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Agilent Technologies 7673 Operating Manual

Automatic liquid sampler
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Operating Manual
Agilent 7673 Automatic Liquid Sampler

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  • Page 1 Operating Manual Agilent 7673 Automatic Liquid Sampler...
  • Page 2 Werden Meß-und Testgeräte mit ungeschirmten of design and the intended use of the instrument. Kabeln und/oder in offenen Meßaufbauten Agilent Technologies assumes no liability for the verwendet, so ist vom Betreiber sicherzustellen, customer’s failure to comply with these daß die Funk-Entströbedingungen unter requirements.

  • Page 3: Table Of Contents

    Contents Chapter 1 Setting Up The modules of the automatic liquid sampler ............3 Preparing the site ...................... 5 Environmental considerations ................. 5 Space considerations ..................5 Electrical power requirements ................ 6 Connecting the controller power cord ............7 Installing the injectors ....................7 Behind the door to the control switches ............
  • Page 4 Contents Filling and placing the bottles ................37 Do you need to read further? .................40 Estimating the maximum number of sample vials ........42 Controlling sample carryover .................47 Selecting and installing syringes ................49 Selecting syringes ....................49 Inspecting syringes ..................51 Installing syringes ....................52 Checking your work ..................53 Maintaining the inlet ....................54 Changing septa ....................54...
  • Page 5 Contents Creating a sequence ..................78 Storing a sequence ..................79 Starting/running a sequence ................80 Special considerations when using an integrator with a 6890 Series GC ..81 3396 integrator with a 5890 GC ................83 Checking your work ..................85 Multitechnique ChemStation control with a 6890 Series GC ........................
  • Page 6 Turret error .....................136 Plunger error ....................137 Incomplete injection ..................138 Bottle in gripper .....................139 Hard tray/injector error .................140 Align LED is On ....................141 Other patterns ....................142 Error messages ......................145 Contacting Agilent Technologies .................147 Obtaining Agilent Technologies service .............147 Shipment or storage ..................148...
  • Page 7 Contents Chapter 6 Special Topics Performing cool on-column injection onto 250-µm and 320-µm columns ..151 Installing the needle into the syringe barrel ..........151 Checking the needle-to-column size ............152 Preparing the cool on-column inlet ............. 153 Using retention gaps and other precolumns ..........158 Preparing the injector ...................
  • Page 8 Contents...

  • Page 9: Setting Up

    Setting Up...
  • Page 10 Setting Up The purpose of this chapter is to: • Introduce you to the names of the major parts associated with installing the automatic liquid sampler and some preventive maintenance tips. • Help you set up the automatic liquid sampler and turn on the power. You must complete the following tasks during installation to be ready to turn on the power.
  • Page 11 Setting Up The modules of the automatic liquid sampler "6890" [type C] tower, tray and controller The modules of the automatic liquid sampler The automatic liquid sampler is made up of three modules: The G1512A controller and communications module supplies power and communications to the injector and tray.

  • Page 12: The Modules Of The Automatic Liquid Sampler

    Setting Up The modules of the automatic liquid sampler Figure 1 illustrates how the automatic liquid sampler is an integral part of the analytical system. One or two injectors With or without the tray With or with out the bar code reader Controller Controller configured to communicate with:...

  • Page 13: Environmental Considerations

    • Relative humidity range: 5% to 95% at 40°C • Altitude ranges: up to 2,300 m Agilent Technologies recommends an environment comfortable for the operators (reasonably constant temperature and humidity) for optimum performance and instrument lifetime. Caution Do not place any instruments that release heat on top of or underneath the controller.

  • Page 14: Preparing The Site

    Setting Up Preparing the site WARNING Place the G1512A controller where you can easily unplug it from the power source. Ventilation and cabling space Top Views Ventilation space All dimensions in centimeters Figure 2. Space considerations Electrical power requirements The controller is the power source for the injector and tray. The controller has an autoranging power supply: •...

  • Page 15: Connecting The Controller Power Cord

    Setting Up Installing the injectors WARNING Any interruption of the grounding conductor or disconnection of the power cord could cause a shock that results in personal injury. Connecting the controller power cord Check the on/off button on the front of the controller. It must be off or flush with the front panel before you plug in the power cord.

  • Page 16: Installing The Injectors

    Setting Up Installing the injectors Electronics assembly Door to control switches Start/stop buttons Fault LEDs Door to syringe Turret Base Figure 3. G1513A injector module...

  • Page 17: Behind The Door To The Control Switches

    Setting Up Installing the injectors Behind the door to the control switches There are control switches behind the door on the injector’s front panel. • You use the rotary switch to set the number of sample vials when no tray is installed and the remaining ten switches to set six injector parameters when the system cannot be controlled by the 6890 Series GC, a computer, or an integrator.

  • Page 18: Before You Start

    Setting Up Installing the injectors Rotary switch Align LED Control switches Figure 4. The parameter control switches Before you start To install an injector, you must first: • Install the tray’s mounting bracket before mounting the injectors (if your automatic liquid sampler includes a tray). The instructions and hardware are packaged together with the tray.
  • Page 19 Setting Up Installing the injectors • Install the injector mounting posts in the front and back locations of the injection bracket on the GC. Mounting the injectors The first part of each step describes how to mount the injector over the front inlet (injection port).

  • Page 20: Mounting The Injectors

    Setting Up Installing the injectors Turn the injector so that the turret is facing toward you. Lower the injector so that the pin in the base enters the hole in the disk on the mounting bracket. Turret Mounting pin Front mounting post Disk Figure 6.

  • Page 21: Checking Your Work

    Setting Up Installing the tray Checking your work Be sure the mounting pin is seated in the hole of the disk. The injector’s feet should touch the mounting bracket. Be sure the gas lines are not routed under the feet or the mounting pin. Turn the turret so you can see the inlet of the GC, and open the door to the syringe.

  • Page 22: Installing The Tray

    Setting Up Installing the tray Quadrant Gripper Gripper jaws Sample vial Figure 7. 18596B tray module Before you start Caution Do not remove the tray’s arm back and forth. Do not move the tray’s gripper up and down. These movements could damage the tray arm. If you need to move the arm, turn it in a clockwise or counterclockwise direction.

  • Page 23: Mounting The Tray

    Setting Up Installing the tray Mounting the tray Thread the cable through the hole in the mounting bracket. Lower the tray onto the bracket. Position the tray so that it sits flat on the bracket with the raised arrow pointing toward the right (the front injector). Move the injector cable out of the way.

  • Page 24: Checking Your Work

    Setting Up Installing the tray Lock the tray into place by pulling each lock up (A), turning each lock (B), and inserting each tab into a slot in the tray (C). Figure 10. Locking the tray Snap the tab of each tray quadrant into a slot on the base of the tray. The numbers on the quadrants should match the numbers on the base.
  • Page 25 Setting Up Installing the controller Installing the controller The G1512A controller provides power and the communication interface for 18593A/B or G1513A injectors and for the 18596A or 18596B/C tray. There are 11 connectors and two sets of switches for defining the communication type.

  • Page 26: Installing The Controller

    Setting Up Installing the controller This section covers connecting the injector and tray cables to the controller, connecting the controller to the GC, connecting the controller to the data handling device, and plugging in the controller. Find the power cord in the controller box. Check the shape of the plug and the source voltage listed on the packing contents sheet.

  • Page 27: Configuration Switch Definitions

    Setting Up Installing the controller Setting the configuration switches There are 16 switches on the back of the controller. Figure 14 and Figure 15 show the switches and settings for five common types of communications. When you are using ChemStation software, you must set the GPIB address switches to a unique address.

