sec
SEC
37
Applications of TSKgel H-TYPE Gel PERMEAtion columns
Shear Degradation
Shear degradation is observed especially when ultra-high molar mass
compounds are analyzed. It tends to occur when analysis is carried out
at high flow rates using a micro-particle size packing material.
FIGURE 33
demonstrates the relationship between shear degradation and particle
size of the packing material, when TSKgel GMH columns were used.
When the flow rate is 1.0 mL/min, normal elution of an ultra-high molar
mass sample (2.06 × 107 Da) is only possible with the TSKgel GMH
HR
-
H(S) column, which has a large particle size. However, with the TSKgel
GMH
XL
and GMH
HR
-H columns, shear degradation does take place and
new peaks appear in the chromatogram on the smaller molar mass side.
Acrylic polymer
Figure 34
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.
figure 33
Shear degradation comparison
0
2
4
6
8
Retention time (minutes)
C
B
A
Detector response (AU)
TSKgel GMH
HR
-H, 5 µm, 7.8 mm ID × 30 cm L; B: TSKgel GMH
XL
, 9 µm, 7.8 mm
ID × 30 cm L; C: TSKgel GMH
HR
-H(S), 13 µm, 7.8 mm ID × 30 cm L
Mobile phase: THF; Flow rate: 1.0 mL/min
Detection: UV @ 254 nm; Temperature: 25 °C
Sample: polystyrene standard F2000 (2.06 x 10
7
Da) 20 µL (0.025%)
figure 34
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:
Temperature:
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
40°C
Column:
A. TSKgel Multi oreH
XL
-M, t .8 m 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 colu ns in series, mixed-bed type;
Sample: acrylic polymer (0.1%, 50 µL); Elution: THF; Flow rate: 1.0 mL/min;
Temperature: 40°C; Detecti n: RI
