Columns - shodex.de

Organic SEC (GPC) Columns (General Analysis) :
DMF
Features
KD-800
• Standard organic solvent SEC (GPC) column
• Supports a wide range of applications from low to high molecular weight compounds
• Corresponds to USP L21
Standard columns
KD-800 series : Shipping solvent Dimethylformamide (DMF)
Product Code
Plate Number
(TP/column)
Product Name
Particle Size
(μm)
Pore Size
(Å)
Column Size (mm)
I.D. x Length
F6028210
GPC KD-801
≥ 17,000
6
50
8.0 × 300
F6028220
GPC KD-802
≥ 17,000
6
150
8.0 × 300
F6028225
GPC KD-802.5
≥ 17,000
6
300
8.0 × 300
F6028230
GPC KD-803
≥ 17,000
6
500
8.0 × 300
F6028240
GPC KD-804
≥ 17,000
7
1,500
8.0 × 300
F6028250
GPC KD-805
≥ 11,000
10
5,000
8.0 × 300
F6028260
GPC KD-806
≥ 11,000
10
10,000
8.0 × 300
F6028290
GPC KD-806M
≥ 13,000
10
10,000
8.0 × 300
F6028270
GPC KD-807
≥ 6,000
18
20,000
8.0 × 300
F6700411
GPC KD-G 4A
(GPC KD-G)
(guard column)
8
−
4.6 × 10
Base Material : Styrene divinylbenzene copolymer
* The columns with ‘L’ or ‘M’ at the end of column names are mixed-gel column capable of
analyzing samples over a wide range of molecular weight distribution.
* See page 62 for applicability of SEC (GPC) columns to solvent replacement.
Target molecular weight range and Exclusion limit
With *PEG/PEO (eluent : DMF)
Product Name
Target Molecular Weight Range
Exclusion Limit
Product Name
Target Molecular Weight Range
Exclusion Limit
KD-801
100 − 1,500
2,500
KD-805
30,000 − **(4,000,000)
**(4,000,000)
KD-802
200 − 4,000
7,000
KD-806
30,000 − **(40,000,000)
**(40,000,000)
KD-802.5
400 − 10,000
20,000
KD-806M
KD-803
1,000 − 50,000
70,000
KD-807
KD-804
4,000 − 200,000
200,000
1,000 − **(40,000,000)
50,000 − **(200,000,000)
* Please use the above table as a rough
indication for the column selection.
**(40,000,000)
**(200,000,000)
*PEG : polyethylene glycol
*PEO : polyethylene oxide
**( ) Estimated value
Solvent-peak Separation Columns for
Organic SEC (GPC)
Features
KF-800D
K-800D
• Use this column in combination with a linear column
• By shifting the elution of monomers, polymer additives, and the solvent-peak in low molecular region,
it reduces interferences in the calculation of the molecular weight distribution of polymers and oligomers
Solvent-peak separation columns
50
Product Code
Product Name
Column Combination
Particle Size
(μm)
Column Size (mm)
I.D. x Length
Shipping Solvent
F6709350
GPC KF-800D
KF-805L, 806L, 806M, 807L
10
8.0 × 100
THF
F6709450
GPC K-800D
K-805L, 806L, 806M, 807L
10
8.0 × 100
Chloroform
Base Material : Styrene divinylbenzene copolymer
Melamine formaldehyde resin
Sample : Polyvinylpyrrolidone 0.2% each
(A) K-30 400μL
(B) K-60 500μL
(C) K-90 500μL
107
Sample : 30μL
Melamine-formaldehyde resin 1%
(A)
05
04
KD
KD
M
06
-8
-8
03
KD
(B)
02
02
.5
01
-8
-8
KD
-8
KD
103
7
-8
-8
104
- 80
KD
KD
105
KD
06
-8
KD
106
Molecular weight (PEG/PEO)
Polyvinylpyrrolidones
(C)
102
5
6
7
8
9
10
11
12
13
10
Elution volume (mL)
Column
:
Eluent
:
Flow rate
:
Detector
:
Column temp. :
0
Shodex GPC KD-800 series
DMF
1.0mL/min
RI
40˚C
10
Column
:
Eluent
:
Flow rate
:
Detector
:
Column temp. :
20
Shodex GPC KD-806M x 2
10mM LiBr in DMF
1.0mL/min
RI
50˚C
20
Column
:
Eluent
:
Flow rate
:
Detector
:
Column temp. :
Celluloses
25 min
Shodex GPC KD-802 x 2
10mM LiBr in DMF
1.0mL/min
RI
50˚C
Phenoxy resin
Sample : 250μL
Phenoxy resin 0.2%
Cellulose is known to be difficult
to dissolve. A cellulose solution
is prepared by repeating solvent
replacement. It is reported that it
requires a long time to dissolve
(1 to 60 days), depending on the
solvent type, crystallinity and
molecular weight.