  • Page 28: Setting The Configuration Switches

    Setting Up Installing the controller GPIB address Communication mode Baud rate Bar code reader position Handshake Figure 14. Setting the address switches ChemStation 6890 Series GC Address = 10 MSD ChemStation (rev 3.70 and above) 3365 ChemStation MSD ChemStation Address = 8 (rev 3.65 and below) HP-UX ChemStations Integrator with INET...
  • Page 29 Setting Up Installing the controller Table 3. Possible GPIB Address Switch Settings Switch Switch GPIB Address Settings GPIB Address Settings 00000 01111 00001 10000 00010 10001 00011 10010 00100 10011 00101 10100 00110 10101 00111 10110 01000 10111 01001 11000 01010 11001 01011...

  • Page 30: Connecting The Injector Cables

    Setting Up Installing the controller back. Be sure the spring clamps on either side of the plug snap onto the connector. Note the TOP label on the connector for orientation purposes. Tray Injector Figure 16. Connecting the injector and tray cables Connecting the tray cable Plug the cable into the tray connector on the back panel of the controller.

  • Page 31: Checking Your Work

    Setting Up Installing the controller Checking your work Be sure the injector and tray plugs are fastened securely. Be sure all the communication cables are installed and fastened securely. Be sure any external control or data handling devices are configured correctly by referring to the appropriate manual.
  • Page 32 this page is from "Agilent 7683B Automatic Liquid Sampler Installation Installation, Operation and Maintenance" 6890A GC Follow the instructions below to properly wire the G2912A controller. See “Procedure 8. Install the G2912A ALS Controller” on page 55 for installation instructions for the G2912A controller including the power supply cord. G2912A Controller Front Back...
  • Page 33 Setting Up Installing the controller...
  • Page 34 Preparing for Operation...

  • Page 35: Preparing Sample Vials

    Preparing for Operation This chapter contains detailed information for preparing the automatic liquid sampler for operation, including: • Preparing sample vials • Using the injector fan • Preparing the solvent and waste bottles • Selecting and installing syringes • Maintaining the inlet •...

  • Page 36: Specifications

    Preparing for Operation Preparing sample vials The location and thickness of a vial label can affect the delivery of the bottles to and from the injector. Agilent Technologies recommends the position and maximum label thickness shown in the following diagram. No label 5.6 0.6...

  • Page 37: Sample Caps And Septum

    Preparing for Operation Preparing sample vials specifications. Some of the dimensions are too difficult to measure without special instruments. Microvial insert Crimp cap sample vial 5 minimum 8.2 maximum 28.4 11.7 0.2 All dimensions in millimeters Figure 18. Dimensions for sample vials and microvial inserts Sample caps and septum Although septa come in different colors, the characteristics are measured by inertness and type of composition.

  • Page 38: Filling Sample Vials

    Preparing for Operation Preparing sample vials Figure 19 illustrates the recommended and minimum diameter for vial cap apertures. 5.58 (0.220 in.) recommended 4.65 (0.183 in.) minimum All dimensions in millimeters Figure 19. Specifications of vial cap aperture Use amber glass vials for light-sensitive samples. The last specification to consider is the total height of the capped vial.

  • Page 39: Crimp Capping Sample Vials

    Preparing for Operation Preparing sample vials For large volumes and multiple injections, you will have to decide how to divide the sample among several vials to obtain reliable results. You have to be aware when sample volume is low. For example, if the vials are less than half full, contaminants from the previous sample injection or solvent washes may affect the sample.
  • Page 40 Preparing for Operation Preparing sample vials Lift the vial into the crimper, and squeeze the handle until the bottom grip reaches the adjuster screw. Handle Adjuster screw Jaws Crimp cap Sample vial Figure 22. Crimping caps Caution Vials that do not have properly crimped caps may cause sampler errors. When a tray is not installed, you may be able to use sample vials with no caps, snap-on caps, or screw-on caps depending on your application.

  • Page 41: Placing Sample Vials In The Standard Injector Turret

    Preparing for Operation Preparing sample vials Cap has a flat septum centered over the top of the vial. • If the septum is not flat, remove the cap, turn the adjusting screw clockwise, and try again. • If the cap is not centered, remove the cap, and make sure the new cap is flat on the top of the vial before you squeeze the crimper.

  • Page 42: Placing Sample Vials In A Tray

    Preparing for Operation Preparing sample vials Place the sample vials into the sample inserts. White sample insert White sample insert for sample 2 for sample 3 Turret Sample 1 Figure 24. Placing sample inserts for three sample vials Placing sample vials in a tray You can place up to 100 samples in the tray’s four quadrants.

  • Page 43: Using The Injector Fan

    Preparing for Operation Using the injector fan For more information, see “Setting the run parameters” in chapter 3. FRONT INJECTOR INJ/BOTTLE 1 > FIRST BOTTLE 1 > LAST BOTTLE 5 > Figure 25. Specifying tray positions with a 3396 integrator and 5890 or 6890 GC Using the injector fan The purpose of the fan is to push cool air over the samples and solvent to keep them cooler.
  • Page 44 Preparing for Operation Using the injector fan Caution This procedure requires protection against electrostatic discharge. Use a static control wrist strap connected to a ground (part no. 9300-0969 for large wrists or part no. 9300-0970 for small wrists). If you do not use static protection, you may damage the electronics of the injector.

  • Page 45: Preparing The Solvent And Waste Bottles

    The injector uses 4-ml bottles with diffusion caps to hold the solvent and waste. You can use diffusion caps or septa on these bottles to reduce evaporation and diffusion of your solvents and waste. Agilent Technologies recommends diffusion caps over septa for two reasons: •...

  • Page 46: Filling And Placing The Bottles

    For many common solvents, the rate of diffusion out of the bottle is less with a diffusion cap than with a septum that has been punctured with a standard syringe needle. Diffusion cap Agilent Technologies recommends using a diffusion cap instead of a septum to reduce solvent contamination and evaporation.
  • Page 47 Preparing for Operation Preparing the solvent and waste bottles Empty and rinse each waste bottle. The syringe can dispense about 4 ml of waste into the waste bottle or about 500 washes for a 10-µl syringe. 4 ml maximum Figure 29. Shows position of syringe tip when dispensing waste Place the bottles in the appropriate positions on the injector turret according to the table on page 40.
  • Page 48 Preparing for Operation Preparing the solvent and waste bottles • If a tray is not installed, place two or three bottles (solvent A, waste A, and solvent B) in the turret positions. Position 3 in the turret can be used as sample 3 or solvent B.

  • Page 49: Do You Need To Read Further

    Preparing for Operation Preparing the solvent and waste bottles Caution When a tray is installed, place a waste bottle in both waste position A and waste position B. The injector alternates dispensing waste between the two positions. With the 6890 Series GC, you can choose A, B, or both. System Solvent Waste...
  • Page 50 Preparing for Operation Preparing the solvent and waste bottles Number of Bottles Solvent Limit Waste Limit Syringe size 5 µl 10 µl 5 µl 10 µl Two bottles 1,000 2,000 1,000 One bottle 1,000 Note: Wash volume is 0.8 times the syringe volume. Figure 31.

  • Page 51: Estimating The Maximum Number Of Sample Vials

    Preparing for Operation Preparing the solvent and waste bottles solvent bottles in both positions and set the run parameters for solvent washes from both positions (e.g., one from solvent A and two from solvent B). Example 3 (tray installed): Your application requires three sample washes, three solvent A washes, and three solvent B washes with a 10-µl syringe.
  • Page 52 Preparing for Operation Preparing the solvent and waste bottles Using the equation to estimate Substitute the parameters of your application into both equations. • If you are using a 5-µl syringe, substitute 0.004 ml/wash for the 0.008 ml/wash in each equation. •...
  • Page 53 Preparing for Operation Preparing the solvent and waste bottles Substitute the parameters of your application into equations S and W. Maximum number of vials = 2.0 ( 0.008 x 2 x 3 ) = 41 Maximum number of vials = 8.0 ( 0.008 x 2 x 7 ) = 71 Calculate the answers for both equations.
  • Page 54 Preparing for Operation Preparing the solvent and waste bottles Number of injections per vial 100+ 100+ 100+ Number solvent washes injection Figure 32. Maximum number of sample vials with one solvent bottle and a 10-µl syringe Go to the W table in Figure 33. In the left-hand column, find the number of solvent wastes and sample washes you need.
  • Page 55 Preparing for Operation Preparing the solvent and waste bottles Number of injections per vial 100+ 100+ 100+ 100+ 100+ 100+ 100+ Number 100+ of pre-and post-solvent washes sample washes per injection Figure 33. Maximum number of sample vials with one waste bottle and a 10-µl syringe Compare the answers from both tables.

