MINIVAP VP - Service - Manual V1.04 - 1.61 - English
MINIVAP VP - Service - Manual V1.04 - 1.61 - English
MINIVAP VP - Service - Manual V1.04 - 1.61 - English
MI N I V AP V P
SER VI C E M A NU A L
1. CALIBRATION ................................................................................................................................... 1
1.1. CALIBRATION OF THE TEMPERATURE MEASUREMENT OF THE PRESSURE TRANSDUCER ....................... 1
1.2. CHECK OF THE CALIBRATION VALUES OF THE TEMPERATURE ............................................................. 2
2. TEST FEATURES............................................................................................................................... 3
2.1 ADJUSTMENT AND CONTROL OF THE OVEN CONTROLLER ................................................................... 4
2.1.1 Adjustment of the span of the oven controller ....................................................................... 5
2.2 LINEARISATION AND COMPENSATION OF THE PRESSURE TRANSDUCER: .............................................. 6
2.3 READING THE VALUES OF THE PLOT .................................................................................................. 9
2.4 PERMANENT STORAGE OF THE CALIBRATION DATA .......................................................................... 10
2.5 MEASUREMENT COUNTER AND PRESSURE THRESHOLD.................................................................... 10
3. MAINTENANCE................................................................................................................................ 12
3.1 CHECK OF POSSIBLE LEAKS ............................................................................................................ 12
3.2 CHECK OF THE COOLING AND HEATING BEHAVIOR ............................................................................ 12
4. TEST MEASUREMENTS ................................................................................................................. 13
4.1. CALIBRATION WITH N-PENTANE ..................................................................................................... 13
4.2. MEASUREMENT WITH CLEAN SOLUTION .......................................................................................... 14
4.3. DVPE-MEASUREMENTS................................................................................................................ 14
5. TROUBLE SHOOTING..................................................................................................................... 15
5.1. EXCHANGING THE MEASURING CELL ASSEMBLY WITH PLATINUM RESISTOR ....................................... 15
6. SETUP FOR DELIVERY................................................................................................................... 16
6.1. SETUP .......................................................................................................................................... 16
7. VAPOR PRESSURE OF PURE COMPOUNDS .............................................................................. 17
1. CALIBRATION
The temperature of the measuring head is measured with the temperature coefficient of resistance
bridge of the pressure transducer.
Prior to the installation of the pressure transducer the temperature coefficient of the resistor bridge is
evaluated in a special thermostat at 10 and 40 ΕC.
The value for the gain is evaluated from this measurement with the following formulae:
****************************************
3 *OK *Z Zero= 0 Gain= 4.6200E 0
ADC= 13612 T(Rb)= 20.02 [C]
****************************************
The correct adjustment of the temperature reading is done by thermostating the measuring head with
the special designed thermostat and adjusting the temperature reading with Zero. If there is no
special thermostat at hand, measurement of the room temperature is sufficient, if the measuring head
is left outside the oven for a longer time to achieve temperature equilibrium with ambient.
Afterwards, the whole measuring head is regulated by the measuring head regulation to 25 C , Zero is
set to 2500. Shift the cursor to *Z and press TASK. T(Rb) shows approx. 25.00 C. Store the
calibration by pressing TASK with the cursor on *OK.
1
1.2. Check of the calibration values of the temperature
This menu is only for checking and completition of the test sheet of the calibration values and also for
regaining the original calibration values.
**********************************************
0 *OK *Z Zero= 0 Gain= 7.2180E-1
ADC= 1319 p= 99,2 [kPa]
**********************************************
an increase the number to 1 to switch-on the calibration menu for the oven temperature:
**********************************************
1 *OK *Z Zero= 0 Gain=-1,0957E 0
ADC= -2828 T= 19.86 [C]
**********************************************
Read the values for *Z, Zero and Gain and write them into the test sheet.
**********************************************
0 *OK *Z Zero= 0 Gain= 5,2180E-1
ADC= 1319 p= 99,2 (kPa)
**********************************************
and increase the value to 2 (with the 8 key). Now you have entered the calibration menu for the
sample temperature.
**********************************************
2 *OK *Z Zero= 0 Gain= 1,0957E 0
ADC= -2828 T= 19.86 [C]
**********************************************
Read the values for *Z, Zero and Gain and write them into the test sheet.
2
2. TEST FEATURES
This test features are mainly installed for use in the manufacturing facility.
Please be very careful when changing numbers for compensation and linearisation. Practically
all numbers in this menus should only be changed when the pressure transducer or the oven
has to be exchanged. This numbers are evaluated in our laboratories and will be given to the
part for exchange. Please be careful when you exchange a part without having this numbers.
