Molecular Weight Distribution of PPO CASE STUDY ... - Jordi Labs
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.
www.jordilabs.com
Page 1
Page 1 of 7
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
Page 2 of 7
Date Client Name Company Name
P: xxx-xxx-xxx E: [email protected]
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).
Page 3 of 7
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.
Table I. Average Molecular Weight Relative to polystyrene standards
Noryl PPO Mn 18,895 18,752
Sample 2012-01-01 01;02;05 PPO 01.vdt 2012-01-01 02;08;53 PPO 02.vdt
Mw 95,454 95,952
Mz 282,436 282,280
Mw/Mn 5.052 5.117
IV 0.0000 0.0000
Rh 0.00 0.00
Overlay Plot: Refractive Index (mV) Vs. Retention Volume (mL) Method: Conventional cal-0003.vcm 206.02 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
206.50
204.00 204.00 202.00 202.00 200.00 200.00
2011-12-31_12;46;52_PS2_01.vdt / Method: Conventional cal-0002.vcm
2011-12-31_11;40;00_PS1_01.vdt / Method: Conventional cal-0003.vcm
198.00
198.00
196.00
196.00
194.00
194.00
192.00
192.00
190.00
190.00
188.00
1 4. 45
1 2. 49 1 2. 78
186.00 1 5. 67
1 1. 26
9.8 0
1 0. 19
184.00
1 1. 87
188.00
186.00
184.00
1 4. 88
182.00
1 6. 78
182.00
180.00
180.00 178.00 178.00 176.00 176.00 174.05
174.53 0.5 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
Retention Volume (mL)
Figure 1: Normalized Overlay of Standards.
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
30.0
Page 4 of 7
2011-12-31_11;40;00_PS1_01.vdt - Calibration Curve View
Conventional cal-0004.vcm
8.000 7.800 7.500 7.200 8.910 e 6 6.900 4.410 e 6 6.600 6.300 1.044 e 6 6.000 454,000
Log Molecular Weight
5.700 5.400
184,000 130,000
5.100 4.800 4.500 17,600 4.200 8,400 3.900 3.600
3,250
3.300 3.000 474
2.700 2.400
2.000 10.000
9.000
11.000
12.000
13.000
14.000
15.000
16.000
17.000
Retention Volume (mL)
Figure 2: Calibration Curve.
13.4
3
181.89 180.95 180.02 179.08 178.15
Refractive Index (mV)
177.21 176.27 175.34 174.40 173.47 172.53 171.60 170.66 169.72 168.79 167.85 0.00
1.43
2.86
2012-01-01_01;02;05_PPO_01.vdt:
4.29
5.71
7.14
8.57
10.00
11.43
12.86 14.29 15.71 Retention Volume (mL)
Refractive Index
Figure 3: Refractive Index (RI) Chromatogram of PPO.
17.14
18.57
20.00
21.43
22.86
24.29
25.71
27.14
28.57 30.00
Page 5 of 7
Overlay Plot: Refractive Index (mV) Vs. Retention Volume (mL) Method: Conventional cal-0004.vcm 186.08
2011-12-31_12;46;52_PS2_01.vdt / Method: Conventional cal-0002.vcm
176.00
177.00
174.00
176.00
184.00
182.00
182.00
181.00
181.00
1 6.7 8
186.00
183.00
183.00
1 4.8 8
188.00
2011-12-31_11;40;00_PS1_01.vdt / Method: Conventional cal-0003.vcm
2012-01-01_02;08;53_PPO_02.vdt / Method: Conventional cal-0004.vcm
184.00
190.00
184.00
1 0.1 9
194.00
192.00
185.00
1 1.8 7
185.00
1 5.6 7
9.8 0
196.00
1 4.4 5
186.00
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
1 2.4 9 1 2.7 8
186.85
198.00
1 1.2 6
199.38
180.00
180.00
179.00
1 3.5 6
182.00
179.00
180.00
178.00
178.00
178.00
177.00
176.00
175.00 172.00 175.00 170.09
174.43
173.83 0.1
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
30.0
Retention Volume (mL)
Figure 4: Normalized Overlay of Standards and PPO sample.
1.00 0.95 0.89 0.84 0.79 0.74 0.68
Cumulative Weight Fraction
0.63 0.58 0.53 0.47 0.42 0.37 0.32 0.26 0.21 0.16 0.11 0.05 0.00 2.00
2.24
2.48
2012-01-01_01;02;05_PPO_01.vdt:
2.71
2.95
3.19
3.43
3.67
3.90
4.14 4.38 4.62 Log Molecular Weight
Cumulative Weight Fraction
Figure 5: cumulative weight fraction curves of PPO.
4.86
5.10
5.33
5.57
5.81
6.05
6.29
6.52
6.76
7.00
7.00
0.41
6.74
0.39
6.47
0.37
6.21
0.35
5.95
0.32
5.68
0.30
5.42
0.28
5.16
0.26
4.89
0.24
4.63
0.22
4.37
0.19
4.11
0.17
3.84
0.15
3.58
0.13
3.32
0.11
3.05
0.09
2.79
0.06
2.53
0.04
2.26
0.02
Normalized Wt Fr
Log Molecular Weight
Page 6 of 7
0.00
2.00 11.04 11.31
11.58
11.85
12.13
2012-01-01_01;02;05_PPO_01.vdt:
12.40
12.67
12.94
Log Molecular Weight
13.21
14.02 13.75 13.48 Retention Volume (mL) Normalized Wt Fr
14.29
14.56
14.83
15.10
15.37
15.64
15.91
16.18 16.45
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.
