Agilent Technologies G3183B Installation And Operation Manual
Agilent Technologies G3183B Installation And Operation Manual

Agilent Technologies G3183B Installation And Operation Manual

Three-way splitter kit

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Agilent G3183B
Three-Way Splitter Kit
Installation and Operation
Guide
Agilent Technologies

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Summary of Contents for Agilent Technologies G3183B

  • Page 1 Agilent G3183B Three-Way Splitter Kit Installation and Operation Guide Agilent Technologies...
  • Page 2 Notices Safety Notices © Agilent Technologies, Inc. 2006 No part of this manual may be reproduced in any form or by any means (including elec- C A U T I O N tronic storage and retrieval or translation into a foreign language) without prior agree-...
  • Page 3 This Installation and Operation Guide contains information for installing and using an effluent splitter on an Agilent 6890 gas chromatograph (GC). The G3183B 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...
  • Page 5: Table Of Contents

    Contents Introduction Overview How It Works Details Calculation of chromatographic parameters Gas Requirements Carrier gas Makeup gas GC Requirements Other Requirements Parts Supplied Part Identification Parts Not Supplied Tools Required Pressure Units Gauge pressure (psig) Absolute pressure (psia) Atmospheric pressure Conversion Installation Prepare the GC...
  • Page 6 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 Disconnect tubing from the splitter Operation An Example Column flow Select restrictors Calculate column flow...
  • Page 7 Makeup gas GC Requirements Other Requirements Parts Supplied Part Identification Parts Not Supplied Tools Required This manual covers the installation and operation of the G3183B effluent splitter with makeup kit on the Agilent 6890 series gas chromatograph (GC). Agilent Technologies...
  • 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

    Tubing dimensions may be determined from 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 G3183B splitter. Inlet Aux EPC Det 1...
  • Page 10: Details

    Details The G3183B kit addresses several limitations of previous approaches to splitting column effluent between three 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: Gas Requirements

    Introduction Gas Requirements Carrier gas The choice of carrier gas is dictated by the chromatographic requirements. Hydrogen and helium are the most common choices for capillary columns. See your GC documentation and other sources for additional carrier gas information. Makeup gas The makeup gas is usually the same as the carrier gas, with one very important exception.
  • Page 13: Parts Supplied

    Introduction Parts Supplied Parts in the G3183B kit are listed in Table Table 1 Parts supplied Part number Description Quantity G1530-01340 Capillary column spring clips G2855-60140 Oven bracket assembly G2855-60560 T-screw oven bracket retainer 0515-0374 Screw, M3 × 10 mm...
  • 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 This assembly is shipped in a plastic bag to keep contaminants Three-way splitter out of the tubing and the fittings.
  • Page 15: Parts Not Supplied

    Introduction Parts Not Supplied Brown-dot frit (19231-60610) Tools Required Side cutter, large Screwdrivers, Phillips Installation and Operation Guide...
  • Page 16: Pressure Units

    Introduction Pressure Units All pressure figures in this manual are given in pounds per square inch. Gauge pressure (psig) This is the pressure as measured by most pressure gauge. It is the pressure in excess of atmospheric pressure. Absolute pressure (psia) This is the actual pressure relative to vacuum.
  • Page 17: Installation

    Agilent G3183B Splitter Kit Installation and Operation Guide 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.
  • Page 18: Prepare The Gc

    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 lid. 2 Remove the valve box cutout using a side cutter (Figure Cut tabs around edges...
  • Page 19 Installation 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 Remove this cutout Figure 4 Remove the insulation cutout 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.
  • Page 20: Install The Column Clips

    Installation Install the Column Clips Install the four column clips on the oven shroud (Figure Clip (1 of 4) Oven shroud Figure 6 Oven clips Installation and Operation Guide...
  • Page 21: Install The Bracket And Splitter

