Hydrophobic Polymers: HFIP Eluent
Calibration curves for GPC HFIP-800 series are shown.
Sample :
PMMA, Poly(methyl methacrylate)
Ethyl methacrylate
Columns : Shodex GPC HFIP-800 series (8.0mmID*300mm each) Eluent : HFIP Flow rate : 1.0mL/min Detector : Shodex RI Column temp. : Room temp.
Calibration curves for HFIP-600 series are shown.
Sample : PMMA, Poly(methyl methacrylate)
Columns : Shodex GPC HFIP-600 series (6.0mmID*150mm) Eluent : 5mM CF3COONa in HFIP Detctor : Shodex RI(small cell volume) Column temp. : 40deg-C
Refractory polymers are usually analyzed using a high-temperature SEC system. However, the high-temperature SEC system is rather expensive and not so easy to use. Since HFIP (hexafluoroisopropanol) dissolves refractory polymers at ordinary temperature, such polymers are preferably analyzed with HFIP eluent without using high-temperature SEC systems. SEC is a method using the principle that larger molecular size (three dimensional volume) of the sample elutes faster. In fact, the actual molecular size of the sample is different according to the solvent in which the sample is dissolved. In case of polymers with ionic functional groups, these groups are repelling each other and the apparent molecular size of the polymers becomes larger. For preventing such ionic interaction, the addition of CF3COONa (sodium trifluoroacetate) to HFIP is recommended.
For the analysis of polyamides or poly(ethylene terephthalate) (PET), the use of HFIP eluent containing CF3COONa is also recommended.
(Refer to Polyamide (1) Nylon6 (HFIP-806M))
(Preparation of the eluent)
Since CF3COONa is not easily dissolved in HFIP, care should be taken to confirm that it has been thoroughly dissolved, otherwise it may damage the columns.
Method for preparing the eluent is as follows:
1) Weigh necessary amount of CF3COONa and dissolve it in HFIP applying ultrasonic vibration. The bottle should be shaken often to ensure thorough ultrasonic vibration.
2) Ultrasonic vibration should be applied for the following time: 10mM CF3COONa in HFIP: 60 min. or more, 5mM CF3COONa in HFIP: 40 min. or more
Polyamide was analyzed using GPC HFIP-806M (a column for organic SEC (GPC)). For preventing ionic interaction, the addition of CF3COONa (sodium trifluoroacetate) to HFIP is recommended.
(Please refer to SEC Analysis with HFIP Eluent)
Sample : Polyamide,Polycaprolactam, Nylon6
Columns : Shodex GPC HFIP-806M (8.0mmID*300mm) x 2 Eluent : HFIP(solid line), 5mM CF3COONa in HFIP(broken line) Flow rate : 1.0mL/min Detector : Shodex RI Column temp. : 40deg-C
Polyamide was analyzed using GPC HFIP-805 + HFIP-803 (columns for organic SEC (GPC)).
Sample : Polyamide,Polyhexamethylene adipamide, Nylon6/6
Columns : Shodex GPC HFIP-805 + HFIP-803 (8.0mmID*300mm each) Eluent : 5mM CF3COONa in HFIP Flow rate : 1.0mL/min Detector : Shodex RI Column temp. : 40deg-C
By using downsized organic SEC (GPC) columns, GPC HFIP-606M (6.0mmID*150mm), the consumption of HFIP solvent will be one third of that of standard type column (8.0mmID*300mmL).
Sample : Polyamide
(left): 0.2% Polyhexamethylene sebacamide, Nylon6/10 (right): 0.2% Polycaprolactam, Nylon6 20micro-L
Columns : Shodex GPC HFIP-606M (6.0mmID*150mm) x 2 Eluent : 5mM CF3COONa in HFIP Flow rate : 0.6mL/min Detector : Shodex RI(small cell volume) Column temp. : 40deg-C
Nylon6/6 was analyzed using GPC LF-604 (a column for organic SEC (GPC)). Please refer to OUTLINE of LF-804.
Sample: 20micro-L
0.2% Polyamide, Polyhexamethylene adipamide, Nylon6/6
Columns : Shodex GPC LF-604 (6.0mmID*150mm) x 2 Eluent : 5mM CF3COONa in HFIP Flow rate : 0.3mL/min Detector : Shodex RI(small cell volume) Column temp. : 40deg-C
Nylon6 was analyzed using GPC LF-604 (a column for organic SEC (GPC)). Please refer to OUTLINE of LF-804.
Sample : 0.2% Polyamide, Polycaprolactam, Nylon6, 20micro-L
Columns : Shodex GPC LF-604 (6.0mmID*150mm) x 2 Eluent : 5mM CF3COONa in HFIP Flow rate : 0.3mL/min Detector : Shodex RI(small cell volume) Column temp. : 40deg-C
By using downsized organic SEC (GPC) columns, GPC HFIP-606M (6.0mmI.D. x 150mm), the consumption of HFIP solvent will be one third of that of standard type column (8.0mmI.D. x 300mmL).
