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Summary of Contents for Agilent Technologies G3180B
- Page 1 Agilent G3180B Two-Way Splitter Kit With Makeup Gas Installation and Operation Guide Agilent Technologies...
- Page 2 Notices ©Agilent Technologies, Inc. 2006 No part of this manual may be reproduced in any form or by any means (including elec- tronic storage and retrieval or translation into a foreign language) without prior agree- ment and written consent from Agilent Technologies, Inc.
- Page 3 In this Guide. . . This Installation and Operation Guide contains information for installing and using an effluent splitter on an Agilent 6890 gas chromatograph (GC). The G3180 splitter is intended for use with capillary columns and uses makeup gas to maintain adequate flows throughout the system.
- Page 4 Installation and Operation Guide...
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Page 5: Table Of Contents
Contents Introduction Hardware Installation Installation and Operation Guide Overview How It Works Details Metal ferrules Microfluidic plate Constant pressure operation Calculation of chromatographic parameters GC Requirements Other Requirements Parts Supplied Part Identification Parts Not Supplied Tools Required Prepare the GC Install the Column Clips Install the Bracket and Splitter Connect the Makeup Gas Supply... - Page 6 Splitter Configurations Operation Typical Configurations Splitting to an MSD Custom Configurations Restrictor id and length Maximum and minimum flows Column outlet pressure Inlet pressure Restrictor and Column Installation Install the column Connect the splitter Disconnect tubing from the splitter An Example Column flow Select restrictors Calculate column flow...
- Page 7 Calculation of chromatographic parameters GC Requirements Other Requirements Parts Supplied Part Identification Parts Not Supplied Tools Required This manual covers the installation and operation of the G3180B effluent splitter with makeup gas kit on the Agilent 6890 series gas chromatograph (GC). Agilent Technologies...
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Page 8: Introduction
Introduction Overview Splitter installation is done in three steps: 1 Hardware installation. This gets the hardware installed and the gas flows connected. 2 Restrictor configuration. You can choose to use a typical, precalculated configuration or create a custom one using software tools supplied on a CD. 3 Restrictor and column installation. -
Page 9: How It Works
Table 2 on page 26 in this manual or from a spreadsheet calculator that is included for calculating tubing dimensions for special situations. Figure 1 shows the plumbing configuration for the G3180B splitter. GC oven Figure 1 Installation and Operation Guide... -
Page 10: Details
Details The G3180B kit addresses several limitations of previous approaches to splitting column effluent between two detectors: Metal ferrules The splitter uses metal column ferrules, which eliminate air leakage into the sample stream. -
Page 11: Calculation Of Chromatographic Parameters
Introduction Calculation of chromatographic parameters Because the pressure at the split point is known and constant, the chromatographic parameters can be calculated before setup. This is especially useful with GC/MSD setups, where there are limitations on the flow rates of carrier gas allowed into the MSD. -
Page 12: Gc Requirements
Introduction GC Requirements The splitter mounts in an Agilent 6890 series GC. The splitter requires an electronically controlled pressure source such as the Three Channel Pressure controller (6890 option 205, 301, or 308) or a Pneumatics Control Module (PCM). Other Requirements The calculator requires Microsof®t Excel 97 (or later), which is not supplied with this kit. -
Page 13: Parts Supplied
Parts Supplied The G3180B kit contains the following parts Table 1 Part number 0100-0124 0100-0241 G1580-00130 G1530-01340 0515-0374 G2855-60140 G2855-60560 G2855-80022 G3180-90120 0100-2354 G3180-61500 G2855-60150 Installation and Operation Guide Parts supplied Description Union, stainless steel, 1/16-inch tubing Union, stainless steel, 1/8 to 1/16-inch reducing... -
Page 14: Part Identification
Introduction Part Identification Most of the kit parts are easily recognized. The unique ones are identified in Figure Capillary column spring clips Valve box blanking plate Oven bracket assembly Compact splitter with makeup gas assembly Figure 2 Part identification This assembly is shipped in a plastic bag to keep contaminants out of the tubing and the fittings. -
Page 15: Parts Not Supplied
Parts Not Supplied Brown-dot frit (19231-60610) Tools Required Side cutter, large Open-end wrenches Installation and Operation Guide Introduction... - Page 16 Introduction Installation and Operation Guide...
- Page 17 Agilent G3180B Splitter Kit Installation and Operation Guide Hardware Installation Prepare the GC Install the Column Clips Install the Bracket and Splitter Connect the Makeup Gas Supply This chapter describes the procedure for installing the splitter hardware and connecting the makeup gas supply.
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Page 18: Hardware Installation
Hardware Installation Prepare the GC Turn the power off and disconnect the power cord before proceeding. WA R N I N G 1 Raise the GC top cover to expose the oven top. 2 Remove the valve box cutout using a side cutter Figure 3 Cut tabs around edges... - Page 19 3 This exposes a layer of soft insulation. Remove it to expose the hard oven insulation. Remove the precut insulation piece at the location shown in Figure Figure 4 4 Replace the soft insulation. Install the valve box blanking plate, using one screw at the front and one at the rear to secure it.