106
105
104
103
6
7
8
9
10
15
11
20
25 min
Elution volume (mL)
Shodex GPC KD-806M
1% LiCl in *DMI
0.5mL/min
RI, MALS (Multi angle light scattering)
60˚C
Data provided by Dr. Masahiko Yanagisawa,
Isogai group,
Graduate School of Agricultural and Life Sciences,
The University of Tokyo
* DMI 1,3-dimethyl-2-imidazolidinone
Potato starch
Column
:
Eluent
:
Flow rate
:
Detector
:
Column temp. :
Sample : 100μL
Potato starch in DMSO 0.1%
* solved at 80°C
Sample : Poly(vinyl chloride)
DOP
(Dioctyl phthalate)
06
Column
: Shodex GPC KD-806M
Eluent
: 10mM LiBr in DMSO/DMF=75/25
Flow rate
: 1.0mL/min
Detector
: RI
Column temp. : 50˚C
0
5
D
103
5
6
7
8
9
10
11
12
13
14
15
Elution volume (mL)
KF-806L + KF-800D
15
min
00
10
-8
104
102
5
KF
L+
6L
15 min
-8
10
80
5
105
KF
0
106
KF
KF-806L
0
Shodex GPC KD-806M x 2
10mM LiBr in DMF
1.0mL/min
RI
50˚C
Effects of solvent-peak separation column
Molecular weight (Polystyrene)
Column
:
Eluent
:
Flow rate
:
Detector
:
Column temp. :
Solvent-peak Separation Columns for Organic SEC (GPC)
Sample : 100μL
Cellulose ca. 0.05% each
107
Molecular mass
15
30 min
Organic SEC (GPC) Columns (General Analysis) : DMF
Calibration curves for KD-800 series
using PEG/PEO
10 min
Column : Shodex GPC KF-806L
Shodex GPC KF-806L + KF-800D
Eluent
: THF
Flow rate : 1.0mL/min
Detector : RI
51
Organic SEC (GPC) Columns :
Linear Calibration Type
Features
LF
• Employs a special packing material with a wide pore size distribution (multi pore type)
• Highly linear calibration curve without inflection points
• Molecular weight distribution can be determined with high precision
• Enables analysis over a broad range of molecular weights
• Column for rapid analysis (LF-604) and column for high performance analysis (LF-404) enabling reduction in
solvent use are also available
• Corresponds to USP L21
Standard columns
Product Code
Product Name
Plate Number
(TP/column)
Particle Size
(μm)
Pore Size
(Å)
Column Size (mm)
I.D. x Length
F6021041
GPC LF-804
≥ 17,000
6
3,000
8.0 × 300
F6709621
GPC LF-G
(guard column)
6
−
4.6 × 10
Base Material : Styrene divinylbenzene copolymer
Shipping Solvent : Tetrahydrofuran (THF)
* See page 62 for applicability of SEC (GPC) columns to solvent replacement.
Rapid analysis downsized column
Use of the LF-604 with semi-micro type devices is recommended.
Product Name
Plate Number
(TP/column)
Particle Size
(μm)
Pore Size
(Å)
Column Size (mm)
I.D. x Length
F6021042
GPC LF-604
≥ 9,000
6
3,000
6.0 × 150
F6709621
GPC LF-G
(guard column)
6
−
4.6 × 10
Product Code
Base Material : Styrene divinylbenzene copolymer
Shipping Solvent : Tetrahydrofuran (THF)
* See page 62 for applicability of SEC (GPC) columns to solvent replacement.
High performance semi-micro column
Use of the LF-404 with semi-micro type devices is recommended.
Product Name
Plate Number
(TP/column)
Particle Size
(μm)
Pore Size
(Å)
Column Size (mm)
I.D. x Length
F6021043
GPC LF-404
≥ 14,000
6
3,000
4.6 × 250
F6709621
GPC LF-G
(guard column)
6
−
4.6 × 10
Product Code
* See page 62 for applicability of SEC (GPC) columns to solvent replacement.
