Degradation of Polyethylene by FTIR and High Temperature ...

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Degradation of Polyethylene by FTIR and High Temperature GPC

CASE STUDY

Degradation of Polyethylene by FTIR

and High Temperature GPC

PROBLEM

The objective of this analysis was to determine if thermal degradation had occurred in a polyethylene sample by

Fourier Transform Infrared Analysis (FTIR) and High Temperature Tetradetection Gel Permeation

Chromatography (GPC-HT).

ANALYTICAL STRATEGY

FTIR is will be used to identify the portion of brown discoloration of the polyethylene sample, while high

temperature GPC will be performed to compare the molecular weights of the sample and a virgin polyethylene.

CONCLUSIONS

The FTIR spectrum of the sample was found to be consistent with oxidized polyethylene. The failed PE sample

was found to show an increase in molecular weight as compared to the virgin material.

Read the following report to see the full analysis.

Final Report

Jordi Labs LLC

Degradation of Polyethylene by FTIR

and High Temperature GPC

Case Study

Date: XX/XX/XX

Released by:

Dr. Mark Jordi

President

Jordi Labs LLC

Report Number: JXXXX

Jordi Labs LLC - Confidential

Page 1 of 33

Date

Client Name

Company Name

Address

Dear Valued Client,

Please find enclosed the test results for your sampled described as:

1. Virgin PE sheet

2. Failed PE Sheet (Lot# 20100913-ASABFY)

The following tests were performed:

1. Fourier Transform Infrared Spectroscopy (FTIR)

2. High Temperature Tetradetection Gel Permeation Chromatography (GPC-HT)

Objective The objective of this analysis was to determine if thermal degradation had occurred in a

polyethylene sample by Fourier Transform Infrared Analysis (FTIR) and High Temperature

Tetradetection Gel Permeation Chromatography (GPC-HT).

Summary of Results Visual observation of the sample shows a brown discoloration in the failed PE sheet as

shown in Image 1. The FTIR spectrum of the sample was compared to our database of

~23,000 entries and found to be consistent with oxidized polyethylene. The peak at 1722

cm-1

is diagnostic for C=O which is consistent with oxidation of the polymer.

Table II shows the molecular weight values as determined by GPC-HT. The failed PE

sample was found to show an increase in molecular weight as compared to the virgin

material. This is at first counter intuitive but is often observed in polyolefin degradation due

to the onset of crosslinking.

Page 2 of 33

Individual Test Results A summary of the individual test results is provided below. All accompanying data,

including spectra, has been included in the data section of this report.

Image 1. Sample Lot# 20100913-ASABFY

FTIR

A thin portion of the sample was extracted using a clean, sharp razor blade and analyzed by

FT-IR. The spectrum was compared to our library database of ~23,000 entries and found to

be consistent with oxidized polyethylene. The presence of additional peaks at 1722 and 1182

cm-1

suggests oxidation. These bands are consistent with C=O and ether functional groups.

Table 1 shows the peak identifications for the failed sample and the virgin polyethylene.

Figure 1 shows the FT-IR spectrum for the failed sample and Figure 2 shows the spectrum

of the virgin polyethylene sample.

Page 3 of 33

Figure 1. FT-IR Spectrum for Lot# 20100913-ASABFY

Table 1

FTIR Peaks and Identifications

IR Frequency (cm-1

Functional Group ) Lot# 20100913-ASABFY Polyethylene Reference

2914 2914 C-H asymmetric Stretch in CH

2846 2

2846 C-H symmetric Stretch in CH

1722 2

C=O stretch

1474 1474 CH2

1376

bend

CH3

1182

bend

C-O-C stretch

720 720 CH2

rock

Page 4 of 33

Figure 2. FT-IR Spectrum for Virgin Polyethylene

Figure 3. FT-IR Spectrum Overlay of Failed (Blue) and Virgin Polyethylene (Red)

Page 5 of 33

Figure 4. FT-IR Spectrum Overlay of Failed Polyethylene (black) and Oxidized

Polyethylene (light blue) Best Match

GPC-HT

Table II shows the results for a series of standards analyzed to demonstrate system

performance. Polystyrene standards were analyzed with weight average molecular weights of

233,643 and 99,420. Confirmation of the accuracy of our calibration was achieved by

running a linear polyethylene standard that was obtained from the National Institute of

Standards and Technology (1475a). Table III shows the results for the samples. The method

of known dn/dc was applied for the samples as the chemistry was known. Overlays are

provided for the polyethylene samples in Figures 5-8.

