S507149 

Test Report 

Measurement of the molecular weights 

”FMN-666(Original) and Stability tested samples” 

TORAY RESEARCH CENTER, INC. 

3-3-7 Sonoyama㧘Otsu City㧘Shiga 520-8567㧘

JAPAN

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  CBI 

   
S507149 

 -1- Toray Research Center, Inc.

ޤSummaryޣ

The GPC measurements of the original sample and the stability tested samples were 

performed. The results are shown in Table A. The content of components having molecular 

weight of less than 1000 was calculated of the original sample. The results are shown in Table B. 

The average molecular weights and the molecular weight distribution curves of the stability 

tested samples were almost same as those of the original sample. 

The content of the component having molecular weight of less than MW 1000 was 0.41% of 

the original sample.

Table A Average molecular weights*1

Sample Mn

*2 Mw*2 Mz*2 Mw / Mn Mz / Mw

pH 1.2 12500 25200 39600 2.02 1.57 

pH 4.0 12300 25000 39300 2.03 1.57 

pH 7.0 12600 25100 39400 1.99 1.57 

pH 9.0 12300 25100 39500 2.04 1.57 

Original 12700 25200 39500 1.98 1.57 

*1 Relative values of polystyrene standards and average of the twice measurements 

*2 Mn : Number average molecular weight 

*2 Mw : Weight average molecular weight 

*2 Mz : Z average molecular weight 

Table B Contents of components less than 

MW 1000 of the original sample* 

Run 1 0.45% 

Run 2 0.36% 

Average 0.41% 

* Calculated values from polystyrene standards 

 molecular weight 

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S507149 

 -2- Toray Research Center, Inc.

1. Sponsor 

Name Daikin Industries, LTD. 

Address 1-1, Nishi-Hitotsuya, Settsu, Osaka 566-8585, Japan 

2. Test Laboratory 

Name Toray Reserch Center, Inc. 

Address 3-3-7 Sonoyama, Otsu City, Shiga, 520-8567, Japan 

3. Objective 

The objective of this measurement are to confirm of having molecular weight change or not 

before and after stability test and to obtain contents of components having molecular weight of 

less than 1000 of FMN-666. 

4. Sample 

Copolymer of 3,3,4,4,5,5,6,6,7,7,8,8,8-tridecafluorooctyl 2-chloro-2-propenate / isobornyl 

methacrylate / stearyl acrylate (Abbreviated title: FMN-666) 

5. Experimental 

5.1 Principle 

 Gel permeation chromatography (GPC) is a family of the liquid chromatography that 

separates molecules of the polymer sample by the difference in their molecular size. The polymer 

molecules are separated in the column packed with the gels that have the pore of the same size as 

the polymer size in dilute solution (hydrodynamic volume). The high molecular weight 

component is eluted faster than the low molecular weight component because the high molecular 

weight component is slightly permeable into the pore of the gel. Therefore GPC provides the 

molecular weight distribution curve and the average molecular weights of the polymer. 

5.2 Measurement Parameters 

Apparatus Gel Permeation Chromatograph (GPC-MALS1) 

Detector Differential refractive index detector RI-8020 (TOSOH)

Data Processing system GPC Data Processing System (Toray research Center) 

Column set Column set of two TSKgel GMHXL and one TSKgel G2500HXL

(TOSOH)

Mobile Phase Tetrahydrofuran

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 -3- Toray Research Center, Inc.

Flow rate 1.0 mL/min 

Temperature 23r2͠

Sample Concentration 0.20% (w/v) 

Solubility Soluble

Filtration 0.45 Pm-Millex-LH (Millipore) 

Injection volume 0.200 mL 

the calibration curve of 

the standards Polystyrene (PS) standards (TOSOH) 

6. Results 

6.1 GPC Curve 

GPC curves of the sample are shown in Fig.1 to Fig.10. The signal of the sample was 

detected from about 20 min. to 31 min. The peaks detected after about 31 min. of the elution time 

were the solvent-composition-change, solvent-impurity and/or the system peak (It was confirmed 

by the GPC measurement of the solvent. See Fig.11).

6.2 Calibration curve of molecular weight 

The calibration curve of polystyrene (PS) standards is shown in Fig.12. The calibration curve 

was obtained from the relationship between the molecular weight and elution time under the 

same GPC conditions. In this report the calculated molecular weights were relative values of PS

standards.

3

3

2

0 1 2 log M A  A  t  A  t  A  t (1) 

where, M : Molecular weight 

t : Elution time 

Ai : Coefficients 

6.3 Calculation of molecular weight distribution (MWD) and average molecular weights

The MWD was originated by the GPC curves of the sample (Fig.1 to Fig.10) and the 

calibration curve (Fig.12) using GPC data processing system. The MWD curves and the average 

molecular weights are shown in Fig.13 to Fig.22 and Table 1. 

The average molecular weights were calculated according to Eqs. (2), (3) and (4). 

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S507149 

 -4- Toray Research Center, Inc.