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Page 20: Install The Column Clips
Hardware Installation Install the Column Clips Install the four column clips on the oven shroud Clip (1 of 4) Oven shroud Figure 6 Oven clips (Figure Installation and Operation Guide... -
Page 21: Install The Bracket And Splitter
Install the Bracket and Splitter The splitter is usually installed on the right side of the oven. The body of the splitter may be discolored as a result of the deactivation process. This is N O T E not a defect. 1 Place the bracket against the side of the oven. - Page 22 Hardware Installation Use extreme care to prevent any fragments of insulation or other material from C A U T I O N entering the makeup gas tubing or the fittings on the splitter assembly. Such materials could block the internal passages in the splitter or the bore of the capillary restrictors. In the following steps, bend the tubing over an object such as your thumb to avoid C A U T I O N kinks.
- Page 23 Hardware Installation 6 Route the prebent tubing against the oven wall and top to keep it clean for future maintenance. It should be behind the back detector location. 7 Screw the splitter assembly to the bracket (three screws). See Figure Makeup gas tubing Mounting screws Splitter assembly...
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Page 24: Connect The Makeup Gas Supply
Hardware Installation Connect the Makeup Gas Supply Connect the makeup gas source to the PCM or Auxiliary Pressure controller. To supply the makeup gas froma PCM 1 Connect the tubing from the PCM to the 1 meter length of stainless steel tubing from the kit with a union. - Page 25 Agilent G3180B Splitter Kit Installation and Operation Guide Splitter Configurations Typical Configurations Splitting to an MSD Custom Configurations Restrictor id and length Maximum and minimum flows Column outlet pressure Inlet pressure Restrictor and Column Installation Install the column Connect the splitter...
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Page 26: Splitter Configurations
Splitter Configurations Typical Configurations The important parameters when setting up a splitter are the lengths and diameters of the restrictor tubes that go to the two detectors. The dimensions of the restrictors are chosen to give the desired split ratio, flow to the detector, and to minimize peak broadening. - Page 27 Table 3 Splitter flows 40 °C Configuration Flow R1, Flow R2, mL/min mL/min 14.7 14.7 25.6 To use the tables, select the configuration you wish to set up. For example, Configuration 1 splits column effluent equally between two atmospheric pressure detectors (FID, TCD, ECD, FPD, and NPD). To plumb this system, 0.544-m lengths of 0.25-mm id uncoated deactivated fused silica tubing are connected as restrictors from the splitter to the two detectors.
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Page 28: Splitting To An Msd
Splitter Configurations For constant pressure methods, first find the maximum flow as above. Use the GC, ChemStation, Flow Calculator Software or the Method Translation Software to find the inlet pressure that gives the maximum flow at the upper temperature of the method (make sure the column outlet pressure is set to 3.8 psig for the calculation). -
Page 29: Custom Configurations
Custom Configurations The CD supplied with this kit contains three software tools: Effluent Splitter Calculator (with Makeup) inside diameter) of restrictors to obtain a desired split ratio Figure 11 Installation and Operation Guide Effluent Splitter Calculator Splitter Configurations Calculates dimensions (length and (Figure 11). - Page 30 Splitter Configurations GC Method Translation operating conditions to another Figure 12 Converts an analytical method from one set of (Figure GC Method Translation 12). Installation and Operation Guide...
- Page 31 Column Pressure/Flow Calculator set of column (or restrictor) dimensions Figure 13 These tools allow you to perform all the calculations needed to create a custom splitter configuration. We recommend that you load the CD software into your PC. 1 Insert the CD into the drive and click the Start icon in the bottom left of the screen.
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Page 32: Restrictor Id And Length
Splitter Configurations Restrictor id and length 1 Run the Effluent Splitter Calculator and enter the following information. The calculator provides a list of possible restrictors. • Column flow. Use the ChemStation, GC, Flow Calculator, or Method Translation Software to determine the column flow in mL/min (with the column outlet at 3.8 psig) at the initial oven temperature. -
Page 33: Maximum And Minimum Flows
Maximum and minimum flows The maximum suggested flow for MSDs depends on the vacuum pump used. For diffusion pump and standard turbo systems, the flow should not exceed 2 mL/min. For performance turbo systems, the flow should not exceed 4 mL/min. These flow limits restrict the column flows and split ratios that can be used with MSDs. -
Page 34: Column Outlet Pressure
Splitter Configurations Column outlet pressure The 6890 GC needs to know the pressure at the end of the column to be able to calculate column flows. Use either the GC keyboard or the ChemStation to set the outlet pressure for the column to 3.8 psig. The ChemStation screen where the column outlet pressure is set is shown in Figure 14 Inlet pressure... -
Page 35: Restrictor And Column Installation
Restrictor and Column Installation Restrictors and the column exit are connected to the splitter assembly using internal nuts N O T E and SilTite ferrules. See Install the column 1 Hang the analytical column on the column clips. The clips hold the outside of the wire “basket”... - Page 36 Splitter Configurations Figure 15 Do not overtighten the fittings. The dashed line in C A U T I O N finger-tight) is usually enough. Restrictor and column connections To makeup gas supply Restrictor 2 to Detector 2 Restrictor 1 to Detector 1 Column exit Figure 16 (about 15°...
