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Khảo sát phản ứng tổng hợp polylactic acid theo phương pháp mở vòng lactide

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Width Plates Resol Select [rnin] [nRIU*s] [nRIU] [rnin] ution ivity... Sample Name: Mau 1Data File.

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4 5 6 7 8 1- 8 9 ' : ; ) ' ' , <# =, +, 7 1' > 4 ?' ; <6 @

+, ' ( ( <6 6 <6, > ; 6 # ( A @-#<.3 /5 B < /' ' , <# ' 4/*1' @ * =/1 6 7 8 1- 8 9 ',) +,- - ' (3

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* = (, = D' 4< =/1 ( ' > ' , 4 ',) ' (3

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Trang 5

  

0< @, 6 > " H ) = ) / E *1 A @-@ ' ' < /* #*)

> @ ' 8<I * <6, 4F J >< A @-#< ( ,)- = 1' > # 6 = @-#< ( ,)- = 1' <( < * 3 0< 4 5 4/ # 6 = /* K# B ) = 4 <, ' <

@-@ ' ' ' 8 8 = <=< ' = '< @- <=,@ =3 >< , < <=,@ = Y < ' < #,# <=,@ ;, = < <8 , <X ;< < .<=< ' 8 <' = <

S, ,.<3

< ;<= <=,@ X ' = <=< ' < ' C < >< < # @<',@ S A @-@ ' ' ' 8 L M3NGG O P# @Q3

Trang 7

G3G3 A ` W OA Q 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3

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G3d3 3 0 < ' < @ ' 8<3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 ! G3d3!3 E *1 @-@ ' ' ' 8 ' ( /) O @-@ ' 8<Q 3 3 3 3 3 3 3 3 3 3 3 3 ! G3d3!3 3 , ,' B ( ',) A 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 ! G3d3!3!3 E *1 A / V@ ' 8< O ?' WV@ ' 8<Q ' 3 3 3 3 3 3 3 ! G3d3G3 l,' ' /5, '* ' E *1 @-@ ' 8<3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 !

d3 3 W \^ 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 G

d3 3 3 ) = / 4 <, ' < @ ' 8< / , <( @ <6, @ ' ' ' 8 3 3 3 3 G d3 3 3 3 ) = /* 4 <, ' < @ ' 8< ( / @ ' ' ' 8 3 3 3 3 3 3 G d3 3 3!3 ) = /* ' < @ ' 8< 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 G d3 3!3 ) = ) / #*) > @ ' 8< @-@ ' ' ' 8 3 3 3 3 3 3 3 3 G d3!3 ^ A \] A ^A W m 0 ^ ^ a c _ 3 3 3 3 3 3 3 3 3 3 3 3 3 3 d

M3 3 3 3 < +, ) E *1 @ ' 8< ( 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 d M3 3 3 3 ) = <6 4 6 ) / ',) 4 1 @ #< 3 3 3 3 3 3 d M3 3 3!3 ) = * ) / 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 d M3 3 3G3 3 ) /*) ',) # @/*1 &,' ' 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 d M3 3!3 3 < +, ) ' < @ ' 8< 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 d M3 3G3 3 < +, ) 4 4 ( +, 1' O A Q3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 M

M3!3 3A 4/*1' E *1 / ' 8< U!3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 M

M3!3 3!3 ) = ) /*) ',) # @/*1 &, '3 3 3 3 3 3 3 3 3 3 3 M M3!3!3 3 A 4/*1' E *1 / ' 8< Ud 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 k

Trang 8

M3!3!3 3 ) = ) /*) ',) * ) / # ( /* B +,-<E 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 k M3!3!3!3 ) = ) /*) ',) # @/*1 &,' ' 3 3 3 3 3 3 3 3 3 3 3 3 3 k M3!3!3G3 3 R = =/1 ) /*) ',) # ( /* ) / 4< A 3 3 3 3 3 k

O *Q 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 N M3!3G3 3 < +, ) ' ,1 E n U 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 N

k3 3 a 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 N k3!3 a f 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 N

m _ 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 j

A [ [ 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 j

A [ [ ! 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 j

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@ E +F G+"$ H H +"H 5%&B( # &Q -+#$%4& $ ' $ 3 -+#$%# +#%4C