Page 7 of 7
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
Kiran Rana, M.S. Chemist Jordi Labs LLC
Mark Jordi, Ph. D. President Jordi Labs LLC
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.
www.jordilabs.com
Page 1
Page 1 of 7
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
Page 2 of 7
Date Client Name Company Name
P: xxx-xxx-xxx E: [email protected]
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).
Page 3 of 7
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.
Table I. Average Molecular Weight Relative to polystyrene standards
Noryl PPO Mn 18,895 18,752
Sample 2012-01-01 01;02;05 PPO 01.vdt 2012-01-01 02;08;53 PPO 02.vdt
Mw 95,454 95,952
Mz 282,436 282,280
Mw/Mn 5.052 5.117
IV 0.0000 0.0000
Rh 0.00 0.00
Overlay Plot: Refractive Index (mV) Vs. Retention Volume (mL) Method: Conventional cal-0003.vcm 206.02 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
206.50
204.00 204.00 202.00 202.00 200.00 200.00
2011-12-31_12;46;52_PS2_01.vdt / Method: Conventional cal-0002.vcm
2011-12-31_11;40;00_PS1_01.vdt / Method: Conventional cal-0003.vcm
198.00
198.00
196.00
196.00
194.00
194.00
192.00
192.00
190.00
190.00
188.00
1 4. 45
1 2. 49 1 2. 78
186.00 1 5. 67
1 1. 26
9.8 0
1 0. 19
184.00
1 1. 87
188.00
186.00
184.00
1 4. 88
182.00
1 6. 78
182.00
180.00
180.00 178.00 178.00 176.00 176.00 174.05
174.53 0.5 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
Retention Volume (mL)
Figure 1: Normalized Overlay of Standards.
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
30.0
Page 4 of 7
2011-12-31_11;40;00_PS1_01.vdt - Calibration Curve View
Conventional cal-0004.vcm
8.000 7.800 7.500 7.200 8.910 e 6 6.900 4.410 e 6 6.600 6.300 1.044 e 6 6.000 454,000
Log Molecular Weight
5.700 5.400
184,000 130,000
5.100 4.800 4.500 17,600 4.200 8,400 3.900 3.600
3,250
3.300 3.000 474
2.700 2.400
2.000 10.000
9.000
11.000
12.000
13.000
14.000
15.000
16.000
17.000
Retention Volume (mL)
Figure 2: Calibration Curve.
13.4
3
181.89 180.95 180.02 179.08 178.15
Refractive Index (mV)
177.21 176.27 175.34 174.40 173.47 172.53 171.60 170.66 169.72 168.79 167.85 0.00
1.43
2.86
2012-01-01_01;02;05_PPO_01.vdt:
4.29
5.71
7.14
8.57
10.00
11.43
12.86 14.29 15.71 Retention Volume (mL)
Refractive Index
Figure 3: Refractive Index (RI) Chromatogram of PPO.
17.14
18.57
20.00
21.43
22.86
24.29
25.71
27.14
28.57 30.00
Page 5 of 7
Overlay Plot: Refractive Index (mV) Vs. Retention Volume (mL) Method: Conventional cal-0004.vcm 186.08
2011-12-31_12;46;52_PS2_01.vdt / Method: Conventional cal-0002.vcm
176.00
177.00
174.00
176.00
184.00
182.00
182.00
181.00
181.00
1 6.7 8
186.00
183.00
183.00
1 4.8 8
188.00
2011-12-31_11;40;00_PS1_01.vdt / Method: Conventional cal-0003.vcm
2012-01-01_02;08;53_PPO_02.vdt / Method: Conventional cal-0004.vcm
184.00
190.00
184.00
1 0.1 9
194.00
192.00
185.00
1 1.8 7
185.00
1 5.6 7
9.8 0
196.00
1 4.4 5
186.00
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
1 2.4 9 1 2.7 8
186.85
198.00
1 1.2 6
199.38
180.00
180.00
179.00
1 3.5 6
182.00
179.00
180.00
178.00
178.00
178.00
177.00
176.00
175.00 172.00 175.00 170.09
174.43
173.83 0.1
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
30.0
Retention Volume (mL)
Figure 4: Normalized Overlay of Standards and PPO sample.
1.00 0.95 0.89 0.84 0.79 0.74 0.68
Cumulative Weight Fraction
0.63 0.58 0.53 0.47 0.42 0.37 0.32 0.26 0.21 0.16 0.11 0.05 0.00 2.00
2.24
2.48
2012-01-01_01;02;05_PPO_01.vdt:
2.71
2.95
3.19
3.43
3.67
3.90
4.14 4.38 4.62 Log Molecular Weight
Cumulative Weight Fraction
Figure 5: cumulative weight fraction curves of PPO.
4.86
5.10
5.33
5.57
5.81
6.05
6.29
6.52
6.76
7.00
7.00
0.41
6.74
0.39
6.47
0.37
6.21
0.35
5.95
0.32
5.68
0.30
5.42
0.28
5.16
0.26
4.89
0.24
4.63
0.22
4.37
0.19
4.11
0.17
3.84
0.15
3.58
0.13
3.32
0.11
3.05
0.09
2.79
0.06
2.53
0.04
2.26
0.02
Normalized Wt Fr
Log Molecular Weight
Page 6 of 7
0.00
2.00 11.04 11.31
11.58
11.85
12.13
2012-01-01_01;02;05_PPO_01.vdt:
12.40
12.67
12.94
Log Molecular Weight
13.21
14.02 13.75 13.48 Retention Volume (mL) Normalized Wt Fr
14.29
14.56
14.83
15.10
15.37
15.64
15.91
16.18 16.45
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.
Page 7 of 7
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
Kiran Rana, M.S. Chemist Jordi Labs LLC
Mark Jordi, Ph. D. President Jordi Labs LLC
