0 

0 

Measurement of the molecular weights 

ICBI 

CBI 
0 

0 

Number average molecular weight (M11) 

Weight average molecular weight (Mw) Z average molecular weight (M2 ) 

Polydispersity (Mwi Mn) 

Polydispersity (M2 I Mw) 

Content of component < MW 1 000 Content of component < MW 500 

*relative values of polystyrene standards 

-1-
0 

3. Objective 

The objective of tllis measurement is to obtain the average molecular weights and contents 

of components having molecular weight of less than 1000 and less than 500 of ... IC_BI __ .....;__. 

4. Sample 

CBI 

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 (hydrodynanlic 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-19) 

Detector Differential refractive index detector RI-8020 (TOSOH) 

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

Column set Column set of three TSKgel MultiporeHXL-M (TOSOH) 

Mobile Phase Tetrahydrofuran 

-2-
0 

0 

6. Results 

6.1 GPC Curve 

The GPC curve of the sample is shown in Fig.1 and Fig.2. The signal of the .eluted sample 

was detected from about 18 min. to 33 min. The peaks detected after about 33 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.3). 

6.2 Calibration curve of molecular weight 

The calibration curve of polystyrene (PS) standards is shown in Fig.4. 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. 

log M 

where, M : Molecular weight 

: Elution time 

Ai : Coefficients 

(1) 

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

The MWD was originated by the RI curves of the sample (Fig. I and Fig.2) and the calibration 

curve (Fig.4) using GPC data processing system. The MWD curve and the average molecular 

weights are shown in Fig.5, Fig.6 and Table A, respectively. 

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

/ 

M ="L-(N· • M·)I<£N· n z z z (2) 

-3-
0 

0 

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

shown in Table A 

where , Mw I Mn : Polydispersity 

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

Mz I Mw : Polydispersity 

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

6.4 Content of the components less than molecular weight 1000 and 500 

The raw data of MWD calculated according to the section 6.3 are shown in Table 1 and 

Table 2. The content of the components having molecular weight of less than 1000 and less than 

500 were ICBI I 

7. Conclusion 

The measurements of the average molecular weights and the contents of components 

molecular weight of less than 1000 and less than 500 ofiCBI I were carried out using GPC. The 

number average molecular weight and the weight ayerage molecular weight of the sample were 

ICBI I respectively. The content of the components having molecular weight of less 

than 1000 and less than 500 were .... IC_BI ____ __, 

-4- .___rs• ____ __.l-
0 

0 

g

y 

; 

/ 

r . 

Study Director : Kazutomo Akasaka 

Signature: Date: 

-5-
0 

Table 1 Molecular Weight Data 

,_,, Flf~ . I ADS:' . Ql() -·''"'I . " llw l . ..: .• , :1 - Ar~a : 278. 00 1V • sec liz : .~-' ~ -:. 

O!lerator: Hamuhise llv : .J: :: · . Oat~ : 2013/9/4 llw/lln: ~-~'i· - .. · llz!l.lw: · -.: .. 

Retention llolecular Intens

ity d!!ei&btl 

Tile leisht IIIVl d LogOftl 

J.i nl 

18. 23 441128 Q. 000 

0. 000 

18. 32 422401 0. 000 D. 000 

18. 40 404469 . 0. 002 . 0. 002 

18.48 387298 0. 003 0. 003 

18. 57 370856 0. 003 0. 003 

18. 65 355113 0. 006 0. 006 

18.73 340038 D. 006 D. 006 

18.82 325602 0. 007 D. 007 

18.90 311780 0. 009 0. 008 

18.98 298544 0. 011 0. 011 

19.07 285870 ' 0. 014 0. 013 

19. 15 273734 0. 015 0. 014 

19. 23 262114 0. 018 0. 017 

19. 32 250986 0. 022 0. 021 

19. 40 240331 0. 025 0.024 

19. 48 230129 0. 027 0. 026 

19. 57 220359 0. 031 0. 029 

19.65 211005 0. 035 0. 033 

19. 73 202047 0. 040 

0. 039 

19. 82 193470 0. 046 0. 044 

19.90 185256 0. 050 D. 048 

19.98 177392 0. 056 0. 054 

20. 07 169861 0. 063 0. 060 

20. 15 162650 0. 069 

0. 066 

20. 23 155745 0.077 D. 073 

20. 32 149134 0. 085 D. 081 

20. 40 142803 0. 092 0. 088 

20. 48 136740 0. 101 D. 096 

20. 57 130935 

0. 111 

0. 106 

20. 65 125377 

0. 120 0. 115 

20.73 120054 0.131 0. 125 

20.82 114958 0. 

