Basic HTML Version
SEC
56
Applications of TSKgel H-type Gel PERMEAtion columns
Acrylic polymer
Figure 26
shows the separation of an acrylic polymer on the TSKgel
MultiporeH
XL
-M column compared with two commercially available
mixed-bed columns. The arrows illustrate the inflections seen in
the chromatograms from mixed-bed columns and the improvement
achieved when using the TSKgel MultiporeH
XL
-M column.
Polymethylmethacrylate
The effect of different pore size distributions in the mixed beds of TSKgel
GMH
HR
-H and TSKgel GMH
HR
-M is illustrated in
Figure 27
. The TSKgel
GMH
HR
-M produces better resolution in the 8 x 10
5
to 1 x 10
4
Da range.
Semi-Micro GPC
Semi-micro columns are referred to as such since their dimensions
are smaller than conventional columns in terms of internal diameter
as well as in length: 4.6 mm or 6 mm ID x 15 cm vs. 7.8 mm ID x 30
cm of conventional GPC columns. As shown in
Figure 28
, a TSKgel
SuperMultiporeHZ-N column provides the same or higher resolution at
a much shorter analysis time than multiple conventional sized columns
linked together.
Columns:
A. TSKgel GMH
HR
-H, 7.8 mm ID x 30 cm L
;
B. TSKgel GMH
HR
-M, 7.8 mm ID x 30 cm L
;
Sample: polymethylmethacrylate: 1. 820,000 Da, 2. 67,000 Da, 3. 10,200 Da,
4.1,950Da;Solvent:5mmol/Lsodiumtrifluoroacetateinhexafluoroisopropanol;
Flow Rate: 1.0 mL/min; Detection: UV@220 nm; Temperature: 40°C
figure 27
Comparison of TSKgel GMH
HR
-H and -M columns with polymethylme-
thacrylate standards
figure 26
Separation of acrylic resin by SEC on TSKgel MultiporeH
XL
-M and
mixed-bed type columns
10
20
100
50
0
A
B
150
C
mV
Minutes
Separation of acrylic resin by SEC
on TSKgel MultiporeH
XL
-M and mixed-bed type columns
Column:
Sample:
Elution:
Flow Rate:
A. TSKgel MultiporeH
XL
-M, two 7.8 mm ID x 30 cm L columns
in series;
B. Competitor P, two 7.5 mm ID x 30 cm L columns in series,
mixed-bed type;
C. Competitor S, two 8.0 mm ID x 30 cm L columns in series,
mixed-bed type
acrylic polymer (0.1%, 50 µL)
THF
1.0 mL/min
Comparison of TSKgel GMH
HR
-H and -M columns wit
Column:
A. TSKgel GMH
HR
-H, 7.8 mm ID x 30 cm L;
HR
-M, 7.8 mm ID x 30 cm L
Sample:
polymethylmethacrylate: 1. 820,000 Da, 2. 67,000 Da
3. 10,200 Da, 4. 1,950 Da
Solvent:
5 mmol/L sodium trifluoroacetate in hexafluoroisopropanol
Flow Rate:
1.0 mL/min
Detection:
UV @ 220 nm
Temperature: 40°C
Minutes
A. TSKgel GMH
HR
-H
B. TSKgel GMH
HR
-M
0 5 10
0
5 10
2
1
1
2
3
4
4
3
Minutes
polymethylmethacrylate standards
B. TSKgel GMH
figure 28
PTMEG Analysis on Conventional and semi-micro TSKgel Columns
-10
10
30
50
70
90
10
20
30
40
(A) Conventional columns
7.8mm ID x 30cm x 4
(B) TSKgel SuperMultiporeHZ-N
4.6mm ID x 15cm x 4
Eluent:
THF
Flow Rate:
(A) 1.0mL/min,
(B) 0.35mL/min
Detector:
RI
Temp.:
40°C
ample:
PTMEG, poly(tetramethyleneether glycol)
Inj. volume:
(A) 60µL
(B) 10µL
Col
Mo
Flo
Tem
Inje
Sa
Columns: A. Conventional columns, 7.8 mm ID x 30 cm L x 4,
B. TSKgel Super-
MultiporeHZ-N, 4.6 mm ID x 15 cm L x 4
;
Mobile phase: THF; Flow rate: (A) 1.0 mL/min (B) 0.35 mL/min; Temperature:
40°C; Injection vol.: (A) 60 μL (B) 10 μL; Sample: poly(teramethylene ether
glycol), (PTMEG 650), 10 μg/μL
Column:
A. TSKgel MultiporeH
XL
-M, two 7.8 mm ID x 30 cm L in series,
B. Competitor P, two 7.5 mm ID x 30 cm L columns in series, mixed-bed type;
C. Competitor S, two 8.0 mm ID x 30 cm L columns in series, mixed-bed type;
Sample: acrylic polymer (0.1%, 50 µL); Elution: THF; Flow Rate: 1.0 mL/min;
Temperature: 40°C; Detection: RI