Koehler K87170 Guide

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: [phone] • Fax: [phone]
http://www.koehlerinstrument.com • e-mail: [e-mail]
Petroleum Testing & Analysis Instrumentation • Custom Design & Manufacturing

ii
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

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. Fluctuations in the power or noise on the power line may cause
equipment malfunctions. Any abnormalities in power should be reported in detail at
the time of ordering.
Nitrogen
As an option, gaseous nitrogen can be used as a bleed gas for vacuum control instead
of air. If nitrogen is to be used as the bleed gas, a gaseous nitrogen source is
required. The cylinder should be equipped with a two stage regulator with a hose
barb adapter to accommodate a 3/8" ID hose. The regulator should measure in 1 lb.
increments, up to 30 lbs.
Manual Cold Trap
The manual cold trap requires dry ice and acetone.
Venting.
A vent to the outside should be provided to vent the vacuum pump exhaust.
Environment
The area in which the instrument is operated should be free from all ignition sources
such as sparks and flames and be well ventilated. Flammable solvents should not be
stored within 5 feet of the system unless those solvents are contained in a flammable
storage cabinet.
The area should also be temperature controlled between 20C (68 F) and 27C(81F)
with a relative humidity less than 80%.
General Information 1-1

Cleaning
A source of reagent toluene or cyclohexane should be available for cleaning the unit
after each run.
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. Please see to it that
it is treated as such.
Please remember that the technician will be traveling a long distance to install and
train laboratory personnel. Having the site properly prepared will lead to quick
installation and allow more valuable time to test the unit and train lab operators!
Please pay careful attention to each of the requirements listed above. If you have any
questions please contact Koehler Instrument for advice. Thank you for your attention
to this matter.
Reporting Damaged Equipment
Damage due to shipment must be reported immediately to both the carrier and
Koehler Instrument Company, Inc. Neither the carrier nor Koehler will be
responsible for damages reported after 14 days from shipment. It is the customer's
responsibility to report any damage to the carrier. Please call 1 631 589 3800 to
report damage to Koehler Instrument.
General Information 1-2

General Information 1-3
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.
Your company should develop standard operating procedures for safe and proper
operation of the D1160 System.
For your protection, never plug in and turn on the power until the installation has
been completed in its entirety.
Laboratories using flammable solvents should be protected with an automatic fire
extinguishing system.
Goggles, gloves, and other protective safety equipment should be provided and used
when handling petroleum products and chemicals.

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).
Receiver and Level Follower: This is where the distillate is collected and the volume
is measured automatically.
Heating Mantle: Provides heat to the pot flask.
Vacuum Sensor: Senses the vacuum level.
Vacuum Bleed Valve: This automatically operated valve allows air or nitrogen into
the distillation system to regulate the vacuum level.
Cold Trap: Filled with dry ice (solid CO2). The cold trap protects the vacuum pump
and pressure sensor from uncondensed gases.
Distillation Column: Column for distilling the sample.
Pot Flask: Flask for distilling the sample.
Figure 2
Electrical connections on back of M690 controller.
Equipment Description 2-1

Equipment Description 2-2

Equipment Description 2-3

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. The metal drip trough should also be
touching the side of the receiver.
3. Verify that the receiver joint is greased.
4. Put dry ice in the cold trap.
5. Check the vacuum pump oil level. It should be near the high mark.
Electrical System Check
1. The Control Unit power should be in the ON position.
2. The Condenser Bath power switch should be in the ON position.
3. The Vacuum Pump power switch should be in the ON position.
System and Sample Preparation 3-1

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. At the
same time vacuum level and various temperatures can be monitored. This is useful for
checking the equipment function and performing maintenance.
Manage Run Data: This area is used to create and edit distillation programs.
View and Print Results: This area allows data from distillations to be viewed or
printed.
Operating the Microprocessor Controller 4-1

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.
Manual Controls
The Manual Controls button launches the Manual Control screen shown below.
Transducers show the current temperatures for the pot temperature probe and the vapor
temperature probe.
Operating the Microprocessor Controller 4-2

