GPC/SEC... 3 GPC... 4 GPC... 5 Agilent PL-SP 260VS... 6 Agilent PL-GPC 220 GPC/SEC... 7 Agilent Cirrus GPC GPC GPC/SEC GPC Agilent PL
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1 GPC/SEC Greg Saunders Ben MacCreath
2 GPC/SEC... 3 GPC... 4 GPC... 5 Agilent PL-SP 260VS... 6 Agilent PL-GPC 220 GPC/SEC... 7 Agilent Cirrus GPC GPC GPC/SEC GPC Agilent PLgel Olexis GPC GPC GPC...20 GPC GPC GPC GPC Cirrus GPC...22 (LLDPE)...24 GPC/FT-IR
3 GPC/SEC [ ] 2 (GPC (SEC) ) 1 () 10 % 1. (Mw) Mw Mw Polymer Laboratories (PL) 1976 GPC/SEC 30 PLgel PL -OH PlusPore PLgel Olexis PolarGel EasiVial PL PL GPC SEC GPC 3
4 GPC 1,2,4- (TCB) 1 4 GPC ºC 4
5 GPC 1 ( ) GPC/SEC 1. GPC 5
6 ( 2)TCB 2. (mg/ml) (ºC) (h) PE PP Agilent PL-SP 260VS PL-SP 260VS GPC ºC ( 2 ºC) ( 10 %) rpm PL-SP 260VS Agilent PL-SP 260VS ( ) ( 2) 2 : ( 1 µm) ( 2) ( µm) 20 ml () PL-GPC ml 4 ml µm 6
7 Agilent PL-GPC 220 GPC/SEC PL-GPC 220 PL-GPC 220 PL-GPC ºC 0.05 ºC GPC PL-GPC 220 THF 140 ºC TCB 0.07 % RI (RI) GPC/SEC RI 220 ºC / ( 3) : : 2 x Agilent PLgel 10 µm MIXED-B 300 x 7.5 mm ( PL ) 1 ml/min : 200 µl : PL-GPC Mp = 1,460,000 = 0.62 mg/ml 2. Mp = 9,860 = 1.08 mg/ml TCB CN x 7.5 mm GPC / GPC/SEC Agilent PL-GPC 220 GPC/SEC 7
8 GPC TREF ( ) FT-IR ( ) ELSD ( ) 4 RI PC 220 ºC PL-GPC 220 PC PC PL-GPC 220 PL-GPC 220 RI PL-GPC 220 PL-GPC L 13 L 30 ºC ( 5) ( 4) 5. Agilent PL-GPC 220 GPC/SEC 4. PL-GPC 220 PL-GPC 220 8
9 2 ml 39 1 % RSD 220 ºC Agilent Cirrus GPC GPC Cirrus GPC/ Polymer Laboratories 1980 GPC Cirrus GPC GPC LC Cirrus GPC LC GPC Cirrus Agilent PL DataStream Cirrus GPC FT-IR (SCB) GPC PC GPC 1 Workbook Cirrus : Cirrus 3 MW % Cirrus QC/ 9
10 Cirrus GPC/ SEC ISO 9001:2000 () GPC (Mp) 3 3. Agilent EasiCal Agilent EasiVial GPC/SEC Yes Yes Yes Yes Yes Yes Yes Yes Yes 10
11 GPC/SEC GPC/SEC 1. GPC/SEC 2. ( ) 3. 2 ( ) PLgel Olexis PLgel Olexis ( ) PLgel 10 µm MIXED-B PLgel MIXED-A PLgel MIXED-B LS PLgel MIXED-A LS PLgel 5 µm MIXED-C PLgel 5 µm MIXED-D PLgel MIXED-A PLgel MIXED-B PLgel () PLgel 5 µm 500Å PLgel () PLgel 5 µm 100Å PLgel PLgel Olexis PLgel 20 µm 4 13 µm 3 10 µm 3 5 µm 2 (PS) (PE) PLgel Olexis 13 µm EasiVial PE 11
12 GPC PLgel Olexis Agilent PLgel Olexis PLgel Olexis 100,000,000 g/mol (THF ) 13 µm 220 ºC PLgel 30,000 /m 13 µm ( 6) PLgel Olexis PLgel Olexis 100,000,000 g/mol ( 7) Log M PLgel Olexis X 6. PLgel Olexis 12
13 1 PLgel Olexis ( 8) 7 Log M 2 14 ( ) PLgel Olexis TCB PLgel Olexis 13