142 0. 136 

20.90 110078 0. 154 0. 147 

20. 98 105405 0. 168 0. 160 

21.07 100930 0. 181 0. 173 

21. 15 96645 

0. 195 0. 187 

21. 23 92542 0. 211 0. 201 

21. 32 88614 0. 227 0. 217 

21. 40 84852 0. 243 0. 232 

21. 48 81250 0. 260 0. 248 

21. 57 77800 0. 278 0. 266 

21. 65 W98 0. 297 0. 283 

-

File : AOS.Iml 

SSD7883 

Weight X 

100. 00 

100.00 

100. 00 

99.99 

99. 99 

99.98 

99. 97 

99. 95 

99.94 ' 

99. 92 I 99. 90 

99.87 

99. 84 

99. 80 

99.76 

99. 71 

99. 66 

99.60 

99. 53 

99. 45 

99. 37 

99. 27 

99. 16 

99. 04 

98. 91 

98. 76 

98. 60 

98. 43 

98. 24 

98. 03 

97.80 

97.55 

97.28 

96. 99 

96. 67 

96. 33 

95. 96 

95

. 57 

95.14 

94. 69 

94. 20 

93.68 

Table 1 Page - 1 

0 

Retention llolecular Intensity 

Ti1e Weiaht (mV) 

IIi n) 

21. 73 71335 0. 316 

21. 82 68307 . 

0. 336 

21. 90 65~07 0. 358 

21. 98 62630 o. 380 

22. 07 59971 

0. 402 

22. 15 57426 

0. 426 

22. 23 54988 0. 449 

22. 32 52653 o ..m 

2Z. 40 50418 0. ~98 

22.48 48278 0. 523 

22. 57 ~6228 0. 548 

22. 65 ~4266 

0. 575 

22.73 ~2387 

0. 602 

22. 82 40587 

0. 628 

22. 90 38864 0. 656 

22. 98 37214 0. 683 

23. 07 35634 

0. 710 

2l. 15 34122 D. 737 

23. 23 32673 o. 765 

23. 32 31286 0. 792 

23. 40 29958 

0. 819 

2l48 28686 0. 845 

23. 57 27468 6.371 

2l65 26302 0. 896 

23. 73 25186 0. 919 

2l. 82 24116 o. 943 

2l. 90 23093 

0. 964 

2198 22112 0. 984 

24. 07 21174 1. 003 

24. 15 20275 

1. 018 

24. 23 19414 

1. 032 

24. 32 18590 

1. 043 

24. 40 17801 1. 051 

24. 48 17045 

1. 056 

24. 57 16321 

1. 058 

24. 65 15629 

1. 057 

24. 73 14965 

1. 054 

24.82 W30 1. 046 

24. 90 13721 1. 035 

2.(. 98 13139 

1. 021 

25. 07 12581 1. 005 

25. 15 12047 0. 985 

25.23 11536 

D. 965 

25. 32 11046 D. 941 

25. 40 10577 Q. 915 

25.48 10128 0. 888 

25. 57 9698 o. 859 

25.65 9286 0. 830 

25.73 8892 0. 799 

f ile : AOS.ItiD 

d !rci&bll 

d Los Mil D. 302 

0. 321 0. 341 

D. 363 

D. 384 

0. 406 

D. 429 

0. 452 

0 475 

0. 499 

0. 524 0. 549 

D. 575 

D. 600 

0. 626 

D. 652 

0.677 

D. 704 

D. 731 0. 756 0. 782 0. 807 

0. 831 0. 855 

D. 878 

D. 900 0. 920 0. 940 

D. 957 0. 972 

D. 985 0. 996 

1. 004 

1. 008 

1. 010 

1. 009 1. 006 

0. 999 0. 988 0. 974 

D. 959 0. 941 

D. 921 

0. 898 0. 874 

D. 848 o. 820 0. 792 o. 763 

S507883 

leiaht X 

93. 13 

92. 54 

91.91 

91.24 

90. 53 

39.79 

88. 99 

88. 16 

87. 28 

86. 36 

85. 39 

84. 38 

83.32 

82. 20 

81.04 

79. 83 

78. 58 

77. 27 

75.92 

1~- 51 

73. 06 

71.56 

70. 01 

68. 41 

66.78 

65. 10 

63. 38 

61. 62 

59. 83 

58.01 

56.17 

54.30 

5Z. 41 

50. 52 

48. 62 

46.71 

44. 82 

42. 93 

41.06 

39. 21 

37. 39 ' 

35. 51 

33.86 

32. 15 

30. 48 

28. 86 

27. 30 

25.78 

24.33 

-; 

(/) 

I 

::><; 

..., 

"' .... 

