Organic SEC (GPC) Columns (General Analysis) : DMF Features KD-800 • Standard organic solvent SEC (GPC) column • Supports a wide range of applications from low to high molecular weight compounds • Corresponds to USP L21 Standard columns KD-800 series : Shipping solvent Dimethylformamide (DMF) Product Code Plate Number (TP/column) Product Name Particle Size (μm) Pore Size (Å) Column Size (mm) I.D. x Length F6028210 GPC KD-801 ≥ 17,000 6 50 8.0 × 300 F6028220 GPC KD-802 ≥ 17,000 6 150 8.0 × 300 F6028225 GPC KD-802.5 ≥ 17,000 6 300 8.0 × 300 F6028230 GPC KD-803 ≥ 17,000 6 500 8.0 × 300 F6028240 GPC KD-804 ≥ 17,000 7 1,500 8.0 × 300 F6028250 GPC KD-805 ≥ 11,000 10 5,000 8.0 × 300 F6028260 GPC KD-806 ≥ 11,000 10 10,000 8.0 × 300 F6028290 GPC KD-806M ≥ 13,000 10 10,000 8.0 × 300 F6028270 GPC KD-807 ≥ 6,000 18 20,000 8.0 × 300 F6700411 GPC KD-G 4A (GPC KD-G) (guard column) 8 − 4.6 × 10 Base Material : Styrene divinylbenzene copolymer * The columns with ‘L’ or ‘M’ at the end of column names are mixed-gel column capable of analyzing samples over a wide range of molecular weight distribution. * See page 62 for applicability of SEC (GPC) columns to solvent replacement. Target molecular weight range and Exclusion limit With *PEG/PEO (eluent : DMF) Product Name Target Molecular Weight Range Exclusion Limit Product Name Target Molecular Weight Range Exclusion Limit KD-801 100 − 1,500 2,500 KD-805 30,000 − **(4,000,000) **(4,000,000) KD-802 200 − 4,000 7,000 KD-806 30,000 − **(40,000,000) **(40,000,000) KD-802.5 400 − 10,000 20,000 KD-806M KD-803 1,000 − 50,000 70,000 KD-807 KD-804 4,000 − 200,000 200,000 1,000 − **(40,000,000) 50,000 − **(200,000,000) * Please use the above table as a rough indication for the column selection. **(40,000,000) **(200,000,000) *PEG : polyethylene glycol *PEO : polyethylene oxide **( ) Estimated value Solvent-peak Separation Columns for Organic SEC (GPC) Features KF-800D K-800D • Use this column in combination with a linear column • By shifting the elution of monomers, polymer additives, and the solvent-peak in low molecular region, it reduces interferences in the calculation of the molecular weight distribution of polymers and oligomers Solvent-peak separation columns 50 Product Code Product Name Column Combination Particle Size (μm) Column Size (mm) I.D. x Length Shipping Solvent F6709350 GPC KF-800D KF-805L, 806L, 806M, 807L 10 8.0 × 100 THF F6709450 GPC K-800D K-805L, 806L, 806M, 807L 10 8.0 × 100 Chloroform Base Material : Styrene divinylbenzene copolymer Melamine formaldehyde resin Sample : Polyvinylpyrrolidone 0.2% each (A) K-30 400μL (B) K-60 500μL (C) K-90 500μL 107 Sample : 30μL Melamine-formaldehyde resin 1% (A) 05 04 KD KD M 06 -8 -8 03 KD (B) 02 02 .5 01 -8 -8 KD -8 KD 103 7 -8 -8 104 - 80 KD KD 105 KD 06 -8 KD 106 Molecular weight (PEG/PEO) Polyvinylpyrrolidones (C) 102 5 6 7 8 9 10 11 12 13 10 Elution volume (mL) Column : Eluent : Flow rate : Detector : Column temp. : 0 Shodex GPC KD-800 series DMF 1.0mL/min RI 40˚C 10 Column : Eluent : Flow rate : Detector : Column temp. : 20 Shodex GPC KD-806M x 2 10mM LiBr in DMF 1.0mL/min RI 50˚C 20 Column : Eluent : Flow rate : Detector : Column temp. : Celluloses 25 min Shodex GPC KD-802 x 2 10mM LiBr in DMF 1.0mL/min RI 50˚C Phenoxy resin Sample : 250μL Phenoxy resin 0.2% Cellulose is known to be difficult to dissolve. A cellulose solution is prepared by repeating solvent replacement. It is reported that it requires a long time to dissolve (1 to 60 days), depending on the solvent type, crystallinity and molecular weight. 