液体クロマ トグラフィ用示差屈折計の開発
Contents
1. Fig 13 BACH oll dN dT dP dT 12. KERMA ORES dN dT 5 mn 2 dN dT LT be 3
3. 2 3 dnz n 1 K4p i9 46x10 94x10 239x109 db yy COMP IC CARE ZM Otr PEXESO RI Fig 21 5x10 back pressure 0 1 2 3 4 atm Fig 21 Eflect of compressibility 67 148 24 2 1980 dn ADO 4n
4. 100 gm 2 2
5. 9 Q sin 1 mE te e Sn 144 RARE 24 2 1980 Fig 9 6x10 D d 3 mm zg 1 5168 4x 10 eJ 4e s Full scale Fig 9 Optical Null glass on 256x k 2x 0 25mm 0 5mm 1 2 1x10 1 3 4x1075 RIU Fig 10
6. 68 Fig 23 ON 6x10 H 5x 10 77 C RI response Temperature control ON 350 e Temperature control OFF o E a 3x10 RIU RU 0 1 2 3 4 5hour Fig 23 Detector response 9 dn lx1079
7. 67 457 150 mm K
8. 5 19624 J Moore 3 Ri 59 140 24 2 nm R K n n 1 KK WAAROBS BIRO n Nm C1ns Carl 2 KEL es n Gladstore Dale g gc 2 1 2 3 c g mZ p
9. dn 9 1 3 4x 10 RIU 128 x10 FS 27 S N 2 0 2x10 RIU rz Fig 25 Fig 27 Fig 25 TSK G2000PW 0 75 cm x 60 cm Sucroce 1 0 gg a 69 130 424 2 980 Column 2000PW 7 5mmID 60cm Solvent Water RI range 2x 10 6 FS Injection volume 10z9 c Sucrose 1 04g 1 1 RI Range 2X10 FES Fig 25 Measurement of sucrose RI Range 2X10 5 FS t f f 1 I RI Range 1X10 i 1 usd SOM eye ere j iuo
10. Turns of optical zero screw 0 5 10 15 Fig 10 Linearity to change in zero glass rotation 256x10 FS CHO 3 Fig 11 Fig 12 15V p Balance VR AWN gt Polalyty SW 15V Range SW Marker SW OUT gt do gt 15V Fig 11 Schematic diagram of amplifier 64 DGEBA NSN RO AUN 145 15V T VC Erenn SW Heater IND Lamp Temp Set VR Fig 12 Schematic diagram of temperature control circuit 4 1 GPC 1 33 1 61 RANILI L NIVEL eS
11. dN dP WADA 2 Fig 13 Fig 22 Fig 22 Structure of the flow cell 2 Fig 13 Fig 22
12. 2 Fig 13 14 Fy eg Fig 15 45 67 Kon avy bil 0 8 mm Fig 13 Structure of the flow cell ERECTO BUR RT REPT ARABS 45 1 0 1 8 Fig 14 Structure of the flow cell C 65 146 SEW EAR 24 2 1980 1 0 lS n 1 8RI Fig 15 Deviation of the image 1x10 67 1 3 1 52 1 3 1 6 2 3 45 2 Acetone in THF v v
13. f 150mm 2 10ug 67 45 O 2 3 Fig 13 Fig 14 Fig 22 1 HLC 803A Fig T Fig 8 2 1 155 Fig 8 Front view of RI 8 Separate Type C 63 2 Fig 4 HAY tO 6 V2A 3 4 V
14. 153 Fig 35 Measurement of Heavy Oil Column GMH6 7 5 mmID 120cm Eluant CHCl Flow rate 1 4 mZ min Sample size 0 1 1 000 ug RI range 32x 107 5 FS Fig 36 Measurement of Dextran Mw 176000 Column G5000 PW 7 5 mmID 60cm Eluant Water Frow rate 10 m min Sample size 0 527 30 ut RI range 32x10 S FS Fig 37 Measurement of Oligosaccharide Column G2000 PW 7 5 mmID 60cm Eluant Water Flow rate 10 mZ min Sample size 0 5 50 uz RI range 32x10 5 FS Fig 38 Measurement of TSK Starda d Polyethylene oxid Column G5000 PW 7 5 mmID 60cm Eluant M 15 phosphate buffer M 10 KCI Flow zate 1 0 mZ min Sample size 0 06 500 gl RI range 64x 10 9FS 73 154 Eur 208 2 1980 Fig 39 Measurement of