Sample : 0.2% Polyamide, Polytirmethyl hexamethylene terephthalamide, Nylon6/T, 20micro-L
Columns : Shodex GPC HFIP-G (4.6mmID*10mm) + HFIP-606M (6.0mmID*150mm) x 2 Eluent : 5mM CF3COONa in HFIP Flow rate : 0.6mL/min Detector : Shodex RI(small cell volume) Column temp. : 40deg-C
By using downsized organic SEC (GPC) columns, GPC HFIP-606M (6.0mmI.D. x 150mm), the consumption of HFIP solvent will be one third of that of standard type column (8.0mmI.D. x 300mmL).
Sample : 0.2% Polyamide, Polyundecanoamide, Nylon11, 20micro-L
Columns : Shodex GPC HFIP-G (4.6mmID*10mm) + HFIP-606M (6.0mmID*150mm) x 2 Eluent : 5mM CF3COONa in HFIP Flow rate : 0.6mL/min Detector : Shodex RI(small cell volume) Column temp. : 40deg-C
By using downsized organic SEC (GPC) columns, GPC HFIP-606M (6.0mmI.D. x 150mm), the consumption of HFIP solvent will be one third of that of standard type column (8.0mmI.D. x 300mmL).
Sample : 0.2% Polyamide, Polyhexamethylene dodecanediamide, Nylon6/12, 20micro-L
Columns : Shodex GPC HFIP-G (4.6mmID*10mm) + HFIP-606M (6.0mmID*150mm) x 2 Eluent : 5mM CF3COONa in HFIP Flow rate : 0.6mL/min Detector : Shodex RI(small cell volume) Column temp. : 40deg-C
By using downsized organic SEC (GPC) columns, GPC HFIP-606M (6.0mmI.D. x 150mm), the consumption of HFIP solvent will be one third of that of standard type column (8.0mmI.D. x 300mmL).
Sample : 0.2% Polyamide, Polyhexamethylene nonanediamide, Nylon6/9, 20micro-L
Columns : Shodex GPC HFIP-G (4.6mmID*10mm) + HFIP-606M (6.0mmID*150mm) x 2 Eluent : 5mM CF3COONa in HFIP Flow rate : 0.6mL/min Detector : Shodex RI(small cell volume) Column temp. : 40deg-C
By using downsized organic SEC (GPC) columns, GPC HFIP-606M (6.0mmI.D. x 150mm), the consumption of HFIP solvent will be one third of that of standard type column (8.0mmI.D. x 300mmL).
Sample : 0.2% Polyamide, Polylaurylactam Nylon12, 20micro-L
Columns : Shodex GPC HFIP-G (4.6mmID*10mm) + HFIP-606M (6.0mmID*150mm) x 2 Eluent : 5mM CF3COONa in HFIP Flow rate : 0.6mL/min Detector : Shodex RI(small cell volume) Column temp. : 40deg-C
Poly(ethylene terephthalate) was analyzed using GPC HFIP-806M (a column for organic SEC (GPC)). PET resin is commonly used as a raw material for beverage bottles. PET usually contains small amounts of oligomers as impurities. For the analysis of PET, CF3COONa should be added to HFIP eluent.
Sample : PET, Poly(ethylene terephthalate)
Column : Shodex GPC HFIP-806M (8.0mmID*300mm) Eluent : 5mM CF3COONa in HFIP Flow rate : 0.5mL/min Detector : Shodex RI Column temp. : 40deg-C
By using downsized organic SEC (GPC) columns, GPC HFIP-606M (6.0mmID*150mm), the consumption of HFIP solvent will be one third of that of standard type column (8mmID* 300mm).
Sample : PET, Poly(ethylene terephthalate)
Columns : Shodex GPC HFIP-606M (6.0mmID*150mm) x 2 Eluent : 5mM CF3COONa in HFIP Flow rate : 0.6mL/min Detector : Shodex RI(small cell volume) Column temp. : 40deg-C
Poly(butylene terephthalate) was analyzed using GPC HFIP-805 + HFIP-803 (columns for organic SEC (GPC)). PBT is a polyester resin used in a wide variety of fields. This chromatogram shows that small amounts of oligomers may affect the characteristics of PBT resin.
Sample : PBT, Poly(butylene terephthalate)
Columns : Shodex GPC HFIP-805 + HFIP-803 (8.0mmID*300mm each) Eluent : 5mM CF3COONa in HFIP Flow rate : 1.0mL/min Detector : Shodex RI Column temp. : 40deg-C
Polyacetal was analyzed using GPC HFIP-806M (a column for organic SEC (GPC)).
Sample : Poly(oxymethylene)
Column : Shodex GPC HFIP-806M (8.0mmID*300mm) Eluent : 5mM CF3COONa in HFIP Flow rate : 0.5mL/min Detector : Shodex RI Column temp. : 40deg-C
Polyacetal was analyzed using GPC HFIP-806M (a column for organic SEC (GPC)).
Sample : Delrin, Poly(oxymethylene)
Column : Shodex GPC HFIP-806M (8.0mmID*300mm) Eluent : 50mM CF3COONa in HFIP Flow rate : 0.5mL/min Detector : Shodex RI Column temp. : 40deg-C
By using downsized organic SEC (GPC) columns, GPC HFIP-606M (6.0mmID*150mm), the consumption of HFIP solvent will be one third of that of conventional column (8.0mmID*300mm).