The failed PE sample was found to show a higher molecular weight as compared to the virgin

resin. A significant increase in the light scattering signal was observed as shown in Figure 6.

This indicates the presence of crosslinking in the degraded sample.

Table II. Standards

Standard Analysis (GPC-T)

(PS 99,420)

Sample Mn Mw Mz Mw/Mn IV Rh

2012-03-02 10;56;18 PS99K 99420Da 02.vdt 99,329 99,921 100,437 1.006 0.4803 9.10

ID dn/dc Conc

PS99K 99420Da 0.0531 2.5920

Page 6 of 33

Standard Analysis (GPC-T)

(PS 233,643)

NIST 1475a Linear Polyethylene Analysis

(Mw = 53,070)

Table III. Analysis of Samples

Virgin PE Sheet (GPC-T)

Failed PE Sheet (GPC-T)


2012-03-02 11;58;09 PS235K 233643Da 01.vdt 108,236 233,287 431,060 2.155 0.7543 13.29

2012-03-02 14;01;55 PS235K 233643Da 03.vdt 108,652 233,599 428,978 2.150 0.7676 13.39

ID dn/dc Conc

PS235K 233643Da 0.0558 5.9760

PS235K 233643Da 0.0567 5.9760


2012-03-02 19;37;55 1475A 02.vdt 19,290 53,970 163,317 2.798 1.1776 9.05

2012-03-02 20;39;49 1475A 03.vdt 19,291 53,959 164,914 2.797 1.1753 9.06

ID dn/dc Conc

1475A 0.1040 2.5200

1475A 0.1040 2.5200


2012-03-16_04;47;59_modified_P 44,050 128,438 620,633 2.916 10.7886 24.89

2012-03-16 06;51;32 modified P 44,915 133,621 614,303 2.975 10.7216 25.05

ID dn/dc Conc

modified 0.1040 2.4898

modified 0.1040 2.4890


2012-03-16 02;44;29 degraded PE 44,481 163,208 1.012 e 6 3.669 11.1475 26.52

2012-03-16 03;46;14 degraded PE 43,500 162,159 1.037 e 6 3.728 11.9730 26.92

ID dn/dc Conc

0.1040 1.8015

0.1040 1.7810

Virgin PE

Virgin PE

Virgin PE

Virgin PE

Failed PE

Failed PE

Failed PE

Failed PE

Page 7 of 33

Figure 5: Overlay of refractive index curves for the virgin PE (green) and Failed PE (red)

samples.

Figure 6: Overlay of Right Angle Light Scattering curves for the virgin PE (green) and

Failed PE (red) samples.

2012-03-16_02;44;29__degraded_PE_sheets_02.vdt: Refractive Index

2012-03-16_04;47;59_modified_PE_sheet_01.vdt: Refractive Index

-260.00

-258.00

-256.00

-254.00

-252.00

-250.00

-248.00

-246.00

-244.00

-242.00

-240.00

-238.00

-236.00

-234.00

-232.00

-230.00

Re

fra

cti

ve

In

de

x (

mV

)

Retention Volume (mL)7.00 7.39 7.77 8.16 8.55 8.93 9.32 9.70 10.09 10.48 10.86 11.25 11.64 12.02 12.41 12.80 13.18 13.57 13.95 14.34 14.73 15.11 15.50

2012-03-16_02;44;29__degraded_PE_sheets_02.vdt: Right Angle Light Scattering

2012-03-16_04;47;59_modified_PE_sheet_01.vdt: Right Angle Light Scattering

298.64

299.70

300.75

301.81

302.87

303.92

304.98

306.04

307.09

308.15

309.21

310.27

311.32

312.38

314.49

Rig

ht

An

gle

Lig

ht

Sc

att

eri

ng

(m

V)


Failed PE = Red

Virgin PE = Green

Failed PE = Red

Virgin PE = Green

Page 8 of 33

Figure 7: Overlay of Viscometry curves for the virgin PE (green) and Failed PE (red)

samples.