Gum Arabic Powder Column G5000 PW 7 5 mmID 60cm Eluant M 15 phosphate buffer M 10 KCI Flow jate 1 0 mZ min Sample size 0 1 500 pl RI range 128x10 5 FS Fig 41 Measurement of Human Serum Column G3000SW 7 5mm 60 cm Eluant 0 1M phosphate buffer 0 3 M NaCl Flow rate 1 0 m2 min Sample size 10 pg RI range 32x 10 8 FS Fig 42 Measuzement of Saccharides Column TSK GEL LS 450 NH Column Size 7 5 mmID x 30cm Mobile Phase CHyCN H20 65 35 Fig 40 Measurement of Pullulan Column G6000PW 7 5mmID 60 cm Eluant M 15 phoshate buffer M 10 KCl Flow rate 1 0m min
15. 9 YO i cos Es sin sin sin e me Gu sin EI cos 9 Sa 1980 n GEBRO DTA 0 9 KM R dg Zorees n cos ey I 2 ng cos 6 n cos B 1 fn cos 9 6 cos By Pora 0 RB Oe zR LTRS na Sin n sin B 8 no n sin 0 9 ze 8 7 SOKO GE To 802 W Labo ato y Data Control LDC SF 1107 model 3 1 3 1 6 Fig 1 LDC SF 1107 amp Fig 2 802 Cell Prism lt 9 Zer
16. 0 1 20 gg THE Fig 28 06mm G2000 H8 THF 0 5 20 Z Table 3 Table 3 Result of theoretical plate check Pigs Die Volume TP F 06mm 14 7900 j o Bum eo 02 Gu soo Table 4 0 6 mm 50cm TSK GMH4 0 75 cm x 60 cm THE 12595 20z2 100 cm Table 4 Result of theoretical plate check Rowe 0 8mm 0 6 mm 0 2mm 3500TP F
17. 107 10 4 Imv 10v biIe 1x Acetone in THF Ie Benzene in THF RI range 128 x Recorder 500 mv FS Fig 16 Measurement of the dynamic range 107 4x107 Fig 16 THE eve 50x 10 RI THF 1x l0 FS 256x10 5 FS x 9 3 0 25 50 100 g 2 2 dazzl07 Injection volume 3 Fig 18 Responce of detector and injection volume 66 5 ares 4 5 WUE sb 797 147 Fig 18 peak hight 3 Saccharides TSK GEL LS 450 NH 0 75 cm x 30 cm CHICN H3O 65 35 1 5mZ min
18. Fig 6 WE Fig 6 Interference Refractometer of the Jamin Type Gi Gs d d DORM n m di d2 dg n n2 ng 4 d 2ngd gC cos B1 cos B5 iq Bi LG Ba Ge ANA Uma Gi EG Bi f DL EF PRAET TDS G Bg DEI Frig 6 Ty Ty og TO TRO ARC Lo COREA UT OPTILAB model 902 546 nm 10 1 0 2 0 02 mm 10 mm 10 52x10 FS HY 5x107 RIU S N 2 1x10 8 RIU
19. 3x10 mm 23x10 9 C RE THE L0 m2 min 1 0m2 min dE 3 without cell e R S 1 0ml min o R 0 S 1 0ml min 2 5X10 temp 30 40 50 60 C Fig 24 Effect of temperature 1075 20 H 149 Fig 24 15mm
20. 133 N i B 5 B fT TH it ie Differential Refractometer for Liquid Chromatography Nobuyuki BAMBA Makoto AIURA Tsutomu HASHIMOTO Widely used as monitor in liquid chromatography is differential refractometer that detects relative content of separated substances from the difference of refractive index between a pure solvent and a solution containg separated substances Recently we have developed a new differential refractometer commercialized as TOYO SODA RI 8 with an improved optical system and temperature control system Full scale deflection of this unit of which fow cell angle is 45 and focal length of lens 150 mm is 1x 10 RIU and noise level of refractive index is less than 1x 107 RIU at optimum condition This paper deals with appraisal of measurement results obtained from experiments 1 GPC DRI GPC