Mn=Ǜ(Ni࡮Mi)/ǛNi (2) 

Mw=Ǜ(Ni࡮Mi

2)/Ǜ(Ni࡮Mi) (3) 

Mz=Ǜ(Ni࡮Mi

3)/Ǜ(Ni࡮Mi

2) (4) 

where, Mn : Number average molecular weight 

Mw : Weight average molecular weight 

Mz : Z average molecular weight 

Ni : Molar fraction at elution time ti

Mi : Molecular weight at elution time ti

The polydispersity (Mw / Mn, Mz / Mw), indicating the index of the dispersion of MWD, is 

shown in Table A. 

where , Mw / Mn : Polydispersity 

(the index of the dispersion in the low molecular weight region) 

Mz / Mw : Polydispersity 

(the index of the dispersion in the high molecular weight region) 

6.4 Content of the components less than molecular weight 1000 of the original sample 

The MWD data are shown in Table 2 and Table 3. The content of the components having the 

molecular weight of less than MW 1000 was 0.41% (average of 0.45% and 0.36%). 

7. Conclusion 

The GPC measurements of the original sample and the stability tested samples were 

performed. The results are shown in Table A. The content of components having molecular 

weight of less than 1000 was calculated of the original sample. The results are shown in Table B. 

The average molecular weights and the molecular weight distribution curves of the stability 

tested samples were almost same as those of the original sample. 

The content of the component having molecular weight of less than MW 1000 was 0.41% of 

the original sample.

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        CBI 

 CBI 
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㪪㪌㪇㪎㪈㪋㪐

1 12400 25100 39500 2.02 1.57 Fig.152 12600 25200 39600 2.00 1.57 Fig.16

Average 12500 25200 39600 2.02 1.57

1 12500 25100 39400 2.01 1.57 Fig.172 12100 24900 39100 2.06 1.57 Fig.18

Average 12300 25000 39300 2.03 1.57

1 12500 25100 39400 2.01 1.57 Fig.192 12700 25100 39300 1.98 1.57 Fig.20

Average 12600 25100 39400 1.99 1.57

1 12500 25100 39400 2.01 1.57 Fig.212 12100 25000 39500 2.07 1.58 Fig.22

Average 12300 25100 39500 2.04 1.57

1 12500 25100 39500 2.01 1.57 Fig.132 12800 25200 39400 1.97 1.56 Fig.14

Average 12700 25200 39500 1.98 1.57

* Relative values of polystyrene standards

Original

Run

pH 7.0pH 9.0

Test solution

pH 1.2pH 4.0

Molecular Weight

Distribution

Table 1 Average Molecular Weight *

M n M w M z M w/M n M z/M w

Toray Research Center, Inc.

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        CBI 
Table 6 Molecular Weight Data

Sample : FMN-666(Original,Run 1) Mn : 12500File : A10.MWD Mw : 25100Area : 500.85 mV・sec Mz : 39500Operator: Hamashige Mv :

Date : 2012/6/28 Mw/Mn: 2.01

Mz/Mw: 1.57

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Retention Molecular Intensity d(Weight) Weight % 

 Time Weight (mV) d Log(MW)  (min)

 20.26 203502 0.000 0.000 100.00 20.33 193142 0.003 0.001 100.00 20.39 183348 0.008 0.003 99.99 20.46 174086 0.013 0.005 99.98 20.53 165326 0.020 0.007 99.97 20.59 157039 0.028 0.010 99.95 20.66 149197 0.038 0.014 99.92 20.73 141774 0.050 0.018 99.89 20.79 134748 0.065 0.024 99.84 20.86 128094 0.083 0.030 99.78 20.92 121793 0.103 0.037 99.70 20.99 115824 0.127 0.046 99.61 21.06 110168 0.155 0.057 99.49 21.12 104808 0.186 0.069 99.35 21.19 99727 0.224 0.083 99.19 21.26 94909 0.267 0.099 98.99 21.32 90341 0.313 0.117 98.75 21.39 86008 0.367 0.137 98.48 21.46 81898 0.427 0.161 98.15 21.52 77998 0.494 0.186 97.78 21.59 74296 0.567 0.215 97.35 21.66 70782 0.649 0.247 96.86 21.72 67446 0.739 0.282 96.29 21.79 64278 0.835 0.320 95.66 21.86 61269 0.940 0.361 94.94 21.92 58410 1.053 0.406 94.13 21.99 55693 1.175 0.454 93.23 22.06 53112 1.305 0.506 92.23 22.12 50658 1.444 0.562 91.12 22.19 48325 1.589 0.620 89.89 22.26 46107 1.742 0.683 88.55 22.32 43997 1.900 0.747 87.08 22.39 41990 2.060 0.812 85.48 22.46 40081 2.222 0.879 83.76 22.52 38264 2.383 0.946 81.90 22.59 36535 2.538 1.010 79.92 22.66 34888 2.686 1.072 77.82 22.72 33321 2.820 1.129 75.61 22.79 31829 2.940 1.181 73.30 22.86 30407 3.039 1.225 70.90 22.92 29053 3.115 1.259 68.43 22.99 27763 3.170 1.285 65.92

Table 6 Page - 1 File : A10.MWD

2 S507149 S506740

Retention Molecular Intensity d(Weight) Weight % 

 Time Weight (mV) d Log(MW)  (min)