****************************************
CCA-VP VERS. 1,xx 25/08/1990 09:37
ABS *memory *setup
****************************************
Depress 9 together with RUN (first 9 and then RUN), the display changes to
****************************************
caution *factory calibration
*Tcal Vers. 1.## 23:06:90
****************************************
The date in this menu is the date when the software version was written.
Move the cursor to the digits after *Tcal, (not visible, but cursor stops) and program the code number
162
****************************************
caution *factory calibration
*Tcal 162 Vers. 1.## 23:06:90
****************************************
and press TASK to initialize the TEST mode. The cursor jumps to the 7. Press TASK again to switch
back to the initial menu.
****************************************
CCA-VP VERS. 1,xx 25/08/1990 09:37
ABS *memory *setup
****************************************
The TEST mode is disabled when the instrument is switched off and on.
When the instrument is opened for the TEST mode (does not show on the display) and in the start-up
mode key 8 and RUN are depressed together, the test-modes are initialized.
3
2.1 Adjustment and control of the oven controller
If the instrument is set in TEST-Mode and 8 and RUN is pressed together, it shows the test features
for adjustment of the oven controller.
****************************************
CCA-VP VERS. 1,xx 25/08/1990 09:37
ABS *memory *setup
****************************************
****************************************
P= 0.750 I= 87% r= 6( 6) Ts= 30.00 C
* Th= 22.87(8+ -1) Tz= 30.1 To= 30.00
****************************************
The constants of the temperature controller are shown and the temperature regulation can be
observed with the high resolution of 0.01 C.
If you have initialized the test mode, you can switch into this menu during "RUN" and monitor the
regulator of the oven and also the pressure transducer compensation. The measuring program is not
interrupted.
ATTENTION: The set temperature remains at the temperature also after leaving the menus.
Switching-off the unit, Ts is set to the injection temperature.
4
2.1.1 Adjustment of the span of the oven controller
The maximum span of the oven controller determines the power consumption of the peltier elements.
If the power consumption of the elements is too high during cooling down, the air cooler elements
cannot dissipate the heat well enough and the hot side temperature of the peltiers becomes too warm.
Since only a limited temperature difference can be achieved, the lowest temperature of the oven is
degraded. Limiting the span of the regulator will lower the power consumption and therefor the heat
dissipation. Cooling is slowed down, but the low temperature limit will be lower. This does not have
much influence, when the instrument is prechilled with tap water.
****************************************
CCA-VP VERS. 1,xx 25/08/1990 09:37
ABS *memory *setup
****************************************
and 8 and RUN is pressed together, it shows the test features for adjustment of the oven controller.
****************************************
P= 0.750 I= 87% r= 6( 6) Ts= 30.00 C
* Th= 22.87(8+ -1) Tz= 30.1 To= 30.00
****************************************
****************************************
*pLcal *Mon lim hi= 255 lo=-220
*copyCal Koven=##### Kprobe=#####
****************************************
5
2.2 Linearisation and compensation of the pressure transducer:
The pressure transducer is of highest quality available but there are still some possibilities of
performance enhancement. Linearity is typically 0.5%, which means a maximum deviation from a
straight curve of 50 hPa. Using state of the art technology, the linearity can be improved by linear
interpolation between calibration points. This high accuracy needs a very high accurate pressure
standard, e.g. a dead weight pressure balance.
Another source of wrong pressure reading is the fact, that during the measurement the measuring
head changes its temperature slightly. This leads to a small deviation from zero. Measuring the
temperature of the measuring head, which is done via the resistance bridge of the piezoresistive
pressure transducer, a correction can be performed in the software.
Due to the measuring arrangement, leaving the measuring head at room temperature and having the
connection tubing to the pressure chamber below the liquid level because of condensation, a small
deviation occurs. As long as the temperature of the pressure cell is below room temperature, the
vapor pressure in the measuring head (being at room temperature, is higher and in the connection
tubing is only gas.
Rising the temperature of the measuring cell above the temperature of the measuring head, the liquid
in the pressure chamber is pressed up to the pressure transducer producing a liquid column in the
connection tubing. This column with a length of 8 cm reduces the pressure reading approx. 8 hPa.
Monitoring the temperature of the measuring head enables to add sequentially this 8 hPa to the
pressure reading in a temperature range around room temperature.
Finally, there is a slight source of error due to the double injection. The volume of the pressure cell for
the dissolved gases is reduced partly by the second injection. Partly, because the liquid is still
containing gas and therefor does not behave like a complete volume reduction. This percentage of
dead volume can be preset.