  • Page 56: Controlling Sample Carryover

    Preparing for Operation Preparing the solvent and waste bottles Go to the S table in Figure 32. In the left-hand column, find the largest number of solvent washes you need from a solvent bottle, answer (3). Read across this row to the column indicating the number of injections you are taking from each vial, answer (2).
  • Page 57 Preparing for Operation Preparing the solvent and waste bottles • Sample washes The injector fills the syringe to eight-tenths of its volume with the next sample and dispenses the contents into one of the waste bottles. Sample washes occur before the injection. When sample is limited, you can use a solvent prewash to wet the syringe before drawing sample.

  • Page 58: Selecting And Installing Syringes

    Preparing for Operation Selecting and installing syringes Selecting and installing syringes Selecting syringes Select the type of syringe you need based on the inlet (injection port) you are using and the volume of sample you want to inject. The syringe needle must have a cone tip. Do not use sharp-tipped needles. These needles tear the inlet septum causing leaks.
  • Page 59 Preparing for Operation Selecting and installing syringes Figure 36 illustrates the shapes of the two fixed needles: 23/26 gauge tapered needle 23 gauge or 26 gauge straight needle Figure 36. Needle shapes Select the appropriate syringe needle gauge. If you need more help in making your selection, refer to chapter 6, “Special Topics.”...

  • Page 60: Inspecting Syringes

    Preparing for Operation Selecting and installing syringes Sample Volume Setting Standard Injection With Nanoliter Adapter Syringe 5 µl 10 µl 5 µl 10 µl Size Figure 38. Injection volumes depend on sample volume setting, syringe size and injection type Caution Failure to use an on-column syringe when injecting into an on-column inlet could damage the injector, syringe and column.

  • Page 61: Installing Syringes

    Preparing for Operation Selecting and installing syringes If there are ridges, polish the needle by pulling it through a folded piece of fine emery paper between your finger and thumb until the ridges are gone. Be careful not to modify the special blunt tip of the syringe. Check for a sticky plunger.

  • Page 62: Checking Your Work

    Preparing for Operation Selecting and installing syringes Move the plunger carrier loop down and tighten the plunger screw. Checking your work Move the plunger carrier up and down. If the syringe plunger does not move along with the carrier, repeat the previous steps. Be sure the plunger carrier screw is tight.

  • Page 63: Maintaining The Inlet

    Preparing for Operation Maintaining the inlet Caution Do not operate the injector without a syringe in place because the syringe latch may interfere with the motor if it is allowed to swing freely. To check the alignment of the syringe needle to ensure an average septum life of 200 injections, follow these instructions: Pull down the syringe carriage until the needle tip is near the top of the inlet septum nut.

  • Page 64: Changing Or Cleaning Liners

    Preparing for Operation Adapting for cool on-column injection Changing or cleaning liners Most samples contain nonvolatile material that accumulates on and partially pyrolyzes on the liner. Replace the liner or clean the liner periodically. Some active components interact with the glass liner and glass wool plug of the capillary liner.
  • Page 65 • Slows the plunger speed to 1/18 the normal speed Complete the following: Install an on-column syringe. Agilent Technologies recommends syringes with a 23/26 gauge tapered-tip needle for injections onto 530-µ columns and 32/26 gauge for 320- and 250-µ columns.

  • Page 66: Chapter 3 Operation

    Operation...
  • Page 67 Operation This chapter contains detailed information for operating the automatic liquid sampler, including: • Setting the run parameters • Starting and stopping the automatic liquid sampler • What happens during a run • Running the samples • Four methods of control •...

  • Page 68: Setting The Run Parameters

    Operation Setting the run parameters Setting the run parameters This section describes each run parameter, lists the range of values for the common controlling devices, and contains three examples. The run parameters tell the injector and the tray what to do. For example, they tell the injector how much sample to inject and tell the tray where to find sample vials.
  • Page 69 Operation Setting the run parameters Number of sample washes Specifies the number of times the syringe is rinsed with sample before the injection. The injector lowers the needle into the sample vial, fills the syringe to eight-tenths its full volume, and empties it into one of the waste bottles. Number of sample pumps Specifies the number of times the syringe plunger is moved up and down while the needle is in the sample to expel air bubbles and improve reproducibility.
  • Page 70 Operation Setting the run parameters Caution Do not set the volume parameter for splitless inlets more than 2 µl. Larger volumes cause sample to be lost through the purge vent and may contaminate carrier inlet lines. Dwell time This setpoint specifies the time delay of the needle in the inlet for both pre- and post-injection.
  • Page 71 Operation Setting the run parameters parameter also holds the syringe in the inlet for 4 seconds after the injection. The plunger speed during the pump and waste dispensing does not change. inj: fast slow Switch setting Sample in needle Fast, no dwell Slow, with dwell Down Figure 42.

  • Page 72: Injection Mode

    Operation Setting the run parameters Sampling depth This setpoint allows you to move the position of the needle tip up or down to approximate locations from the nominal position of zero (default). Default is the standard position (see Figure 43). Standard position 1 ml 3.6 mm*...
  • Page 73 Operation Setting the run parameters Position This setpoint indicates which tower is on which inlet (front or back). Typically, the location of the injector cable in the controller box, front or back, is the position associated with that injector. With an INET integrator and dual injectors, this setpoint specifies which injector, front or back, is associated with the INET data channel and which is associated with the auxiliary data channel.
  • Page 74 Operation Setting the run parameters Table 4. Range of Values for Common Controlling Devices 6890 and Multitechnique 3396 INET Parameter ChemStation* Integrator 3365 ChemStation** Injections per vial 1 to 99 0 to 15 1 to 99 Position of first and last vials (front) 1-3, 101-103, or 1-100 1-3 or 1-100 1-3 or 1-100...

  • Page 75: What Happens During A Run

    Operation What happens during a run? What happens during a run? In the following description, the run parameters that determine the automatic liquid sampler’s actions are surrounded by quotes (“run parameter”). From the point when you start the run, the automatic liquid sampler does the following: The syringe carriage, plunger carrier, injector turret, tray arm, and gripper move to their home positions.
  • Page 76 Operation What happens during a run? The injector waits until the GC sends a ready signal to continue. Steps 1, 2, and 3 through 9 are repeated according to the “injections per vial.” With a tray, the steps are repeated until the tray returns the last sample to the “position of last vial.”...

  • Page 77: Checklist

    Operation Checklist Checklist Use this checklist to make sure the sampler is ready before you begin. Sample vials are half full Cap centered, no wrinkles, septum is flat Sample inserts and vials match the run parameters Tray quadrants snapped in place 4.5 ml of fresh solvent in each solvent bottle Waste bottles are clean and empty Two waste bottles (with tray)

  • Page 78: Running The Samples

    Operation Running the samples Running the samples This section describes starting and stopping a run or sequence and the movements of the automatic liquid sampler during a run. Starting a run or sequence After completing the checklist above, start the run or sequence by pressing the start button on the injector or entering the appropriate command at your controlling device.

  • Page 79: Using Two Injectors

    Operation Using two injectors To restart an aborted sequence from the point of interruption: Identify the last sample vial that was run successfully. Check the vial number of the last successful chromatogram. Reset the parameter that identifies the first sample vial to the next vial number.
  • Page 80 Operation Using two injectors When you set up the run parameters, you must identify which data channel is for which injector. Different communication devices assign the position and data channel differently. • Using a 6890 Series GC, the channel is assigned when you set up the sequence.

