Downsized organic SEC (GPC) Columns: KF-600

(Eluent: THF)

Calibration curves for GPC KF-600 series are shown.

Sample : PS, Polystyrene

Column : Shodex GPC KF-600 series (6.0mmID*150mm each)
Eluent : THF

Downsized organic SEC (GPC) Column, GPC KF-602 (6.0mmID*150mm) and standard type column KF-802 (8.0mmID*300mm) are comapred using styrene oligomer. The required analysis time is 10 min. for KF-602 and 20 min. for KF-802. This means the analysis time for KF-602 is about half of that for KF-802. The solvent consumtion is 6mL (0.6mL/min x 10min.) for KF-602 and 20mL (1.0mL/min x 20min.) for KF-802. This means the solvent consumption for KF-602 is less than one third of that for KF-802.

Sample: Styrene oligomer

              (Above)                                  (Below)
Columns      : Shodex GPC KF-602 (6.0mmID*150mm) x 2  : Shodex GPC KF-802 (8.0mmID*300mm) x 2
Eluent       : THF                                    : THF
Flow rate    : 0.6mL/min                              : 1.0mL/min
Detector     : Shodex RI(small cell volume)           : Shodex RI
Column temp. : 40deg-C                                : 40deg-C

For GPC KF-602, the relaion between HETP (height equivalent to a theoretical plate) and temperature is shown here. In the range of 30 to 50 deg-C, HETP changes very little. This is also true for other grades of Shodex GPC KF-series columns. When using the columns replacing the in-column solvent from original solvent (THF) to other solvents, check the physical characteristics (viscosity, melting point, boiling point, etc.) of the solvent to be used because the pressure may exceed the maximum usable pressure by vaporization or solidification of a part of the solvent in the column. Usually, the use of KF-series columns in the range of room temperature to 45 deg-C is recommended.

Sample : 0.1% Dicyclohexylphthalate, 5micro-L

Column       : Shodex GPC KF-602 (6.0mmID*150mm)
Eluent       : THF
Flow rate    : 0.5mL/min 
Detector     : UV(254nm)(small cell volume)
Column temp. : 40deg-C

For GPC KF-602, the relation between HETP (height equivalent to a theoretical plate) and flow rate is shown here. The value of HETP is almost the same in the range of 0.4 to 0.8mL/min. However, outside of the range, the value of HETP is higher. This is true for other grade of Shodex GPC KF-series columns. When using the columns replacing the in-column solvent from original solvent (THF) to other solvents, check the pressure not to exceed the maximum usable pressure because the pressure will be higher if the viscosity of the replaced solvent is higher.
Generally, the use of KF-series columns in the range of 0.4 to 0.6 mL/min is recommended.

Sample : 0.1% Dicyclohexyl phthalate, 5micro-L

Column       : Shodex GPC KF-602 (6.0mmID*150mm)
Eluent       : THF 
Detector     : UV(254nm)(small cell volume)
Column temp. : 40deg-C

For GPC KF-606M, the effect of sample concentration on lution volume and peak-width is shown here. The effect of sample concentration is marked for the sample of larger molecular weight. When the injection volume is 10 micro-L, the sample concentration smaller than 0.05% is recommended for the sample of which maolecular weight is smaller than 6,750,000.

Sample : PS, Polystyrene, 10micro-L

Column       : Shodex GPC KF-606M (6.0mmID*150mm)
Eluent       : THF 
Column temp. : 40deg-C

For GPC KF-606M, the effect of injection volume on elution volume and peak-width is shown here. When the injection volume is changed, the elution volume changes very little, however, the peak-width inceases markedly when the injection volume exceeds 20 micro-L. Therefore, the use of sample concentration lower than 0.05% and the injection volume smaller than 20 micro-L is recommended.

Sample : PS, Polystyrene
(Elution Volume)
1.7K(0.05%), 4.8K(0.05%), 28.5K(0.05%), 66K(0.05%), 156K(0.03%), 514K(0.03%), 2950K(0.01%), 6750K(0.01%)
(Peak-width)
1.7K(0.05%), 4.8K(0.05%), 28.5K(0.05%), 66K(0.05%), 156K(0.01%), 514K(0.01%), 2950K(0.01%)

Column       : Shodex GPC KF-606M (6.0mmID*150mm)

Eluent       : THF 

Column temp. : 40deg-C

Polystyrene standards were analyzed using GPC KF-601, a downsized organic SEC (GPC) column.