Figure 8: Overlay of weight fraction and log molecular weight curves for the virgin PE

(green) and Failed PE (red) samples.

2012-03-16_02;44;29__degraded_PE_sheets_02.vdt: Viscometer - DP

2012-03-16_04;47;59_modified_PE_sheet_01.vdt: Viscometer - DP

-226.95

-218.09

-209.22

-200.35

-191.49

-182.62

-173.76

-164.89

-156.03

-147.16

-138.29

-129.43

-120.56

-111.70

-102.83

-93.97V

isc

om

ete

r -

DP

(m

V)


2012-03-16_02;44;29__degraded_PE_sheets_02.vdt: Log Molecular Weight Normalized Wt Fr

2012-03-16_04;47;59_modified_PE_sheet_01.vdt: Log Molecular Weight Normalized Wt Fr

3.00

3.21

3.42

3.63

3.84

4.05

4.26

4.47

4.68

4.89

5.11

5.32

5.53

5.74

5.95

6.16

6.37

6.58

6.79

7.00

Lo

g M

ole

cu

lar

We

igh

t

0.00

0.03

0.05

0.08

0.11

0.13

0.16

0.19

0.21

0.24

0.27

0.30

0.32

0.35

0.38

0.40

0.43

0.46

0.48

0.51

No

rma

liz

ed

Wt

Fr

Retention Volume (mL)9.22 9.59 9.96 10.33 10.70 11.07 11.44 11.80 12.17 12.54 12.91 13.28 13.65 14.02 14.38 14.75 15.12 15.49 15.86 16.23 16.60

Failed PE = Red

Virgin PE = Green

Page 9 of 33

Analysis Conditions Information on the specific conditions used to perform the analysis is typically listed in this

section of the report.

Closing Comments

Deformulation of an unknown material is intended to provide a best estimate of the chemical

nature of the sample. All chemical structures are supported by the evidence presented but are

subject to revision upon receipt of additional evidence. Additional factors such as material

processing conditions may also affect final material properties.

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.

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

Laurie Scharp

Laurie Scharp

Chemist

Jordi Labs LLC

Page 10 of 33

Appendix

Table of Contents

• - 14 – System Calibration using PS 99,420 (PS99K)

• Page 13 - 15 – PS 235K Standard Analysis (233,643)

• Page 16 - 18 – NIST 1475a Linear Polyethylene Standard

• Page 17 - 21 – Samples

• Page 22 - 29 – FTIR Data

Page 11 of 33

System

Calibration

using PS

99,420

(PS99K)

Page 12 of 33

System Calibration using PS 99,420 (PS99K)

PS 99K: RI, RALS, LALS DP Overlay Chromatogram

PS99K: Cumulative Weight Fraction Curve

2012-03-02_10;56;18_PS99K_99420Da_02.vdt: Refractive Index Right Angle Light Scattering Low Angle Light Scattering

Viscometer - DP

242.93

247.18

251.43

255.68

259.94

264.19

268.44

272.69

276.95

281.20

285.45

289.70

293.95

298.21

302.46

306.71

Re

fra

cti

ve

In

de

x (

mV

)

253.65

254.45

255.24

256.03

256.82

257.61

258.40

259.19

259.98

260.77

261.56

262.35

263.14

263.93

264.72

265.51

Rig

ht

An

gle

Lig

ht

Sc

att

eri

ng

(m

V)

714.33

714.93

715.53

716.13

716.73

717.33

717.93

718.53

719.12

719.72

720.32

720.92

721.52

722.12

722.72

723.32L

ow

An

gle

Lig

ht

Sc

att

eri

ng

(m

V)

-343.07

-320.86

-298.64

-276.42

-254.20

-231.98

-209.76

-187.54

-165.33

-143.11

-120.89

-98.67

-76.45

-54.23

-9.80

Vis

co

me

ter

- D

P (

mV

)

Retention Volume (mL)0.00 1.47 2.94 4.41 5.88 7.35 8.82 10.29 11.76 13.24 14.71 16.18 17.65 19.12 20.59 22.06 23.53 25.00

13.0

1

2012-03-02_10;56;18_PS99K_99420Da_02.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

Cu

mu

lati

ve

We

igh

t F

rac

tio

n

Log Molecular Weight4.00 4.10 4.19 4.29 4.38 4.48 4.57 4.67 4.76 4.86 4.95 5.05 5.14 5.24 5.33 5.43 5.52 5.62 5.71 5.81 5.90 6.00