Base Material : Styrene divinylbenzene copolymer
Shipping Solvent : Tetrahydrofuran (THF)
Target molecular weight range and Exclusion limit
With Polystyrene (eluent : THF)
Product Name
Target Molecular Weight Range
Exclusion Limit
LF-804
300 − 2,000,000
2,000,000
LF-604
300 − 2,000,000
2,000,000
LF-404
300 − 2,000,000
2,000,000
* Please use the above table as a rough indication for the column selection.
Schematic diagram of linear calibration type packing
Connecting linear calibration type columns (LF series)
The linear calibration type column covers a broad range
of molecular weights with only one kind of packing (column).
Connecting mixed-gel columns (KF-804L, etc.)
56
Connecting different grades columns
(KF-804 + KF-803 + KF-802, etc.)
107
106
106
105
104
-40
4
102
103
102
5
6
7
8
9
10
11
12
1.0
13
1.5
2.0
Elution volume (mL)
Column
:
Eluent
:
Flow rate
:
Detector
:
Column temp. :
2.5
3.0
0
3.5
Shodex GPC LF-804
THF
1.0mL/min
RI
40˚C
Column
Eluent
Flow rate
: Shodex GPC LF-604, LF-404
: THF
: 0.5mL/min (LF-604)
0.3mL/min (LF-404)
Detector
: RI (small cell volume)
Column temp. : 40˚C
Sample : Xylan 0.1%, 100μL
10
15
10
Column
:
Eluent
:
Flow rate
:
Detector
:
Column temp. :
Polyamide (Nylon6/6)
5
5
15
20 min
Elution volume (mL)
Xylan
0
4
103
105
LF
104
Sample : Polyurethane 0.1%, 20μL
-60
Molecular weight (Polystyrene)
107
Polyurethane
LF
Molecular weight (Polystyrene)
Calibration curves for LF-604 and
LF-404 using polystyrene
20
Shodex GPC LF-404 x 2
THF
0.3mL/min
RI (small cell volume)
40˚C
Polymethyl methacrylate
Sample : NylonTM 6/6 0.1%, 20μL
0
25 min
Column
Eluent
: Shodex GPC LF-804
: 20mM H3PO4 + 20mM LiBr in
(DMSO/DMF=80/20)
Flow rate
: 0.6mL/min
Detector
: RI
Column temp. : 50˚C
5
10
Column
:
Eluent
:
Flow rate
:
Detector
:
Column temp. :
Organic SEC (GPC) Columns : Linear Calibration Type
Calibration curve for LF-804 using
polystyrene
15
20
Sample : 100μL
Polymethyl methacrylate
25
min
0
5
10
Column
:
Eluent
:
Flow rate
:
Detector
:
Column temp. :
Shodex GPC LF-404
5mM CF3COONa in HFIP
0.15mL/min
RI (small cell volume)
40˚C
15
20
25
30
min
Shodex GPC LF-804 x 2
Methyl ethyl ketone
1.0mL/min
RI
40˚C
Comparison of polystyrenes separation with different numbers
of LF-404
Polyamic acid
4
Sample : Poly(pyromellitic dianhydride-co-4,4'-oxydianiline), 100μL
5
3
Sample : 10μL
1. Polystyrene (Mw : 1,030,000)
2. Polystyrene (Mw : 152,000)
3. Polystyrene (Mw :
66,000)
4. Polystyrene (Mw :
22,000)
5. Polystyrene (Mw :
5,050)
6. Polystyrene (Mw :
580)
7. Ethylbenzene
6
7
2
1
LF-404 x 1
Column
: Shodex GPC LF-404 x n
Eluent
: THF
Flow rate
: 0.3mL/min
Detector
: RI (small cell volume)
Column temp. : 40˚C
4
5
3
7
6
2
1
LF-404 x 2
0
5
10
15
20
25
30
35
40
45
min
4
3
Column
:
Eluent
:
Flow rate
:
Detector
:
Column temp. :
Shodex GPC LF-804 x 2
30mM LiBr + 30mM H3PO4 in NMP
0.7mL/min
RI
50˚C
6
1
LF-404 x 3
0
7
5
2
5
10
15
20
25
30 min
57