Agilent PL Rapide Organic GPC Columns Data Sheet
Contents
1. concentrations than lower polydispersity samples Overloading will not damage the column but distorted peaks and hence spurious results will be obtained 3 a Agilent Technologies Excessive injector loop volume will contribute to band broadening and reduce system performance Agilent s injection volume recommendations are shown in Table 2 When heating or cooling columns in high viscosity eluents for example TCB NMP DMF a low solvent flow rate must always be maintained Typically 0 2 mL min for 7 5 mm id and 0 4 mL min for 10 0 mm id should be used prior to raising the tem Table 2 Injection Volume Recommendations perature A useful stepwise guide is provided in Figure 3 Recommended Table 3 Flow Rate Conversions Recommended injection Column type concentration pL per column PL Rapide 7 5 mm id PL Rapide 10 0 mm id PL Rapide 7 5 mm id 0 05 0 50 20 0 2 mL min 0 35 mL min PL Rapide 10 0 mmid 0 05 0 50 20 0 5 mL min 0 88 mL min 1 0 mL min 1 77 mL min Eluents PL Rapide gel is compatible with an extensive range of organic solvents having solubility parameters in the range 7 14 Mixed organic solvent systems can also be used but water should not be used except at concentrations less than 10 by volume in a misci ble organic eluent All eluents should be of high purity and should be filtered and degassed prior to use PL Rapide columns are nor mally supplied in ethylbenzene unless otherwise stated and can be flushed2. Installation Tubing and connectors Stainless steel tubing of 1 16 in od and 0 010 in id or 0 007 in id is recommended for column connections Connecting tubing lengths between columns detectors and injection volumes should be minimized to avoid excessive dead volume which will diminish system performance Column connections should be made using Parker compatible 1 16 in nuts and ferrules The compatibility of column connectors is illustrated in Figure 1 0 090 0 210 p E Figure 1 Compatible connectors The distance x for the standard column end fitting is 0 090 in and a minimum male nut length of 0 210 in is required Some fit tings from other manufacturers may not be compatible for exam ple Waters and Rheodyne If unsure please contact your local Agilent office Column connection Connect the GPC column in the eluent flow direction indicated and tighten the 1 16 in nut and ferrule using wrenches on the 1 16 in nut and the actual end fitting It is recommended that several drops of eluent have been pumped before the column outlet is connected to another column or detector to clean out the end fitting of any particulate matter which may be present To avoid loosening the end fittings and causing leaks wrenches must be used on the end fitting adjacent to the connecting nut and NOT on the column barrel or the opposite end fitting as illustrated in Figure 2 Agilent PL Rapide Rapid Organic GPC Columns Data Shee
3. Rapide PL Rapide Specifications F L M H Typical operating pressure psi bar 350 25 225 15 75 5 75 5 Maximum operating pressure psi bar 1500 90 1100 75 1100 75 1100 75 Maximum operating temperature C2 150 150 220 220 Efficiency ppm gt 40 000 gt 80 000 gt 60 000 gt 35 000 1 Based on THF at 20 C PL Rapide 150 x 7 5 mm at 1 0 mL min and for PL Rapide 100 x 10 0 mm at 1 8 mL min using butylated hydroxy toluene BHT as a test probe 2 At very high temperatures column lifetimes are likely to be reduced Storage On removing the column from the system the end plugs must be replaced to prevent the column from drying out by evaporation since subsequent shrinkage of the gel and disruption of the pack ing will occur The end plugs need only be applied finger tight All eluents mentioned previously are suitable for storage but unstabilized THF should not be used Warranty The columns are covered by warranty for 90 days following deliv ery For columns used at or above 170 C the warranty period is reduced to 30 days Agilent cannot accept liability from improper handling or use For a full warranty statement please request Agilent s General Conditions of Sale Maintenance Deterioration in column performance may occur as a result of damage to the packed bed or as a result of blockage in the column frits In the case of frit blockage the column can be reverse flushed at 1 0 mL min for 1 minu