106 105 104 103 6 7 8 9 10 15 11 20 25 min Elution volume (mL) Shodex GPC KD-806M 1% LiCl in *DMI 0.5mL/min RI, MALS (Multi angle light scattering) 60˚C Data provided by Dr. Masahiko Yanagisawa, Isogai group, Graduate School of Agricultural and Life Sciences, The University of Tokyo * DMI 1,3-dimethyl-2-imidazolidinone Potato starch Column : Eluent : Flow rate : Detector : Column temp. : Sample : 100μL Potato starch in DMSO 0.1% * solved at 80°C Sample : Poly(vinyl chloride) DOP (Dioctyl phthalate) 06 Column : Shodex GPC KD-806M Eluent : 10mM LiBr in DMSO/DMF=75/25 Flow rate : 1.0mL/min Detector : RI Column temp. : 50˚C 0 5 D 103 5 6 7 8 9 10 11 12 13 14 15 Elution volume (mL) KF-806L + KF-800D 15 min 00 10 -8 104 102 5 KF L+ 6L 15 min -8 10 80 5 105 KF 0 106 KF KF-806L 0 Shodex GPC KD-806M x 2 10mM LiBr in DMF 1.0mL/min RI 50˚C Effects of solvent-peak separation column Molecular weight (Polystyrene) Column : Eluent : Flow rate : Detector : Column temp. : Solvent-peak Separation Columns for Organic SEC (GPC) Sample : 100μL Cellulose ca. 0.05% each 107 Molecular mass 15 30 min Organic SEC (GPC) Columns (General Analysis) : DMF Calibration curves for KD-800 series using PEG/PEO 10 min Column : Shodex GPC KF-806L Shodex GPC KF-806L + KF-800D Eluent : THF Flow rate : 1.0mL/min Detector : RI 51 Organic SEC (GPC) Columns : Linear Calibration Type Features LF • Employs a special packing material with a wide pore size distribution (multi pore type) • Highly linear calibration curve without inflection points • Molecular weight distribution can be determined with high precision • Enables analysis over a broad range of molecular weights • Column for rapid analysis (LF-604) and column for high performance analysis (LF-404) enabling reduction in solvent use are also available • Corresponds to USP L21 Standard columns Product Code Product Name Plate Number (TP/column) Particle Size (μm) Pore Size (Å) Column Size (mm) I.D. x Length F6021041 GPC LF-804 ≥ 17,000 6 3,000 8.0 × 300 F6709621 GPC LF-G (guard column) 6 − 4.6 × 10 Base Material : Styrene divinylbenzene copolymer Shipping Solvent : Tetrahydrofuran (THF) * See page 62 for applicability of SEC (GPC) columns to solvent replacement. Rapid analysis downsized column Use of the LF-604 with semi-micro type devices is recommended. Product Name Plate Number (TP/column) Particle Size (μm) Pore Size (Å) Column Size (mm) I.D. x Length F6021042 GPC LF-604 ≥ 9,000 6 3,000 6.0 × 150 F6709621 GPC LF-G (guard column) 6 − 4.6 × 10 Product Code Base Material : Styrene divinylbenzene copolymer Shipping Solvent : Tetrahydrofuran (THF) * See page 62 for applicability of SEC (GPC) columns to solvent replacement. High performance semi-micro column Use of the LF-404 with semi-micro type devices is recommended. Product Name Plate Number (TP/column) Particle