  • Page 81: Without A Tray

    Operation Using two injectors Injection Number Front Injector Back Injector Vial 1 Idle Vial 2 Vial 1 Vial 3 Vial 2 Vial n Vial n-1 Last Idle Vial n Figure 44. Synchronous N-1 injection mode To inject the same sample into the front and back inlet in the same run, you must do the following: Prepare two sets of sample vials, two vials for each sample.

  • Page 82: Four Methods Of Control

    Operation Four methods of control Four methods of control There are a number of ways to control the automatic liquid sampler. Each controlling device allows different functionality when using the G1513A or 18593B injectors. Always check the manual of your chosen controlling device for exact feature sets.

  • Page 83: Examples Of Operation

    Operation Examples of operation Examples of operation This section describes the basic steps to set up your automatic liquid sampler using different methods of control. The following examples are for three specific systems with one injector module mounted over the front inlet. For more information on other types of configurations, see the manual of your controlling device.

  • Page 84: 6890 Series Gc Control

    Operation 6890 Series GC Control 6890 Series GC Control The following procedure allows you to configure the setpoints associated with the injector waste bottle and tower positions. Configure tower position Injector cables are connected to either the INJ1 (front) or INJ2 (back) port on the controller.

  • Page 85: Injector Parameter Setpoints

    Operation 6890 Series GC Control Injector parameter setpoints To enter injector setpoints: Press [Front Injector] or [Back Injector]. Scroll to the desired setpoint. Enter a setpoint value, or turn the setpoint on or off. *The Offset line appears only when “On” is selected. Sample tray setpoints Press [Sample Tray] to access the sample tray and bar code reader setpoints.

  • Page 86: Storing Injector Setpoints

    Operation 6890 Series GC Control Storing injector setpoints After setting up injector setpoints, sample tray setpoints, and bar code reader configurations, store them as part of a method. This method becomes a part of the sequence used to run the samples. Press [Method], and scroll to the method number you wish to use.

  • Page 87: Creating A Sequence

    Operation 6890 Series GC Control Creating a sequence A sequence specifies which samples to run and the stored method to be used for each. It is divided into subsequences, each of which uses a single method plus a priority sequence and postsequence events. The sequence definition control table is accessed by pressing [Seq].

  • Page 88: Storing A Sequence

    Operation 6890 Series GC Control When in the sequence control table, you will find the [Info] key useful if an explanation of sequence parameters is needed. Storing a sequence Up to five sequences can be stored. To store a sequence, press [Store][Seq]. This opens the Store Sequence control table.

  • Page 89: Starting/Running A Sequence

    Operation 6890 Series GC Control • Cancel the store, and return to the STORED SEQUENCES status table. Sequences can also be stored from within the STORED SEQUENCES status setpoint table by scrolling the cursor to the appropriate sequence number and pressing the [Store] key.

  • Page 90: Special Considerations When Using An Integrator With A 6890 Series Gc

    Operation Special considerations when using an integrator with a 6890 Series GC Special considerations when using an integrator with a 6890 Series GC The definitions of sequence are not the same in the 6890 Series GC and in the 3396 integrator. The following points must be considered when sequences are used with this GC/integrator combination: •...
  • Page 91 Operation Special considerations when using an integrator with a 6890 Series GC Figure 46 shows an example of the injector parameter portion of a method printout using a 6890 Series GC, a 3396 integrator, and a G1513A injector in the front position and a 18593B in the back position.

  • Page 92: 3396 Integrator With A 5890 Gc

    Operation 3396 integrator with a 5890 GC 3396 integrator with a 5890 GC Set the run time to 0.1 minutes by pressing [TIME] [.] [1] [STOP]. Begin the dialog to prepare a sequence by pressing the keys for [PREP] [SEQ]. Answer yes to INET SAMPLER CONTROL by pressing [Y] [ENTER].
  • Page 93 Operation 3396 integrator with a 5890 GC 10. Set the viscosity delay to zero. VISCOSITY --> Press [0] [ENTER]. 11. Set the sample size (injection volume) to 1 ml. VOLUME --> Press [1] [ENTER]. 12. Set the injection speed to fast. SLOW INJECTION -->...

  • Page 94: Checking Your Work

    Operation 3396 integrator with a 5890 GC Checking your work List the parameters by pressing the keys for [LIST][SEQ]. LIST: SEQ @ ALS INFORMATION INET SAMPLER CONTROL ..EQUILIBRATION TIME IN SECONDS . . 7673C SAMPLER: LOOP ADDRESS: ENABLE TRAY (1=YES)

  • Page 95: Multitechnique Chemstation Control With A 6890 Series Gc

    Operation Multitechnique ChemStation control with a 6890 Series GC Multitechnique ChemStation control with a 6890 Series GC The following is an example of the multitechnique ChemStation control of the G1513A injector in the front position and a 18593B injector in the back position with a 6890 Series GC.

  • Page 96: Washes

    Operation Multitechnique ChemStation control with a 6890 Series GC Washes Sample (preinjection) Number of times the syringe is rinsed with the next sample following any preinjection solvent washes. For each wash, the syringe is filled to eight-tenths its full volume (4 µl for the 5-µl syringe and 8 µl for the 10-µl syringe), and then emptied into a waste vial.

  • Page 97: Extended Injector Parameters Dialog Box

    Operation Multitechnique ChemStation control with a 6890 Series GC Injection Volume Injection Volume is the volume (in µl) of sample you want to be injected. The number of stops is automatically calculated based on your entry for injection volume and syringe size. You can indicate whether or not you are using a Nanoliter Adapter at the Injector Configuration dialog box.
  • Page 98 Operation Multitechnique ChemStation control with a 6890 Series GC Click on the [More...] button to display the Extended Parameters dialog box. Figure 51. Extended Injector Parameters dialog box Viscosity Number of seconds the syringe plunger should pause between the last pumping stroke and the injection stroke.

  • Page 99: Start A Run

    Operation Multitechnique ChemStation control with a 6890 Series GC PreInjection Dwell Time in hundredths of a minute for the needle to stay in the inlet before the plunger is depressed to inject sample. Valid entries: 0.00 to 1.00. PostInjection Dwell Time in hundredths of a minute for the needle to stay in the inlet after the plunger is depressed to inject sample.

  • Page 100: Standalone Control

    Standalone Control...

  • Page 101: Setting The Run Parameters

    Standalone Control Standalone control means using the automatic liquid sampler’s electronics to control its own operation. The controls are switches located above the START button of the injector module and are shown in Figure 52. The G1512A controller has two standalone configurations, synchronous and asynchronous. (For more information on configuring the controller, see “Installing the controller”...
  • Page 102 Standalone Control Setting the run parameters • Number of sample washes—There are two switches for 0, 2, 6, or 10 sample washes • On-column injection mode—There is one no/yes switch. • Number of solvent washes—There two switches for 0, 2, 6, or 10 solvent washes.
  • Page 103 Standalone Control Setting the run parameters Open the door to the injector control switches (where the start and stop buttons are located). The door hinge is on the left-hand side. sample solvent pre-wash post-wash col: One switch for changing the on-column injection mode Two switches for setting the number of solvent washes Figure 52.

  • Page 104: Sample Size

    Standalone Control Setting the run parameters Sample size Set the sample size with the two switches below the sample size label shown in Figure 53. The following table shows the injection volumes for each of the switch settings. Tenths of Syringe Volume Switch Setting Both up Left up, right down...

  • Page 105: Injection

    Standalone Control Setting the run parameters Injection Set this switch to specify the speed of the syringe plunger during the injection strokes and whether or not the syringe needle stays in the inlet after injection of the sample. This enables you to reduce the average speed of the plunger by a factor of 18 and, with a split/splitless inlet, hold the syringe needle in the inlet for 4 seconds after the injection.

