From the Box to Packing in 30 minutes Pack-in-a-Box components • Remove components and assemble bracket as shown • Follow the instructions to pack your first column and learn how to use the system Additional Equipment & Chemicals • • • • • • • • • • • • ¼” wrench 5/8” wrench 7/16” wrench Phillips head screwdriver 30ml beaker Waste container Methanol Chloroform Spatula Balance Computer Ultrasonic bath Column Packer Assembly • Pre assembled for supplied SSI column hardware. Mounting Packing Stand to Pump • Screw stand to side of pump using the two #6 screws provided. Plumbing the Pump Priming pumps Use MeOH for this column • Open prime purge valve press prime button • With prime purge valve open use the supplied syringe to draw solvent through the pump • Prime pump • When pump is primed close the prime purge valve Packing Ring Seal Installation • Place ring in adapter as shown • Make sure ring is flat in bottom of adapter Packer Mounted to Stand • Mount packer to stand and tighten wing nuts • No wrenches are required to seal reservoir • Hand tighten end nuts Column Assembly • Assemble lower fitting of column and add frit to top end fitting and set aside to put on column after it is packed. System Assembled Correctly • The use of the Quick-Set software is not required but gives the most flexibility and will be used for this example Installing Quick Set • Insert Disk • Run the Quick-Set “setup.exe” program file & follow prompts. • Due to the many versions of Windows in use, your PC may have newer files than the ones being loaded. You will be prompted for a course of action, when in doubt, “keep” your existing files or “ignore” other messages. • Connect RS 232 Cable provided to the computer and pump • Turn on pump Click QuickSet • Go to Start/Programs • Click on Quick-Set • The screen below appears with the information on the program Automatic Set Up Initial screen is for locating the SSI / LA pump If communication does not initialize or if the pump is not on this list: Click on the “Poll Com Port For Device” button. This will scan 9 possible PC COM ports for the attached device. When the device is found, click on the” Continue” button. Getting To CP Screen Setting Flow and Pressure • Set to pressure limited ramp and click ‘send’ • Set upper pressure to 9999 psi; click ‘send’ • Set lower pressure to 0 psi; click ‘send’ • Set ramp speed to 100; click ‘send’ • Set max flow and pressure from table Adding Steps Packing program to load Pressure Flow Rate Time 9000 24 1 9000 23 5 9000 22 30 Send to pump Saving Your Packing Program • Click on “Save Settings” • Enter file name • Save Mounting Column • Make sure packing ring seal is in adapter • Hand tighten column in adapter • Place plug in bottom of column • Remove plug just prior to starting pump Tighten Column on Packer • Use a ¼” wrench and 5/8” or adjustable wrench to snug column to packer • Do not over tighten ¼ turn past snug is fine • Fill column with 3 mL MeOH Setting up Graphing and Data Collection Saving Packing Data • Select Log data • Give file a name Making the Slurry • Weigh 3 gm of silica into 30 mL beaker • Add 20 ml of 50:50 Chloroform:Methanol (Straight MeOH can be used but is not as efficient) • Use a spatula to break up packing • Place in ultrasonic bath until uniformly dispersed • Pour in packing reservoir as soon as possible and pack column Adding Slurry • Use 20 mL of silica slurry and pour carefully into reservoir • Fill reservoir with washings of beaker and close Is It Closed? • Make sure the reservoir is full with slurry • Remove silica from threads • Hand tighten top nut Make Sure You Are Ready • Is the program loaded? • Is the pump primed? • Is there a waste collection vessel below the column? • Did you tighten the fittings? • Is there slurry in the reservoir and is the reservoir closed? • Are you set to graph the process and save your data? • If so, proceed Packing The Column • To run program, click on “Pump;” or if program is loaded click on “Start” Initial Packing Profile Running a Column Packing Profile Removing the Column • Stop the pump and let the pressure drop to 0 psi • Carefully unscrew the column, and using a flat spatula or razor blade, remove excess silica • Remove silica from threads if present • Place end fitting and frit on column and seal Removing Excess Silica • Work quickly with a spatula edge or razor blade Getting Ready to Pack Again • Pump remaining silica from precolumn for reuse or disposal • Empty reservoir • Install next column and repeat steps