Trang 49

K+Q/ F `7 $1 ;7 H ("$

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U

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! T 6 E&Q$ R(+F 5 S Q% - ) H +' $ F #(F+ 0+l( O +#$%4& 6\

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UY

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=P

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! T ` E&Q$ R(+F 5 S Q% - ) H +' $ F #(F+ 0+l( UO +#$%4& @\

Trang 81

=Y

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! T 6; E&Q$ R(+F 5 VK #(F+ 6777HH0\ U U E

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! T 6T E&Q$ R(+F 5 VK #(F+ 6777HH0\ 6@

Trang 85

SP

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B B V *DDV(

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Cirrus GPC Sample Injection Report

Generated by: LAMDONGANH Tuesday, December 22, 200910:13 AM

Workbook: D:\QUOC VIET\Duong Chuan\Poly pore\THF\EsiVial

PS\POL YPOREO04-23- THF-EASIVIALPS-1711 07\POL YPOREO04-23- THF-EASIVIALPS-1711 07.plw

Sample Details

Sample Name: 500ppm 6H N2 6H CK Batch Name: PHU

THF 0.800000 Concentration: 0.10

-/ 1 Injection Volume 100.0 ul K of Sample: 14.1000 Alpha of Sample: 0.7000

Analysis Using Method: POL YPOREO04-23- THF-EAsiVIALPs-1711 07

Area (mV secs) 9407.23 578.155

% Area

1

2

87.2052 12.7948

94.21 5.79002

Trang 103

Cirrus GPC Sample Injection Report

Generated by: LAMDONGANH Tuesday, December 22, 200911 :21 AM

Workbook: D:\QUOC VIET\Duong Chuan\Poly pore\THF\EsiVial

PS\POL YPOREO04-23- THF-EASIVIALPS-1711 07\POL YPOREO04-23- THF-EASIVIALPS-1711 07 plw

Sample Details

Sample Name: 1000ppm 6H N2 6H CK Batch Name: PHU

THF 0.800000 Concentration: 0.10

-, , Injection Volume: 100.0 ul K of Sample: 14.1000 Alpha of Sample: 0.7000

Analysis Using Method: POL YPOREO04-23- THF-EASIVIALPs-1711 07

90 1.3-

1.1 70 1-

% Height Area

(mV.secs) 9536.58 423.533

% Area

1

2

88.7882 11.2118

95.7477 4.25229

103 Max RT (mins) 10.33 14.55

Trang 104

Cirrus GPC Sample Injection Report

Generated by: LAMDONGANH Tuesday, December 22, 2009 11 :24 AM

Workbook: D:\QUOC VIET\Duong Chuan\Poly pore\THF\EsiVial

PS\POL YPORE004-23- THF-EASIVIALPS-171107\POL YPOREO04-23- THF-EASIVIALPS-171107.plw

Sample Details

Sample Name 2000PP 6N2 6CK Batch Name: PHU

THF 0.800000 Concentration: 0.10

-, , Injection Volume 100.0 ul K of Sample: 14.1000 Alpha of Sample 0.7000

Analysis Using Method: POL YPOREO04-23- THF-EASIVIALPS-1711 07

10.15 13.47 157.95 96.236 14.50 14.95 6.17783 3.76402

Mn 11629 126 Stan RT (mins) 8.93 13.73

Area % Area (mV.secs)

11721.4 98.4599 183.35 1.54014 1

2

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Cirrus GPC Sample Injection Report

Generated by: LAMDONGANH Wednesday, December 23, 20092:52 PM

Workbook: D.\QUOC VIET\Duong Chuan\Poly pore\THF\EsiVial

PS\POL YPOREO04-23- THF-EASIVIALPS-1711 07\POL YPOREO04-23- THF-EASIVIALPS-1711 07 plw

Sample Details

Sample Name: 3000ppm 6h N 6H CK Batch Name: PHU

THF 0.800000 Concentration: 0.10

-' 0 Injection Volume: 100.0 ul K of Sample: 14.1000 Alpha of Sample: 0.7000

Analysis Using Method: POL YPOREO04-23- THF-EAsiVIALPs-1711 07

Mz 13401 128 Max RT (mins) 11.15 14.57

Mz+1 18192 141 End RT (mins) 14.25 14.93

Area (mV.secs) 8302.97 197.829

% Area 1

2

93.5151 6.48488

97.6728 2.32718

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Cirrus GPC Sample Injection Report