-< 

0 

)> 

-u:+ 

.. .. ... (l 

.. ::r ...,3 

-..... <> -;:l. 

...,~ 

Table 1 Page - 2 
0 

$507883 

Retention Molecular lntensi ty dllei&btl Weight f 

Ti11e Weisht !IIVJ d Logllfl 

Ill in! 

25.82 8515 o. 768 

0. 733 22.92 

25. 90 8153 0. 738 0. 704 

21.57 

25. 98 7807 0. 707 

0. 675 20. 28 

26.07 7476 0. 675 0. 645 19.04 

.. 26. 15 7158 0. 646 0. 

616 l7. 86 

26. 23 6&54 0. 615 0. 587 16. 73 

26.32 6563 0. 585 0. 559 

15.66 

26. 40 6285 

0. 556 0. 531 14.64 

26. 48 6018 0. 527 0. 503 13. 67 

26.57 5762 0. 499 0.477 12.75 

26. 65 5518 0. 474 

D. 452 11.88 

26.73 5284 0. 448 0. 428 11.05 

26. 82 5059 0.423 0. 404 10. 28 

26. 90 4U5 

0. 399 0. 381 9. 54 

26. 98 4639 0. 376 D. 359 

8. 85 

27. 07 ~442 0. 355 

0. 338 

8. 19 

27. 15 4253 

0. 334 0. 319 7. 58 

27. 23 ~073 0. 312 

0. 298 7. 00 

27. 32 3900 0. 294 

0. 280 

6. 46 

27. 4D 3734 

0. 274 D. 262 5. 95 

27.48 3576 

0. 255 0. 244 

5. 48 

27.57 3424 

0. 239 0. 228 5. 04 

27. 65 3279 0. 222 

0. 212 4. 63 

27.73 3139 o. 206 0. 197 4. 25 

27.82 3006 

0. 192 0. 183 3.89 

27. 90 2879 0.177 0. 169 

3. 56 

27. 98 2756 0. 162 0. 155 3. 26 

28. 07 2639 0. 151 

0. 144 

2. 98 

28. 15 2527 o: 139 

0. 133 2. 72 

28. 23 2420 0. 129 

o. 123 2.49 

28.32 2317 0.117 0. 112 

2. 27 

28.40 2219 0. 107 0. 102 

2. 07 

28.48 2125 0. 100 0. 095 1.88 

28. 57 2035 0. 091 0. D87 1.71 

28. 65 1948 

o. 083 0. 080 

1. 56 

28. 73 1865 0.077 0. 073 l. 42 

23. 82 1786 0. 069 0. 066 

I. 29 

28. 90 1710 0. 063 

0. 060 l. 17 

23. 98 1638 0. 058 

0. 055 l. 06 

29. 07 1568 o. 052 D. 050 o. 96 

29. 15 1502 0. 047 o. 045 D. 87 29. 23 1438 0. 043 0. 041 o. 79 

29. 32 1377 o. 039 0. 037 o.n 

29. 40 1318 

o. 035 0. 034 o. 65 

29.48 1262 D. 033 0. 031 0. 59 

29. 57 1209 o. 029 0. 028 0. 54 

29. 65 1158 0. 027 0. 025 o. 49 

29. 73 1108 D. 024 0. 023 o. 44 

29. 82 1061 0. 02Z D. 021 0. 40 

Fi I e : AOS.IIMl Table 1 Poage 

- 3 

0 

Relent ion lololecular I ntens i IY 

Tl•e Ieight (•VJ 

fllin) 

29. 90 --------ifgf:··-

1016 --·--------973 ______ 0. 020 ---.-----ii"li18 

-----

30. 07 932 0. 016 

30. 15 892 D. 016 

30. 23 854 D. 014 

30. 32 

818 0. 013 

30.40 783 0. 014 

30. 48 750 

0. 013 

30. 57 718 

0. 013 

30. 65 688 0. 014 

30.73 659 0. 013 

30.82 631 0. 