Page 13 of 33

PS99K: MW Distribution Curve

2012-03-02_10;56;18_PS99K_99420Da_02.vdt: Log Molecular Weight Normalized Wt Fr

4.00

4.11

4.21

4.32

4.42

4.53

4.63

4.74

4.84

4.95

5.05

5.16

5.26

5.37

5.47

5.58

5.68

5.79

5.89

6.00

Lo

g M

ole

cu

lar

We

igh

t

0.00

0.09

0.18

0.26

0.35

0.44

0.53

0.62

0.70

0.79

0.88

0.97

1.05

1.14

1.23

1.32

1.41

1.49

1.58

1.67

No

rma

liz

ed

Wt

Fr


Page 14 of 33

PS 235K

Standard

Analysis

(233,643)

Page 15 of 33

PS 235K Standard Analysis (233,643)

PS 235K: RI, RALS, LALS DP Overlay Chromatogram

PS 235K: Cumulative Weight Fraction Curve

2012-03-02_11;58;09_PS235K_233643Da_01.vdt: Refractive Index Right Angle Light Scattering Low Angle Light Scattering

Viscometer - DP

252.80

256.43

260.05

263.68

267.31

270.94

274.56

278.19

281.82

285.45

289.07

292.70

296.33

299.96

303.58

Re

fra

cti

ve

In

de

x (

mV

)

255.30

256.93

258.56

260.19

261.82

263.45

265.08

266.71

268.34

269.97

271.60

273.23

274.86

276.49

278.12

Rig

ht

An

gle

Lig

ht

Sc

att

eri

ng

(m

V)

715.22

716.28

717.34

718.40

719.47

720.53

721.59

722.66

723.72

724.78

725.84

726.91

727.97

729.03

730.09

Lo

w A

ng

le L

igh

t S

ca

tte

rin

g (

mV

)

-416.99

-379.08

-341.16

-303.25

-265.33

-227.42

-189.51

-151.59

-113.68

-75.77

-37.85

0.06

37.98

75.89

113.80

Vis

co

me

ter

- D

P (

mV

)

Retention Volume (mL)0.00 1.56 3.13 4.69 6.25 7.81 9.38 10.94 12.50 14.06 15.63 17.19 18.75 20.31 21.88 23.44 25.00

12.6

8

2012-03-02_11;58;09_PS235K_233643Da_01.vdt: Cumulative Weight Fraction

0.00

0.06

0.11

0.17

0.22

0.28

0.33

0.39

0.44

0.50

0.56

0.61

0.67

0.72

0.78

0.83

0.89

0.94

1.00

Cu

mu

lati

ve

We

igh

t F

rac

tio

n

Log Molecular Weight3.00 3.20 3.40 3.60 3.80 4.00 4.20 4.40 4.60 4.80 5.00 5.20 5.40 5.60 5.80 6.00 6.20 6.40 6.60 6.80 7.00

Page 16 of 33

PS 235K: MW Distribution Curve

PS 235K: Mark Houwink Plot

2012-03-02_11;58;09_PS235K_233643Da_01.vdt: Log Molecular Weight Normalized Wt Fr

3.00

3.22

3.44

3.67

3.89

4.11

4.33

4.56

4.78

5.00

5.22

5.44

5.67

5.89

6.11

6.33

6.56

6.78

7.00

Lo

g M

ole

cu

lar

We

igh

t

0.00

0.03

0.06

0.10

0.13

0.16

0.19

0.23

0.26

0.29

0.32

0.35

0.39

0.42

0.45

0.48

0.52

0.55

0.58

No

rma

liz

ed

Wt

Fr

Retention Volume (mL)10.62 10.94 11.26 11.59 11.91 12.23 12.56 12.88 13.21 13.53 13.85 14.18 14.50 14.82 15.15 15.47 15.80 16.12 16.44 16.77