21. 0 1 2 3 4 Fig 17 Responce of detector and solutioa 4 coacentration THF Be te Fig 17 2 0 6 dn v7 A 1000c G3000H8 0 75 cm x 30 cm THE 1 0 m min 1005 2 3x107 Pesk licht 9 2x10 RIU JO C RI
22. Fig 19 3 4 5 DRI Fructose Sucrose Glucose Maltose Maltotriose Injection volume gg Fig 19 Responce of detector and injection volume FERE EERE ATA 1X10 RIU 2X 107 RIU 4X10 RIU 8X 107 RIU Fig 20 Noise level of RI 8 150mm dN dT 1 x10 Art Fig 20 1x10 RIU
23. Table 1 Table 1 7 8 3 FSUE Fig 5 4 mo 1 n Ru Ry ROAX Ty Th 4R AT Fig 5 Interference of parallel plate AR n cos B 4 2 nt sif 2 02 AT 2dn cos 29 2 ginza 03 24 2 sin2g 2 W 4 2dy n sinfa 2N 3 Bj XE3BDXC 43 BLN 20 12 d e Jamin
24. 500 He S N DRI 45 AUBRE 150 mm DRI TSK Model RI 8 1x108 RIU 2x10 RIU 10 20 4 3 gt 5 2 KAD BEBE S i
25. T B 1 W Heller J Phisicai Chem 69 1123 1965 2 H E Jones L E Ashman E E Srahly Anal Chem 21 1470 1949 3 H W Johnson Jr V A Campanile H A Lefebre Anal Chem 39 32 1967 4 U S Pat 2780131 1957 5 ibid 3386332 1968 6 Brit Pat 1271172 1972 7 Henri Colin et al J Chromatogr Sci 17 485 1979 8 Milos Krejei et all J Chromatogr 73 105 1972 9 Minard Bakken Virgil I Stenberg J Chro matogr Sci 9 603 1971 10 H5 26 1969 11 E M Barrall M J R Cantow J F Johnson J Api Polym Sci 12 1373 1968 12 H L Wanger C A J Hoeve J Po ym Sci A 2 9 1763 1971 C 75
26. Xv 5 10 1 2 Table 2 Table 2 Compare of temperature effect Drift No 1 No 2 Condition Pioto type Proto type TC OFF 2 5x10 6 C 2x10 7 C Without Cell TC ON 5x10 7 C ILx10 7 C With Cell TC OFF 1 5x107 C 2x10 7 C R S 1 0 mZ min 4 THF G2000 TC ON 5x1077 C 1x1077 C 6 sucrose 220mg 27 elt 16x 107 RIU 128x 10 6 FS 12 5
27. n bi 2 ni 1 81 4 be na 1 02 5 gz gc Gov qme GPC Mi Ni 11 RHEE DC dR dn
28. 2ftana An 09 e 6 e Null glass Photosensor Fig 3 Const uction of differential refractometer o by y f tan w 0 XE cy eg cg Roc ooa n uU ui Fig 4 The schematic diagram of the TSK model RI 8 Table 1 Chazacteristic properties of the DRI Detectors Maker amp Measure Cell Noise Drift peen p Attenua Pressure Signal Light rupe imi out pu Model Range Volume no flow RIU H s n 2 ES FS psi E source range e cx um 1 0 1 8 10 1x10 8 3x107 2x10 0 1x 100 100 tungsten R T 60 RI 8 9 step BEN uii Shodex 1 0 Jg E 25 256 x water SE 11 1 75 8 3x10 5x10 6x10 oad 10 100
29. 10 4 4I 4n n 1 Cc AT 09 c liquid thermal expansion GPC THF 6 5x10 C KG 7x10 5 6x10 9 lx 107 RIU 1 5x10 5 C L
30. 4900TP F 5300TP F 4700TP F 1 0 mf min l6m min 3200TP F 5000TP F 8 GPC 71 1 1D19 Fig 29 T TSK GMH6 0 75 cm x120 cm THF 0 7 m min TSK 0 05 500 gg UV 254 nm Lj 10 10 cB peak area polystyrene My 10 10 10 107 10 Fg 29 Eflect of molecular weight 9 GPC THE Fig 30 Fig