 23.06 26534 3.197 1.299 63.37 23.12 25362 3.198 1.304 60.82 23.19 24246 3.174 1.298 58.28 23.26 23181 3.128 1.282 55.76 23.32 22166 3.063 1.259 53.30 23.39 21198 2.986 1.231 50.89 23.46 20274 2.900 1.199 48.55 23.52 19394 2.814 1.166 46.28 23.59 18553 2.732 1.135 44.07 23.66 17751 2.654 1.105 41.93 23.72 16986 2.586 1.080 39.85 23.79 16255 2.525 1.057 37.81 23.86 15558 2.467 1.035 35.83 23.92 14892 2.413 1.015 33.88 23.99 14256 2.358 0.994 31.98 24.06 13648 2.298 0.971 30.13 24.12 13068 2.231 0.945 28.33 24.19 12514 2.157 0.916 26.58 24.26 11984 2.075 0.883 24.90 24.32 11478 1.985 0.847 23.29 24.39 10994 1.891 0.808 21.75 24.46 10532 1.793 0.768 20.29 24.52 10090 1.691 0.726 18.91 24.59 9667 1.592 0.685 17.61 24.66 9263 1.494 0.644 16.39 24.72 8877 1.401 0.605 15.24 24.79 8507 1.311 0.567 14.17 24.86 8153 1.223 0.530 13.17 24.92 7815 1.140 0.495 12.23 24.99 7491 1.063 0.462 11.36 25.06 7182 0.989 0.431 10.55 25.12 6885 0.921 0.402 9.79 25.19 6601 0.856 0.374 9.09 25.26 6330 0.797 0.349 8.44 25.32 6070 0.739 0.324 7.83 25.39 5821 0.687 0.302 7.27 25.46 5582 0.638 0.281 6.74 25.52 5354 0.591 0.260 6.26 25.59 5135 0.548 0.242 5.81 25.66 4926 0.508 0.224 5.39 25.72 4725 0.469 0.208 5.00 25.79 4533 0.435 0.193 4.65 25.86 4349 0.402 0.178 4.32 25.92 4172 0.374 0.166 4.01 25.99 4003 0.345 0.153 3.73 26.06 3841 0.319 0.142 3.46 26.12 3685 0.295 0.131 3.22 26.19 3536 0.272 0.121 3.00 26.26 3394 0.251 0.112 2.79

Table 6 Page - 2 File : A10.MWD

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Retention Molecular Intensity d(Weight) Weight % 

 Time Weight (mV) d Log(MW)  (min)

 26.32 3257 0.230 0.103 2.60 26.39 3125 0.212 0.095 2.43 26.46 2999 0.196 0.088 2.27 26.52 2879 0.180 0.081 2.12 26.59 2763 0.165 0.074 1.98 26.66 2652 0.151 0.068 1.86 26.72 2545 0.140 0.063 1.74 26.79 2443 0.129 0.058 1.63 26.86 2345 0.118 0.053 1.54 26.92 2251 0.109 0.049 1.45 26.99 2161 0.100 0.045 1.36 27.06 2074 0.091 0.041 1.29 27.12 1991 0.083 0.037 1.22 27.19 1911 0.076 0.034 1.16 27.26 1835 0.070 0.032 1.10 27.32 1761 0.064 0.029 1.05 27.39 1691 0.060 0.027 1.00 27.46 1623 0.054 0.024 0.95 27.52 1558 0.052 0.023 0.91 27.59 1496 0.049 0.022 0.87 27.66 1436 0.049 0.022 0.83 27.72 1379 0.048 0.022 0.80 27.79 1324 0.050 0.022 0.76 27.86 1271 0.051 0.023 0.72 27.92 1220 0.057 0.026 0.67 27.99 1171 0.064 0.029 0.62 28.06 1124 0.070 0.032 0.57 28.12 1079 0.072 0.032 0.51 28.19 1036 0.070 0.031 0.45 28.26 994 0.062 0.028 0.40 28.32 954 0.053 0.024 0.36 28.39 916 0.043 0.019 0.32 28.46 879 0.033 0.015 0.29 28.52 844 0.026 0.012 0.27 28.59 810 0.020 0.009 0.25 28.66 777 0.017 0.008 0.24 28.72 746 0.015 0.007 0.22 28.79 716 0.012 0.005 0.21 28.86 687 0.011 0.005 0.20 28.92 659 0.010 0.004 0.20 28.99 633 0.010 0.004 0.19 29.06 607 0.008 0.004 0.18 29.12 583 0.010 0.005 0.17 29.19 559 0.014 0.006 0.16 29.25 536 0.020 0.009 0.15 29.32 515 0.023 0.010 0.13 29.39 494 0.025 0.011 0.11 29.45 474 0.024 0.011 0.09 29.52 454 0.021 0.009 0.07

Table 6 Page - 3 File : A10.MWD

S507149 S506740

Retention Molecular Intensity d(Weight) Weight % 

 Time Weight (mV) d Log(MW)  (min)