14 PLgel PL-GPC 220 (MWD) PLgel Olexis : : : : 3 x PLgel Olexis 300 x 7.5 mm ( PL ) TCB % BHT 1 ml/min : 200 µl : 160 ºC : PL-GPC 220 (RI) + PLgel Olexis MWD ( 9) PLgel Olexis dw/d Log M 9. PLgel Olexis 10 PLgel Olexis dw/d Log M Log M PLgel Olexis ( 11) 1 dw/d Log M 3 Log M PLgel Olexis 0 3 Log M PLgel Olexis 14
15 2 GPC GPC GPC 12 3 : : : : 2 x Agilent PLgel 5 µm 100Å 300 x 7.5 mm ( PL ) TCB 1 ml/min : 145 ºC : PL-GPC C 36 H C 22 H C 14 H : : : : 2 x Agilent PLgel 3 µm 100Å 300 x 7.5 mm ( PL ) TCB : 20 µl 0.8 ml/min : 145 ºC : PL-GPC C C C C C PLgel 100Å GPC 4,000 ( ) 400,000 PLgel MIXED-D 5 µm PLgel 15
16 14 PLgel 5 µm MIXED-D : : : : 2 x Agilent PLgel 5 µm MIXED-D 300 x 7.5 mm ( PL ) TCB 1 ml/min : 200 µl : 160 ºC : PL-GPC (HDPE) PL-SP 260VS 2 mg/ml 160 ºC 2 8 PL-GPC 220 PL-GPC ºC 80 ºC ( 16) : : : 3 x PLgel 10 µm MIXED-B 300 x 7.5 mm ( PL ) TCB % BHT 1 ml/min : 200 µl : 160 ºC : PL-GPC HDPE 8 : 2 x PLgel 5 µm MIXED-D 300 x 7.5 mm ( PL ) : THF : 1 ml/min : 40 ºC : RI PLgel 5 µm MIXED-D 16
17 4 TCB 1 = K x 12.1 x 10-5 = TCB 2 = K x 40.6 x 10-5 = HDPE 8 Mn Mp Mw 1 17,289 76, , ,988 77, , ,428 77, , ,521 77, , ,348 76, , ,487 77, , ,898 77, , ,457 77, ,923 17,302 77, , ,048 % (HDPP) PL-SP 260VS 1.5 mg/ml 160 ºC 2 6 PL-GPC 220 PL-GPC ºC 80 ºC 18 HDPP HDPP 6 17 HDPE 8 PLgel 10 µm MIXED-B PL-GPC 220 dw/d Log M 2 Log M HDPE 8 17
18 5 TCB 1 = K x 12.1 x 10-5 = TCB 2 = K x 19.0 x 10-5 = HDPP 6 Mp Mn Mw 1 127,132 65, , ,893 65, , ,673 66, , ,062 67, , ,625 69, , ,227 69, , ,202 67, ,691 1,693 1,815 1,239 % : : : 3 x PLgel 10 µm MIXED-B 300 x 7.5 mm ( PL ) TCB BHT 1 ml/min : 200 µl : 160 ºC : PL-GPC HDPP 6 PLgel 10 µm MIXED-B PL-GPC 220 dw/d Log M 3 Log M HDPP 6 1 H. Coll and D. K. Gilding (1970) Universal calibration in GPC: a study of polystyrene, poly- -methylstyrene, and polypropylene. Journal of Polymer Science Part A-2: Polymer Physics, 8, T. G. Scholte, N. L. J. Meijerink, H. M. Schoffeleers and A.M.G. Brands (1984) Mark-Houwink equation and GPC calibration for linear short chain branched polyolefins, including polypropylene and ethylene-propylene copolymers. Journal of Applied Polymer Science, 29,
19 GPC GPC GPC PL-GPC 220 GPC GPC 1 2 ( x ) 1 : x 2 : Log (MW x ) VS. log ( ) VS. PLgel Olexis ( 20) 9 Log (Mw x IV) ( ) GPC PL-GPC 220 GPC GPC 3 3 : R = CM (dn/dc) 2 P K R CM x dn/dc P K 15º 90º 2 10 nm 20. PLgel Olexis GPC 19
20 GPC PL-GPC 220 GPC 15º 90º 2 10 nm GPC GPC GPC GPC GPC GPC GPC GPC GPC GPC GPC GPC GPC 20
21 GPC LDPE 1930 ( 2 %) GPC LDPE HDPE LDPE HDPE LDPE HDPE LLDPE LLDPE LDPE GPC LLDPE 24 GPC-FT-IR GPC Rg IV ( ) ( ) ( ) 4 (MW ) (MW ) 4 : g = Rg Rg g = g = g (1/ ) IV IV MW MW () = g ( g ( 0.75) ) ( 1000 ) : g = [(1 + B n /7) 1/2 + 4B n /9 ] -1/2 B n =
