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MKC-500 KF
Operation Manual
83 pgs761.02 Kb1

KEM MKC-500 KF Operation Manual

Operation Manual
MKC-500 KF Moisture Titrator
Ver.04
#595-0006
Contents Page
1. SAFETY MEASURES........................................................................................................................................... 1
2. FOREWORD.......................................................................................................................................................... 2
3. MEASUREMENT PRINCIPLE............................................................................................................................. 3
4. SETTING UP THE SYSTEM................................................................................................................................ 4
5. INSTALLING THE TITRATION CELL ............................................................................................... .............. 11
6. METHOD CONFIGURATION............................................................................................................................13
6.1.1 Basic structure.......................................................................................................................................... 13
6.1.2 Structure of the parameter configuration ................................................................................................. 14
6.1.3 Initial parameters .....................................................................................................................................16
6.2.1 t(stir)[s], t(wait)[s], t(max)[s]................................................................................................................... 18
6.2.2 Drift stop : (rel / abs / off)........................................................................................................................ 18
6.3.1 Calculation formula (by unit)................................................................................................................... 21
6.3.2 Weight : (fix / var)...................................................................................................................................22
6.3.3 Drift comp : (auto / off / manu)................................................................................................................ 22
6.3.4 Blank........................................................................................................................................................ 22
6.3.5 Factor....................................................................................................................................................... 22
7. EXAMPLE OF ACTUAL OPERATION............................................................................................................. 27
8. SETUP.................................................................................................................................................................. 33
9. FUNCTION.......................................................................................................................................................... 43
10. INITIALIZING PARAMETERS AND DEFAULT VALUES.......................................................................... 50
11. SPECIAL KEYS................................................................................................................................................. 51
12. MAINTENANCE............................................................................................................................................... 54
12.8.1 Cleaning steps........................................................................................................................................ 56
12.8.2 Drying steps........................................................................................................................................... 57
12.8.3 Adjusting the length between anode and membrane.............................................................................. 57
13. KARL FISCHER REAGENT.............................................................................................................................59
14. TROUBLESHOOTING......................................................................................................................................61
15. DISPLAY MESSAGES LIST............................................................................................................................69
16. PARTS LIST ...................................................................................................................................................... 72
17. SYSTEM CONNECTIONS ............................................................................................................................... 76
18. SPECIFICATIONS.............................................................................................................................................77
19. CONNECTION DIAGRAM..............................................................................................................................78
20. WARRANTY PROVISION FOR TERMS AND CONDITIONS..................................................................... 79
1. Safety measures
Measures for your safety
− Ensure that you plug the supplied power cable into a sock et which is grounded! In the absence of grounding, a technical fault could be lethal.
− Switch the instrument off and disconnect the power cable if you change blown fuses!
An electrical shock could be fatal.
− Never work in a hazardous area! The housing of the titrator is not gastight (explosion hazard through spark formation, corrosion by gas diffusion into the instrument).
Measures for operational safety
− Check the set operating voltage before you switch on the instrument (see chapter 4.2)! The instrument will be damaged if the operating voltage does not match the line voltage.
− Use only fuses of the specified type if you need to change them!
− Let the titrator be opened and maintained by Service only!
− Exclude the following environmental influences:
⋅ Powerful vibrations ⋅ Direct sunlight ⋅ High atmospheric humidity ⋅ Temperatures below 5°C and above 35°C ⋅ Powerful electric or magnetic fields which influence the power supply through large
load fluctuations!
1
2. Foreword
Moisture in sugar or salt influences its pouring properties. Traces of moisture in brake fluid adversely affect the function of the vehicle brakes. Small amounts of water in aircraft hydraulic oil increase the risk of an emergency. Traces of moisture usually influence the quality of products and it is therefore often very important to know the exact value of the moisture content. With the MKC-500 you can easily determine traces of water with a very high degree of accuracy.
You can change the titration parameters and get the results from computer by RS-232C.
The MKC-500 offers the possibility of entering the sample weight before or after the titration; manually or transferred automatically from the connected balance.
The MKC-500 has an automatic drift determination, which is reconciled in the result calculation.