 29.59 436 0.016 0.007 0.06 29.65 418 0.011 0.005 0.05 29.72 401 0.008 0.003 0.04 29.79 384 0.005 0.002 0.04 29.85 369 0.004 0.002 0.04 29.92 353 0.002 0.001 0.03 29.99 339 0.001 0.001 0.03 30.05 325 0.002 0.001 0.03 30.12 311 0.002 0.001 0.03 30.19 299 0.003 0.001 0.03 30.25 286 0.003 0.001 0.03 30.32 274 0.005 0.002 0.02 30.39 263 0.005 0.002 0.02 30.45 252 0.005 0.002 0.01 30.52 241 0.005 0.002 0.01 30.59 231 0.004 0.002 0.01 30.65 222 0.003 0.001 0.00 30.72 212 0.003 0.001 0.00 30.79 203 0.002 0.001 0.00

Table 6 Page - 4 File : A10.MWD

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Table 7 Molecular Weight Data

Sample : FMN-666(Original,Run 2) Mn : 12800File : A11.MWD Mw : 25200Area : 493.61 mV・sec Mz : 39400Operator: Hamashige Mv :

Date : 2012/6/28 Mw/Mn: 1.97

Mz/Mw: 1.56

S506740

Retention Molecular Intensity d(Weight) Weight % 

 Time Weight (mV) d Log(MW)  (min)

 20.26 203502 0.000 0.000 100.00 20.33 193142 0.003 0.001 100.00 20.39 183348 0.006 0.002 99.99 20.46 174086 0.012 0.004 99.99 20.53 165326 0.020 0.007 99.97 20.59 157039 0.028 0.010 99.95 20.66 149197 0.037 0.014 99.93 20.73 141774 0.050 0.018 99.89 20.79 134748 0.065 0.024 99.84 20.86 128094 0.081 0.030 99.78 20.92 121793 0.100 0.037 99.71 20.99 115824 0.125 0.047 99.61 21.06 110168 0.152 0.057 99.50 21.12 104808 0.184 0.069 99.36 21.19 99727 0.221 0.083 99.19 21.26 94909 0.261 0.099 98.99 21.32 90341 0.309 0.117 98.76 21.39 86008 0.362 0.137 98.48 21.46 81898 0.421 0.161 98.16 21.52 77998 0.487 0.187 97.79 21.59 74296 0.559 0.215 97.36 21.66 70782 0.639 0.247 96.86 21.72 67446 0.727 0.281 96.30 21.79 64278 0.823 0.320 95.66 21.86 61269 0.927 0.361 94.94 21.92 58410 1.039 0.406 94.14 21.99 55693 1.159 0.455 93.23 22.06 53112 1.287 0.507 92.23 22.12 50658 1.424 0.562 91.12 22.19 48325 1.568 0.621 89.90 22.26 46107 1.719 0.683 88.55 22.32 43997 1.875 0.748 87.08 22.39 41990 2.033 0.814 85.48 22.46 40081 2.194 0.881 83.75 22.52 38264 2.354 0.948 81.89 22.59 36535 2.508 1.013 79.91 22.66 34888 2.654 1.075 77.80 22.72 33321 2.787 1.133 75.58 22.79 31829 2.905 1.184 73.27 22.86 30407 3.003 1.228 70.86 22.92 29053 3.080 1.263 68.39 22.99 27763 3.132 1.288 65.87

Table 7 Page - 1 File : A11.MWD

3 S507149 S506740

Retention Molecular Intensity d(Weight) Weight % 

 Time Weight (mV) d Log(MW)  (min)

 23.06 26534 3.160 1.303 63.31 23.12 25362 3.161 1.308 60.75 23.19 24246 3.137 1.301 58.20 23.26 23181 3.091 1.286 55.68 23.32 22166 3.029 1.263 53.21 23.39 21198 2.952 1.235 50.79 23.46 20274 2.869 1.203 48.44 23.52 19394 2.784 1.170 46.16 23.59 18553 2.702 1.139 43.95 23.66 17751 2.627 1.110 41.80 23.72 16986 2.559 1.084 39.71 23.79 16255 2.498 1.061 37.66 23.86 15558 2.443 1.040 35.67 23.92 14892 2.389 1.020 33.72 23.99 14256 2.333 0.998 31.81 24.06 13648 2.274 0.975 29.95 24.12 13068 2.206 0.948 28.14 24.19 12514 2.133 0.919 26.39 24.26 11984 2.052 0.886 24.70 24.32 11478 1.963 0.849 23.09 24.39 10994 1.869 0.810 21.54 24.46 10532 1.773 0.770 20.08 24.52 10090 1.672 0.728 18.69 24.59 9667 1.573 0.686 17.39 24.66 9263 1.477 0.646 16.16 24.72 8877 1.384 0.606 15.02 24.79 8507 1.292 0.567 13.94 24.86 8153 1.206 0.530 12.94 24.92 7815 1.124 0.495 12.00 24.99 7491 1.047 0.462 11.13 25.06 7182 0.975 0.431 10.32 25.12 6885 0.907 0.402 9.57 25.19 6601 0.844 0.374 8.86 25.26 6330 0.785 0.349 8.21 25.32 6070 0.728 0.324 7.60 25.39 5821 0.676 0.301 7.04 25.46 5582 0.627 0.280 6.52 25.52 5354 0.581 0.259 6.03 25.59 5135 0.538 0.241 5.58 25.66 4926 0.498 0.223 5.17 25.72 4725 0.460 0.206 4.79 25.79 4533 0.426 0.192 4.43 25.86 4349 0.395 0.177 4.10 25.92 4172 0.365 0.164 3.80 25.99 4003 0.335 0.151 3.52 26.06 3841 0.309 0.139 3.26 26.12 3685 0.285 0.129 3.02 26.19 3536 0.262 0.118 2.80 26.26 3394 0.240 0.109 2.60