Size (μm) Pore Size (Å) Column Size (mm) I.D. x Length F6021043 GPC LF-404 ≥ 14,000 6 3,000 4.6 × 250 F6709621 GPC LF-G (guard column) 6 − 4.6 × 10 Product Code * See page 62 for applicability of SEC (GPC) columns to solvent replacement. Base Material : Styrene divinylbenzene copolymer Shipping Solvent : Tetrahydrofuran (THF) Target molecular weight range and Exclusion limit With Polystyrene (eluent : THF) Product Name Target Molecular Weight Range Exclusion Limit LF-804 300 − 2,000,000 2,000,000 LF-604 300 − 2,000,000 2,000,000 LF-404 300 − 2,000,000 2,000,000 * Please use the above table as a rough indication for the column selection. Schematic diagram of linear calibration type packing Connecting linear calibration type columns (LF series) The linear calibration type column covers a broad range of molecular weights with only one kind of packing (column). Connecting mixed-gel columns (KF-804L, etc.) 56 Connecting different grades columns (KF-804 + KF-803 + KF-802, etc.) 107 106 106 105 104 -40 4 102 103 102 5 6 7 8 9 10 11 12 1.0 13 1.5 2.0 Elution volume (mL) Column : Eluent : Flow rate : Detector : Column temp. : 2.5 3.0 0 3.5 Shodex GPC LF-804 THF 1.0mL/min RI 40˚C Column Eluent Flow rate : Shodex GPC LF-604, LF-404 : THF : 0.5mL/min (LF-604) 0.3mL/min (LF-404) Detector : RI (small cell volume) Column temp. : 40˚C Sample : Xylan 0.1%, 100μL 10 15 10 Column : Eluent : Flow rate : Detector : Column temp. : Polyamide (Nylon6/6) 5 5 15 20 min Elution volume (mL) Xylan 0 4 103 105 LF 104 Sample : Polyurethane 0.1%, 20μL -60 Molecular weight (Polystyrene) 107 Polyurethane LF Molecular weight (Polystyrene) Calibration curves for LF-604 and LF-404 using polystyrene 20 Shodex GPC LF-404 x 2 THF 0.3mL/min RI (small cell volume) 40˚C Polymethyl methacrylate Sample : NylonTM 6/6 0.1%, 20μL 0 25 min Column Eluent : Shodex GPC LF-804 : 20mM H3PO4 + 20mM LiBr in (DMSO/DMF=80/20) Flow rate : 0.6mL/min Detector : RI Column temp. : 50˚C 5 10 Column : Eluent : Flow rate : Detector : Column temp. : Organic SEC (GPC) Columns : Linear Calibration Type Calibration curve for LF-804 using polystyrene 15 20 Sample : 100μL Polymethyl methacrylate 25 min 0 5 10 Column : Eluent : Flow rate : Detector : Column temp. : Shodex GPC LF-404 5mM CF3COONa in HFIP 0.15mL/min RI (small cell volume) 40˚C 15 20 25 30 min Shodex GPC LF-804 x 2 Methyl ethyl ketone 1.0mL/min RI 40˚C Comparison of polystyrenes separation with different numbers of LF-404 Polyamic acid 4 Sample : Poly(pyromellitic dianhydride-co-4,4'-oxydianiline), 100μL 5 3 Sample : 10μL 1. Polystyrene (Mw : 1,030,000) 2. Polystyrene (Mw : 152,000) 3. Polystyrene (Mw : 66,000) 4. Polystyrene (Mw : 22,000) 5. Polystyrene (Mw : 5,050) 6. Polystyrene (Mw : 580) 7. Ethylbenzene 6 7 2 1 LF-404 x 1 Column : Shodex GPC LF-404 x n Eluent : THF Flow rate : 0.3mL/min Detector : RI (small cell volume) Column temp. : 40˚C 4 5 3 7 6 2 1 LF-404 x 2 0 5 10 15 20 25 30 35 40 45 min 4 3 Column : Eluent : Flow rate : Detector : Column temp. : Shodex GPC LF-804 x 2 30mM LiBr + 30mM H3PO4 in NMP 0.7mL/min RI 50˚C 6 1 LF-404 x 3 0 7 5 2 5 10 15 20 25 30 min 57
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