The MKC-500 has two kinds of report format, Short/GLP. (Note: Printer is optional )
2
3. Measurement principle
In the Karl Fisher moisture content measurement, water reacts with iodine and sulfur dioxide in the presence of a base and alcohol.
H
In the volumetric titration, iodine is added as a titrant. In the coulometric technique, iodine is electrolytically generated in the anolyte, which contains iodide.
2I¯
As long as water is present in the titration cell the generated iodine reacts according to (1). As soon as all the water has reacts, a small excess of iodine appears in the anolyte. This iodine is detected by the double platinum pin electrode and the iodine production is stopped. According to Faraday's law, the quantity of iodine produced is proportional to the current generated. In equation (1), I proportion 1:1. Therefore a mole of water (18 g) is equivalent to 296500 coulombs, or 10.72 coulombs/ 1 mg H of moisture can thus be determined by measuring the total consumption of electricity.
O + I2 + SO2 + CH3OH + 3RN [RNH]SO4CH3 + 2[RNH]I (1)
2
→
I2 + 2 e ¯ (2)
and H2O react with each other in
2
O. The total amount
2
Catholyte
Cathode
Membrane
Detection/
Control unit
Microconputer Display
Detection electrode (double platinum pin electrode)
Titration cell
Anolyte
Anode
Rotor
3
4. Setting up the system
4.1 Supplied parts
The carton box that has been delivered to you contains the MKC-500 and supplied parts including Operating manual as per below list. Please identify the supplied parts with the list, and if you should find any part missing or broken, contact your local dealer.
MKC-500 MKC-500
2-component cell 1-component cell
1. Main unit.................................................................................MKC-500 1 unit 1 unit
2. Power cord with earth wire (AC100/120V area) ....................#320-3198 1 pce 1 pce
(AC220/230/240 area)................#320-3461
(for UK)......................................#320-4199
3. AC 3-pin Adapter (AC100V only)..........................................#320-3199 1 pce 1 pce
4. Earth wire (AC100V only)......................................................#433-3331 1 pce 1 pce
5. Titration cell unit....................................................................#433-0005 1 set ⎯
6. Titration cell unit....................................................................#433-0071 ⎯ 1 set
7. Drain bottle.............................................................................#500-3134 1 pce ⎯
8. Funnel.....................................................................................#500-3159 1 pce ⎯
9. Stirrer spinner (35mm)...........................................................#500-3362 1 pce 1 pce
10. KF grease (5g)......................................................................#433-3138 1 pce 1 pce
11. Septum...................................................................................#523-3161S 10 pcs 10 pcs
12. Anode tool.............................................................................#075-3411 1 pce ⎯
13. Power fuse (T3.15A/250V for AC100/ 120V ).......................#338-5028 2 pcs 2 pcs
(T1.6A/250V for AC220/230/240V) ..................#338-3252 2 pcs 2 pcs
13. Operating manual..................................................................#595-0006 1 copy 1 copy
14. Warranty................................................................................ 1 copy 1 copy
15.Manual solvent exchanger......................................................MLC-500 ⎯ 1 unit
4
4.2 Parts name and functions
g
t
Detection electrode
measures potential in the cell to detec endpoint.
Fuse box where power fuse is replaced with new one.
Desiccator keeps air dried.
Inner burette(anode and cathode electrode combined into one unit) generates iodine and titrates
moisture content.
Injection port(for syringe) allows the sample injected into the cell.
Titration cell in which iodine and water react for coulometric titration.
Cell holder secures the titration cell.
Display screen shows measurement results or mode of the instrument.
Keypad Enter desired parameters and controls titration. Input for inner burette Plug in the connector from inner burette.
Input for detection electrode Plug in the cable end from the electrode.
Port for Printer Plug in the printer cable here.
Port for Balance
in the cable from Balance.
Plu
5
Voltage selector
Power switch
RS-232C connector Interface for communication with PC or other external device.
Connector for power cable
Key to enter Titration parameter. Press the key again when finishing parameter setting. Key to enter parameters for Calculation or Report. Press the key again when finishing parameter setting. Key to enter Sample No., Lot No. or Sample weight. Press the key again when finishing parameter setting. Key to set up Function parameter. Press the key when closing parameter setup.
0.Reagent Capacity
1.Recalculation
2.Factor
3.Memory clear
Key to enter Setup parameter. Press the key when closing parameter setup.