2012-03-02_11;58;09_PS235K_233643Da_01.vdt: Log Intrinsic Viscosity

-0.80

-0.74

-0.68

-0.63

-0.57

-0.51

-0.45

-0.39

-0.34

-0.28

-0.22

-0.16

-0.11

-0.05

0.01

0.07

0.13

0.18

0.24

0.30

Lo

g I

ntr

ins

ic V

isc

os

ity

Log Molecular Weight3.00 3.20 3.40 3.60 3.80 4.00 4.20 4.40 4.60 4.80 5.00 5.20 5.40 5.60 5.80 6.00 6.20 6.40 6.60 6.80 7.00

Page 17 of 33

NIST 1475a

Linear

Polyethylene

Page 18 of 33

NIST 1475a Linear Polyethylene

NIST 1475a Linear Polyethylene: RI, RALS, LALS DP Overlay Chromatogram

NIST 1475a Linear Polyethylene: Cumulative Weight Fraction Curve

2012-03-02_19;37;55_1475A_02.vdt: Refractive Index Right Angle Light Scattering Low Angle Light Scattering

Viscometer - DP

-285.12

-283.05

-280.99

-278.92

-276.86

-274.79

-272.73

-270.66

-268.60

-266.53

-264.47

-262.40

-260.34

-258.27

-256.21

-254.14R

efr

ac

tiv

e I

nd

ex

(m

V)

256.34

256.88

257.42

257.97

258.51

259.05

259.59

260.14

260.68

261.22

261.76

262.30

262.85

263.39

263.93

264.47

Rig

ht

An

gle

Lig

ht

Sc

att

eri

ng

(m

V)

716.03

716.51

717.00

717.48

717.97

718.46

718.94

719.43

719.92

720.40

720.89

721.37

721.86

722.35

722.83

723.32

Lo

w A

ng

le L

igh

t S

ca

tte

rin

g (

mV

)

-380.54

-361.70

-342.87

-324.04

-305.21

-286.38

-267.55

-248.72

-229.89

-211.06

-192.23

-173.39

-154.56

-135.73

-116.90

-98.07

Vis

co

me

ter

- D

P (

mV

)


13.1

3

2012-03-02_19;37;55_1475A_02.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

Cu

mu

lati

ve

We

igh

t F

rac

tio

n


Page 19 of 33

NIST 1475a Linear Polyethylene: MW Distribution Curve

NIST 1 475a Linear Polyethylene: Mark Houwink Plot

2012-03-02_19;37;55_1475A_02.vdt: Log Molecular Weight Normalized Wt Fr

3.00

3.21

3.42

3.63

3.84

4.05

4.26

4.47

4.68

4.89

5.11

5.32

5.53

5.74

5.95

6.16

6.37

6.58

6.79

7.00

Lo

g M

ole

cu

lar

We

igh

t

0.00

0.03

0.05

0.08

0.11

0.13

0.16

0.19

0.21

0.24

0.27

0.30

0.32

0.35

0.38

0.40

0.43

0.46

0.48

0.51

No

rma

liz

ed

Wt

Fr


2012-03-02_19;37;55_1475A_02.vdt: Log Intrinsic Viscosity

-0.70

-0.61

-0.53

-0.44

-0.36

-0.27

-0.19

-0.10

-0.02

0.07

0.15

0.24

0.32

0.41

0.49

0.58

0.66

0.75

0.83

0.92

1.00

Lo

g I

ntr

ins

ic V

isc

os

ity


Page 20 of 33

Samples

Page 21 of 33

Modified PE sheet

Modified PE sheet: RI, RALS, LALS DP Overlay Chromatogram

Modified PE sheet: Cumulative Weight Fraction Curve

2012-03-03_13;09;33_degraded_modified_PE_sheet_01.vdt: Refractive Index Right Angle Light Scattering Low Angle Light Scattering

Viscometer - DP

-278.63

-277.10

-275.57

-274.04

-272.51

-270.98

-269.45

-267.92

-266.39

-264.85

-263.32

-261.79

-260.26

-258.73

-257.20

-255.67

Re

fra

cti

ve

In

de

x (

mV

)

255.00

255.69

256.38

257.07

257.76

258.46

259.15

259.84

260.53

261.22

261.91

262.61

263.30

263.99

264.68

265.37

Rig

ht

An

gle

Lig

ht

Sc

att

eri

ng

(m

V)

715.46

716.09

716.71

717.33

717.96

718.58

719.21

719.83

720.46

721.08

721.71

722.33

722.96

723.58

724.21

724.83

Lo

w A

ng

le L

igh

t S

ca

tte

rin

g (

mV

)

