Lab Catalog - page 28

SEC
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TSKgel GMPW and TSKgel GMPWXL
When the molecular weight range of the sample is broad or unknown,
Tosoh Bioscience offers mixed-bed and multipore columns for
analysis. The mixed bed column TSKgel GMPW and its high resolution
counterpart, TSKgel GMPWXL, are packed with the G2500, G3000 and
G6000 PW or corresponding PWXL resins. They offer a broad molecular
weight separation range. As shown on page 42, the calibration curve
for polyethylene glycols and oxides on these columns is fairly shallow
and is linear over the range of 100-1,000,000 Da. The introduction
of mixed-bed columns has facilitated the analysis of polydisperse
samples. Previously, two-column systems such as TSKgel G3000PW
and TSKgel G6000PW, were required to achieve good resolution with
wide MW-range samples. The substitution of a TSKgel GMPW series
column can save both time and money compared with multi-column
systems.
TSKgel SuperMultiporePW
TSKgel SuperMultiporePW columns incorporate the multi-pore
particle synthesis technology developed by Tosoh scientists in which
monodisperse particles exhibit a broad range of pore sizes. See page
54 for additional information on multipore technology. Each particle,
by design, has an extended linear calibration curve, thereby greatly
diminishing the appearance of chromatograms with inflection points.
This allows better reproducibility when determining molecular mass
and molecular mass distribution of polymers.
Three semi-micro (6.0 mm ID x 15 cm L) columns are available within the
TSKgel SuperMultiporePW series containing 4, 5 or 8 μm particles. This
enables high speed separation for aqueous polymers and low solvent
consumption compared to the conventional SEC columns. In addition,
a wide separation range can be analyzed with the three different
columns, from high molecular mass aqueous polymers to oligomers.
Multi-pore, semi-micro SEC columns provide high resolution and
smooth peak shapes without shoulders of inflection points. This leads
to better accuracy and reproducibility when determining the molecular
mass distribution of water soluble polymers
Comparison with conventional GPC columns
FIGURE 20 shows the SEC analysis of a real sample Polyvinyl-
pyrrolidone (PVP) K-30- on a series of conventional TSKgel G3000PWXL
and G5000PWXL columns compared to the one obtained with a
single TSKgel SuperMultiporePW-M linear SEC column (MW range
600,000 – 1,500,000). On a series of conventional SEC columns the
Polyvinylpyrrolidone peak shows an inflection point, which does not
appear on the SuperMultiporePW-M column. Analysis is much faster
and more sensitive when applying the new multi-pore packing.
A mixture of polyethylene oxide (PEO) and polyethylene glycol (PEG)
was analyzed on a semi-micro TSKgel SuperMultiporePW-M column
and on conventional-sized TSKgel G3000PWXL and TSKgel G5000PWXL
columns in series. As shown in FIGURE 21, the analysis using the
TSKgel SuperMultiporePW-M column was completed in half the time
and with higher resolution than the analysis performed using the
TSKgel G3000PWXL and TSKgel G5000PWXL columns. This is due to the
semi-micro dimensions (6.0 mm ID x 15 cm L) and the smaller particle
size (5 μm) of the TSKgel SuperMultiporePW-M column compared to
the 7.8 mm ID x 30 cm L size and 7 and 10 μm particle size of the TSKgel
G3000PWXL and TSKgel G5000PWXL columns respectively.
Columns for Specific Applications
figure 21
Comparison of analysis of a mixture of PEO and PEG
0
40
80
120
1 3 5 7 9 11
Elution time (minutes)
mV
1 (MW = 879,000)
1
4 (MW = 194)
3 (MW = 3,000)
2 (MW = 39,000)
2
3
4
Columns: A: TSKgel SuperMultiporePW-M, 6.0mm ID x 15cm
B: TSKgel G5000PWXL + G3000PWXL, each 6.0mm ID x 15cm
Mobile phase: H2 O
Flow rate: 0.6mL/min
Detection: RI
Temperature: 25°C
A
B
Column: TSKgel SuperMultiporePW-M, 6.0 mm ID x 15 cm L;
TSKgel G5000PWXL + G3000PWXL, each 6.0 mm ID x 15 cm L;
Mobile phase: H2 O; Flow rate: 0.6 mL/min; Detection: RI; Temperature: 25°C;
Injection vol.: A: 20 μL, B: 100 μL; Samples: mixture of PEO and PEG
figure 20
Analysis of polyvenylpyrrolidone
Columns: TSKgel SuperMultiporePW-M, 6 mm ID x 15 cm L x 1 (red)
TSKgel G3000PWXL & G5000PWXL, each 7.8 mm ID x 30 cm L in line (blue);
Sample: Polyvinylpyrrolidone (K-30); Mobile phase: 0.1 mol/L NaNO3 ;
Flow rate: 0.6 mL/min; Detection: RI