  • Page 106: Number Of Injections Per Vial

    Standalone Control Setting the run parameters Caution The slow setting is only recommended for a few specific splitless and cool on- column applications. For most applications, set this switch to “fast.” A setting of “slow” for other applications may cause peak area discrimination and reduced quantitative precision.

  • Page 107: Number Of Sample Prewashes

    Standalone Control Setting the run parameters Number of sample prewashes Set the number of sample washes to 0, 2, 6, or 10 sample washes per injection. The following table shows the number of sample washes for each of the switch settings.

  • Page 108: On-Column Injection Mode

    Standalone Control Setting the run parameters On-column injection mode There are two injection modes: no (normal) and yes (on-column). Normal is used with packed and split/splitless inlets. On-column mode is used with on- column inlets and changes the carriage speed and the position over the inlet. Injection Mode Switch Setting Up or no...

  • Page 109: Number Of Solvent Postwashes

    Standalone Control Setting the run parameters Number of solvent postwashes Set the number of solvent washes to 0, 2, 6, or 10 solvent washes per injection. The table shows the number of solvent washes for each switch setting. Number of Solvent Washes Switch Setting Both up Left up, right down...

  • Page 110: Example Of Setting The Injector Switches

    Standalone Control Setting the run parameters Example of setting the injector switches Draw in the position of the switches for the following run parameters. sample injections size #/vial inj: fast slow Run parameters: • 1.5 ml with a 5 ml syringe •...

  • Page 111: Setting The Position Of The Last Vial

    Standalone Control Setting the run parameters Setting the position of the last vial When using a tray, the tray arm delivers sample vials starting from position 1 and continues to deliver vials until it cannot find the next vial in the quadrant. For example, if sample vials are in positions 1 to 10 and 15 to 30, the tray delivers samples 1 to 10 and then stops at position 11.

  • Page 112: Running The Samples

    Standalone Control Running the samples Running the samples This section describes starting and stopping a run or sequence and the movements of the automatic liquid sampler during a run when using standalone control. Starting a run or sequence Start the run or sequence by pressing the start button on the injector. What happens during a run? From the point when you start the sequence, the automatic liquid sampler does the following:...

  • Page 113: Stopping Or Interrupting A Run Or Sequence

    Standalone Control Running the samples the waste into both waste positions. During one run, it dispenses all of the waste into one position. During the next run, it dispenses all of the waste into the other position. If a tray is not installed, the injector takes all the washes from the solvent A bottle and expels the waste into the waste A bottle.
  • Page 114 Standalone Control Running the samples For more information, see chapter 5, “Preventive Maintenance and Troubleshooting.” The sampler does not remember which sample vial was associated with the interruption. When you restart an interrupted sequence, the sampler returns any vials that were left in the injector turrets and begins a new sequence. To restart the sequence from the point of interruption: Identify the last sample vial that was run successfully.

  • Page 115: Using Two Injectors

    Standalone Control Using two injectors Using two injectors Using standalone control, you can operate two injectors and a tray. The standalone configuration of a tray with two injectors has the following characteristics: • Input and output signals are shared. • The system sends only one INJECTOR READY signal to the GC when both injectors are ready and one START signal at the beginning of the injection stroke.

  • Page 116: Asynchronous Mode

    Figure 62. General-purpose cable (part no. 35900-60670) The asynchronous standalone control configuration with two injectors but without a tray is only supported by Agilent Technologies for isothermal analyses. Because there is no direct connection to the GC, this system only waits for readiness from an analog-to-digital (A/D) converter or other data handling device.
  • Page 117 Standalone Control Using two injectors sample injections size #/vial inj: fast slow solvent sample post-wash pre-wash col: Switch settings for the example on page 101: • 1.5 µl with a 5-µl syringe • 2 injections per sample vial • Injection set to “fast” •...

  • Page 118: Example Of Standalone Control Setup

    Standalone Control Example of standalone control setup Example of standalone control setup Set the GC to minimize the time between injections. Open the door to the injector control switches. sample injections size #/vial Number of Sample Vials inj: fast Align Mode sample injections size...
  • Page 119 Standalone Control Example of standalone control setup Set the number of injections per sample vial to one. injections #/ vial Set the number of sample washes per sample vial to two. sample pre-wash Left switch up, right switch down The number of pumps is preset to six. The viscosity delay is preset to zero.
  • Page 120 Standalone Control Example of standalone control setup Set the injection mode col: For a packed or split/splitless inlet, switch up For an on-column inlet, switch down...

  • Page 121: Checking Your Work

    Standalone Control Checking your work Checking your work Before you start the sequence, check the run parameters. Standalone control Check the injector control switches that you set. The switches should look like the following: sample injections size #/vial inj: fast slow solvent sample...

  • Page 122: Chapter 5 Preventive Maintenance And Troubleshooting

    Preventive Maintenance and Troubleshooting...

  • Page 123: Preventive Maintenance

    Preventive Maintenance and Troubleshooting Preventive maintenance This section contains some suggestions for ensuring good performance. The maintenance interval varies with the use of the instrument. Caution Do not use any lubricants on the automatic liquid sampler. They may affect the chemical performance of the GC and damage the instruments.

  • Page 124: Turret Exchange

    Preventive Maintenance and Troubleshooting Preventive maintenance • Clean the needle guide and nearby surfaces of the injector. Dust and dirt accumulate in these areas and can be picked up easily by the syringe needle and carried into the inlet. • Clean the sample vial inserts for the turret.

  • Page 125: Alignment Procedure

    Preventive Maintenance and Troubleshooting Preventive maintenance Restore power, and check for the green tower ready light. For proper needle depth in the sample vial, the syringe carriage height calibration must be carried out each time the turret is changed. See the following section, “Alignment procedure.”...
  • Page 126 Preventive Maintenance and Troubleshooting Preventive maintenance Remove the syringe, and carefully remove the needle support rod from the injector. Press the STOP button. The red LED will start flashing a double flash. Press STOP three times more, moving through displays of three, four, and five flashes.

  • Page 127: Troubleshooting

    Troubleshooting Troubleshooting Find the illustration in Figure 67 that best identifies your problem, and then turn to the appropriate page. For information on how to obtain service from Agilent Technologies, see page 147. Page Bent syringe needle Dropped sample vial...

  • Page 128: Bent Syringe Needle

    Preventive Maintenance and Troubleshooting Bent syringe needle Bent syringe needle When you find a bent syringe needle, check: • Was the syringe installed properly in the syringe carriage? • Was the syringe needle straight? Roll the syringe on a flat surface and watch the tip of the needle.

  • Page 129: Dropped Sample Vial

    Preventive Maintenance and Troubleshooting Dropped sample vial Dropped sample vial When you find a mishandled sample vial, check: • Are there folds or wrinkles in the crimp cap, especially near the neck of the sample vial? For more information, see “Crimp capping sample vials” on page 30.

  • Page 130: Chromatographic Symptoms

    Preventive Maintenance and Troubleshooting Chromatographic symptoms Chromatographic symptoms You may suspect a problem in the automatic liquid sampler based on what you see in a chromatogram or by comparing chromatograms. Each of the five parts of this section is named after a chromatographic symptom. Each part contains a list of possible causes and recommended solutions.
  • Page 131 Preventive Maintenance and Troubleshooting Chromatographic symptoms • The injector bracket is not aligned to the injection port. See the appropriate link manual that describes the installation. Syringe is worn or dirty If the syringe looks dirty or the plunger is sticking, clean the syringe with an appropriate solvent, or follow the syringe manufacturer’s cleaning instructions.
  • Page 132 Preventive Maintenance and Troubleshooting Chromatographic symptoms If this does not help and the sample is viscous, try the following: • Reset the viscosity run parameter. See “Viscosity delay” on page 60. • Use the tray quadrants to warm the sample. •...