22 1000 ( ) PL-GPC 220 LDPE HDPE LLDPE Log IV 0 : : : 3 x PLgel Olexis 300 x 7.5 mm ( PL ) TCB % BHT 1.0 ml/min : 200 µl : 160 ºC : PL-GPC 220 (RI) + + Cirrus GPC dw/d Log M Log M (HDPE LLDPE LDPE ) Log M (HDPE LLDPE LDPE ) HDPE LLDPE K () () GPC LDPE HDPE LLDPE LDPE Cirrus GPC ( 6 ) 22
23 PL-GPC 220 GPC/3 (HDPE 1 LDPE 2 ) 2 1 SRM 1475 Cirrus GPC g ( ) : : : : 3 x PLgel Olexis 300 x 7.5 mm ( PL ) TCB % BHT 1.0 ml/min : 200 µl : 160 ºC : dw/d Log M PL-GPC 220 (RI) ( ) Log M 8 6 : g = IV IV 1/ Log IV Log M
24 1 g ( ) 2 g g 1000 Cirrus GPC g g g ( ) Log Mw (LLDPE) (FT-IR) FT-IR FT-IR FT-IR 1 GPC PL-HTGPC-FT-IR PL-GPC 220 FT-IR 0.5 ºC 175 ºC FT-IR MCT () Log Mw () 24
25 GPC/FT-IR ( 135 ºC ) GPC (TCB) TCB >C-H 3,500 2,700 cm -1 FT-IR GPC CH >C-H >CH 2 CH 3 CH 3 >CH 2 (SCB) 1 SCB 6 GPC SCB SCB CH 3 >CH 2 SCB SCB FT-IR GPC ( ) SCB GPC/FT-IR Agilent FT-IR PL-GPC 220 : : : 200 µl : 2 x PLgel Olexis 300 x 7.5 mm ( PL ) (BHT ) 1.0 ml/min : 160 ºC : Agilent Resolutions Pro 8.0 cm ,500 2,700 cm -1 : Agilent PL-HTGPC-FT-IR MCT Agilent FT-IR Cirrus GPC-FT-IR SCB SCB FT- IR 27 FT-IR 0.6 dw/d Log M Log Mw CH 3 /CH 2 1 P.J. DesLauriers, D.C. Rohlfing and E.T. Shieh (2002) Quantifying short chain branching microstructures in ethylene-1-olephin copolymers using size exclusion chromatography and Fourier transform infrared spectroscopy (SEC-FTIR). Polymer, 43,
26 Agilent PLgel 3 µm 100Å 300 x 7.5 mm Agilent PLgel 5 µm 100Å 300 x 7.5 mm Agilent PLgel 5 µm MIXED-D 300 x 7.5 mm Agilent PLgel 10 µm MIXED-B 300 x 7.5 mm PLgel 10 µm MIXED-B LS 300 x 7.5 mm PLgel 20 µm MIXED-A 300 x 7.5 mm PLgel 20 µm MIXED-A LS 300 x 7.5 mm Agilent PLgel Olexis 300 x 7.5 mm Agilent PS-H EasiVial 2 ml Agilent PS-M EasiVial 2 ml Agilent E-M x 0.2 g Agilent E-MW x 0.1 g Agilent E-SCB 10 x 0.1 g PL PL PL PL PL LS* PL PL LS* PL PL PL PL PL PL Agilent PL-SP 260VS ** Agilent PL-GPC 220 GPC/SEC Agilent PL-HTGPC-FT-IR** Agilent PL-BV 400HT Agilent PL-HTLS 15/90 Agilent ** Agilent Cirrus GPC Agilent Cirrus GPC Agilent GPC-FT-IR SCB * PL PL PL PL PL PL ** 26
27 GPC FT-IR 600-IR 600-IR (ATR) Agilent ATR Agilent 600-IR NMR Agilent NMR 1D 2D NMR 2D NMR Agilent 400-MR DirectDrive DirectDigital 400-MR Agilent 600-IR 27
28 Agilent Technologies, Inc Printed in Japan January 28, JAJP
GPC/SEC
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RS-AP1[操作説明書]
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