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Molecular Weight Distribution of PPO

CASE STUDY Molecular Weight Distribution of PPO

PROBLEM The purpose of this work was to determine the molecular weight distribution of a modified Polyphenylene Oxide (PPO) sample. ANALYTICAL STRATEGY High Temperature Gel Permeation Chromatography (GPC-H) was employed to characterize the PPO sample in terms of number average molecular weight (Mn), weight average molecular weight (Mw), and Z average molecular weight (Mz). CONCLUSIONS Molecular weights are provided, along with a refractive index chromatogram for the sample, a cumulative weight fraction curve and a molecular weight distribution curve. Read the following report to see the full analysis.

Final Report

Jordi Labs LLC Case Study

Molecular Weight Distribution Determination of Modified

Polyphenylene Oxide (PPO) Sample Using High Temperature Gel Permeation Chromatography (GPC-H)

Date: xx/xx/xx

Released by: Dr. Mark Jordi

President Jordi Labs LLC

Company Name Confidential

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Date Client Name P: xxx-xxx-xxx Company Name E: xxxxx@xxxx.com Dear Client, Please find enclosed the test results for your sample described as:

1. Noryl PPO (modified Polyphenylene Oxide)

The following test was performed:

1. High Temperature Gel Permeation Chromatography (GPC-H) Summary of Results The purpose of this work was to determine the molecular weight distribution of a modified Polyphenylene Oxide (PPO) sample using High Temperature Gel Permeation Chromatography (GPC-H). Table I shows the resulting molecular weight values. Individual Test Results A summary of the individual test results is provided below. All accompanying data, including spectra, has been mailed in the full version of this report. GPC

Background:

A polymer is a large molecule which is formed using a repeating subunit. A polymeric sample does not have a single molecular weight but rather a range of values and thus an average value is used to indicate its molecular weight.

Three different molecular weight averages are commonly used to provide information about polymers. These are the number average molecular weight (Mn), the weight average molecular weight (Mw), and the Z average molecular weight (Mz).

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Mn provides information about the lowest molecular weight portion of the sample. Mw is the average closest to the center of the peak and Mz represents the highest molecular weight portion of the sample. The different molecular weight averages can each be related to specific polymer properties such as material toughness, tensile strength, and total elongation. By comparing the different averages, it is possible to define a fourth parameter called the polydispersity index (PDI). This parameter gives an indication of how broad a range of molecular weights are in the sample. Results:

Enclosed is a refractive index chromatogram for the sample, as well as a cumulative weight fraction curve and a molecular weight distribution curve. A calibration curve and chromatographic overlay of the standards are included. The molecular weights are summarized in Table I.

Relative to polystyrene standards Table I. Average Molecular Weight

Noryl PPO

Figure 1: Normalized Overlay of Standards.

Sample Mn Mw Mz Mw/Mn IV Rh2012-01-01 01;02;05 PPO 01.vdt 18,895 95,454 282,436 5.052 0.0000 0.002012-01-01 02;08;53 PPO 02.vdt 18,752 95,952 282,280 5.117 0.0000 0.00

174.05

206.02

176.00

178.00

180.00

182.00

184.00

186.00

188.00

190.00

192.00

194.00

196.00

198.00

200.00

202.00

204.00

20

11

-12

-31

_1

1;4

0;0

0_

PS

1_

01

.vd

t / M

eth

od

: Co

nve

ntio

na

l ca

l-0

00

3.v

cm

174.53

206.50

176.00

178.00

180.00

182.00

184.00

186.00

188.00

190.00

192.00

194.00

196.00

198.00

200.00

202.00

204.00

20

11

-12

-31

_1

2;4

6;5

2_

PS

2_

01

.vd

t / M

eth

od

: Co

nve

ntio

na

l ca

l-0

00

2.v

cm

0.5 30.0Retention Volume (mL)

1.0 2.0 3.0 4.0 5.0 6.0 7.0 8.0 9.0 10.0 11.0 12.0 13.0 14.0 15.0 16.0 17.0 18.0 19.0 20.0 21.0 22.0 23.0 24.0 25.0 26.0 27.0 28.0 29.0

Overlay Plot: Refractive Index (mV) Vs. Retention Volume (mL)Method: Conventional cal-0003.vcm

9.8

0

11.

26

12.

49

14.

45

15.

67

10.

19 11.

87

12.

78

14.

88

16.

78

2011-12-31_11;40;00_PS1_01.vdt : Conventional cal-0003.vcm 2011-12-31_12;46;52_PS2_01.vdt : Conventional cal-0002.vcm

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Figure 2: Calibration Curve.

Figure 3: Refractive Index (RI) Chromatogram of PPO.