0.Interface
1.Date & Time
2.Name
3.Serial No.
Key to activate Printer for printing.
Key to control Stirring speed. Press the key again finishing rotating speed se tt i ng. Key to perform Pre-titration.
Key to start Titration.
Key to turn the instrument into reset condition.
Key to select menu with ↑ mark or characters, and to show cell potential.
Key to select and reverse dot or character.
6
Key to select numerals.
~
Key to move the cursor.
Key to confirm the key entry.
Key to return the parameters on display to the previous screen.
Key to reverse a character or number by one space.
Key to clear the key entry that has been made.
7
4.3 Checking the operating voltage
Before switching on the instrument for the first time, make sure the voltage selector is set to the appropriate line voltage. If it should be set to a wrong voltage, correct it by the following procedure:
(1) Open the cover of power inlet using a flat head screw driver. (2) Pull out the voltage selector wheel, and put it back to the box so that the selected voltage can be seen when
the cover is closed.
(3) Close the cover and recheck the voltage display on the box.
Insert the driver and Pull out the voltage Close the cover. open the cover. selector wheel.
Voltage selector
Make sure the power fuse conforms to the below rating chart. For more details, see 12.10 Replacement of Power Fuse.
AC Line voltage Fuse Hz
100 V 90 - 120 V T3.15 A/250 V 50/60
120 V 103 - 132 V T3.15 A/250 V 50/60
220 V 198 - 242 V T 1.6 A/250 V 50/60
230 V 207 - 253 V T 1.6 A/250 V 50/60
240 V 216 - 264 V T 1.6 A/250 V 50/60
Voltage can be selected by the selector on the rear panel.
CAUTION
For continued protection against risk of fire, replace only with same type and ratings of fuse.
Fuse
8
4.4 Turning on the power
(1) Make sure the power switch is in OFF position.
(2) Plug in the connector of supplied power cord to the unit.
(3) Plug in the other end of power cord to the power outlet.
<For 3-P consent> <For 2-P consent>
The 3-pin plug has an earth terminal First, plug in the AC-3P adapter to AC plug, so that grounding by wire is not necessary. and then ground the green wire to the earth.
(4) Turn ON the power switch of the unit.
WARNING
Be sure to ground the earth line. If not earthed, there will be danger of electric shock.
9
4.5 Initial display at start
When the power is turned on, the message (1) will appear on display for about two seconds. Then, the message (2) on product version number will be shown for two seconds. Then, the message (3) will blink, which keeps blinking until pre-titration starts.
(1)
(2)
(3)
C . M o i s t u r e T i t r .
V e r 1 .01
Pre-Tit r
4.6 How to confirm product version number
The product ver. number varies depending on what options and specifications you have selected for your MKC-500. Follow the below procedure to check its number:
With power turned on, make sure it shows Initial message or Main display. Then, press [ 0 ], [ 0 ], [ 0 ] and press [ ↵ ] key. The product number will appear for two seconds.
( 4.5 (2) )
Note!
This procedure must be worked on Initial display or main display.
10
5. Installing the titration cell
5.1 Installation 2-comoponent cell
(1) Put the stirring spinner in the cell, and insert the inner burette and the detection electrode. Apply KF grease
around jointing parts.
Inner burette port
Detection electrode port
Sample injection port
Apply KF grease
Desiccator
Apply KF grease
Titration cell
(2) Supply 100mL anolyte into Titration cell, and seal it after KF grease is applied around the injection p ort.
(The lower level line outside the titration cell shows 100mL line.) (3) Supply 5mL catholyte into Inner burette, and seal it by the desiccant tube. (4) Position the measuring cell in the cell holder.
Then, plug the cables of the electrode and the inner burette to the ports at the rear panel. (See next page)
Inner burette (with diaphragm)
Detection electrode
Sample port stopper
CAUTION
KF grease must be applied around all the jointed parts including the inner
burette, the detection electrode, sample port inlet and the low end of
desiccant tube. Check the jointed parts once a week. (See 12.1)
Neglegence of such maintenance will lead to solidification of those parts.
Note!
The protective seal on Desiccator must be peeled off.