If the instrument is set in TEST-Mode
****************************************
CCA-VP VERS. 1,xx 25/08/1990 09:37
ABS *memory *setup
****************************************
and 8 and RUN is pressed together, it shows the test features for adjustment of the oven controller
****************************************
P= 0.750 I= 87% r= 6( 6) Ts= 30.00 C
* Th= 22.87(8+ -1) Tz= 30.1 To= 30.00
****************************************
****************************************
*pLcal *Mon lim hi= 255 lo=-220
*copyCal Koven=##### Kprobe=#####
****************************************
6
Shift the cursor to *pLcal and press TASK
****************************************
*OK Nr:0 pi= 200.0 ps= 200.0 [kPa]
KpTk= 340 [ppm/C] (T=Tk-20)
****************************************
Typically, the linearisation is 0.5 % (this means a maximum deviation of 5 kPa). Entering a
linearisation curve and a linear interpolation, it is possible to avoid also this small inaccuracy.
To determine the non-linearity, you can use a dead weight pressure balance. You must program at
minimum five pairs of points that are measured by the dead weight pressure balance.
**********************************************
*OK Nr:# pi= ###,# ps= ###,# [kPa]
KpTk=#### [ppm/C] (T=Tk-20)
**********************************************
**********************************************
CCA-VP VERS. 1,xx 25.08.1990 09:37
ABS *memory *setup
**********************************************
Press 8 and RUN together and you reach the test features for the adjustment of the oven regulator:
7
**********************************************
P= 0.750 I= 87% r= 6( 6) Ts= 30.00 C
* Th= 22.87(8+ -1) Tz= 30.1 To= 30.00
**********************************************
Shift the cursor to the number (8) of Th= ##.##(8+ 0). Pressing 9 is switching-off the correction of the
liquid column.
**********************************************
P= 0.750 I= 87% r= 6( 6) Ts= 30.00 C
* Th= 22.87(off ) Tz= 30.1 To= 30.00
**********************************************
8
2.3 Reading the values of the plot
To read the values of the data to be plotted the following menu can be used:
****************************************
CCA-VP VERS. 1,xx 25/08/1990 09:37
ABS *memory *setup
****************************************
press 8 and RUN together to open the menu for the oven controller
****************************************
P= 0.750 I= 87% r= 6( 6) Ts= 30.00 C
* Th= 22.87(8+ -1) Tz= 30.1 To= 30.00
****************************************
****************************************
*pLcal *Mon lim hi= 255 lo=-220
*copyCal Koven=##### Kprobe=#####
****************************************
****************************************
Plotval nr. ### = ##### [hPa]
Location nr.#####= ##
****************************************
9
2.4 Permanent storage of the calibration data
After finishing the calibration with the quartz thermometer, the calibration data are stored in a
separate range of the EE-PROM for a later reading.
Enter the test mode and the initialization menu:
**********************************************
CCA-VP VERS. 1,xx 25.08.1990 09:37
ABS *memory *setup
**********************************************
Press and RUN and you reach the test features for the adjustment of the oven regulator.
**********************************************
P= 0.750 I= 87% r= 6( 6) Ts= 30.00 C
* Th= 22.87(8+ -1) Tz= 30.1 To= 30.00
**********************************************
**********************************************
*pLcal *Mon lim hi= 255 lo=-220
*copyCal Koven=##### Kprobe=#####
**********************************************
Shift the cursor to *copyCal and press TASK. Switch back to the initialization menu. Now the factory
calibration values are stored in the EEPROM.
In the setup menu shift the cursor to *preset and press TASK.
****************************************
T=[F] p=[psi] english *preset
*loc *com *clk display= 15
****************************************
****************************************
Tinj = ### [C] solubility= ## [%]
Equilibrium time = #### [sec]
****************************************
Move the cursor to the end of the second line and press TASK.
****************************************
delta =2.00kPa
nr. meas.: ###
****************************************
delta= ... pressure threshold for EN measurement. After the equilibrium time the
pressure reading should not change more than 2.0 kPa within one
minute. Otherwise the equilibrium time will be extended until the
pressure change is less than 2.0kPa.
10
The measurement counter can be reset if the code 163 is programmed in the following menu:
In the start up menu press 9 and RUN, shift the cursor in the second line and program the code 163.
****************************************
caution *factory calibration
*Tcal 163 Vers. 1.## 23:06:90
****************************************
Press TASK, shift the cursor back into the *setup and *preset menu and enter the menu of the
measuring counter. Exit and enter it again. Now the measurement counter is set to zero.