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Page 37: Disconnect Tubing From The Splitter
Figure 16 Disconnect tubing from the splitter Loosen and remove the internal nut from the splitter fitting. Usually the tubing and ferrule will fall out of the fitting. Occasionally the ferrule will stick in the fitting. If this happens, use a pointed object like a pen or a paper clip and insert it in the ferrule release hole in the side of the fitting breaks free. - Page 38 Splitter Configurations Protect the column and restrictors Column and restrictor tubes with swaged metal ferrules can be disconnected and reconnected several times. To protect the tubing end, use one of the brass-sealing caps from the kit. Tighten to finger-tight plus 15 degrees. Protect the splitter Seal the ports of the splitter assembly with plugs when the splitter is not connected.
- Page 39 Agilent G3180B Splitter Kit Installation and Operation Guide Operation An Example Column flow Select restrictors Calculate column flow Calculate ECD restrictor flow Calculate MSD restrictor flow Changing Columns Without Venting the MSD Backflushing the Column This chapter contains a worked-through custom configuration, plus some special topics.
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Page 40: Operation
Operation An Example Assume we have a method that uses an HP-5MS column (30 m × 250 µm id × 0.25-µm film thickness) to measure pesticides with an MSD. The initial oven temperature is 70 °C and is programmed to 280 constant pressure mode at 19.44 psig inlet pressure and the carrier gas is helium. - Page 41 Operation Figure 18 Calculating column flow The outlet pressure entered for the new splitter method must be in absolute pressure units. Since the outlet of the column will be 3.8 psig, we need to convert this to psia for the method translator. Absolute pressure = gauge pressure + 14.696.
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Page 42: Select Restrictors
Operation Select restrictors Start up the spreadsheet "splitter_calc.xls" in Excel. We will choose to have 2 mL/min go to the ECD initially. With a split ratio of 3, this will send 6 mL/min to the MSD. This flow is acceptable with a performance turbo system but will give somewhat degraded detection limits. -
Page 43: Calculate Column Flow
Operation The calculator lists the lengths required for the different sizes of uncoated, deactivated, fused-silica, restrictor tubing available. Choose the id tubing that gives the shortest length of at least 0.3 m for most detectors and 0.8 m for MSDs. In this case 0.18-mm id is the choice, requiring 0.912 m for the ECD restrictor and 0.824 m for the MSD restrictor. -
Page 44: Calculate Ecd Restrictor Flow
Operation Calculate ECD restrictor flow The flow through the ECD restrictor at 280 °C is calculated to be 0.88 mL/min (Figure 21). Figure 21 This flow is higher than the minimum 0.72 mL/min suggested for helium in 0.18-mm id tubing. ECD restrictor flow calculation Installation and Operation Guide... -
Page 45: Calculate Msd Restrictor Flow
Operation Calculate MSD restrictor flow The flow through the MSD restrictor (Figure 22) at 280 °C is: Figure 22 MSD restrictor flow calculation The flow to the MSD at 280 °C is 2.65 mL/min. This flow is higher than the minimum 0.72 mL/min suggested for helium in 0.18-mm id tubing. -
Page 46: Changing Columns Without Venting The Msd
Operation Changing Columns Without Venting the MSD For systems that use an MSD attached to the splitter, one added advantage is the GC column can be changed without venting the MSD. When the column is disconnected from the splitter plate, the makeup gas purges air out of the fitting, preventing air from reaching the MSD. -
Page 47: Backflushing The Column
Backflushing the Column One useful feature available with EPC control of the makeup is the ability to backflush unwanted higher boiling analytes from the column. Use of this feature requires that the split/splitless inlet be used. Backflushing reduces the hold at the end of the run to clean out the column. To backflush, the splitter makeup pressure is time-programmed to rise rapidly after elution of the last peak of interest while the inlet pressure decreases rapidly. - Page 48 Operation The restrictor to the MSD was 0.824 m of 0.18-mm id tubing. The backflushing temperature used here is the hold temperature at the end of the run in the original method (280 °C). The flow calculator makeup pressure can be programmed to 17.4 psig at 280 °C. Figure 23 The time required for complete backflushing of heavy materials is then determined empirically.
- Page 49 Index Absolute pressure, Aux EPC, Auxiliary Pressure controller, Backflushing, Changing columns, Column connections, flow, 10, 26, 27, outlet pressure, Column clips, Column effluent, Configuration, custom, 25, typical, 25, Constant flow mode, Constant pressure mode, Constant pressure operation, Custom configuration, Example, Detector Above atmospheric pressure, Atmospheric pressure,...
- Page 50 Installation and Operation Guide...
- Page 52 Agilent Technologies © Agilent Technologies, Inc. Printed in USA, April 2006 G3180-90120...