Cell holder Inner burette
holder Detection
electrode holder
CAUTION
To prevent the inner burette from breaking by handhold, do not snatch the housing (black resin) and desiccant tube by fingers. You may get hurt if it is broken.
11
5.2 Installation 1-comoponent cell
(1) Put the stirring spinner in the cell, and insert the inner burette and the detection electrode. Apply KF grease
around jointing parts.
Inner burette port
Detection electrode port
35mm spinner
Flask stopper port
Sample injection port
Apply KF grease
Desiccator
Apply KF grease
Titration cell
(2) Supply 150mL anolyte into Titration cell, and seal it after KF grease is applied around the injection p ort.
(The lower level line outside the titration cell shows 150mL line.) (3) Position the measuring cell in the cell holder.
Then, plug the cables of the electrode and the inner burette to the ports at the rear panel. (See next page)
Inner burette (Diaphragmless)
Detection electrode
Sample port stopper
CAUTION
KF grease must be applied around all the jointed parts including the inner
burette, the detection electrode, sample port inlet and the low end of
desiccant tube. Check the jointed parts once a week. (See 12.1)
Neglegence of such maintenance will lead to solidification of those parts.
Note!
The protective seal on Desiccator must be peeled off.
Cell holder Inner burette
holder Detection
electrode holder
CAUTION
To prevent the inner burette from breaking by handhold, do not snatch the housing (black resin) and desiccant tube by fingers. You may get hurt if it is broken.
12
6. Method configuration
6.1 General
The MKC-500 has some parameters which are used for the titration, the calculation and the record of a titration. These parameters can be modified to meet the requirements of individual titrations using the three function keys, Titration, Result and Sample.
In a new MKC-500 parameters are initialized with default value (see 10.). With these parameters you can start a titration without any change of parameter configuration.
6.1.1 Basic structure
The parameters can be selected with the three function keys, Titration, Result and Sample.
Function key Description
Titration (parameters for controlling the titration)
Result (parameters for the result calculation)
(parameters for the result print out)
Sample (parameters for the sample)
13
6.1.2 Structure of the parameter configuration
For entering and changing these display lines, see the chapters 6.2, 6.3, 6.4, 6.5.
Routine measurement by MKC-500 is simply started by [ Start ] key, and can be aborted by [Reset ] key.
Display messages and key entry are related like this: Parameters of message ending with "↑" is selected on display by [-/Disp. ] key, and confirmed by [↵ ] key. For parameters ending with "?", use numeric key and confirm by [↵ ] key.
The contents of each parameter are shown below:
t(stir) [s] ( 0 - 999 s ) t(wait) [s] (15 - 9999 s ) t(max) [s] ( 0 - 999 s )
Drift stop : rel ↑/ abs ↑/ off↑
Calculation↑
Unit : μg↑ /mg↑ /ppm↑ /%↑ Weight : fix↑ /var↑ Drift comp : auto↑ /off↑/ manu
Abs?(0.00 - 9.99)
Rel?(0.00 - 9.99)
↑
Drift?(0.0000 - 999.9)
14
Report ↑
Short
↑/ GLP ↑
Date & Time Date & Time Sample No. Serial No. Sample Weight Sample No. Result Lot No. Sample Weight Factor Result Titr.Time Drift Blank Name
Sample No. ? (00 - 00
99 - 99) Lot ? (xxxxxxxxxx) Wt1 ? (0.000000 - 999.9999) Wt2 ? (0.000000 - 999.9999)
15
6.1.3 Initial parameters
Parameters Initial value
Titration
Result Calculation
Report
Sample
t(stir) [s]? t(wait) [s]? t(max) [s]? Drift stop
Unit Weight Drift comp
Drift comp:manu↑
Drift ?
Blank ?
Sample No. ? Lot ? Wt1 ? Wt2 ?
0s
15s
0s
rel 0.1μg / s
Calculation↑
μg↑
f ix↑
auto↑
0.0μg / s 0μg
Short↑
00 - 00
5.0000g
0.0000g
16
6.2 Titration parameters
Here you can set the control parameters for the titration.
Entry Key Display Description
t(stir)[s]? 0 titration active, stirrer, no I
t(wait)[s]? 15
t(max)[s]? 0 time limit of titration, termination criteria. (0s
Drift stop : rel ↑ rel : stop s when drift is below.
