Ionic functional groups found on polymers repel each other and/or aggregation take place, and therefore, the apparent molecular size of the polymers seems larger than actual. When analyzing such polymers by a organic SEC column (GPC KD-806M) with DMF as the eluent, the peak may elute early and/or abnormal peak shape may be obtained. The addition of salts such as LiBr is know to be effective for preventing ionic dissociation. Although the optimal concentration of LiBr is considered to be around 10 mM, no systematic study has been performed. The following study was used to determine the optimal concentration range of LiBr in DMF for polyvinylpyrrolidone. It is confirmed that the concentration of 10 mM which has been used traditionaly is in the range of optimal concentration range. The chromatograms show the output from RI detector and "x" marks show the output from MALS (multi angle light scattering) detector. The table shows the calculation result from the data of MALS detector. The inaccurate molecular weight and larger molecular size components are mesured when the LiBr concentration is low from 0 to 0.001 mM compared with the case when the LiBr concentration is higher from 0.5 to 50 mM. From the result, we can say that apparent large molecular weight components exist because of ion repellent within the polymer, electrostatic with column packing material and aggregation of the polymers when LiBr concentration is not enough.
Please refer to the case of cellulose acetate.
Sample: 100 μL
0.01 % Polyvinylpyrrolidone
LiBr conc. | Mw (x104) | Mn (x104) | Rw (nm) | Rz(nm) |
---|---|---|---|---|
0 mM | (750) | (297) | (222) | (371) |
0.001 mM | (220) | (132) | (243) | (259) |
0.01 mM | 95.6 | 54.1 | 67.3 | 92.0 |
0.1 mM | 78.2 | 36.2 | 48.9 | 58.9 |
0.5 mM | 78.5 | 32.5 | 48.3 | 56.7 |
1 mM | 79.0 | 25.5 | 40.0 | 56.8 |
10 mM | 79.2 | 29.2 | 44.7 | 56.8 |
50 mM | 78.9 | 23.4 | 37.2 | 56.8 |
- Column
- :Shodex GPC KD-806M (8.0 mm I.D. x 300 mm)
- Eluent
- :LiBr in DMF
- Flow rate
- :1.0 mL/min
- Detector
- :RI, MALS
- Column temp.
- :40 ℃
Sample Name Index
Operation Manual / Certificate of Analysis
Operation Manuals and Certificate of Analysis / Inspection Certificate for the following products can be downloaded here.
Product Name Index
Applications
- Polystyrene Standards (9) (KD-802)
- Polystyrene Standards (21) (GF-HQ : THF, Chloroform and DMF)
- Poly(Ethylene Oxide) Standards (KD-806M + KD-802)
- Poly(Ethylene Glycol) Standards (2) (DMF Eluent) (KD-802 + KD-801)
- Phenol Resin (2) (KD-803 + KD-802)
- Phenoxy Resin (2) (KD-806M)
- Phenoxy Resin (3) (LF-604)
- Melamine Resin (KD-802)
- Melamine-Formaldehyde Resin (DMF Eluent) (KD-802)
- Polyvinylpyrrolidone (1) (DMF Eluent: KD-806M)
- Poly(vinylidene Fluoride) (KD-806M)
- Cellulose Acetate (1) (KD-806M)
- Cellulose Acetate (4) (DMF Eluent: Effects of LiBr Concentration) (KD-806M)
- Cellulose Acetate (5) (SB-806M HQ)
- Chlorinated Rubber (KD-806M)
- Styrene Allylalcohol Copolymer (1) (KD-803 + KD-802)
- Styrene Maleic Anhydride Copolymer (KD-806M)
- Styrene Acrylonitrile Copolymer (1) (KD-806M)
- N-Vinylpyrrolidone Vinyl Acetate Copolymer (KD-806M)
- Vinyl Chloride Vinyl Acetate Copolymer (1) (KD-806M)
- Vinylidene Chloride Acrylonitrile Copolymer (1) (KD-806M)
- Vinylidene Chloride Acrylonitrile Copolymer (2) (Comparison of KD-800 and SB-800 HQ)
- Poly(-N,N-Dimethylaminomethyl Styrene) (1) (DMF Eluent) (Comparison KD-800 with SB-800 HQ)
- Phenol Formaldehyde Resin (Comparison of KD-800 and SB-800 HQ)
- Ethylene Maleic Anhydride Copolymer (Comparison of KD-800 and SB-800 HQ)
- Polycarbonate Resin (2) (Comparison of SB-800 HQ and KD-800)
- Poly(4-Vinylpyridine) (LF-804)
- Poly(4-vinylpyridine) (HK-404L)
- Poly(2-Vinylpyridine-co-styrene) (LF-804)
- Poly(Vinyl Butyral) (3) (LF-604)
- Copovidone (SB-806M HQ)
Applications (Related Information)
- Calibration Curves for KD-800 Series (DMF Eluent: PEG, PEO)
- Calibration Curves for KD-800 Series (DMF Eluent: PMMA)
- Calibration Curves for HK-400 Series (DMF Eluent: PEG, PEO)
- Calibration Curve for LF-804 (DMF Eluent: PEG, PEO)
- Calibration Curves for KF-806L (Various Eluents: PS)
- Comparison of Calibration Curves for KD-800 Series and SB-800 HQ Series (DMF Eluent)
- Comparison of Calibration Curves for KD-802.5 and SB-802.5 HQ (DMF Eluent: PEG, PEO and PS)
- Calibration Curves for SB-800 HQ Series (DMF Eluent: PEG, PEO)
- Calibration Curves for SB-800 HQ Series (DMF Eluent: PMMA)
- Calibration Curves for SB-800 HQ Series (DMF Eluent: PS)
- Calibration Curves for SB-806M HQ (DMF Eluent: PEG, PEO and PS)
- Calibration Curves for LB-800 Series (DMF Eluent: PEG, PEO)
- Calibration Curves for GF-HQ Series (DMF Eluent: PS)
- Calibration Curve for GF-510 HQ + GF-310 HQ (DMF Eluent: PS)
- Calibration Curves for GF-HQ Series (DMF Eluent: PEG, PEO)
- Calibration Curves for GF-HQ Series (DMF Eluent: PMMA)