Table 7 Page - 2 File : A11.MWD

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Retention Molecular Intensity d(Weight) Weight % 

 Time Weight (mV) d Log(MW)  (min)

 26.32 3257 0.220 0.100 2.42 26.39 3125 0.204 0.092 2.25 26.46 2999 0.188 0.085 2.09 26.52 2879 0.174 0.079 1.94 26.59 2763 0.160 0.072 1.81 26.66 2652 0.146 0.067 1.69 26.72 2545 0.133 0.061 1.58 26.79 2443 0.123 0.056 1.47 26.86 2345 0.113 0.051 1.38 26.92 2251 0.103 0.047 1.29 26.99 2161 0.093 0.042 1.21 27.06 2074 0.086 0.039 1.14 27.12 1991 0.077 0.035 1.08 27.19 1911 0.070 0.032 1.02 27.26 1835 0.064 0.029 0.97 27.32 1761 0.060 0.028 0.92 27.39 1691 0.054 0.025 0.87 27.46 1623 0.050 0.023 0.83 27.52 1558 0.047 0.022 0.79 27.59 1496 0.046 0.021 0.75 27.66 1436 0.045 0.021 0.71 27.72 1379 0.044 0.020 0.68 27.79 1324 0.045 0.020 0.64 27.86 1271 0.047 0.021 0.61 27.92 1220 0.052 0.024 0.57 27.99 1171 0.059 0.027 0.52 28.06 1124 0.064 0.029 0.47 28.12 1079 0.066 0.030 0.42 28.19 1036 0.063 0.029 0.36 28.26 994 0.055 0.025 0.32 28.32 954 0.046 0.021 0.28 28.39 916 0.036 0.016 0.24 28.46 879 0.027 0.012 0.22 28.52 844 0.020 0.009 0.20 28.59 810 0.015 0.007 0.19 28.66 777 0.012 0.005 0.18 28.72 746 0.008 0.004 0.17 28.79 716 0.007 0.003 0.16 28.86 687 0.005 0.002 0.16 28.92 659 0.006 0.003 0.15 28.99 633 0.005 0.002 0.15 29.06 607 0.006 0.003 0.15 29.12 583 0.009 0.004 0.14 29.19 559 0.011 0.005 0.13 29.25 536 0.015 0.007 0.12 29.32 515 0.020 0.009 0.10 29.39 494 0.021 0.009 0.09 29.45 474 0.020 0.009 0.07 29.52 454 0.017 0.008 0.06

Table 7 Page - 3 File : A11.MWD

S507149 S506740

Retention Molecular Intensity d(Weight) Weight % 

 Time Weight (mV) d Log(MW)  (min)

 29.59 436 0.014 0.006 0.04 29.65 418 0.011 0.005 0.03 29.72 401 0.007 0.003 0.03 29.79 384 0.004 0.002 0.02 29.85 369 0.002 0.001 0.02 29.92 353 0.000 0.000 0.02 29.99 339 0.000 0.000 0.02 30.05 325 0.000 0.000 0.02 30.12 311 0.000 0.000 0.02 30.19 299 0.000 0.000 0.02 30.25 286 0.002 0.001 0.02 30.32 274 0.003 0.001 0.02 30.39 263 0.003 0.001 0.02 30.45 252 0.004 0.002 0.01 30.52 241 0.004 0.002 0.01 30.59 231 0.004 0.002 0.01 30.65 222 0.003 0.001 0.00 30.72 212 0.002 0.001 0.00 30.79 203 0.001 0.000 0.00

Table 7 Page - 4 File : A11.MWD

S507149

㼀㻿㻙㻲㻠㻠㻠㻸㻷 㻭㼠㼠㼍㼏㼔㼙㼑㼚㼠㻌㻝

㻼㼍㼓㼑㻌㻌㻝㻝㻛㻞㻞
15 20 25 30 35 40

0

1

2

3

4

5

6

7

8

Date :

Column : Operator :

Apparatus : Temperature :

Injection Volume : Detector :

Concentration : Flow Rate :

Sample : Solvent :

2012/06/28

TSKgel GMHXL(2),G2500HXL(1) Hamashige

GPC-MALLS(1) 23.0°C

0.200 mL RI 32x 

0.20 % 1.0 mL/min

FMN-666(Original,Run 1) THF

Fig . 2-1 Gel Permeation Chromatogram

Toray Research Center Inc.

File: A10

Retention Time (min)

RI Intensity

m

V

1

15 20 25 30 35 40

0

1

2

3

4

5

6

7

8

Date :

Column : Operator :

Apparatus : Temperature :

Injection Volume : Detector :

Concentration : Flow Rate :

Sample : Solvent :

2012/06/28

TSKgel GMHXL(2),G2500HXL(1) Hamashige

GPC-MALLS(1) 23.0°C

0.200 mL RI 32x 

0.20 % 1.0 mL/min

FMN-666(Original,Run 2) THF

Fig . 2-2 Gel Permeation Chromatogram

Toray Research Center Inc.