-386.29

-367.02

-347.76

-328.50

-309.23

-289.97

-270.71

-251.45

-232.18

-212.92

-193.66

-174.39

-155.13

-135.87

-116.60

-97.34

Vis

co

me

ter

- D

P (

mV

)


12.7

4

2012-03-03_13;09;33_degraded_modified_PE_sheet_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

Cu

mu

lati

ve

We

igh

t F

rac

tio

n


Page 22 of 33

Modified PE sheet: MW Distribution Curve

Modified PE sheet: Mark Houwink Plot

2012-03-03_13;09;33_degraded_modified_PE_sheet_01.vdt: Log Molecular Weight Normalized Wt Fr

2.00

2.32

2.63

2.95

3.26

3.58

3.89

4.21

4.53

4.84

5.16

5.47

5.79

6.11

6.42

6.74

7.05

7.37

7.68

8.00

Lo

g M

ole

cu

lar

We

igh

t

0.00

0.02

0.05

0.07

0.09

0.11

0.14

0.16

0.18

0.20

0.23

0.25

0.27

0.29

0.32

0.34

0.36

0.38

0.41

0.43

No

rma

liz

ed

Wt

Fr


2012-03-03_13;09;33_degraded_modified_PE_sheet_01.vdt: Log Intrinsic Viscosity

-0.50

-0.42

-0.35

-0.27

-0.20

-0.12

-0.05

0.03

0.10

0.18

0.25

0.33

0.40

0.48

0.55

0.63

0.70

0.77

0.85

0.92

1.00

Lo

g I

ntr

ins

ic V

isc

os

ity


Page 23 of 33

Degraded PE Sheet

Degraded PE Sheet: RI, RALS, LALS DP Overlay Chromatogram

Degraded PE Sheet: Cumulative Weight Fraction Curve

2012-03-03_10;03;57_modified_PE_Sheet_01.vdt: Refractive Index Right Angle Light Scattering Low Angle Light Scattering

Viscometer - DP

-277.41

-275.39

-273.37

-271.36

-269.34

-267.32

-265.30

-263.28

-261.26

-259.24

-257.22

-255.20

-253.18

-251.16

-247.12

Re

fra

cti

ve

In

de

x (

mV

)

254.46

255.31

256.15

257.00

257.84

258.69

259.53

260.37

261.22

262.06

262.91

263.75

264.60

265.44

266.28

267.13

Rig

ht

An

gle

Lig

ht

Sc

att

eri

ng

(m

V)

714.01

714.79

715.56

716.34

717.11

717.89

718.66

719.44

720.21

720.99

721.76

722.54

723.31

724.09

724.86

725.64

Lo

w A

ng

le L

igh

t S

ca

tte

rin

g (

mV

)

-413.45

-383.63

-353.81

-323.99

-294.17

-264.35

-234.53

-204.71

-174.89

-145.07

-115.25

-85.43

-55.61

-25.79

4.03

33.85

Vis

co

me

ter

- D

P (

mV

)


12.6

0

2012-03-03_10;03;57_modified_PE_Sheet_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

Cu

mu

lati

ve

We

igh

t F

rac

tio

n


Degraded PE Sheet-01.vdt.


Page 24 of 33

Degraded PE Sheet: MW Distribution Curve

Degraded PE Sheet: MW Distribution Curve

2012-03-03_10;03;57_modified_PE_Sheet_01.vdt: Log Molecular Weight Normalized Wt Fr

3.00

3.26

3.53

3.79

4.05

4.32

4.58

4.84

5.11

5.37

5.63

5.89

6.16

6.42

6.68

6.95

7.21

7.47

7.74

8.00

Lo

g M

ole

cu

lar

We

igh

t

0.00

0.03

0.05

0.08

0.11

0.13

0.16

0.19

0.21

0.24

0.27

0.30

0.32

0.35

0.38

0.40

0.43

0.46

0.48

0.51

No

rma

liz

ed

Wt

Fr


2012-03-03_10;03;57_modified_PE_Sheet_01.vdt: Log Intrinsic Viscosity

-0.30

-0.23

-0.15

-0.08

0.00

0.08

0.15

0.23

0.30

0.38

0.45

0.53

0.60

0.68

0.75

0.83

0.90

0.98

1.05

1.13

1.20

Lo

g I

ntr

ins

ic V

isc

os

ity




Page 25 of 33

FTIR Data

Page 26 of 33

4000 3800 3600 3400 3200 3000 2800 2600 2400 2200 2000 1800 1600 1400 1200 1000 800 600 400

10

20

30

40

50

60

70

80

90

100

2914 2

848

1718

1472

1462

1368

1178

730

718

604

Lot# 20100913-ASABFY

Copr. © 1980, 1981-1993 Sadtler. All Rights Reserved.