Sample : PMMA, Poly(methyl methacrylate) 0.02% each, 20micro-L
Columns : Shodex GPC HFIP-606M (6.0mmID*150mm) x 2 Eluent : 5mM CF3COONa in HFIP Flow rate : 0.6mL/min Detector : Shodex RI(small cell volume) Column temp. : 40deg-C
By using downsized organic SEC (GPC) columns, GPC HFIP-606M (6.0mmID*150mm), the consumption of HFIP solvent will be one third of that of conventional column (8.0mmID*300mm).
Sample : 0.2% Polyacetal, poly(oxymethylene), 20micro-L
Columns : Shodex GPC HFIP-606M (6.0mmID*150mm) x 2 Eluent : 5mM CF3COONa in HFIP Flow rate : 0.6mL/min Detector : Shodex RI(small cell volume) Column temp. : 40deg-C
Poly(vinyl alcohol) was analyzed using GPC HFIP-805 + HFIP-803 (columns for organic SEC (GPC)).
Sample : Poly(vinyl alcohol)
Columns : Shodex GPC HFIP-805 + HFIP-803 (8.0mmID*300mm each) Eluent : HFIP Flow rate : 1.0mL/min Detector : Shodex RI Column temp. : 40deg-C
Ethylene vinyl acetate copolymer was analyzed using GPC HFIP-806M (a column for organic SEC (GPC)).
Sample : Ethylene vinyl acetate copolymer
Columns : Shodex GPC HFIP-806M (8.0mmID*300mm) x 2 Eluent : HFIP Flow rate : 0.5mL/min Detector : Shodex RI Column temp. : 40deg-C
The calibration curves for downsized organic SEC (GPC) columns using PMMA are shown. In the case of the analysis for polymer whose MW is 1,000,000 or less, GPC LF-604 or LF-404 is suitable. When it is needed to separate low MW polymer and high MW polymer and low MW polymer is the purpose for the analysis, GPC HFIP-603 is suitable.
Please refer to Comparison of Analysis of PMMA with Down-sized SEC Columns
Sample : PMMA, Poly(methyl methacrylate) standards, 50micro-L
Columns : Shodex GPC LF-604 (6.0mmID*150mm) x 2
Shodex GPC LF-404 (4.6mmID*250mm) x 2
Shodex GPC KF-405LHQ (4.6mmID*250mm) x 2
Shodex GPC KF-406LHQ (4.6mmID*250mm) x 2
Shodex GPC HFIP-603 (6.0mmID*150mm) x 2
Shodex GPC HFIP-606M (6.0mmID*150mm) x 2
Eluent : 5mM CF3COONa in HFIP
Flow rate : 0.3mL/min
Detector : Shodex RI(small cell volume)
Column temp. : 40deg-C
The calibration curves for downsized organic SEC (GPC) columns using PMMA are shown. In the case of the analysis for polymer whose MW is 1,000,000 or less, GPC LF-604 or LF-404 is suitable. When it is needed to separate low MW polymer and high MW polymer and low MW polymer is the purpose for the analysis, GPC HFIP-603 is suitable.
Please refer to Comparison of Calibration Curves for Down-sized SEC Columns (HFIP Eluent: PMMA)
Sample : 50micro-L
1. PMMA, Poly(methyl methacrylate) (MW: 1,944,000)
2. PMMA, Poly(methyl methacrylate) (MW: 281,700)
3. PMMA, Poly(methyl methacrylate) (MW: 79,250)
4. PMMA, Poly(methyl methacrylate) (MW: 13,300)
5. PMMA, Poly(methyl methacrylate) (MW: 1,960)
Columns : Shodex GPC LF-604 (6.0mmID*150mm) x 2
Shodex GPC LF-404 (4.6mmID*250mm) x 2
Shodex GPC KF-405LHQ (4.6mmID*250mm) x 2
Shodex GPC KF-406LHQ (4.6mmID*250mm) x 2
Shodex GPC HFIP-603 (6.0mmID*150mm) x 2
Shodex GPC HFIP-606M (6.0mmID*150mm) x 2
Eluent : 5mM CF3COONa in HFIP
Flow rate : 0.3mL/min
Detector : Shodex RI(small cell volume)
Column temp. : 40deg-C
Polyacetal was analyzed using GPC LF-404 (a column for organic SEC (GPC)).
Sample : Polyacetal, 20micro-L
Column : Shodex GPC LF-404 (4.6mmID*250mm) Eluent : 5mM CF3COONa in HFIP Flow rate : 0.15mL/min Detector : Shodex RI(small cell volume) Column temp. : 40deg-C
Poly(ethylene terephthalate) was analyzed using GPC LF-404 (a column for organic SEC (GPC)).
Sample : PET, Poly(ethylene terephthalate), 20micro-L
Column : Shodex GPC LF-404 (4.6mmID*250mm) Eluent : 5mM CF3COONa in HFIP Flow rate : 0.15mL/min Detector : Shodex RI(small cell volume) Column temp. : 40deg-C