012 

30.90 604 

0. 010 

30. 98 578 

0. 007 

31. 07 554 

0. 006 

31. 15 530 0. 004 _______ JUL ... __________ jjljl__ ____ __________ O,_Q9L ... 31. 32 486 0. 002 

31. 40 465 0. 002 

31. 48 446 0. 001 

31.57 427 0. 001 

31. 65 409 0. 000 

31. 73 391 0. 000 

31. 82 375 0. 000 

31. 90 359 0. 000 

31.98 344 

0. 000 

32. 07 329 0. 001 

32. 15 315 0. 000 

32. 23 302 0. 

001 

32. 32 289 0. 002 

32. 40 277 0. 001 

32. 48 265 0. 001 

32.57 254 0. 000 

32.65 243 

0. 000 

32.73 233 0. 000 

32.82 223 0. 000 

32.90 213 0. 000 

32.98 204 0. 000 

Fi I e : AOS. t.1JD 

d !lei sbtl 

d Los om 

0. 019 ----------ii"oi 1"------

0. 016 

0. 015 

0. 013 0. 013 

0. 013 

0. 012 

0. 013 

0. 013 0. 013 

0.011 0. 009 

0. 007 

0. 005 

0. 004 

___ _______ !l.,_QOL ••.••• 

0. 002 

0. 002 

0. 001 

0. 001 

0. 000 

0. 000 

0. 000 

0. 000 

0. 000 

0. 001 

0. 000 

D.n01 

0. 002 

0. 001 

0. 001 

0. 000 

o. 000 

0. ODO 

0. 000 

0. 000 

0. 000 

S507883 

Weight f 

---. ·---~c~L .. ---- 0. 33 o. 30 0. 27 

0. 25 

0. 22 o. 20 

0.18 

0.15 

0. 13 

0. 10 

0. 08 

o. 06 

0. 05 0. 04 

0. 03 ________ Qj)_2. _______ o. 02 

0. 02 

o. 01 

0. 01 0. 01 

o. 01 0. 01 

o. 01 

0. 01 

0. 01 

0. 01 

D. 01 

0. 00 

o. 00 

0. 00 

0. 00 

0. 00 

o. 00 

o. 00 

0. 00 

0. 00 

Table 1 Page - 4 

-i 

Cll 

I 

"' ..... 

00 

~ 0 

)> 

-u::l= 

.. "' "' 0 .. :r 003 

'" -;?. 

..... _ 
0 

Table 2 Molecular Weight Dar:t:=a"""""":"'"""= 

Sa•ple :I _,·- lXI nl lin . ;

7 -~-; &l 

File XUS: 1110 llw ,,.., - Areo 289.85 •V ·sec liz -·~::.,..h~ 

Operator Hamshi&e llv ·.::"£-_: ~-.. Date 2013/9/4 llw/lhl : --•···· · · llz/llw: ·. ·•.- •.· · 

Relent ion llol ecular IntensIty d !t:cisbll 

Ti•e Ieicht 

linin) 

(•Vl d log OM 

18. 23 441128 0. ODD 0. 000 

18. 32 422401 0. 001 0. 001 

18. 40 404469 

0. 002 0. 002 

18. 48 387Z98 

0. 003 0. 

003 

18.57 370356 0. 005 

0. 004 

18. 65 355113 0. 005 0. OD5 

18.73 340038 0. 007 0. 007 . 18. 82 325602 0. 009 0. OD8 

18. 9D 311780 

0. 010 0. 009 

18.98 298544 

0. 014 

D. 013 

19. 07 285870 0. 016 

D. 015 

19. IS 273734 

0. 019 0. 017 

19. 23 262114 

0. 021 

D. 019 

19. 32 250986 0. 024 

D. 022 

19.40 240331 

0. 028 0. 025 

19.48 230129 

o. 032 

0. 029 

19.- 57 220359 0. 035 0 032 

19. 65 

211005 0. 039 

0. 036 

19.73 202047 

0. 043 0. 040 

19. 82 193470 

o. 049 0. 045 

19. 90 185256 0. 053 0. 049 

19. 98 177392 

o. 060 0. 055 

20. 07 169861 0. 067 0. 061 

20. 15 162650 

o. 074 0. 068 

20. 23 155145 

0. 082 

0. 075 

20. 32 149134 

0. 090 0. 083 

20. 40 142803 -. 