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. The current temperature is displayed
in the Temperature field. The Serial Data field shows the current serial communications
between the computer and the bath.
Drop Count displays the number of drops the have been detected by the IBP detector.
The Heating Mantle heaters can be turned on by checking the box next to the word
Power. Enter the percentage of the total Wattage desired in the Heat Percent field.
The Level Follower has a number of manual control options. Find Upper Limit sends
the level follow to the top of its range. Up Slow sends the level follower up slowly.
Track mode instructs the level follower to find the current liquid volume in the receiver
and follow it if it increases. Down Slow sends the level follower down slowly. Find
Base sends the level follower down till the base is found. Standby cancels previous
commands and leaves the level follower in the rest position.
There are also a variety of outputs from the level follower. Counts tells how many steps
the level follower is from the base. Sensor indicates if the level follower eye is blocked
(liquid is blocking the light from the emitter to the detector). Clear indicates liquid is not
blocking the light from the emitter to the detector. Volume tells the volume of liquid that
corresponds to the current level follower position. Lower Limit indicates if the lower
limit detector is blocked (on) or not blocked (off).
Operating the Microprocessor Controller 4-3

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

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. The value is a percentage
of the total available wattage for the heating mantle. The default value
is 50%. If the distillation rate is too high during the beginning of the
distillation then lower this value. If the distillation rate is too low
during the beginning of the distillation then raise this value.
c. Initial Take Off Heat Rate: This is the amount of heat that will be
applied to the pot flask from the the time that first drop is detected till
10% of the volume is distilled. If the distillation rate is too high
during the this time then lower this value. If the distillation rate is too
low during this time then raise this value.
d. Target Distillation Rate: This is the desired distillation rate in
ml/min. ASTM D1160 specifies an averaged distillation rage of 6-8
mL/min.
e. Maximum Pot Temperature: This is the maximum pot temperature
allowed for this distillation. The default value is 300 ºC. The
maximum allowable value is 350 ºC for borosilicate flasks and 400 ºC
for quartz flasks. If the pot temperature exceeds 300 ºC for a
borosilicate flask during a distillation it should be checked for strain
before being returned to service.
Operating the Microprocessor Controller 4-5

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. Pressure step down begins at
100 mmHg and is reduced from there at the desired rate. Slow
reduction in pressure helps to prevent foaming by allowing the sample
to slowly degas before the distillation begins.
h. Maximum Vapor AET: This is an optional field in case there is a
need to stop the distillation at a specific vapor temperature. If the field
is left blank, it appears grey and is ignored. If the field has a value
entered then, the distillation will stop at that atmospheric equivilant
temperature (AET).
i. Distillation PID Bias: This is the starting point for the distillation
rate control. If the distillation rate is too high then lower this value. If
the distillation rate is too low during then raise this value. Normally
the default value is suitable.
j. Stop by volume: If this box is checked, then an additional field
appears. This is an optional field in case there is a need to stop the
distillation at a specific volume % distilled. If the box is not checked
then the field is ignored. If the box is checked the the distillation will
stop at the volueme % entered in the field.
k. Stop on cracking detection: This is an optional function. When
check, the system will monitor the system for signs of cracking of the
sample. If sample cracking is observed, the distillation will stop
automatically. If the box is left unchecked, then this function is
disabled.
Operating the Microprocessor Controller 4-6

“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. The first set is for pressures above 10 mmHg, the second for
1-10 mmHg and the third for pressures below 1 mmHg.
a. Vacuum KP: This is the proportional control constant for the vacuum
control. The default value is normally adequate and should not need to
be changed. If you are having problems with vacuum control contact
your local representative for advice.
b. Vacuum KI: This is the integral control constant for the vacuum
control. The default value is normally adequate and should not need to
be changed. If you are having problems with vacuum control contact
your local representative for advice.
c. Distillation Rate KP: This is the proportional control constant for the
distillation rate control. Normally this value does not need to be
changed. If you are having problems with distillation rate control
contact your local representative for advice.
d. Distillation Rate KI: This is the integral control constant for the
distillation rate control. Normally this value does not need to be
changed. If you are having problems with distillation rate control
contact your local representative for advice.
e. Distillation Rate KD: This is the differential control constant for the
distillation rate control. Normally this value does not need to be
Operating the Microprocessor Controller 4-7

Operating the Microprocessor Controller 4-8

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.
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.
Operating the Microprocessor Controller 4-9

System Options
System Options for the fully automatic D1160 should be set as seen below.
Operating the Microprocessor Controller 4-10

Calibration
The main calibration screen has options for calibrating temperature, pressure and volume.
Operating the Microprocessor Controller 4-11