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