0. 098 0. 089 

20.48 136740 0. 107 

0. 098 

20. 57 

130935 0.117 0. 108 

20. 65 t253n 0. 127 0. 116 

20. 73 120054 

D. 137 0. 126 

20. 82 11 4958 0. 150 0. 137 

20. 90 110078 0. 161 a. 148 

20. 98 105405 

0. 175 a. 160 

21. 07 100930 

0. 189 Q.173 

21. 15 96645 

o. 203 0. 186 

21. 23 92542 0. 219 0. 200 

21.32 88614 0. 235 

o. 215 

21.40 84852 0. 252 0. 230 

21.48 81250 0. 271 a. 248 

21.57 77800 

0. 288 0. 264 

21. 65 74498 0. 309 

o. 283 

File : A06.1ltll 

S5D7883 

Weight X 

I 

10D. 00 

100.00 

10D. 00 

99.99 

99. 98 

99.98 

99. 96 

99. 95 

99. 93 

99. 91 

99.89 

99. 86 

99. 82 

99.78 

99.74 

99. 69 

99. 63 

99. 56 

99. 49 

99.41 

99. 32 

99. 23 

99. 11 

98. 99 

98.86 

98. 71 

98.54 

98. 36 

98. 17 

97. 96 

97. 73 

97.48 

97. 21 

96. 92 

96.60 

96. 26 

95. 89 

95. 50 

95. 07 

94. 62 

94. 13 

93. 62 

Table 2 Page 

- 1 

0 

Retention llo lecular lntensi tY 

Ti•e Wcl&ht t.Vl 

t.inl 

21. 73 71335 0. 328 

21.82 68307 0. 350 

21.90 65407 0. 371 

21. 98 62630 0. 394 

22. 07 59971 0.417 

22. 15 57426 0.441 

22. 23 54988 0. 465 

22. 32 52653 0. 489 

22.40 50418 0. 516 

22.48 48278 0. 542 

22. 57 46228 0. 568 

22. 65 44266 0. 596 

22.73 42387 0. 623 

22.82 40587 0. 650 

22. 90 38864 0. 678 

22.98 37214 0. 706 

23. 07 35634 0. 

735 

23. 15 34122 0. 763 

23. 23 32673 0. 792 

23. 32 31286 0. 820 

23.40 29958 0. 846 

2U8 28686 0. 874 

23. 57 27468 0. 902 

23. 65 26302 0. 929 

2173 25186 0. 954 

23.82 24116 0. 979 

219D 23093 

1. 002 

23.98 22112 1. 022 

24.07 21174 1. 042 

24. 15 20275 1. 059 

24. 23 19414 1. 075 

24. 32 18590 1. 087 

24. 4D i7801 1. 095 

24.48 17045 1. 101 

24.57 16321 1. 102 

24. 65 15629 1. 102 

24.73 14965 1. 098 

24.82 14330 1. 089 

24.-90 13721 I. 079 

24. 98 13139 I. 065 

25. 07 12581 1. 048 

25. 15 12047 I. 028 

25. 23 11536 1. 005 

25.32 110<46 0. 980 

25.40 10577 0. 953 

25.48 10128 0. 926 

25. 57 9698 0. 895 

25. 65 9286 a. 865 

25.73 8892 a. 832 

File : A06.1ltll 

dllcisbll 

d Locom 

0. 301 

0. 320 

0. 340 

0. 361 

0. 382 

0.404 

o.m 

0. 448 

0. 472 

0. 496 0. 52D 0. 546 

0. 571 0. 595 

0. 621 

0. 647 0. 673 0. 699 

0.725 

0. 751 

0. 775 

0. 80D 

0. 826 

0.850 

0. 874 

0. 896 

0. 917 

0. 936 

0. 954 

0. 970 

0.934 

0. 995 

1. 003 

1. 008 

1. 009 

1. OD9 

I. 005 

0. 998 

0. 988 

0. 975 

0. 959 

0. 941 

. 0. 921 

0. 897 

0. 873 

0. 848 

0. 820 

0. 792 

0. 762 

-

S507883 

Ieight % 

93. 06 

92. 47 

91.85 

91. 18 

90.44 

89. 74 

88. 95 

88. 13 

87.25 

86. 34 

85. 34 

84. 37 

8131 

82.21 

81.06 

79. 86 

78. 61 

77. 31 

75.97 

74. 57 

73. 13 

71.64 

70. 11 

68. 52 

66. 89 

65. 22 

63. 51 

61.76 

59.98 

58. 16 

56. 32 

54.45 

52.57 

50. 67 

48. 77 

46. 87 

44.97 

43. 09 

41.22 

39.37 

37.55 

35. 76 

34. 01 

32. 31 

30.64 

29. 03 

27. 46 

25. 95 

24. 49 

-t 

(/) 

I 

;>;; 

...... 

