Chinese Journal of Chromatography ›› 2024, Vol. 42 ›› Issue (8): 812-818.DOI: 10.3724/SP.J.1123.2023.12005
• Teaching Research • Previous Articles
QIAO Congde*(), YANG Wenke, LI Zhongwei, LIU Qinze, YAO Jinshui
Received:
2023-12-08
Online:
2024-08-08
Published:
2024-08-01
CLC Number:
QIAO Congde, YANG Wenke, LI Zhongwei, LIU Qinze, YAO Jinshui. Experimental teaching reform of polymer molar mass determination using gel permeation chromatography coupled with light scattering[J]. Chinese Journal of Chromatography, 2024, 42(8): 812-818.
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URL: https://www.chrom-china.com/EN/10.3724/SP.J.1123.2023.12005
Fig. 1 (a) Chromatograms of polystyrene sample, and (b) Zimm plot for one data slice from the LS peak LS: light scatting detection; dRI: refractive index detection. Conditions: solvent, 0.05 mol/L LiBr in DMF; flow rate, 1.0 mL/min; column temperature, 60 ℃. Results: slice index, 354; model, Zimm; fit degree, 1; abscissa position, 11.725 min; mass concentration, 0.1565 mg/mL; molar mass, (4.691±0.007)×105 g/mol; radius of gyration, (22.5 ± 0.2) nm; dn/dc, 0.159 mL/g; R2= 0.9957.
Fig. 2 Curves of (a) molar mass versus elution time and (b) radius of gyration versus elution time for polystyrene sample Conditions: solvent, 0.05 mol/L LiBr in DMF; flow rate, 1.0 mL/min; column temperature, 60 ℃.
Molecular structural parameter | Content | Result | Uncertainty |
---|---|---|---|
Molar mass moments/(g/mol) | Mn | 1.686×105 | 0.2% |
Mp | 3.045×105 | 0.1% | |
Mw | 2.959×105 | 0.1% | |
Mz | 4.381×105 | 0.3% | |
Polydispersity | Mw/Mn | 1.755 | 0.2% |
Mz/Mn | 2.599 | 0.4% | |
Radius of gyration/nm | Rgn | 13.7 | 4% |
Rgw | 17.9 | 2% | |
Rgz | 22.2 | 1% |
Table 1 GPC-LS test items and results of polystyrene sample
Molecular structural parameter | Content | Result | Uncertainty |
---|---|---|---|
Molar mass moments/(g/mol) | Mn | 1.686×105 | 0.2% |
Mp | 3.045×105 | 0.1% | |
Mw | 2.959×105 | 0.1% | |
Mz | 4.381×105 | 0.3% | |
Polydispersity | Mw/Mn | 1.755 | 0.2% |
Mz/Mn | 2.599 | 0.4% | |
Radius of gyration/nm | Rgn | 13.7 | 4% |
Rgw | 17.9 | 2% | |
Rgz | 22.2 | 1% |
Fig. 3 (a) Chromatograms and (b) differential weight fraction curves of two polyacrylonitrile (PAN) samples Conditions: solvent, 0.05 mol/L LiBr in DMF; flow rate, 1.0 mL/min; column temperature, 60 ℃.
Fig. 4 Chromatograms of polyethylene glycol with different molar masses Conditions: solvent, 0.1 mol/L NaNO3 and 0.2 g/L NaN3 in water; flow rate, 0.5 mL/min; column temperature, 35 ℃.
Label Mw/(g/mol) | Determined Mw/(g/mol) | Uncertainty |
---|---|---|
1000 | 1260 | 13% |
2000 | 2210 | 12% |
4000 | 4450 | 12% |
6000 | 7760 | 9% |
10000 | 8130 | 10% |
20000 | 17430 | 6% |
Table 2 Determination results of polyethylene glycol with different molar masses
Label Mw/(g/mol) | Determined Mw/(g/mol) | Uncertainty |
---|---|---|
1000 | 1260 | 13% |
2000 | 2210 | 12% |
4000 | 4450 | 12% |
6000 | 7760 | 9% |
10000 | 8130 | 10% |
20000 | 17430 | 6% |
Fig. 5 Scaling relationship between radius of gyration and molar masses for different polymer samples PMMA: polymethyl methacrylate; poly(β-CD): poly(β-cyclodextrin). Conditions: solvent, 0.05 mol/L LiBr in DMF; flow rate, 1.0 mL/min; column temperature, 60 ℃.
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