Drift stop : abs ↑
Drift stop : off ↑
Drift stop : rel ↑
rel[μg/s]? 0.1
titration active, no termination during this time. (more than 15s)
endless)
(entered value + drift value)
abs : stops when drift is below entered value.
off : no drift stop, termination after
{ t(stir) + t(wait) + t(max) }
- generation.
2
Note!
Do not select Drift Stop:off and t(max)=0 at the same time. If selected, the alarm will beep when titration starts.
Note!
All parameters with the ↑ sign can be changed with the [ -/Disp. ] key. All parameters with the ? sign require entry of a numeric value.
17
6.2.1 t(stir)[s], t(wait)[s], t(max)[s]
Start End
t(stir) t(wait) t(max)
No I2 generation I2 generation
a) t(stir) is the time that just stirrer is active. b) t(wait) is the first possible time of titration termination.
Titration terminates here if drift stop level is reached.
c) t(max) is the time limit of titration.
titration time = t(stir) + t(wait) + t(max)
6.2.2 Drift stop : (rel / abs / off)
With the MKC-500 you have two possibilities to determine an endpoint.
a) Time Limit ( t(wait) + t(max) )
You define a fixed titration time. The titration stops after the defined time.
b) Drift stop
You define a drift stop. When the drift stop is reached, and the time "t(wait)"elapses, the titration stops.
You must define t(max) or Drift stop, or both.
If you define nothing, in other words t(max) 0 and Drift stop off, you get an error message: Para set miss!
Remarks regarding Drift stop
A high value of the Drift stop reduces the titration time, but the titration error increases, especially if the sample releases its moisture slowly. Repeated analysis of an oil sample sometimes causes a shift to a higher drift. In this case a low Drift stop setting results in failure to detect the endpoint. In the case of titrations with a sluggish approach towards the endpoint (due to side-reactions), a higher Drift stop can help reduce the error.
18
Titration curves of a rapid and a slow moisture release with two Drift stop :
μgH2O/s
L1
L2
A
End2 End2 Start Start End1 End1
A : Drift L1 : High value for Drift stop L2 : Low value for Drift stop End1 : Endpoint with L1 End2 : Endpoint with L2
19
6.3 Calculation parameters
The four calculation parameters are part of the result parameters you can select in a method.
Entry Key Display Description
Calculation ↑
Unit :μg ↑ Set the calculation result unit
Unit : mg ↑
Unit : ppm ↑
Unit : % ↑
Weight : fix ↑ Select fixed or variable
Weight : var ↑
Drift comp : auto ↑ Set the drift compensation
Drift comp : off ↑
Drift comp : manu ↑
Drift? 0
Drift? 1.0
Blank? 0
Blank? 1.0
Calculation ↑
Drift is entered here [μg/s]
Blank is entered here [μg]
Note!
All parameters with the ↑ sign can be changed with the [ -/Disp. ] key. All parameters with the ? sign require entry of a numeric value.
20
6.3.1 Calculation formula (by unit)
(
(
)
Formula No. Description Formula
1
2 Concent rat ion calculation for weighed
Formula No. is selected automatically by result unit.
Calculation Result unit Formula No.
μg or mg
ppm or %
Data : Result of th e titration (μg) DL : Drift Level (μg/s)
T : Measurement time (s)
Blank : The value for subtraction of result (μg) Wt1 : Weight of syringe with sample in it Wt2 : Weight of empty syringe
Therefore, the sample weight = Wt1-Wt2
Moisture calculation Result in μg or mg.
liquid or solid samples. Result in ppm or %
1 2
When Drift comp:auto is selected, this value represents the drift at time [ Start ] key is pressed. When Drift comp:manu is selected,this is manually input value.
When Drift stop:off ↑ is selected,t=(t(stir)+t(wait)+t(max)) (s) When Drift stop:rel ↑ /abs ↑ is selected, t=<
Factor Data DL t Blank×−×−
Factor
t(stir)+t(wait)+t(max) (s)
Data DL t Blank
×
−×−
Wt1 Wt2
−
)
(ppm)
Note!
21
Even when ppm or % is selected for calculation results, if Wt1-Wt2=0, the display will show the results in mg and printout in μg and mg.
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