File: A11

Retention Time (min)

RI Intensity

m

V

2

㼀㻿㻙㻲㻠㻠㻠㻸㻷 㻭㼠㼠㼍㼏㼔㼙㼑㼚㼠㻌㻝

㻼㼍㼓㼑㻌㻌㻝㻞㻛㻞㻞
15 20 25 30 35 40

0

1

2

3

4

5

6

7

8

Date :

Column : Operator :

Apparatus : Temperature :

Injection Volume : Detector :

Concentration : Flow Rate :

Sample : Solvent :

2012/06/28

TSKgel GMHXL(2),G2500HXL(1) Hamashige

GPC-MALLS(1) 23.0°C

0.200 mL RI 32x 

0.20 % 1.0 mL/min

FMN-666(pH 1.2-1) THF

Fig . 2-3 Gel Permeation Chromatogram

Toray Research Center Inc.

File: A14

Retention Time (min)

RI Intensity

m

V

3

15 20 25 30 35 40

0

1

2

3

4

5

6

7

8

Date :

Column : Operator :

Apparatus : Temperature :

Injection Volume : Detector :

Concentration : Flow Rate :

Sample : Solvent :

2012/06/28

TSKgel GMHXL(2),G2500HXL(1) Hamashige

GPC-MALLS(1) 23.0°C

0.200 mL RI 32x 

0.20 % 1.0 mL/min

FMN-666(pH 1.2-2) THF

Fig . 2-4 Gel Permeation Chromatogram

Toray Research Center Inc.

File: A18

Retention Time (min)

RI Intensity

m

V

4

㼀㻿㻙㻲㻠㻠㻠㻸㻷 㻭㼠㼠㼍㼏㼔㼙㼑㼚㼠㻌㻝

㻼㼍㼓㼑㻌㻌㻝㻟㻛㻞㻞
15 20 25 30 35 40

0

1

2

3

4

5

6

7

8

Date :

Column : Operator :

Apparatus : Temperature :

Injection Volume : Detector :

Concentration : Flow Rate :

Sample : Solvent :

2012/06/28

TSKgel GMHXL(2),G2500HXL(1) Hamashige

GPC-MALLS(1) 23.0°C

0.200 mL RI 32x 

0.20 % 1.0 mL/min

FMN-666(pH 4.0-1) THF

Fig . 2-5 Gel Permeation Chromatogram

Toray Research Center Inc.

File: A15

Retention Time (min)

RI Intensity

m

V

5

15 20 25 30 35 40

0

1

2

3

4

5

6

7

8

Date :

Column : Operator :

Apparatus : Temperature :

Injection Volume : Detector :

Concentration : Flow Rate :

Sample : Solvent :

2012/06/28

TSKgel GMHXL(2),G2500HXL(1) Hamashige

GPC-MALLS(1) 23.0°C

0.200 mL RI 32x 

0.20 % 1.0 mL/min

FMN-666(pH 4.0-2) THF

Fig . 2-6 Gel Permeation Chromatogram

Toray Research Center Inc.

File: A19

Retention Time (min)

RI Intensity

m

V

6

㼀㻿㻙㻲㻠㻠㻠㻸㻷 㻭㼠㼠㼍㼏㼔㼙㼑㼚㼠㻌㻝

㻼㼍㼓㼑㻌㻌㻝㻠㻛㻞㻞
15 20 25 30 35 40

0

1

2

3

4

5

6

7

8

Date :

Column : Operator :

Apparatus : Temperature :

Injection Volume : Detector :

Concentration : Flow Rate :

Sample : Solvent :

2012/06/28

TSKgel GMHXL(2),G2500HXL(1) Hamashige

GPC-MALLS(1) 23.0°C

0.200 mL RI 32x 

0.20 % 1.0 mL/min

FMN-666(pH 7.0-1) THF

Fig . 2-7 Gel Permeation Chromatogram

Toray Research Center Inc.

File: A16

Retention Time (min)

RI Intensity

m

V

7

15 20 25 30 35 40

0

1

2

3

4

5

6

7

8

Date :

Column : Operator :

Apparatus : Temperature :

Injection Volume : Detector :

Concentration : Flow Rate :

Sample : Solvent :

2012/06/28

TSKgel GMHXL(2),G2500HXL(1) Hamashige

GPC-MALLS(1) 23.0°C

0.200 mL RI 32x 

0.20 % 1.0 mL/min

FMN-666(pH 7.0-2) THF

Fig . 2-8 Gel Permeation Chromatogram

Toray Research Center Inc.

File: A20

Retention Time (min)

RI Intensity

m

V

8

㼀㻿㻙㻲㻠㻠㻠㻸㻷 㻭㼠㼠㼍㼏㼔㼙㼑㼚㼠㻌㻝

㻼㼍㼓㼑㻌㻌㻝㻡㻛㻞㻞
15 20 25 30 35 40

0

1

2

3

4

5

6

7

8

Date :

Column : Operator :

Apparatus : Temperature :

Injection Volume : Detector :

Concentration : Flow Rate :

Sample : Solvent :

2012/06/28

TSKgel GMHXL(2),G2500HXL(1) Hamashige

GPC-MALLS(1) 23.0°C

0.200 mL RI 32x 

0.20 % 1.0 mL/min

FMN-666(pH 9.0-1) THF

Fig . 2-9 Gel Permeation Chromatogram

Toray Research Center Inc.