00 

... 

-< 

0 

)> 

-u:+ 

.. .. .. 0 .. :r 

"'3 

...... .. -;:?. 

...... 

Table 2 Page - 2 
0 

S507883 

Retent

ion Uol ecular Intens

ity d rfci tbll Weicht s Ti•e lei !ht (mV) d locaftl 

f.inl 

25.82 8515 

o. 800 0. 733 23. 09 

25.90 8153 0. 767 0. 702 21.74 

25. 98 7807 0. 73. 0.672 20. ~5 

26.07 7476 

o. 702 0. 642 19

. 22 

26. 15 7158 0. 670 0..613 18.04 

26.23 685~ 0. 638 0. 585 16.92 

26. 32 6563 0. 6D7 0. 556 15

. 85 

26. 40 6285 0. 577 0. 529 14. 8.4 

26.48 6018 0. 548 0. 

501 13.87 

26. 

57 5762 0. 518 

0. 474 12.96 

26. 65 . 5518 0. 490 0.~9 12

. 09 

26. 73 528. 0. 465 0. 426 11.21 

26. 82 5059 

0. 439 0. 402 10. 50. 26.90 4845 0. 415 0. 380 9. 76 

26. 98 4639 0. 391 

0. 358 

9. 07 

27.07 4442 0. 369 0. 337 3.42 

27. 15 4253 0. 345 0. 316 7. 81 

27.23 4073 0. 324 0. 297 7. 24 

27. 32 3900 0. 304 0. 278 6.70 

27.40 3734 0. 285 0. 261 6. 19 

27.48 3576 0. 267 0. 244 

5. 72 

27

. 57 3424 0. 249 0. 228 

5. 28 

27.65 3279 0. 232 0. 213 4. 87 

27. 73 

3

139 0. 216 0. 198 4. 49 

27. 82 3006 0. 201 0.184 

4. 13 

27.90 2879 0. 186 0. 170 3. 80 

27.98 2756 0.172 0.158 3. 49 

28.07 2639 

0. 158 0. 145 3. 21 

28. 15 2527 

D. 147 0. 134 

2. 95 

28. 23 2420 0. 136 0. 125 2. 71 

28.32 2317 o. 126 0. 11 5 2. 

48 

28.

40 2219 D. 116 0. 

1

D6 

2. 28 

28.48 

2

125 0. 108 0. 098 

2. 08 

28.57 2035 

0. 099 0. 091 1.91 

28.65 1948 0. 091 0. 084 1.75 

28.73 1865 0. 083 0. 076 

1. 6D 

28.82 1786 0. 076 0. 070 1. 46 

2&. 90 1710 

0. 070 0. 064 1.34 

2&. 98 1638 0. 065 0. 059 1. 22 

29.07 1568 0. 058 0. 053 1.12 

29. 15 1502 0. 053 0. 048 1. 02 

29. 23 1438 0. 048 0.044 0. 93 

29.32 13n 0. 045 0. 041 0. 85 

29.

40 1318 0. 040 0. 037 

o. 78 

29.48 m2 0. 036 0. 033 0. 72 

29.57 1209 0. 034 0. 031 

o. 66 

29.65 1158 0. 030 0. 028 

o. 60 

29.73 1108 0. D28 0. 025 

0. 55 

29.82 1061 0. 02~ 0. 022 

0. 51 

Fi

le : A06.1Ml Table 2 Page 

- 3 

0 

Re

tention llol ecular 

Intensity 

Tl•e lelaht (mV) 

C.inl 

29. 90 

---

----if9f ____ 

10

16 

---

---

----973 ______ 0. 022 -------·-o:-o22 _____ 

30.07 932 0. 019 . 30. 15 892 0. 018 

30. 23 854 0. 

0

17 

30. 32 

8

18 O.D17 

30.40 783 0. DIS 

30.48 750 0. 

0

16 

30. 57 

7

18 0. 017 

30.65 688 0. 016 

30.73 659 0. D17 

30.82 631 0. DIS 

30. 9D 6D4 0. D13 

30. 98 SIS 0. D11 

31. D7 554 0. D09 

31. 15 530 0.008 

--------~U.L .. __________ jp_s_ 

___ ________ JLQP

_6 ____ _ 

31.32 486 0.004 

31.40 465 0. 005 31. 48 446 0. 003 31. 57 427 0. DD3 31. 65 409 0. DD2 31. 73 391 0. 002 

31. 82 375 0. 001 

31.90 359 0. DO D 

31

. 98 344 0. ODI 

32. 07 329 0. 