    Installation Install the Bracket and Splitter The body of the splitter may be discolored as a result of the deactivation process. This is not a defect. The splitter is usually installed on the right side of the oven. 1 Place the bracket against the side of the oven. The two notches should be up and the standoffs should face the center of the oven.
  • Page 22 Installation In the following steps, bend the tubing over an object such as your thumb to avoid C A U T I O N kinks. 3 Open the plastic bag and remove the splitter assembly. Install a plastic cap on the end of the makeup gas tubing. Place small pieces of tape over the open end of the fittings.
  • Page 23 Installation Makeup gas tubing Mounting screws Note: Picture shows a two-way splitter. Mounting details are the same for both. Splitter assembly Ferrule release hole Mounting screw Figure 9 Installing the splitter assembly 8 After the splitter is installed and the makeup gas tubing is routed, trim the tubing above the oven top, leaving at least 10 cm.
  • Page 24: Connect The Makeup Gas Supply

    Installation Connect the Makeup Gas Supply Connect the makeup gas source to the Pneumatic Control Module or Auxiliary Pressure controller. To supply the makeup gas from a Pneumatic Control Module (PCM) 1 Connect the tubing from the PCM to the length of stainless steel tubing from the kit with a union.
  • Page 25 Agilent G3183B 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...
  • 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 three detectors. The dimensions of the restrictors are chosen to give the desired flow (split) ratio, flow to the detector, and to minimize peak broadening.
  • Page 27 Splitter Configurations Table 3 Splitter flows 40 °C 200 °C 300 °C Configur- Flow R1, Flow R2, Flow R3, Flow R1, Flow R2, Flow R3, Flow R1, Flow R2, Flow R3, ation mL/min mL/min mL/min mL/min mL/min mL/min mL/min mL/min mL/min 0.71 0.71...
  • Page 28: Splitting To An Msd

    Splitter Configurations The column flow at 200 °C should be no more than 2 mL/min. This becomes important when the column is run in constant flow mode. If constant flow mode is used with Configuration 1 and the method programmed to 300 °C, the column flow should not exceed 1.13 mL/min ([0.71 + 0.71 + 0.71] –1).
  • Page 29: Custom Configurations

    Splitter Configurations Custom Configurations The CD supplied with this kit contains three software tools: Effluent Splitter Calculator (with Makeup) Calculates dimensions (length and inside diameter) of restrictors to obtain a desired split ratio (Figure 11). Figure 11 Effluent Splitter Calculator Installation and Operation Guide...
  • Page 30 Splitter Configurations GC Method Translation Converts an analytical method from one set of operating conditions to another (Figure 12). Figure 12 GC Method Translation Installation and Operation Guide...
  • Page 31 Splitter Configurations Column Pressure/Flow Calculator Calculates flows and pressures for a given set of column (or restrictor) dimensions (Figure 13). Figure 13 Column Flow/Pressure Calculator 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.
  • 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

    Splitter Configurations 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.
  • 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 Figure 14...
  • Page 35: Restrictor And Column Installation

    Splitter Configurations Restrictor and Column Installation Restrictors and the column exit are connected to the splitter assembly using internal nuts and SilTite ferrules. Install fittings on the column exit and one end of each restrictor as described in “Swaging SilTite Ferrules” on the CD.
  • Page 36: Disconnect Tubing From The Splitter

    Splitter Configurations Restrictor to detector 3 Restrictor to detector 2 Restrictor to detector 1 To makeup gas supply Column in Figure 15 Detector and column connections Do not overtighten the fittings. One-eighth of a turn (about 15° clockwise from C A U T I O N finger-tight) is usually enough.
  • Page 37 Splitter Configurations 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 (Figure 16). Press firmly. The ferrule will click when it breaks free.
  • Page 38 Splitter Configurations Installation and Operation Guide...
  • Page 39 Agilent G3183B Splitter Kit Installation and Operation Guide Operation An Example Column flow Select restrictors Calculate column flow Calculate MSD restrictor flow Calculate FPD restrictor flow Calculate ECD restrictor flow Changing Columns Without Venting the MSD Backflushing the Column Other Uses for Three-Way Splitter Setup...
  • 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 performance turbo system. The initial oven temperature is 70 °C and is programmed to ο...
  • Page 41 Operation Figure 17 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.
  • Page 42: Select Restrictors