  • Page 133: Contamination Or Ghost Peaks

    Preventive Maintenance and Troubleshooting Chromatographic symptoms Contamination or ghost peaks Figure 69. Contamination or ghost peaks Vial cap septum is dissolving in solvent Ghost peaks sometimes appear in the chromatogram when small pieces of vial septum material dissolve in the sample. Make several “blank” runs to determine the presence or absence of the ghost peaks.
  • Page 134 Preventive Maintenance and Troubleshooting Chromatographic symptoms Injection port septum is giving off volatiles Make several “blank” runs with a small piece of aluminum foil backing the inlet septum. If the contamination peaks disappear, they were probably due to the septum. Try replacing the septum you usually use with another type. Column is contaminated High molecular weight samples that contain residues may cause the syringe, the inlet liner, or the first few inches of column to become contaminated.

  • Page 135: Peak Area Discrimination (Smaller Or Larger Peaks Than Expected)

    Preventive Maintenance and Troubleshooting Chromatographic symptoms Peak area discrimination (smaller or larger peaks than expected) Automated injection C 34 C 10 Manual injection Figure 70. Smaller or larger peaks than expected You are comparing a chromatogram without needle fractionation against one with needle fractionation In the normal injection mode, the automatic liquid sampler uses fast injection to deliver a representative amount of the sample.
  • Page 136 Preventive Maintenance and Troubleshooting Chromatographic symptoms You are using a packed inlet and a 530-µm column Capillary columns used with packed inlets do have some inherent sample discrimination characteristics. See “Suggestions for packed inlets with 530-µm columns” on page 55. You are using a packed column Double-check the following: •...

  • Page 137: Sample Carryover

    Preventive Maintenance and Troubleshooting Chromatographic symptoms Detector response has changed Recalibrate the detector. Absolute response factors can change several percentage points during the day depending on the type of detector in use. Sample carryover Figure 71. Blank run showing carryover peaks Number or type of washes is insufficient Check the run parameters for the number of sample and solvent washes.

  • Page 138: No Signal/No Peaks

    Preventive Maintenance and Troubleshooting Chromatographic symptoms Syringe is worn or dirty If the syringe looks dirty or the plunger is sticking, clean the syringe with an appropriate solvent, or follow the syringe manufacturer’s cleaning instructions. If the syringe seems worn, replace it. Samples (vial-to-vial) are of immiscible types In this situation, the sample and solvent washes may not rinse the syringe properly.

  • Page 139: Fault Light Symptoms

    Preventive Maintenance and Troubleshooting Fault light symptoms Fault light symptoms Four light-emitting diodes (LEDs) on the injector indicate the status of the injector. Two LEDs on the controller module indicate the status of the controller and the tray if it is installed. During normal operation, the controller’s green LED and the injector’s green LED are on.

  • Page 140: Fault Light Locations, Colors, And Patterns

    Preventive Maintenance and Troubleshooting Fault light symptoms Fault light locations, colors, and patterns FAULT Yellow READY Green Yellow Green Figure 72. Location and pattern of LEDs during normal operation...
  • Page 141 Preventive Maintenance and Troubleshooting Fault light symptoms Throughout the rest of this section, an icon is used to represent the fault lights and beeps. The following are examples of the four basic patterns. A number indicates the number of flashes or double flashes that occur between the pauses.

  • Page 142: Responding To The Fault Lights

    Preventive Maintenance and Troubleshooting Fault light symptoms Responding to the fault lights Use the following instructions to try to solve the problem before obtaining Agilent service: Find the icon on this and the following pages that describes the LED pattern on the injector and controller. Read the information under the icon.

  • Page 143: Injector Door Open/Not Mounted

    Preventive Maintenance and Troubleshooting Fault light symptoms Injector door open/not mounted Probable causes • The injector door is open. • The injector is mounted incorrectly on the bracket. Suggested actions Ensure that the injector door is closed. Ensure that the injector is mounted properly. For more information, see “Installing the injectors”...

  • Page 144: Syringe Error

    Preventive Maintenance and Troubleshooting Fault light symptoms Syringe error Probable causes • The syringe carriage motor has a problem. • The syringe carriage cannot find its home position. • The syringe carriage sensor is inoperable. • The improper injection mode was used. For information on the syringe carriage home positions, see the Glossary.

  • Page 145: Turret Error

    Preventive Maintenance and Troubleshooting Fault light symptoms Turret error Probable causes • Something has interfered with the turret rotation. • The turret motor/encoder assembly is inoperable. • The turret type was changed without performing the alignment procedure on the injector. For information on the turret’s home positions, see the Glossary.

  • Page 146: Plunger Error

    Preventive Maintenance and Troubleshooting Fault light symptoms Plunger error Probable causes • The plunger carrier is out of position. • The plunger carrier sensor(s) is inoperable. • The plunger motor wires are disconnected. • The plunger carrier is operating incorrectly. •...

  • Page 147: Incomplete Injection

    Preventive Maintenance and Troubleshooting Fault light symptoms Incomplete injection Probable causes • There was an incomplete injection. • The plunger or syringe carrier is operating incorrectly during injection. Suggested actions If the syringe needle is bent, check the list of actions on page 119. Remove the syringe from the injector, and check the plunger for stickiness or binding.

  • Page 148: Bottle In Gripper

    Preventive Maintenance and Troubleshooting Fault light symptoms Bottle in gripper 3 beeps Probable cause • The sample vial was not delivered properly and stayed in the tray gripper. Suggested actions Remove the vial and return it to its position in the tray. Ensure that the tray quadrants are snapped into place.

  • Page 149: Hard Tray/Injector Error

    Preventive Maintenance and Troubleshooting Fault light symptoms Hard tray/injector error 4 beeps Probable causes • The tray is not able to move. • The injector is not responding to signals from the controller. Suggested actions Remove any obstructions from the tray that might keep the arm from moving through its full motion.

  • Page 150: Align Led Is On

    Preventive Maintenance and Troubleshooting Fault light symptoms Align LED is On Probable causes • The type of turret was changed without performing the alignment procedure. • The system was not initialized. • There is an injector memory error. • The injector main board was replaced. Suggested action Perform the alignment procedure.

  • Page 151: Other Patterns

    Preventive Maintenance and Troubleshooting Fault light symptoms Other patterns For any of the following patterns, obtain Agilent service. Probable cause There is an injector board failure. Probable causes • There is an injector memory error. • The injector main board is malfunctioning. Probable cause •...
  • Page 152 Preventive Maintenance and Troubleshooting Fault light symptoms Probable causes • The 18-V fuses have blown on the power supply board. • The 18-V supply is not operable. beep Probable cause ± • It failed the 13 V self-test. 2 beeps Probable cause ±...
  • Page 153 Preventive Maintenance and Troubleshooting Fault light symptoms 3 beeps Probable cause • It failed the fan self-test. Both fans failed. Probable causes • It failed the application test. • In service mode Alternating Flashes Continuous beep Probable cause • It failed the RAM test.

  • Page 154: Error Messages

    Preventive Maintenance and Troubleshooting Error messages Error messages This section is an alphabetical listing of possible error messages. BOTTLE NOT FOUND • The gripper did not find a sample vial in the injector turret during a removal attempt. DOWNLOAD NOT COMPLETE FILE TOO LONG •...
  • Page 155 Preventive Maintenance and Troubleshooting Error messages FRONT INJECTOR RESET ± • There is an interruption in the 18 V from the controller. Obtain Agilent service. FRONT INJECTOR DOOR OPEN/NOT MOUNTED • Go to page 134. REAR INJECTOR COMMUNICATIONS ERROR • There is a communications error between the rear injector and the controller.

  • Page 156: Contacting Agilent Technologies

    Obtaining Agilent Technologies service To obtain service, contact your local sales or support office. If you compile the following information before you call, Agilent Technologies can give you better service: •...