Generated by: LAMDONGANH Wednesday, December 23, 20093:03 PM

Workbook: D:\QUOC VIET\Duong Chuan\Poly pore\THF\EsiVial

PS\POL YPOREO04-23- THF-EASIVIALPS-1711 07\POL YPOREO04-23- THF-EASIVIALPS-1711 07 ,plw

Sample Details

Sample Name: 2000ppm 6h N 6h CK 130C Batch Name: PHU

THF 0.800000 Concentration: 0.10

-0- , , Injection Volume' 100.0 ul K of Sample: 14.1000 Alpha of Sample: 0.7000

Analysis Using Method: POL YPOREOO4-23- THF-EASIVIALPS-171107

-30 0.6-

-20 0.4-

% Height Area

(mV.secs) 6770.95 878.598

% Area

1

2

75.926 24.074

88.5144 11.4856

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9.30 10.50 13.70 123.328 91.311 14.27 14.55 14.98 11.7357 8.68902

% Area

Area (mV.secs) 10074.7 253.014

97.5501 2.44987

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Cirrus GPC Sample Injection Report

Generated by: LAMDONGANH Tuesday, December 22, 2009 11 :25 AM

Workbook: D:\QUOC VIET\Duong Chuan\Poly pore\THF\EsiVial

PS\POL YPOREO04-23- THF-EASIVIALPS-1711 07\POL YPOREO04-23- THF-EASIVIALPS-1711 07 plw

Sample Details

Sample Name: 500ppm 12H N2 Batch Name: PHU

THF 0.800000 Concentration: 0.10

-, , Injection Volume: 100.0 ul K of Sample: 14.1000 Alpha of Sample: 0.7000

Analysis Using Method: POL YPOREOO4-23- THF-EASIVIALPS-171107

(mV.secs) 9743.22 458.653

% Area

1

2

87.918 12.082

95.5042 4.49578

Trang 109

Cirrus GPC Sample Injection Report

Generated by: LAMDONGANH Tuesday, December 22, 2009 11 :26 AM

Workbook: D:\QUOC VIET\Duong Chuan\Poly pore\THF\EsiVial

PS\POL YPOREO04-23- THF-EASIVIALPS-1711 07\POL YPOREO04-23- THF-EASIVIALPS-1711 07 plw

Sample Details

Sample Name 1000ppm N2 12H Batch Name: PHU

THF 0.800000 Concentration: 0.10

-, , Injection Volume: 100.0 ul K of Sample: 14.1000 Alpha of Sample: 0.7000

Analysis Using Method: POL YPOREOO4-23- THF-EAsiVIALPs-111101

(mV.secs) 6921.33 408.318

% Area

1

2

85.0935 14.9065

94.4292 5.57078

Cirrus GPC Version 3.0 Page 1 12/22/2009 11 :26 AM

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Cirrus GPC Sample Injection Report

Generated by: LAMDONGANH Wednesday, December 23, 20092:50 PM Workbook: D:\QUOC VIET\Duong Chuan\Poly pore\THF\EsiVial

PS\POL YPOREO04-23- THF-EASIVIALPS-1711 07\POL YPOREO04-23- THF-EASIVIALPS-1711 07.plw

Sample Details

Sample Name: 2000ppm 12h N Batch Name: PHU

THF 0.800000 Concentration: 0.10

-/ 1 Injection Volume 100.0 ul K of Sample: 14.1000 Alpha of Sample: 0.7000

Analysis Using Method: POL YPOREO04-23- THF-EASIVIALPS-1711 07

Mw Mz

28583 39825

111 114 Max RT End F (mins) (min!

(mV.secs) 8816.28 257.78

% Area

1

2

89.5606 10.4394

97.1592 2.84085

Trang 111

Cirrus GPC Sample Injection Report

Generated by: LAMDONGANH Tuesday, December 22, 2009 11 :27 AM

Workbook: D:\QUOC VIET\Duong Chuan\Poly pore\THF\EsiVial

PS\POL YPOREO04-23- THF-EASIVIALPS-1711 07\POL YPOREO04-23- THF-EASIVIALPS-1711 07 plw

Sample Details

Sample Name 3000PP 12H N2 Batch Name: PHU

THF 0.800000 Concentration: 0.10

-, , Injection Volume 100.0 ul K of Sample: 14.1000 Alpha of Sample: 0.7000

Analysis Using Method: POL YPOREOO4-23- THF-EASIVIALPS-171107

% Area

1

2

98.1741 1.82595

PO 2.41207 1.01709

% Height

94.409 5.59098

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Cirrus GPC Sample Injection Report