File: A17

Retention Time (min)

RI Intensity

m

V

9

15 20 25 30 35 40

0

1

2

3

4

5

6

7

8

Date :

Column : Operator :

Apparatus : Temperature :

Injection Volume : Detector :

Concentration : Flow Rate :

Sample : Solvent :

2012/06/28

TSKgel GMHXL(2),G2500HXL(1) Hamashige

GPC-MALLS(1) 23.0°C

0.200 mL RI 32x 

0.20 % 1.0 mL/min

FMN-666(pH 9.0-2) THF

Fig . 2-10 Gel Permeation Chromatogram

Toray Research Center Inc.

File: A21

Retention Time (min)

RI Intensity

m

V

10

㼀㻿㻙㻲㻠㻠㻠㻸㻷 㻭㼠㼠㼍㼏㼔㼙㼑㼚㼠㻌㻝

㻼㼍㼓㼑㻌㻌㻝㻢㻛㻞㻞
15 20 25 30 35 40

0

1

2

3

4

5

6

7

8

Date :

Column : Operator :

Apparatus : Temperature :

Injection Volume : Detector :

Concentration : Flow Rate :

Sample : Solvent :

2012/06/28

TSKgel GMHXL(2),G2500HXL(1) Hamashige

GPC-MALLS(1) 23.0°C

0.200 mL RI 32x 

- 1.0 mL/min

Solvent THF

Fig . 2-11 Gel Permeation Chromatogram

Toray Research Center Inc.

File: A13

Retention Time (min)

RI Intensity

m

V

11

18 20 22 24 26 28 30 32

0

1

2

3

4

5

6

7

8

9

10

Flow Rate :

Solvent : Date :

Column : Operator :

Apparatus : Temperature :

Sample : Detector :

1.0 mL/min

THF 2012/06/28

TSKgel GMHXL(2),G2500HXL(1) Hamashige

GPC-MALLS(1) 23.0°C

Polystyrene RI 32x

Fig . 2-12 Calibration Curve

Toray Research Center Inc.

File: C02.BXX

Log(MW) = A(0) + A(1)T + A(2)T2+ A(3)T3+・・・ Coefficient(Order: 3)

 A(0) : 20.32576

 A(1) : -1.333435

 A(2) : 3.871096E-02

 A(3) :-4.679954E-04

Molecular Weight Data

 RT(min) MW

19.29 427000

20.38 190000

21.34 96400

22.54 37900

23.56 18100

24.41 10200

25.32 5970

26.81 2630

28.24 1010

29.09 578

Retention Time (min)

L

o

g

M

olecular Weight

12

㼀㻿㻙㻲㻠㻠㻠㻸㻷 㻭㼠㼠㼍㼏㼔㼙㼑㼚㼠㻌㻝

㻼㼍㼓㼑㻌㻌㻝㻣㻛㻞㻞

  CBI 
102 103 104 105 106

0.0

0.2

0.4

0.6

0.8

1.0

1.2

1.4

1.6

1.8

2.0

Mz : Mz/Mw :

Mw : Mw/Mn : Date :

Mn : Mv : Operator :

 39500 1.57

 25100 2.01 2012/06/28

 12500 Hamashige

Sample: FMN-666(Original,Run 1)

Fig . 2-13 Molecular Weight Distribution Curve

Toray Research Center Inc.

File: A10.MWD

Molecular Weight

d

W

/

d

L

o

g

M

13

102 103 104 105 106

0.0

0.2

0.4

0.6

0.8

1.0

1.2

1.4

1.6

1.8

2.0

Mz : Mz/Mw :

Mw : Mw/Mn : Date :

Mn : Mv : Operator :

 39400 1.56

 25200 1.97 2012/06/28

 12800 Hamashige

Sample: FMN-666(Original,Run 2)

Fig . 2-14 Molecular Weight Distribution Curve

Toray Research Center Inc.

File: A11.MWD

Molecular Weight

d

W

/

d

L

o

g

M

14

㼀㻿㻙㻲㻠㻠㻠㻸㻷 㻭㼠㼠㼍㼏㼔㼙㼑㼚㼠㻌㻝

㻼㼍㼓㼑㻌㻌㻝㻤㻛㻞㻞

CBI

CBI

CBI

CBI

CBI CBI
102 103 104 105 106

0.0

0.2

0.4

0.6

0.8

1.0

1.2

1.4

1.6

1.8

2.0

Mz : Mz/Mw :

Mw : Mw/Mn : Date :

Mn : Mv : Operator :

 39500 1.57

 25100 2.02 2012/06/28

 12400 Hamashige

Sample: FMN-666(pH 1.2-1)

Fig . 2-15 Molecular Weight Distribution Curve

Toray Research Center Inc.

