weighing
19. Dry the PER content at 105 ± 5 oC under 10 mHg for 1 hour with the
stirring rod remaining in it.
20. After completion of drying, take out the stirring rod, allow the PER
content only to cool for 30 min in a constant temperature room. Precipitate
21. Precisely weigh the PER content to 0.1 mg  take the weight as “b”

Calculation
PER Content = b/a x 100 (wt%).
Report
Report to first decimal place. (e.g. 1.0 %, 10.0 %)