    Operation Select restrictors Start up the spreadsheet "splitter3_calc_rev1.xls" in Excel. Select the “3-Way (Makeup)” worksheet. We will choose to have 4 mL/min go to the MSD initially. This flow is acceptable with a performance turbo system. Fill in the input column as shown (Figure 18) with the MSD assumed to be Detector 1, the FPD...
  • 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 for the MSD and the FPD. A length of 1.236 m is calculated for the MSD restrictor and 0.456 m for the FPD restrictor.
  • Page 44: Calculate Msd Restrictor Flow

    Operation The column flow drops to 1.38 mL/min at 280 °C. Calculate MSD restrictor flow The flow through the MSD restrictor at 280 °C is calculated to be 1.77 mL/min (Figure 20). Figure 20 MSD restrictor flow calculation This flow is higher than the minimum 0.72 mL/min suggested for helium in 0.18-mm id tubing.
  • Page 45: Calculate Fpd Restrictor Flow

    Operation Calculate FPD restrictor flow The flow through the FPD restrictor (Figure 21) is also 1.77 mL/min at 280 °C. Figure 21 FPD restrictor flow calculation This flow is higher than the minimum 0.72 mL/min suggested for helium in 0.18-mm id tubing. Installation and Operation Guide...
  • Page 46: Calculate Ecd Restrictor Flow

    Operation Calculate ECD restrictor flow The flow through the ECD restrictor (Figure 22) is 0.18 mL/min at 280 °C. Figure 22 ECD restrictor flow calculation This flow is below the minimum 0.4 mL/min suggested for helium in 0.10-mm id tubing. In practice, this setup still gives acceptable peak shapes on the ECD, so it will be used.
  • Page 47: 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 forces air out of the fitting, preventing air from reaching the MSD.
  • Page 48: Backflushing The Column

    Operation 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.
  • Page 49 Operation The restrictor to the MSD was 1.236 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 (Figure 23) shows that the makeup pressure can be programmed to 47.5 psig at 280 °C.
  • Page 50: Other Uses For Three-Way Splitter Setup

    Operation Other Uses for Three-Way Splitter Setup While the most common use of the hardware discussed here is as a three-way splitter, the device can also be used for other purposes. The following configurations are examples. Three-way splitter Figure 24 shows the typical three-way splitter configuration for reference.
  • Page 51: Two Columns In/Two Detectors Out

    Operation In this case, port 1 is plugged and the column is connected to port 2. The two detector restrictors are connected to ports 3 and 4. Calculations for a two-way splitter are similar to those for the three-way. See the manual for the G3180B Micro-Fluidic Effluent Splitter with Makeup Gas provided on the CD that came with this product for setting up a two-way split.
  • Page 52: Two Different Columns In/Two Detectors Out

    Operation Two different columns in/Two detectors out Inlet 1 Inlet 2 Aux EPC Det 1 Column 2 Column 1 Splitter Figure 27 Two different columns in/two detectors out With this setup, a method can inject into Inlet 1 (and Column 1) while Column 2 is unused.
  • Page 53 Index Absolute pressure, Effluent Splitter Calculator, 29, 32, Aux EPC, Electronic pneumatic control, Auxiliary Pressure controller, Excel, Backflushing, Ferrule release hole, Flow column, 10, 26, detector, makeup, Changing columns, maximum and minimum, Column Flow Calculator, connections, flow, 10, 26, 28, outlet pressure, Column clips, Column effluent,...
  • Page 54 Parameter calculation, Parts supplied, PCM, 12, 24, Peak broadening, 26, Plugs, Pneumatic Control Module, 12, Pressure controller, psia, psig, Restrictor, dimensions, flow, 44, Retention times, Software tools Column Pressure/Flow Calculator, Effluent Splitter Calculator, GC Method Translation, loading, Split ratio, 9, 26, 28, Splitter connections, Spreadsheet calculator, Tailing,...
  • Page 56 Agilent Technologies © Agilent Technologies, Inc. Printed in USA, April 2006 G3183-90120...

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