File: A14.MWD

Molecular Weight

d

W

/

d

L

o

g

M

15

102 103 104 105 106

0.0

0.2

0.4

0.6

0.8

1.0

1.2

1.4

1.6

1.8

2.0

Mz : Mz/Mw :

Mw : Mw/Mn : Date :

Mn : Mv : Operator :

 39600 1.57

 25200 2.00 2012/06/28

 12600 Hamashige

Sample: FMN-666(pH 1.2-2)

Fig . 2-16 Molecular Weight Distribution Curve

Toray Research Center Inc.

File: A18.MWD

Molecular Weight

d

W

/

d

L

o

g

M

16

㼀㻿㻙㻲㻠㻠㻠㻸㻷 㻭㼠㼠㼍㼏㼔㼙㼑㼚㼠㻌㻝

㻼㼍㼓㼑㻌㻌㻝㻥㻛㻞㻞

CBI CBI

CBI

CBI

CBI

CBI
102 103 104 105 106

0.0

0.2

0.4

0.6

0.8

1.0

1.2

1.4

1.6

1.8

2.0

Mz : Mz/Mw :

Mw : Mw/Mn : Date :

Mn : Mv : Operator :

 39400 1.57

 25100 2.01 2012/06/28

 12500 Hamashige

Sample: FMN-666(pH 4.0-1)

Fig . 2-17 Molecular Weight Distribution Curve

Toray Research Center Inc.

File: A15.MWD

Molecular Weight

d

W

/

d

L

o

g

M

17

102 103 104 105 106

0.0

0.2

0.4

0.6

0.8

1.0

1.2

1.4

1.6

1.8

2.0

Mz : Mz/Mw :

Mw: Mw/ Mn : Dat e :

Mn: Mv: Oper at or :

 39100 1. 57

 24900 2. 06 2012/ 06/ 28

 12100 Hamashi ge

Sample: FMN-666(pH 4.0-2)

Fig . 2-18 Molecular Weight Distribution Curve

Toray Research Center Inc.

File: A19.MWD

Molecular Weight

d

W

/

d

L

o

g

M

18

㼀㻿㻙㻲㻠㻠㻠㻸㻷 㻭㼠㼠㼍㼏㼔㼙㼑㼚㼠㻌㻝

㻼㼍㼓㼑㻌㻌㻞㻜㻛㻞㻞

CBI

CBI

CBI

CBI

CBI

CBI
102 103 104 105 106

0.0

0.2

0.4

0.6

0.8

1.0

1.2

1.4

1.6

1.8

2.0

Mz : Mz/Mw :

Mw : Mw/Mn : Date :

Mn : Mv : Operator :

 39400 1.57

 25100 2.01 2012/06/28

 12500 Hamashige

Sample: FMN-666(pH 7.0-1)

Fig . 2-19 Molecular Weight Distribution Curve

Toray Research Center Inc.

File: A16.MWD

Molecular Weight

d

W

/

d

L

o

g

M

19

102 103 104 105 106

0.0

0.2

0.4

0.6

0.8

1.0

1.2

1.4

1.6

1.8

2.0

Mz : Mz/Mw :

Mw : Mw/Mn : Date :

Mn : Mv : Operator :

 39300 1.57

 25100 1.98 2012/06/28

 12700 Hamashige

Sample: FMN-666(pH 7.0-2)

Fig . 2-20 Molecular Weight Distribution Curve

Toray Research Center Inc.

File: A20.MWD

Molecular Weight

d

W

/

d

L

o

g

M

20

㼀㻿㻙㻲㻠㻠㻠㻸㻷 㻭㼠㼠㼍㼏㼔㼙㼑㼚㼠㻌㻝

㻼㼍㼓㼑㻌㻌㻞㻝㻛㻞㻞

CBI

CBI

CBI

CBI

CBI

CBI
102 103 104 105 106

0.0

0.2

0.4

0.6

0.8

1.0

1.2

1.4

1.6

1.8

2.0

Mz : Mz/Mw :

Mw : Mw/Mn : Date :

Mn : Mv : Operator :

 39400 1.57

 25100 2.01 2012/06/28

 12500 Hamashige

Sample: FMN-666(pH 9.0-1)

Fig . 2-21 Molecular Weight Distribution Curve

Toray Research Center Inc.

File: A17.MWD

Molecular Weight

d

W

/

d

L

o

g

M

21

102 103 104 105 106

0.0

0.2

0.4

0.6

0.8

1.0

1.2

1.4

1.6

1.8

2.0

Mz : Mz/Mw :

Mw : Mw/Mn : Date :

Mn : Mv : Operator :

 39500 1.58

 25000 2.07 2012/06/28

 12100 Hamashige

Sample: FMN-666(pH 9.0-2)

Fig . 2-22 Molecular Weight Distribution Curve

Toray Research Center Inc.

File: A21.MWD

Molecular Weight

d

W

/

d

L

o

g

M

22

㼀㻿㻙㻲㻠㻠㻠㻸㻷 㻭㼠㼠㼍㼏㼔㼙㼑㼚㼠㻌㻝

㻼㼍㼓㼑㻌㻌㻞㻞㻛㻞㻞

   CBI    CBI

   CBI 

   CBI    CBI

   CBI