Generated by: LAMDONGANH Thursday, December 31, 2009 1 :35 PM

Workbook: D:\QUOC VIET\Duong Chuan\Poly pore\THF\EsiVial

PS\POL YPOREO04-23- THF-EASIVIALPS-1711 07\POL YPOREO04-23- THF-EASIVIALPS-1711 07 plw

Sample Details

Sample Name 2000ppm 24hN2 Batch Name: PHU

THF 0.800000 Concentration" 0.10

-,. , Injection Volume 100.0 ul K of Sample" 14.1000 Alpha of Sample: 0.7000

Analysis Using Method: POL YPOREO04-23- THF-EASIVIALPS-1711 07

Area (mV.secs) 8690.33

% Area Peak No

Trang 113

Generated by LAMDONGANH Thursday, December 31, 20091.59 PM

-, ,

Area (mV.secs) 9799.79

% Area

Cirrus GPC Version 3.0

Trang 114

at'; Fil~ C:\HPCHEM\1\DATA\COTMIXA\61000007.D Sample Name: mau 1 lOOOppm

Multiplier

Dilution

[nstrurnent 110/12/2009 1:06:02 PM

Trang 115

" 'f 0.

~ 0 z

Molar mass

mau 1 1000ppm

C :\H PC H EM\G PC\cali b\colum n500A CAL 6.312 ml Integration to : 1.000E+O MHK- K (Cal.):

Flowrate : Inject volume : Delay volume : Acquisition interval :

1.000 gll RID A, Refractive Index Signal

~

rid1A Mn:

0.000000 mllg 7.5023eO ml 4.2504e3 glmol 9.5648e3 ml*V 1.5391 e3 glmol 2.6964e3 glmol 3.7375e3 glmol 4.9973e3 glmol 7.1901e3 glmol C:\HPCHEM\ 1 \DA T A\COTMIXA\61 000007 D Monday 10112109 13:06:52

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)at8 File C:\HPCHEM\1\DATA\COTMlXA\61000008.D Sample Name: mau 2 2000ppm

Area Percent Report with Performance

Multiplier

Dilution

1.0000 1.0000

RetTirne kt Area Height Syrnrn Width Plates Resol Select

[rnin] [nRIU*s] [nRIU] [rnin] ution ivity

Trang 117

1.8814e3 3.2525e3 4.6803e3 3.2525e3 1.7287eO O.OOOOOO 7.7472eO 3.1234e3 8.9624e3 9.4763e2 1.8824e3 2.7772e3 3.954ge3 6.1954e3

mi/g mi glmoi ml*V glmol glmoi glmoi glmoi glmol

C:\HPCHEM\ 1 \OA T A\COTMIXA\61 000008.0 Monday 10/12/0913:11:01

Path :

~

Trang 118

Sample Name: Mau 1

Data File C:\HPCHEM\1\DA.TA.\COTMIXA\20080001.D

:================================================================

Multiplier

Dilution

1.0000 1.0000

[nRIU*s]

Height [nRIU]

5713.68457

=====================================================================

Trang 119

" 1%: c

" of u Q.

~ Q :1;

THF Flowrate : 1.000 gn Inject volume : RID A, Refractive Index Signal Delay volume :

Acquisition interval :

rid1A

5.0137e3 9.g260e3 2.0g02e4

glmol glmol glmol glmol

mUg ml glmol ml*V glmol glmol glmol glmol glmol

Path : C:\HPCHEM\1\DA TA\COTMlXA\20080001.D

Trang 120

Sample Name: Mau 2

D-;t!a File C: \HPCHEM\1.\DATA\COTMIXA\20080002 D

Injection Date: i1/21/2009 4:07:19 PM

Sample Name: Mau 2 Location :

Instrument 1 11/21/20094:22:18 PM Page 1 of 1

Trang 121

" cr: c

"

'f Q.

~ Q.

4.3247e3 6.1748e3 8.7927e3 1.4625e4

~

Path :

mi/g mi glmol ml*V glmoi glmol glmol glmoi glmol C:\HPCHEM\ 1 \DA T A \COTMlXA \20080002 D

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