Page 27 of 33

4000 3800 3600 3400 3200 3000 2800 2600 2400 2200 2000 1800 1600 1400 1200 1000 800 600 400

10

20

30

40

50

60

70

80

90

100

2914 2

848

1718

1472

1462

1368

1178

730

718

604

Lot# 20100913-ASABFY (in black) Oxidized Polyethylene (in green)


Page 28 of 33

4000 3800 3600 3400 3200 3000 2800 2600 2400 2200 2000 1800 1600 1400 1200 1000 800 600 400

10

20

30

40

50

60

70

80

90

100

2916

2848

1472

720

OM #1; A-C POLYETHYLENE 316


Name(s): A-C POLYETHYLENE 316

Source Of Sample: ALLIED FIBERS AND PLASTICS COMPANY, ALLIED CORPORATION

Technique: FILM (CAST FROM o-DICHLOROBENZENE)

Density: 0.98

Classification: Polymers: POLYETHYLENES

Solution Data: Acid Number: 16

Viscosity Data: (Brookfield): (140C) 12000 CPS

Softening Point: 140C

Comments: Chemical Description: OXIDIZED ETHYLENE HOMOPOLYMER

Page 29 of 33

Index HQI Chemical Name Spectrum

OM #46 792.44 PETROLITE C-4040

OM #15 783.16 DISLON 4200-10

OM #19 780.81 PETROTHENE NL 409-00

OM #613 775.89 CERAMER 5005

OL #63 772.95 BAYLON V22H764*LOW DENSITY POLYETHYLENE

OM #5 769.00 POLY-ETH 2255

RC #142 768.84 ROCK F T WAX

OM #1 766.55 A-C POLYETHYLENE 316

OM #4 765.84 POLY-ETH 2205

QF #97 765.28 HEPTACOSANE

OL #1976 752.22 M-P-A 60-T (TOLUENE)

OM #13 752.06 HOSTALEN GK9050 HO

AS #1858 749.98 DAF 618 FILM FORMULATED WITH AN ADHESI...

OM #1215 749.61 ESCOR ATX 310

OL #2 746.78 PARVAN 3150, F.N. 3502*REFINED PARAFFI...

SR #167 746.78 PARVAN 3150, F.N. 3502*REFINED PARAFFI...



PL #1471 745.41 WAX X-12 : MIXTURE OF STRAIGHT CHAIN F...

AS #1275 745.12 AREMCO #562

OM #17 743.97 PETROTHENE HD 5002

AS #1526 743.18 THERMOGRIP 1317

Page 30 of 33

lscharp

Typewritten Text

Best Match Hit List for Lot# 20100913-ASABFY

lscharp

Typewritten Text

Index HQI Chemical Name Spectrum

OL #47 739.60 POLY EM 40*PH STABLE ANIONIC POLYETHYL...

OM #26 738.27 VOLARA 2E

OL #4 737.75 PARVAN 4550, F.N. 3519*REFINED PARAFFI...

Page 31 of 33

4000 3800 3600 3400 3200 3000 2800 2600 2400 2200 2000 1800 1600 1400 1200 1000 800 600 400

40

45

50

55

60

65

70

75

80

85

90

95

100

2916

2848

1472

716

Polyethylene

Page 32 of 33

lscharp

Typewritten Text

4000 3800 3600 3400 3200 3000 2800 2600 2400 2200 2000 1800 1600 1400 1200 1000 800 600 400

40

45

50

55

60

65

70

75

80

85

90

95

100

2914

2848

1718

1472

1462 7

30

718

Lot# 20100913-ASABFY (in black) Polyethylene Reference (in red)

Page 33 of 33

Degradation of Polyethylene by FTIR and High Temperature ...

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