001 

32. 15 315 0. 001 

32. 23 302 0. OD1 

32. 32 289 0. 001 

32.40 277 0. 

D01 

32. 48 265 0. 

D01 

32. 57 254 0. DOD 

32.65 243 0. DOD 

32. 73 233 0. DOD 

32. 82 223 0. DOO 

32. 90 213 0. DOD 

32. 98 204 0. DOD 

File : A06.1110 

d [lcitb!l 

d loc 111'111 

0. 021 ---------o:-oiil ___

___ 

0. 018 

0. 016 0. 016 

0. 015 

0. 014 

0. 015 

0. 015 

0. 015 

0. 015 

0. D14 

0. 012 

0. 010 

0. 008 

0. D07 _____ _____ o"_qoL 

_____ 

o. oo• 0. 004 

0. 003 

0. 002 

0. 002 

0. 001 

0. 001 

0. 000 

0. 001 D. 001 0. D01 

0. 

D01 

0. 001 

0. 001 

0. 

001 

0. 000 

0. DOD 

0. 000 

0. 000 

0. 000 0. DOD 

S507883 

Wei&ht S 0. 47 -------·o:4r

··-

-

o. 40 o. 36 0. 33 0. 30 ' D. 28 

D. 25 

o. 22 0. 19 D. 16 

D. 14 

D. 11 0. 09 0. 08 0. 06 ________ QJl_L __

__ 

0. 04 o. 03 

0. 03 

0. 02 0. 02 

0. 02 

0. 01 0. 01 

0. 01 

0. 

01 

0. 

D1 

0. 

D1 

o. 

00 

o. 00 

0. 00 0. 00 

D. 00 I D. OD 0. OD 

0. OD D. 00 

-i 

en 

I 

"' ...... 

co 

~ 

. 0 

"0)> 

:: ~ -;:,- " 0 

03 ' " 

: 

Table 2 

Page 

- 4 
> 

E 

» 

.... 

(/) 

c 

Cl) 

.... 

c 

0:: 

6 

5 

4 

3 

2 

1 

0 

Fig . 1 

10 

Sample 

Concentration 

Injection Volume 

Apparatus 

Column 

15 

,...... I') 

Gel Permeation Chromatogram 

20 25 30 

Retention Time (min) 

So I vent 

Flow Rate 

Detec tor 

Temperature 

Opera tor 

Date 

35 

: THF 

: 1. 0 ml/mi n 

: R I 32x 

: 23. o·c 

: Hamash i ge 

: 2013/ 09/ 04 

40 

File: A05 

45 

--i 

(/) 

I 

;><; 

..... 

co 

:!( 

0 

..... 

J'~ n o - ::T 

-3 

' "' ~: 
{ 

» 

..... 

en 

c 

<I> 

+' 

c 

cr: 

6 

5 

4 

3 

2 

1 

0 

Fig. 2 

10 

Sample 

Concentrat ion 

Inj ect ion Volume 

Apparatus 

Col umn 

15 

('\ 0 

Gel Permeation Chromatogram 

: u:--zu-x 

: 0. 200 ml 

: GPC (19) 

: TSKge I Mu It i poreHXL -M (3) 

20 25 30 

Retention Time (min) 

Solven t 

Fl ow Rate 

Detector 

Temperature 

Operator 

Da te 

35 

: THF : 1. 0 mllmi n 

: R I 32x 

: 23. o·c 

: Hamash i ge 

: 2013/ 09/ 04 

40 

File: A06 

45 

-1 

C/) 

I 

;>< 

_, 

CX> 

!< 

0 

-o> 

.. ::t ... .. ct 0 

- :r N3 

' " :::: 
> 

E 

._, 

>. 

+' 

·-

(/) 

c 

Q) 

+' 

c 

... 