11
3. MAINTENANCE
Connect vacuum
Turn valve several times between V and F and stay at M
Check the pressure increase (max 0.5 kPa in 3 min.)
3.2 Check of the cooling and heating behavior (Test sheet: test thermostat)
Testing procedure:
Start the measuring program with an initial temperature of - 50 ΕC
The unit tries to cool down to this temperature (it is not possible with a water cooling of 13 C).
Wait apr. 20 min to achieve the lowest temperature possible. The delta-T for cooling
(=minimum temperature - temperature of the cooling element) can be recorded in the test
sheet.
The program can be interrupted by pressing STOP.
To check delta-T heating, repeat the procedure with an initial temperature of 150 ΕC
If the instrument is ok, it will reach this 150 C
12
4. TEST MEASUREMENTS
This feature was built-in for our customers to enable them the possibility of a calibration at high
temperatures without using a quartz thermometer.
In the quality control, this automatic calibration is done only for controlling purposes.
**********************************************
CCA-VP VERS. 1,xx 25.08.1990 09:37
ABS *memory *setup
**********************************************
shift the cursor to *Absolut and press TASK to switch-on the measuring method for absolute vapor
pressure. Increase the program number No: to C1.
**********************************************
Nr:C1 *CAL-nPentan Ta= 30 C Te=100 C
I= 5C:2 C/min v1=v2=1.0 ml Tp1=*****C
**********************************************
Evacuate the measuring cells and fill 1 ml n-Pentane each according to the filling procedure.
*******************************************************
Use clean, water-free n-Pentane only.
*******************************************************
After the filling procedure, please pay attention to the gas correction Pgas that should be at approx. 7
kPa (depending on the sample temperature). If the deviation of the gas correction is higher, the
program should be interrupted since in this case a calibration is not useful.
The whole measurement is done according to the determination of the absolute vapor pressure. If a
printer is connected, the measured values are printed. After reaching the final temperature, the oven
regulates the cell temperature (after an equilibrium time of 3 minutes) in such a way that the
theoretical absolute vapor pressure of n-Pentane is reached. The necessary temperature is shown at
the display.
**********************************************
PREG *OK To=100.6 C Tp=100.5 C
Pabs=589.3 Pgas= 13.4 Ptot=367.7 kPa
**********************************************
PREG means that the automatic regulation of the oven temperature is done due to a balance of the
absolute vapor pressure to the desired value.
The oven and sample temperature at the first CAL-procedure after calibration of the thermometer will
between 100.1 C and 100.9 C.
13
Literature values for the absolute vapor pressure of n-Pentane:
100 C ... 589.3 kPa
80 C ... 367.1 kPa
38 C ... 108.1 kPa
The deviation that are recognized during the calibration must be filled into the test sheet.
4.3. DVPE-measurements
with neo-Hexane
14
5. TROUBLE SHOOTING
1. Remove the black cover of the pressure transducer held by 2 screws on the bottom side.
2. On the opposite side of the pressure transducer the 2 wires of the Pt100 are visible.
Remove the black tube which is for the insulation of the soldering joint and lose the
connection.
3. Unscrew the 4 screw holding the Pt100 assembly on the measuring head.
4. Exchange the Pt100 assembly, fix it with the 4 screws on the measuring head and connect
the Pt100 by soldering the 2 wires (do not forget to insulate).
15
6. SETUP FOR DELIVERY
6.1. Setup
****************************************
CCA-VP VERS. 1,xx 25/08/90 09:37
ABS *memory *setup
****************************************
****************************************
T=(C) p=(kPa) Deutsch *preset
*loc. *com *clk *format *display= 10
****************************************
****************************************
T=(C) p=(kPa) Deutsch *preset
*loc. *com *clk *format *display= 10
****************************************
Frankreich
220 V AC
1 AT
****************************************
T=(C) p=(kPa) Francaice *preset
*loc. *com *clk *format *display= 10
****************************************
USA
120 V AC
2 AT
****************************************
T=(F) p=(psi) English *preset
*loc. *com *clk *format *display= 10
****************************************
JAPAN
100 V AC
2 AT
****************************************
T=(C) p=(ata) English *preset
*loc. *com *clk *format *display= 10
**********************************************
16
7. VAPOR PRESSURE OF PURE COMPOUNDS
P/T-Behavior
Vapor
Pressure kPa
17
Vapor Pressure of Pure Solvents
P/T-Behavior
Vapor
Pressure psi
18