| Douglas Instruments Version 1.1
 Optimization - using
microbatch
 Step by Step Instructions for Beginners
 Hardware Preparation 
   
    Use a ground glass syringe or pipette to dispense 6 ml
      of light paraffin oil into a Nunc HLA plate. Tip the plate and remove 4.5 ml of excess
      paraffin, leaving paraffin in the wells. Place the Nunc HLA plate in the left side of the
      stainless steel frame on the Plate Loader as shown below. 
	 
    Connect a 5-channel Microtip to the 5 channels
      of IMPAX. Place the tip in the 5-channel "collet" on the Z-arm of the Plate
      Loader. Place a small glass vial under the tip to collect waste.Fill the ground glass syringes of the upper valves
      with degassed pure water and replace them. 
	 Creating an Experiment File  
    Switch on the computer, and wait until XTGOLD is
      loaded. Move to the directory where you want to keep your optimization files (e.g.
      C:\EXPTS\X-FILES) and press F9. Select "XSTEP - Optimization" from
      the menu. (Alternatively you can enter XSTEP at the DOS prompt.)The Main Menu of XSTEP will appear. If you want to
      create a new file, select Files, then New File and provide a
      name for the new file (8 letters or numbers, with no extension.) 
    Alternatively, to work with an existing file, select Files,
    then Load a File. Type in the directory that you want (if it does not
    appear) and press Enter. Move the cursor to the file that you want, press Enter
    to select it, and then Enter to load it.  Finally, press Esc to return to the previous menu. 
    If you have created a new file, or if you want to
      modify the names or concentrations of the stock solutions of an old file, press I
      to select the Ingredients option. Press A (or S or D for a pH
      experiment), then modify the concentrations and names of the ingredients displayed. Fill
      in the viscosities of PEG solutions etc. As a guide, the viscosity of 40% PEG 8K is 40,
      while the viscosity of water is 1. Finally, press Esc, Y (to keep the changes) and
      Esc to return to the Main Menu.The simplest type of dispensing is when the
      "Laying On" option is disabled. Select Dispensing Parameters. If Laying
      On is enabled, press L. Press Esc to return to the Main Menu. (If you do
      use Laying On, you must use the Laying On tool to remove excess oil - see Laying On in the
      Protein Crystallization manual.)From the main menu, select Spreadsheet.
      Each group of numbers shows the concentrations of the 5 ingredients in a well. Move to a
      well and press Enter to edit its values. To interpolate values between the two most
      recently edited wells select Interpolate. To optimize around a point, select
      Expand. See "Spreadsheet" in the manual for other options. When
      the experiment is ready, select Save to save it to disk. Finally press
      Esc to return to the Main Menu Liquid Handling Calibration 
    Move the cursor up to the flashing option entitled
      "CALIBRATION NECESSARY", and press Enter. Turn the valves to the
      positions shown, and press R. The positions of the motorized syringes are now shown.
      If you suspect that any motor positions are not correct, press Z, then S to
      rezero the syringes, and P to rezero the Plate Loader. Finally press Esc.At the beginning of each day the system will require
      debubbling. Place a small bottle or vial under the Microtip in the Z-arm and press D.
      Press Enter to start debubbling. After about five seconds press Enter again.
      Any air bubbles that were present at the top of the motorized syringes should have passed
      out into the connecting tubing. Now remove the air bubbles from the connecting tubing
      as follows:- Remove the PTFE tubing from the needles of debubbled motorized syringes.
 - Expel water and air bubbles from the tubing using the ground glass syringe.
 - Reconnect the tubing carefully, ensuring no air bubbles re-enter.
 When this is completed, press P.
 
    If there are bubbles between the upper and lower valves, turn the top
    valves to the flush position (|- ) and flush the
    bubbles out through the microtip with the ground glass syringes. Then return the top
    valves to the fill position ( l ). 
    A routine for preparing the motorized syringes appears. Motorized
      syringes 2 - 5 should be moved to their lowest positions to be ready to dispense buffers,
      etc. Motorized syringe 1 should be nearly empty so that it will be ready to suck up
      protein solution. Press P again to move syringes to these positions. When the
      syringes stop moving, press any key.You should now manually flush the bores of the microtip with
      solutions. The microtip acts as a reservoir of solution. Press Y, turn the valves
      to the positions shown, and press R. Using disposable syringes, flush all bores
      with water. Leave water in the channels 1 and 5. Flush the other channels with air, then
      the appropriate ingredient. Press any key, again turn the valves to the positions shown,
      and press R.You should now have returned to the Main Menu. If you suspect that the
      5-channel Microtip is not set to the correct height select Liquid Handling.
      Press A to select Adjust/Change Microtip. The arm will move to its lowest
      position. Follow the instructions on the screen: (1) adjust the height of the Microtip
      until it is just touching the table. (2) Tighten the collet. (3) Mark the height by
      moving the two o-rings down to the top of the collet. Press Esc to return to the
      Main Menu. Execution of the Experiment 
    From the main menu, select Spreadsheet. To execute the
      experiment, press the Caps Lock key to obtain a new (red) menu. Ensure that there
      is no droplet on the end of the Microtip. Then press L to load protein, and press
      Enter four times to accept the default settings and load air. (The air separates the
      protein to be loaded from the water in the Microtip.) Undo the thumbscrew securing the
      Microtip, remove the Microtip from the Plate Loader, and place the tip into protein
      solution, avoiding any precipitate. Press any key to load the protein. Replace the
      Microtip in the Z-arm of the Plate Loader and tighten the thumbscrew.Press X to execute the experiment automatically. This will
      take about 5 minutes for 24 wells. On completion, press Y to save the file if you
      have not already done so. If you have a printer attached to the computer, press Y
      again to get a report print out. Release Caps Lock.Add 5 ml paraffin
      to the HLA plate (or 5 ml 50:50 silicone and paraffin mixture to allow slow evaporation).
      Place the plate in an incubator at the desired temperature.You must not turn off your computer without quitting XSTEP or the
      motor positions will be lost. To quit XSTEP press Esc until you reach the main
      menu. Press Esc again, then Q. Note: The valve positions shown here indicate the desired
connections between the three valve ports. For the old-style valves with levers, the lever
should point to the blocked port. For example, the flush position ( |- ) corresponds to the lever pointing to the left ( ==o ) on an old-style valve. 
 |