31. 32 i Fig 33 Fig 85 GPC PW Fig 36 Fig 40 SW Fig 41 Saccharides Fig 42 Ree AA 152 Applications REEERE 24 2 1980 Examples of measurement are shown as follows 100000 10200 Fig 30 Measurement of Standard Polystyrenes Fig 31 Fig 32 Fig 33 Fig 34 Column Eluant Flow rate Sample size RI range Measurement Column Eluant Flow rate Sample size RI range Measurement Column Eluant Flow rate Sample size RI range Measurement Column Eluant Flow rate Sample size RI range Measurement Column Eluant Flow rate Sample size RI range GMH6 7 5 mmID 120 cm 2880000 THF 1 0 mZ min 0 01 100 ge 16 x 107 5 FS of Silicon Oil G6000H3 7 5 mmID 120 cm THF 1 4me min 525 100 ug 32x 107 5 FS of Poly methyl methacrylate G6000H3 7 5 mmID 120 cm THF 1 4 mZ min 0 016 1 000 we 32x 10 FS of Melamine Resin GMH6 7 5 mmID 120 cm CHCl gt 1 4m min 0 1 1 000 ne 32x 10 8 FS of Silicon Varnish GMH 6 7 5 mmID 120 cm CHCl 1 4 MZ min 0 1 1 000 uz 82x10 9 FS 72
32. 2 3 RI 8 C 62 eo 9 4 a RAMEE OA 143 1 2 3 4 5
33. i an PAPEL nti arias ae i 0 2 4 6 8 10 12 14 Hinutes Fig 28 Measurement of Glycerin Fig 26 TSK G2000SW 0 75 cm x 30 cm Glycerin 1 0 4g Fig 27 TSK LS 410 Hz O MeoH 20 80 Napthalene 0 1 gg TSK HLC 803A CHs haw Non l 3 d T a ee ee 3 Fig 28 0 1 mm Fig 27 Measurement of napthalene 80cm M gt i eee aL Minutes C 70 Bk n i757 4 AOR 151 peak width flow rate ml min 0 1 2 3 4 5 Fig 28 Peak width vs flow rate 0 6mm Ex 50cm
34. tungsten bath Waters 1 0 2x d 1 x10 39 6x 1078 128 x water nam Pags 10 3 6 10 71 65 10 7 4 xno p 025 100 10 100 tungsten c Knauer l 25 6 X luminescent 8 7 8 ENS 5100 8 2x10 1x10 5x10 oS o 10 100 diode 900 nm 10 60 IOTA Me cen EM ER AsGa 1 F x107 sGa 21078 eG 910nm Miczom kon j m ilio pe m 4 BOOx 7l eritics 1 85 11 2x10 6x10 4x10 1x8 step 200 10 tungsten ALTEX i 64x LED 8 5x10 8 5x10 8 1x107 0 1x 100 10 50 156 E 8 step 900 nm B JAT s 8 q H28x RI 2 50 8x10 3x10 2x10 h x8 step 1 10 100 tungsten S T 50 C61 142 _SOERREDEENA Hob 2S 1980 nu OBE An An nsP lt 1 dn n 4n210 Fig 4
35. Sample size 0 05 500 gg RI range 64x 10 8 FS Sample Sample Size 2 5 mg m 50 uu Flow Rate 1 5 mZ min Pressure Kg cm Temperature R T Chart Speed 5 0mm min Detector RI 32x10 8 RIU SANI 9snon esoiong SL W C74 4 155 6 2x10 RIU D RUG 2 1x10 RIU 1 x10 C WERE RT 60 C 0 15 me 150 C 200 mZ min Ho 2 mm HCL OX SD 3 SU ABO 5
36. o glass Adj I2 L1M2 Zero glass MC D E Projector Fay movement fyc M e SL Fine Adj 7 C Fig 1 the schematic diagram of the LDC model SF 1107 T NETS cos 0 1 sin 2 rcgi Cnt 2 sin f sin 9 ITAL Lamp f y 6 Fig 2 The schematic diagiam of the TSK y sin 0 model HLC 802 C 60 7T C rete Mirror Cell Lens ye Ai 2 ci cz ci c 8 An Fig 3 a koc 24 di 6
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