Sample : 5micro-L
1. PS (MW: 6,200) (0.03%)
2. PS (MW: 300) (0.2%)
3. n-Propylbenzene (MW: 120) (0.08%)
4. Benzene (MW: 78) (0.08%)

Column       : Shodex GPC KF-601 (6.0mmID*150mm)
Eluent       : THF
Flow rate    : 0.5mL/min
Detector     : UV(254nm)(small cell volume) 
Column temp. : Room temp.

Polystyrene standards were analyzed using GPC KF-602, a downsized organic SEC (GPC) column.

Sample : 5micro-L
1. PS (MW: 42,800) (0.04%)
2. PS (MW: 2,800)(0.1%)
3. PS (MW: 300) (0.2%)
4. n-Propylbenzene (MW: 120) (0.1%)
5. Benzene (MW: 78) (0.1%)

Column       : Shodex GPC KF-602 (6.0mmID*150mm)
Eluent       : THF
Flow rate    : 0.5mL/min
Detector     : UV(254nm)(small cell volume)
Column temp. : Room temp.

Polystyrene standards were analyzed using GPC KF-602.5, a downsized organic SEC (GPC) column.

Sample: 5micro-L
1. PS (MW: 107,000) (0.04%)
2. PS (MW: 10,200) (0.08%)
3. PS (MW: 2,800) (0.1%)
4. PS (MW: 580) (0.2%)
5. n-Propylbenzene (MW: 120) (0.1%)
6. Benzene (MW: 78) (0.1%)

Column       : Shodex GPC KF-602.5 (6.0mmID*150mm)
Eluent       : THF
Flow rate    : 0.5mL/min
Detector     : UV(254nm)(small cell volume)
Column temp. : Room temp.

Polystyrene standards were analyzed using GPC KF-603, a downsized organic SEC (GPC) column.

Sample : 5micro-L
1. PS (MW: 422,000) (0.04%)
2. PS (MW: 42,800) (0.06%)
3. PS (MW: 16,700) (0.07%)
4. PS (MW: 6,200) (0.08%)
5. PS (MW: 1,050) (0.15%)
6. n-Propylbenzene (MW: 120) (0.1%)

Column       : Shodex GPC KF-603 (6.0mmID*150mm)
Eluent       : THF
Flow rate    : 0.5mL/min
Detector     : UV(254nm)(small cell volume)
Column temp. : Room temp.

Polystyrene standards were analyzed using GPC KF-604, Downsized organic SEC (GPC) Column.

Sample : 5micro-L
1. PS (MW: 1,260,000) (0.01%)
2. PS (MW: 186,000) (0.02%)
3. PS (MW: 42,800) (0.03%)
4. PS (MW: 10,200) (0.04%)
5. PS (MW: 1,050) (0.05%)
6. n-Propylbenzene (MW: 120) (0.05%)

Column       : Shodex GPC KF-604 (6.0mmID*150mm)
Eluent       : THF
Flow rate    : 0.5mL/min
Detector     : UV(254nm)(small cell volume)
Column temp. : Room temp.

Polystyrene standards were analyzed using GPC KF-606M, a downsized organic SEC (GPC) column.

Sample : 5micro-L
1. PS (MW: 4,480,000) (0.01%)
2. PS (MW: 422,000) (0.02%)
3. PS (MW: 107,000) (0.03%)
4. PS (MW: 16,700) (0.04%)
5. PS (MW: 2,800) (0.05%)
6. n-Propylbenzene (MW: 120) (0.05%)

Column       : Shodex GPC KF-606M (6.0mmID*150mm)
Eluent       : THF
Flow rate    : 0.5mL/min
Detector     : UV(254nm)(small cell volume)
Column temp. : Room temp.

Two kinds of polystyrene standard, RAPRA and NBS 706 were analyzed using GPC KF-606M, a downsized organic SEC (GPC) column.

Sample : PS, Polystyrene, (Left): RAPRA, (Right): NBS 706, 0.1% each, 20micro-L

Columns      : Shodex GPC KF-606M (6.0mmID*150mm) x 2
Eluent       : THF 
Flow rate    : 0.6mL/min
Detctor      : Shodex RI(small cell volume)
Column temp. : 40deg-C

Two kinds of epoxy resin, epokote 1001 and epikote 1004 were analysed using conventional type organic SEC (GPC) column (GPC KF-803L) and downsized organic SEC (GPC) columns (GPC KF-603 + KF-602.5). Using downsized GPC columns, better separation could be obtained in shorter time. For downsized GPC columns, an RI detector of small cell volume type was used.