2.000

8.000

2.400

2.700

3.000

3.300

3.600

3.900

4.200

4.500

4.800

5.100

5.400

5.700

6.000

6.300

6.600

6.900

7.200

7.500

7.800L

og

Mo

lecu

lar

We

igh

t

9.000 17.000Retention Volume (mL)

10.000 11.000 12.000 13.000 14.000 15.000 16.000

2011-12-31_11;40;00_PS1_01.vdt - Calibration Curve View Conventional cal-0004.vcm

8.910 e 6

4.410 e 6

1.044 e 6

454,000

184,000

130,000

17,600

8,400

3,250

474

2012-01-01_01;02;05_PPO_01.vdt: Refractive Index

167.85

168.79

169.72

170.66

171.60

172.53

173.47

174.40

175.34

176.27

177.21

178.15

179.08

180.02

180.95

181.89

Ref

ract

ive

Inde

x (m

V)

Retention Volume (mL)0.00 1.43 2.86 4.29 5.71 7.14 8.57 10.00 11.43 12.86 14.29 15.71 17.14 18.57 20.00 21.43 22.86 24.29 25.71 27.14 28.57 30.00

13.

43

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Figure 4: Normalized Overlay of Standards and PPO sample.

Figure 5: cumulative weight fraction curves of PPO.

170.09

199.38

172.00

174.00

176.00

178.00

180.00

182.00

184.00

186.00

188.00

190.00

192.00

194.00

196.00

198.0020

12-0

1-01

_02;

08;5

3_P

PO

_02.

vdt /

Met

hod:

Con

vent

iona

l cal

-000

4.vc

m

173.83

186.08

175.00

176.00

177.00

178.00

179.00

180.00

181.00

182.00

183.00

184.00

185.00

2011

-12-

31_1

1;40

;00_

PS

1_01

.vdt

/ M

etho

d: C

onve

ntio

nal c

al-0

003.

vcm

174.43

186.85

175.00

176.00

177.00

178.00

179.00

180.00

181.00

182.00

183.00

184.00

185.00

186.00

2011

-12-

31_1

2;46

;52_

PS

2_01

.vdt

/ M

etho

d: C

onve

ntio

nal c

al-0

002.

vcm

0.1 30.0Retention Volume (mL)

1.0 2.0 3.0 4.0 5.0 6.0 7.0 8.0 9.0 10.0 11.0 12.0 13.0 14.0 15.0 16.0 17.0 18.0 19.0 20.0 21.0 22.0 23.0 24.0 25.0 26.0 27.0 28.0 29.0

Overlay Plot: Refractive Index (mV) Vs. Retention Volume (mL)Method: Conventional cal-0004.vcm

13.

56

9.8

0 11.

26

12.

49

14.

45

15.

67

10.

19

11.

87

12.

78

14.

88

16.

78

2012-01-01_02;08;53_PPO_02.vdt : Conventional cal-0004.vcm 2011-12-31_11;40;00_PS1_01.vdt : Conventional cal-0003.vcm 2011-12-31_12;46;52_PS2_01.vdt : Conventional cal-0002.vcm

2012-01-01_01;02;05_PPO_01.vdt: Cumulative Weight Fraction

0.00

0.05

0.11

0.16

0.21

0.26

0.32

0.37

0.42

0.47

0.53

0.58

0.63

0.68

0.74

0.79

0.84

0.89

0.95

1.00

Cum

ulat

ive

Wei

ght F

ract

ion

Log Molecular Weight2.00 2.24 2.48 2.71 2.95 3.19 3.43 3.67 3.90 4.14 4.38 4.62 4.86 5.10 5.33 5.57 5.81 6.05 6.29 6.52 6.76 7.00

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Figure 6: Mw distribution curves.

Analysis Conditions Information on the specific conditions used to perform the analysis is typically listed in this section of the report. Closing Comments Jordi Labs’ reports are issued solely for the use of the clients to whom they are addressed. No quotations from reports or use of the Jordi name is permitted except as authorized in writing. The liability of Jordi Labs with respect to the services rendered shall be limited to the amount of consideration paid for such services and do not include any consequential damages.

2012-01-01_01;02;05_PPO_01.vdt: Log Molecular Weight Normalized Wt Fr

2.00

2.26

2.53

2.79

3.05

3.32

3.58

3.84

4.11

4.37

4.63

4.89

5.16

5.42

5.68

5.95

6.21

6.47

6.74

7.00

Log

Mol

ecul

ar W

eigh

t

0.00

0.02

0.04

0.06

0.09

0.11

0.13

0.15

0.17

0.19

0.22

0.24

0.26

0.28

0.30

0.32

0.35

0.37

0.39

0.41

Nor

mal

ized

Wt F

r

Retention Volume (mL)11.04 11.31 11.58 11.85 12.13 12.40 12.67 12.94 13.21 13.48 13.75 14.02 14.29 14.56 14.83 15.10 15.37 15.64 15.91 16.18 16.45

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Jordi Labs specializes in polymer testing and has 30 years experience doing complete polymer deformulations. We are one of the few labs in the country specialized in this type of testing. We will work closely with you to help explain your test results and solve your problem. We appreciate your business and are looking forward to speaking with you concerning these results.

Sincerely,

Kiran Rana Mark Jordi

Chemist President Kiran Rana, M.S. Mark Jordi, Ph. D.

Jordi Labs LLC Jordi Labs LLC

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