  • Page 157: Shipment Or Storage

    Preventive Maintenance and Troubleshooting Contacting Agilent Technologies Shipment or storage Original factory or authorized Agilent Technologies containers and packing materials should be used for either shipping or storage. If other packaging materials are used, they must meet the following requirements.

  • Page 158: Chapter 6 Special Topics

    Special Topics...
  • Page 159 Special Topics The automatic liquid sampler allows injection onto 250-µm and 320-µm columns in addition to 530-µm columns. This section explains how to adapt the GC and the automatic liquid sampler to use the smaller columns. Specifically, it outlines the following: •...

  • Page 160: Performing Cool On-Column Injection Onto 250-Μm And 320-Μm Columns

    Special Topics Performing cool on-column injection onto 250-µm and 320-µm columns Performing cool on-column injection onto 250-µm and 320-µm columns Installing the needle into the syringe barrel The stainless steel needles used for 250-µm and 320-µm injections must be inserted into a glass syringe barrel (part no. 5182-0836 [5 µl]). Select the correct needle for the column you will use.

  • Page 161: Checking The Needle-To-Column Size

    Special Topics Performing cool on-column injection onto 250-µm and 320-µm columns Checking the needle-to-column size You need to check the needle-to-column fit because some manufacturers provide columns with internal diameters that are too small. You will bend the syringe if you try to inject into a column that is smaller than the needle. You use the insert that is the same size as the syringe needle you will use in the analysis to verify that the column you plan to use is the correct size.

  • Page 162: Preparing The Cool On-Column Inlet

    Special Topics Performing cool on-column injection onto 250-µm and 320-µm columns Insert the column into one end of the insert as shown in Figure 75. Syringe Insert Column Figure 75. Checking the needle-to-column size Insert the syringe needle through the other end of the insert and into the column.
  • Page 163 Special Topics Performing cool on-column injection onto 250-µm and 320-µm columns the size of the column and syringe needle you will use. (See the previous section to identify the correct insert.) Use the following steps to remove an incorrect insert and to install a new one: Lower the temperature of the GC oven.
  • Page 164 Special Topics Performing cool on-column injection onto 250-µm and 320-µm columns Replace the spring on top of the insert. Figure 76. Inlet assembly You will align and install the inlet septum nut in the next section. Aligning the septum nut For 250-µm and 320-µm on-column injections, the septum nut requires a 5-mm through-hole septum.
  • Page 165 Special Topics Performing cool on-column injection onto 250-µm and 320-µm columns Turn the needle over. Insert the wire, inlet septum nut and through-hole septum into the inlet. Step 1 Step 2 Inlet septum nut This end is inserted into the inlet Needle This end is inserted into...
  • Page 166 Special Topics Performing cool on-column injection onto 250-µm and 320-µm columns WARNING Flying glass particles can cause eye injuries. Always wear safety glasses when cutting fused silica columns. 1. Score the column with a carbide knife. 2. Support opposite score 3.

  • Page 167: Using Retention Gaps And Other Precolumns

    Special Topics Performing cool on-column injection onto 250-µm and 320-µm columns on-column injections. If this is the case, reinstall the insert and the column. Syringe 12 mm or less Septum nut Figure 79. Verifying column installation If you are using a retention gap, read the following section. Using retention gaps and other precolumns Precolumns are columns connected in front of the analytical column.
  • Page 168 Special Topics Performing cool on-column injection onto 250-µm and 320-µm columns retention gap. The retention gap should be wetted by the solvent, which means it should be deactivated with a material of similar polarity. Fused silica tubing is commercially available in a range of diameters and deactivations. Press-fit connectors Press-fit connectors are easy-to-use, general-purpose connectors for coupling capillary columns of the same or different diameters.

  • Page 169: Preparing The Injector

    Special Topics Performing cool on-column injection onto 250-µm and 320-µm columns each other inside the ferrule during tightening, exposure to ferrule material is minimized. Purged connectors Purged connectors are commercially available for column connection. The most complex of connector types, they purge the connection area and, thus, minimize contamination.
  • Page 170 Special Topics Performing cool on-column injection onto 250-µm and 320-µm columns Swing the syringe latch counterclockwise to unlock the syringe. Plunger carrier Plunger carrier screw Slide Flange guide Hold here to remove Syringe latch Syringe clip Needle support foot Figure 80. Removing the needle support assembly With your finger under the upper portion of the syringe barrel (just above the syringe latch), pull the syringe up, and gently remove it.
  • Page 171 Special Topics Performing cool on-column injection onto 250-µm and 320-µm columns Caution Be careful not to pull the assembly by its metal shaft. The shaft is easily bent. Installing the 250/320-µm needle support assembly Hold the new needle support assembly in your right hand, and insert the upper end of the rod into the plastic guide to the right of the plunger carrier.
  • Page 172 Special Topics Performing cool on-column injection onto 250-µm and 320-µm columns Push the assembly gently down into place. Make sure the slide lies flat on syringe carriage so that it glides up and down the tracks as shown in the illustration below.
  • Page 173 Special Topics Performing cool on-column injection onto 250-µm and 320-µm columns Pass the syringe needle through the hole of the small needle guide in the needle support foot as shown below. Needle guide Figure 83. Needle support for 250-µm injection Align the syringe flange with the flange guide and syringe clip, and gently press the syringe into place, keeping the needle in the hole of the needle guide.

  • Page 174: Replacing The Needle Guide In The Needle Support Foot

    Special Topics Performing cool on-column injection onto 250-µm and 320-µm columns Check to make sure the needle is aligned with the needle guide in the foot by moving the slide up and down. The needle should slide smoothly in the needle guide.
  • Page 175 Special Topics Performing cool on-column injection onto 250-µm and 320-µm columns Remove the small metal plate from the foot. Remove the needle guide, and replace it with a new one. Replace the metal plate. Replace and finger-tighten the screw. Finish tightening the screw with a 2-mm Allen wrench. Screw Metal plate Needle guide...

  • Page 176: Troubleshooting 250-Μm And 320-Μm Systems

    Special Topics Performing cool on-column injection onto 250-µm and 320-µm columns Troubleshooting 250-µm and 320-µm systems Symptom Possible Cause Corrective or Preventive Action Bent needle Incorrectly installed needle Check needle support assembly installation. support assembly Defective needle Check each syringe before installation to make sure the needle is straight.

  • Page 177: Controlling Sample Vial Temperatures

    Special Topics Performing cool on-column injection onto 250-µm and 320-µm columns Symptom Possible Cause Corrective or Preventive Action Poor precision, Worn syringe barrel Replace the syringe. poor repeatability, or large standard deviation Loose removable needle Make sure the syringe barrel caps are screwed on tightly and that the Teflon disk is wrapped tightly as shown in this chapter.
  • Page 178 Special Topics Performing cool on-column injection onto 250-µm and 320-µm columns Caution Ensure that the drainage tube is attached to the base of the tray, and remove any modules from underneath the tray. When controlling for a low sample temperature with a high ambient temperature or high humidity, water condensation from the quadrants and tray could damage equipment under the tray.
  • Page 179 Special Topics Performing cool on-column injection onto 250-µm and 320-µm columns Connecting the tray quadrants The recommended plumbing used to connect the tray quadrants is shown in Figure 87. Use 6.35-mm id (1/4-in.) tubing. TEE manifold Figure 87. Tray quadrant plumbing Calculating the water bath temperature The temperature of the sample vials depends on several factors, including the ambient temperature of the air around the tray and the temperature of the...
  • Page 180 Special Topics Performing cool on-column injection onto 250-µm and 320-µm columns Caution If the sample temperature is critical for accuracy, experiments should be performed to validate water bath settings. Actual heat transfer varies with vial material, humidity, condensation on the vial, and flow rates. To calculate the temperature needed for the water bath, complete the next four tasks.
  • Page 181 Special Topics Performing cool on-column injection onto 250-µm and 320-µm columns From the intersection of desired vial temperature and ambient temperature, draw a vertical line down to the x-axis of the graph and read the temperature needed for the water bath. 40 C 30 C 25 C...
  • Page 182 Special Topics Performing cool on-column injection onto 250-µm and 320-µm columns Caution Do not allow the inlet pressure and inlet temperature to exceed these limits. If you operate the bath outside this range, the quadrants could be damaged and cause sample vial delivery problems. Inlet Pressure (psi)