4. ate column in new eluent at required flow rate 4 Operate column in new eluent at 60 C 4 Operate column in 4 Operate column at new eluent at 70 C required flow rate using required flow rate maximum using required flow rate Figure 3 Eluent transfer guide for PL Rapide 7 5 mm id columns Column Testing and Specifications Every PL Rapide column is supplied with a test certificate indicat ing the test conditions and the column performance Measurements of column performance are described below 7 Efficiency 1 2 ht Plates m N 5 54 t 2 L W2 7 i t Efficiency 5c Plates m N 25 W5o 2 L rs Symmetry a b where t is the peak elution time W is the peak width at half peak height W5o is the peak width at 4 4 of peak height L is the column length in meters and a and b are the peak widths either side of the perpendicular measured at 10 of peak height Column efficiency is dependent on many experimental factors system dead volume eluent flow rate test probe temperature etc and test results may differ slightly from those quoted on the column certificate due to variability in these parameters Band broadening effects are more severe when using high efficiency columns It is vital to ensure that the system dispersion is mini mized in order to obtain the full potential of PL Rapide columns Column specifications are listed in Table 4 Table 4 Column Specifications PL Rapide PL Rapide PL
5. directly from ethylbenzene to THF at 0 5 mL min Unstabilized THF for example HPLC grade is not recommended as an eluent due to the attack of peroxide on the gels PL Rapide columns can be transferred to other eluents with no deterioration in performance When transferring to another eluent miscibility and viscosity of the new eluent are of primary consideration See Figure 3 for 7 5 mm id columns For other id columns apply the flow rate conversion shown in Table 3 Column supplied in ethylbenzene Transfer to o DCB TCB Transfer to Transfer to Transfer to Hexane Dichloromethane DMAC Perfluoroalkanes Cyclohexane Pyridine Dichloromethane DMF DMSO NMP o CP m Cresol MEK Ethyl acetate Chloroform 1 Flush column with acetone at 0 5 mL min 1 Increase column for 2 column volumes 1 Flush column with temperature to 50 C acetone at 0 5 mL min for 2 column volumes 2 Flush with new eluent at 0 1 mL min for 2 column volumes 1 Flush column with acetone at 0 5 mL min for 2 column volumes 2 Flush with new eluent at 0 2 mL min 2 Flush with new for 2 column volumes eluent at 0 2 mL min for 2 column volumes 2 Flush with new eluent at 0 5 mL min for 2 column volumes 3 Increase column temperature to 60 C f 3 Increase column at 1 C min Increase column temperature to 110 C 150 C as required temperature to 70 C for analysis at at 1 C min 1 C min 3 Oper
6. t Flats a ee ee ris ee Figure 2 Don t use wrenches on the flats Eluent Flow Rate For conventional GPC columns using 7 5 mm id columns 1 0 mL min is an optimum flow rate for most separations With 10 0 mm id columns a flow rate of 1 8 mL min is the optimum flow rate When column id is increased or decreased the volu metric flow rate should be adjusted accordingly in order to give an equivalent linear velocity through the column The recommended flow rates are given in Table 1 however higher viscosity eluents should be used at reduced flow rates or elevated temperature Flow rates should be changed progressively and pressure pulses limited At no time should the maximum operating pressure of the column be exceeded see Table 4 Table 1 Recommended Flow Rate Typical flow rates Recommended flow rate Column type mL min mL min PL Rapide 7 5 mmid 0 5 1 5 1 0 PL Rapide 10 0 mmid 2 0 5 0 2 0 Sample Preparation and Injection If maximum resolution and expected column lifetime are to be achieved care must be taken in sample preparation To avoid blockage of the column frits sample filtration is recom mended 0 5 2 0 um depending on MW An in line filter will further protect the columns with little detrimental effect on performance Optimum sample volumes and concentrations are best deter mined for each type of analysis and are dependent on sample MW Broad distribution polymers can generally be injected at higher
7. te to remove loosely retained material For further technical assistance or to use the Column Repair Service please contact your local Agilent Technologies office Agilent Ordering Information For more information on our products visit our web site at www agilent com chem gpcsec www agilent com chem Agilent shall not be liable for errors contained herein or for incidental or consequential damages in connection with the furnishing performance or use of this material Information descriptions and specifications in this publication are subject to change without notice Agilent Technologies Inc 2011 Printed in the USA February 2011 PK011 z Agilent Technologies
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Agilent PL Rapide Organic GPC Columns Data Sheet