0::: 

6 

5 

4 

3 

2 

1 

0 

Fig. 3 

10 

Sample 

Concentration 

Inject ion Volume 

Appara tus 

Col umn 

15 

,.-.., (', 

Gel Permeation Chromatogram 

: So I ven t 

: 0. 200 ml 

: GPC (19) 

: TSKge I Mu It i poreHXL -M (3) 

20 25 30 

Retention Time (min) 

So lven t 

Flow Ra te 

Detector 

Tempe ratu re 

Opera tor 

Date 

35 

~ 

: THF 

: 1. 0 ml/ mi n 

: R I 32x 

: 23. o·c 

: Ham ash i ge 

: 2013/ 09/ 04 

r 

40 

File: A07 

45 

-t 

Ul 

I 

"' 

.... 

co 

:!< 

0 

-o > .. ~ .. .. " 0 - ::r 

'"' 3 -..... o .... 

-~ _ 
10 

9 

8 

+' 7 

.s: 

b.O 

-

~ 6 

I.. 

ro 

- 5 

:::J 

0 

Q) 

-

~ 4 

....__, 

b.O 

0 3 

_J 

2 

1 

0 

Fig. 4 

Samp le 

Appa ratus 

Column 

Solvent 

Flow Rate 

" 

Calibration 

: Polystyrene 

: GPC (191 

: TSKge l Multi poreHXL-M(3) 

: THF : 1. 0 ml/mi n 

Curve 

Log(MW) = A(O) + A(1 )T + A(2)T2+ A(3)T3+ · · · 

17 19 21 23 25 

(\ 

Det ector 

Temperature 

Operator 

Da te 

Coefficient( Order: 1) 

A(O) : A(l) : 

27 

9.766658 

-0.2260746 

Retention Time (min) 

29 

: Rl 32x 

: 23. o·c 

: Hamash ige 

: 2013/ 09/04 

File: C02.BXX 

Molecular Weight Data 

RT(min) MW 

18.13 427000 

19.75 190000 

21 .22 96400 

23.08 37900 

24.68 16200 

25.55 10200 

26.60 5970 

28.18 2630 

29.77 1010 

30.77 590 

31 33 

-l 

en 

I 

;>; 

..... 

(X) 

:!( 

0 

-c> 

:: ~ " n -::r 

"'" 3 ' " ~: 
........._, ("""\ 

-1 

(/) Fig. 5 Molecular Weight Distribution Curve I 

;>:; 

..... 

"' ~ 

-< 

0 

Mn [] 

.. Mv Ooerator : Hamash ige , ·- Mw .... : . .._ Mw/Mn : 2. 56 Oate : 2013/ 09/ 04 Mz • ~ .: J 

. ' ". -· Mz/Mw : 2. 38 

2.0 File: A05.MWD 

1.8 

1.6 

1.4 

~ 

bD 1.2 

0 

_J 

"'C 1.0 

~ " 0.8 

"'C 

0.6 

0.4 

I I \ I 

-ul> 

.. :+ .. .. 0.2 ~ / '\. I " 0 - :T "'3 

'..... 

-~ " 

_ I . ___.,..- ............_ I 0.0 

102 103 104 105 106 107 

Molecular Weight 
,......., 

"' 

-t 

(/) 

Fig . 6 Molecular Weight Distribution Curve i 

2 

Mn ~ Mv Operator : Hamashige lAw . Mw/ Mn : 2. 64 Da te : 2013/ 09/ 04 

IAz . Mz/ Mw : 2. 41 

File: A06.MWD 2.0 

1.8 

1.6 

1.4 

bO 1.2 

0 

~ 

"0 1.0 

'\. 

~ 0.8 

"0 

0.6 

0.4 I I \ I 

-< 

0 

-o> 

~ 6f 

I n n 0.2 ~ / '\. a; § -... n -~ 

I ~ ..........__ I 

.... _ 0.0 

1~ 1~ 1~ ~ 1~ 1~ 

Molecular Weight 
Fig. 7 

Sample 

CJ -

2.0 

1.8 

1.6 

1.4 

~ 

bD 1.2 

0 

..J 

iJ 1.0 

'\. 

~ 0.8 

iJ 

0.6 

0.4 

0.2 

0.0 

102 10

3 

r- f'l 

Molecular Weight Distribution Curve 

Mn 

n u []

Mw 

lXI 

. [J (JM . . (") 

.

. . ·. . ··-...... lXI . . ·. ·.·· .. .::_ I •.. 

104 105 

Molecular Weight 

10

6 

Mz/Mw 

[] . 

. . 

File: A05 A06 

107 

-1 

(/) 

I 

;><; 

_, 

00 

~ 

-< 

0 

'0)> 

.. ::1: ... .. (I 0 ~ ;T 

_,3 

, .. ::j: