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Koehler K87170 Operation And Instruction Manual

Automatic vacuum distillation system
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K87170
Automatic Vacuum Distillation System
Operation and Instruction Manual
Koehler Instrument Company, Inc.
1595 Sycamore Avenue • Bohemia, New York 11716-1796 • USA
Toll Free: 1-800-878-9070 (US only) • Tel: +1 631 589 3800 • Fax: +1 631 589 3815
http://www.koehlerinstrument.com • e-mail: info@koehlerinstrument.com
Petroleum Testing & Analysis Instrumentation • Custom Design & Manufacturing

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Summary of Contents for Koehler K87170

  • Page 1 K87170 Automatic Vacuum Distillation System Operation and Instruction Manual Koehler Instrument Company, Inc. 1595 Sycamore Avenue • Bohemia, New York 11716-1796 • USA Toll Free: 1-800-878-9070 (US only) • Tel: +1 631 589 3800 • Fax: +1 631 589 3815 http://www.koehlerinstrument.com •...

  • Page 2: Table Of Contents

    Contents General Information ....................... 1-1 Description of Equipment ....................2-1 System Preparation ......................3-1 Operating the Controller ....................4-1 Performing a Distillation ....................5-1 Maintenance and Trouble Shooting................6-1 Replacement Parts......................7-1 Glossary..........................8-1...

  • Page 3: General Information

    Requirements for Installation of Automatic D1160 System Electrical Requirements. Two single phase 120 or 220/240 VAC., 50 Hz/60 Hz, dedicated electrical outlets within 3 feet of the installation site. The amperage required depends on the particular system ordered. Please specify Voltage and Hz when ordering. The electrical power must be clean.
  • Page 4 Freight This equipment is very fragile. There are many delicate glass pieces and electronics packed with the unit. Koehler takes great care and expense in packing this equipment. The customer should take all possible precautions to ensure that the equipment is handled carefully and given a smooth ride during shipment. Keep in mind that this is a very delicate and valuable piece of equipment.
  • Page 5 Cautions Read all instructions carefully before unpacking your system. Installation and training is provided by a trained technician. All operators should be trained in the safe and proper operation of the system. Training is provided during installation, but you may feel that more training is necessary at a later date. To arrange for further training, please contact us.
  • Page 6 Equipment Description Description Fully Automatic D1160 Components Figure 1 Vapor Temperature Probe: This temperature probe measures the actual vapor temperature. Pot Temperature Probe: This temperature probe measures the temperature of the liquid in the pot flask. Controller: Controlls the distillation system and includes display and keyboard. IBP Sensor: Automatically detects first drop (Initial Boiling Point).
  • Page 7 Equipment Description 2-2...
  • Page 8 Equipment Description 2-3...

  • Page 9: System Preparation

    System Preparation Preparing the System Operational Checks 1. Check the condenser bath level. The level should be maintained above the coil inside the bath. 2. Verify that a clean receiver is in place and empty. The metal drip trough should be pointing directly to the front of the unit.
  • Page 10 Software Operation General The D1160 control software is designed to make vacuum distillation as easy as possible. The Main Screen is displayed when the program is started. It gives various options for common tasks Manual Controls: This area is used for manually operating all aspects of the equipment. The vacuum pump, bath, level follower and so forth can be manually operated.
  • Page 11 Start Vacuum Distillation: This area is used to start a vacuum distillation run. System Options: This area is used to turn on/off the various options available with this equipment Start Cleaning Run: This area is used to start a cleaning cycle. Calibration: This area is used to calibrate the pressure, temperature and volume measurements.
  • Page 12 Vacuum Control area is used for testing the vacuum system. Once the pump is turned on enter the desired vacuum level in the Set Point field. The current pressure can be viewed in the Pressure field. The Condenser Bath can be turned on by checking the box next to the word Power. Enter the desired temperature in the Set Point field.
  • Page 13 Manage Run Data To edit or create a distillation program select LOAD from the File menu. Select the desired program from the list. Operating the Microprocessor Controller 4-4...
  • Page 14 Edit the parameters as desired and then save the distillation program with the desired program name. a. Pressure Set Point: the range is 1 to 50 mmHg. The default is 10 mmHg. b. Initial Heat Rate: This is the amount of heat that will be applied to the pot flask until the first drop is detected.
  • Page 15 f. Condenser Temperature: Set the temperature of the condenser coolant to at least 30 ºC below the lowest vapor temperature to be observed in the test. A suitable coolant temperature for most distillations is 60 ºC. g. Pressure Step Down Rate: This the rate at which pressure will be reduced before the distillation begins.
  • Page 16 “Hidden” Parameters There are some parameters that rarely need adjustment. These are normally “hidden” from view to avoid clutter and confusion. To view or edit the parameters, click the Show Tunig Parameters button. Then these parameters will be visible. There are 3 sets of PID control parameters for the automatic vacuum control.
  • Page 17 Operating the Microprocessor Controller 4-8...
  • Page 18 Print and View Results The primary Print and View Results Screen is below. The Print Volume Graph button allows a graph of Temperature versus Volume to be printed. The View Volume Results button allows the temperature versus volume data to be viewed.
  • Page 19 System Options System Options for the fully automatic D1160 should be set as seen below. Operating the Microprocessor Controller 4-10...
  • Page 20 Calibration The main calibration screen has options for calibrating temperature, pressure and volume. Operating the Microprocessor Controller 4-11...
  • Page 21 Temperature Calibration Operating the Microprocessor Controller 4-12...
  • Page 22 Pressure Calibration Operating the Microprocessor Controller 4-13...
  • Page 23 Volume Calibration Calibration of the receiver volume is performed from the screen shown above. 1. Put the empty receiver in place and select Find Base. 2. After the level follower finds the base, select Stand By. 3. Remove the receiver and use a class A pipette to deliver a known volume of toluene into the receiver.
  • Page 24 8. Click on the File menu in the upper left hand corner of the screen and select Save File. 9. Enter the file name of VCal.dat and click on Save. 10. Now the calibration data is saved. You can check the calibration in Manual Controls.

  • Page 25: Performing A Distillation

    Performing a Distillation 1. From the density of the sample determine the weight, to the nearest 0.1 gram, equivalent to 200 ml of the sample at the temperature of the receiver. Weigh this quantity of oil into the distillation flask. Add boiling chips. 2.
  • Page 26 9. Using the file menu choose LOAD Performing a Distillation 5-2...
  • Page 27 10. Then choose the desired distillation program from the list. Performing a Distillation 5-3...
  • Page 28 11. Once the program is selected, the distillation program will begin. You will be prompted for a folder name where the results will be stored. The default folder name is the current date and time. This may be changed as desired. The name must have letters and numbers only.
  • Page 29 13. Once the distillation has started the following screen will by displayed. On the left side of the screen is a display of the results for this distillation including IBP (Initial Boiling Point), various distillation points and the FBP (Final Boiling Point). On the right side is a list of the control parameters.
  • Page 30 Distillation Rate KP is a proportional control constant for the distillation rate control. If you are having problems with distillation rate control contact Koehler Instrument or your local representative for advice. Distillation Rate KI is an integral control constant for the distillation rate control.
  • Page 31 At the bottom of the screen is a display of the current system status. Pot Temperature field displays the liquid temperature in the boiling (pot) flask. Vapor Temperature field displays the vapor temperature in the distillation column. Vapor AET field displays the current atmospheric equivalent temperature of the head (vapor).
  • Page 32 19. If a sudden increase in pressure is observed, coupled with the formation of white vapors and a drop in the vapor temperature, the material being distilled is showing significant cracking. Discontinue the distillation immediately and record the fact. If necessary, re-run the distillation with a fresh sample at a lower operating pressure.
  • Page 33 Other display options during distillation. By Clicking on the screen, different screens can be viewed during the distillation. Graph Display 1 Atmospheric Equivalent Vapor Temperature vs. Volume % Graph Display 2 Vapor Temperature, Pot Temperature and Atmospheric Equivalent Vapor Temperature vs. Time Performing a Distillation 5-9...
  • Page 34 Process Diagram Display Performing a Distillation 5-10...
  • Page 35 Run Data Performing a Distillation 5-11...

  • Page 36: Maintenance And Trouble Shooting

    Maintenance Schedule Daily  Follow pre-run checklist  Carefully document any abnormalities in operation  Grease Vapor Probe Connection  Check Condenser Bath Coolant Level  Check Vacuum Pump Oil Level  Check all glassware for scratches, chips or any defects and replace immediately ...

  • Page 37: Replacement Parts

    If any items need replacement, please contact us or your local distributor. Description Part # Glassware 200 ml Receiver K87170-1 500 ml Borosilicate Pot K87170-2 Flask 500 ml Quartz Pot Flask K87170-3...
  • Page 38 Trouble Shooting Problem Solution Poor Distillation Rate Control Drip trough not in place or not turned so it faces forward. Distillation Rate kP too high Distillation vapor temperature appears too high Vapor temperature probe holder nut not tightened enough. Temperature probe is getting “sucked” down.

  • Page 39: Glossary

    Glossary AET: Atmospheric equivalent temperature is the temperature adjusted for pressure. Atmospheric pressure: Unit of pressure equivalent to 760 torr (mm Hg). Boil up: The point at which reflux begins in the head of the still. The vapor temperature will rise rapidly as this occurs. Charge: The sample in the pot flask to be distilled.