Sample : Epikote (Epoxy reisne)

Columns      : Shodex GPC KF-803L (8.0mmID*300mm) x 2   
Eluent       : THF                                     
Flow rate    : 1.0mL/min                                
Detector     : UV(254nm)(conventional type)                         
Column temp. : Room temp.
 
Columns      : Shodex GPC KF-603 + KF-602.5 (6.0mmID*150mm each)  
Eluent       : THF                             
Flow rate    : 0.6mL/min
Detector     : Shodex RI(small cell volume) 
Column temp. : 40deg-C

(Eluent: Toluene)

Polydimethylsiloxane was analyzed using GPC KF-606KF-604 and KF-603, downsized organic SEC (GPC) Columns.

Sample : Polydimethylsiloxane
1. visco.=10,000
2. visco.=350

Columns      : Shodex GPC KF-606 + KF-604 + KF-603 (6.0mmID*150mm each)
Eluent       : Toluene
Flow rate    : 0.6mL/min
Detector     : Shodex RI(small cell volume) Polarity: (-)
Column temp. : 40deg-C

(Eluent: DMF)

Cellulose acetate was analyzed using GPC KF-606M, a downsized organic SEC (GPC) Column.

Sample : Cellulose acetate

Columns      : Shodex GPC KF-606M (6.0mmID*150mm) x 2               
Eluent       : 0.01M LiBr in DMF  
Flow rate    : 0.5mL/min                        
Detector     : Shodex RI(small cell volume)  
Column temp. : 40deg-C

Poly(vinylpyrrolidone) was analyzed using GPC KF-606M, a downsized organic SEC (GPC) Column.

Sample : Poly(vinylpyrrolidone)

Columns      : Shodex GPC KF-606M (6.0mmID*150mm) x 2               
Eluent       : 0.01M LiBr in DMF  
Flow rate    : 0.5mL/min                        
Detector     : Shodex RI(small cell volume)  
Column temp. : 40deg-C

Styrene acrylonitrile copolymer was analyzed using GPC KF-606M, a downsized organic SEC (GPC) Column.

Sample : Styrene acrylonitrile (30:70) copolymer

Columns      : Shodex GPC KF-606M (6.0mmID*150mm) x 2               
Eluent       : 0.01M LiBr in DMF  
Flow rate    : 0.5mL/min                        
Detector     : Shodex RI(small cell volume)  
Column temp. : 40deg-C

Styrene allylalcohol copolymer were analyzed using GPC KF-606M, a downsized organic SEC (GPC) Column.

Sample : Styrene allylalcohol copolymer

Columns      : Shodex GPC KF-606M (6.0mmID*150) x 2               
Eluent       : 0.01M LiBr in DMF  
Flow rate    : 0.5mL/min                       
Detector     : Shodex RI(small cell volume)  
Column temp. : 40deg-C

Vinyl chloride vinyl acetate copolymer were analyzed using GPC KF-606M, a downsized organic SEC (GPC) Column.

Sample : Vinyl chloride vinyl acetate (90:10) copolymer

Columns      : Shodex GPC KF-606M (6.0mmID*150mm) x 2               
Eluent       : 0.01M LiBr in DMF  
Flow rate    : 0.5mL/min                        
Detector     : Shodex RI(small cell volume)  
Column temp. : 40deg-C

(Eluent: NMP)

Polyimide was analyzed using GPC KF-606M a d ownsized organic SEC (GPC) Column.

Sample : 0.1% Polyimide, 10micro-L

Columns      : Shodex GPC KF-606M (6.0mmID*150mm) x 2
Eluent       : 0.01M LiBr in NMP
Flow rate    : 0.5mL/min
Detector     : Shodex RI(small cell volume)
Column temp. : 60deg-C

Poly(vinylpyrrolidone) (PVP) were analyzed using GPC KF-606M, a downsized organic SEC (GPC) Column.

Sample : Poly(vinylpyrrolidone) (PVP) 0.1%, 10micro-L
(A) PVP (K 15)
(B) PVP (K 30)
(C) PVP (K 60)
(D) PVP (K 90)

Columns      : Shodex GPC KF-606M (6.0mmID*150mm) x 2               
Eluent       : 0.01M LiBr in NMP  
Flow rate    : 0.5mL/min                        
Detector     : Shodex RI(small cell volume)
Column temp. : 60deg-C
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