  • Page 183: Tray Control Commands

    Special Topics Performing cool on-column injection onto 250-µm and 320-µm columns • If you use a built-in pump, it must be suitable for external circulation of liquid and for connection of 6.35 mm id (1/4-inch) tubing. • If you use a pressure pump, it must maintain a pressure between 1.5 and 2.5 psi.
  • Page 184 Special Topics Performing cool on-column injection onto 250-µm and 320-µm columns • The firmware in the controller evaluates your commands. If there are no syntax errors, the tray responds with A NO ERRORS. If there are syntax errors, the tray responds with A and a description of the error. Syntax and description MOVE x,y Picks up the bottle in position x and places it in position y.
  • Page 185 Special Topics Performing cool on-column injection onto 250-µm and 320-µm columns MANUAL The MANUAL SEQUENCE command bypasses the normal SEQUENCE sample sequencing performed by the automatic liquid sampler. Once manual sequencing mode has been activated, it is possible to manipulate sample bottles, moving them to and from the injectors with the MOVE command, and then inject from the bottles currently in the injectors simply by starting a sequence.
  • Page 186 Special Topics Performing cool on-column injection onto 250-µm and 320-µm columns TURRET x,y The turret position values may be any integer from 0 to 10. When either value is omitted, that turret is not affected by (continued) the command. If both are omitted, the command performs no function.
  • Page 187 Special Topics Performing cool on-column injection onto 250-µm and 320-µm columns Example program with a bar code reader and tray This program illustrates the following: • Using bar code reader commands to read a bottle label • Examining the bar code reader message for a specific character and agitating the sample if it is found •...
  • Page 188 Special Topics Performing cool on-column injection onto 250-µm and 320-µm columns PRINT PRINT "ENTER THE INET ADDRESS OF THE SAMPLER." INPUT AD REM ***** SET THE AUTOMATIC LIQUID SAMPLER TO MANUAL OPERATION INET_IO AD,"MAN",JUNK$ REM ******************************** SET UP THE VIAL SEQUENCE PRINT "ENTER THE FIRST VIAL NUMBER:"...
  • Page 189 Special Topics Performing cool on-column injection onto 250-µm and 320-µm columns PRINT " BEGIN ANALYSIS" PRINT " "&RESP$ PRINT "==============================" PRINT IF POS(RESP$,"+")<>0 THEN INET_IO AD,"AGIT",JUNK$ INET_IO AD,"MOVE EXT3,FRONT",JUNK$ START SEQ_NOW INET_IO AD,"MOVE FRONT,"&STR$(I),JUNK$ PRINT "==============================" PRINT " END ANALYSIS" PRINT "...
  • Page 190 Glossary...

  • Page 191: Glossary

    Glossary angular axis: the direction describing the rotation (clockwise and counterclockwise) of the tray’s arm. The tray uses this motion to place the vial gripper above a group of five vials or in the proper orientation to the bar code reader or injector turret.
  • Page 192 Glossary Reducing the amount of vaporization from the needle may result in unexpected changes in your chromatogram. • The peak areas of your chromatograms may be smaller. Automatic fast injection delivers the desired setpoint volume of sample. Without fast injection, residual amounts of sample boil out of the needle and enter the inlet.
  • Page 193 Glossary For more information on the performance of the automatic liquid sampler, order the following technical papers from your Agilent representative: Publication No. 43-5953-1843: Snyder, W. Dale. Fast Injection with the HP 7673A Automatic Injector: Chemical Performance, Technical Paper 108, June 1985. Publication No.
  • Page 194 Glossary home positions: each of the moving parts has a reference point from which it moves to pick up, deliver, or inject samples. The parts move to their home positions between each run, when power is turned on, and when a run is started.
  • Page 195 Glossary homing: the process of the turret, syringe carriage, syringe plunger, vial gripper, and tray arm moving to their home positions. INET: an acronym which stands for instrument network. injection: the injector motion that delivers the sample to the inlet or column of the gas chromatograph.
  • Page 196 Glossary radial axis: a direction describing the horizontal (forward and backward) movement of the tray’s arm. The tray uses this motion to position the vial gripper at the correct distance from the center of the tray. See also home positions. retention time: the time it takes from the moment of injection until a compound elutes and is detected at the peak maximum.
  • Page 197 Glossary The third chromatogram shows the result of washing the syringe with four solvent washes. The carryover peaks disappear. Sample #1: 20 mg/ml of solute in methanol Sample #2a: Methanol blank without washes Carryover peaks Sample #2b: Methanol blank after 4 washes septum bleed: the inherent baseline noise level emanating from a column due to decomposition or volatilization of low molecular weight products mainly from the stationary phase.
  • Page 198 Glossary sequence: a set of instructions that defines how a piece of equipment, for example an integrator, performs more than one automated run. These instructions usually include the automatic liquid sampler parameters, instrument equilibration time, method name, and a sample information table. Note that sequences can be recursive, that is, one sequence can contain another sequence.
  • Page 199 Glossary...

  • Page 200: Index

    Index Numerics 250-µm/320-µm on-column injections, 151 cables 3396 integrator, operating with a 5890 GC, 83 injector cable, 21 530-µm on-column injection, 55 tray cable, 22 6890 GC calculating the water bath temperature creating a sequence, 78 See water bath temperature examples, 74 capillary column, 182 injector setpoints, 76...
  • Page 201 Index examples estimating the maximum number of detector response, 128 sample vials, 41, 43, 46 drainage tube fitting, 169 standalone control, 100 dropped sample vial, 120 tray control commands, 178 dual injectors description, 70 mounting, 11 standalone control, 106 fan, turning on/off, 34 synchronous injection, 72 fast injection with a tray, 70...
  • Page 202 Index injection mode inlet septum, replacing, 54 normal mode, 63 inserts, inlet, 152 on-column mode, 55, 63 integrator injection parameters See 3396 integrator See run parameters interaction, 186 injection port See inlet injection volume, 29, 60 injection, definition, 186 leaks, 127 injections See also inlet, 121 250-µm and 320-µm, 150...
  • Page 203 Index on-column injection mode, 77 radial axis, 187 operation relative humidity range, 5 examples, 74 replace needle guide, 165 starting, 69 retention gaps, 158 stopping or interrupting, 69 retention time, 187 run, 187 run parameter description, 59 injection, 96 P6 jumper switch, 35 injections per vial, 59, 97 packed inlets, with 530-µm columns, 55 number of solvent A and B washes, 60...
  • Page 204 Index septum bleed, 188 septum life, 188 sample, 187 sequence, definition, 189 sample carryover, 47, 128 service, 147 definition, 187 setpoints sample insert, 102 sample tray,6890 GC, 76 sample size shipping requirements, 148 See injection volume slide, 163 sample stability, 122, 125 slow injection, 61 sample tray setpoints slow plunger, 62...
  • Page 205 Index synchronous injection, 72 turret, 176 synchronous mode, 106 controlling sample vial temperature, 168 syringe description, 13 bent syringe needle, 119 drainage tube fitting, 169 injection volumes, 50 installing, 13 inspecting, 51 mounting, 15 installing, 52 tray lock, 15, 16 installing into the foot, 163 tray quadrant nanoliter injection, 51...
  • Page 206 Index washes ChemStation, 87 waste bottle, limited volume, 40 waste bottle limited volume, 42 water bath pressure range, 172 pump requirements, 173 temperature range, 172 water bath temperature, 170...
  • Page 207 Index...

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