Standard Method for Karl Fisher Titration
Sequence of Select the Method
1. Select the method of ‘if initial filling’ by pressing the ‘Mode’ from the main menu if this
is the first time to fill the titre into the cylinder;
2. Select the method of ‘Rinsing’ by pressing the ‘Mode’ from the main menu after filling
the reagent bottle and connect it to the titrator;
3. Select the method of ‘titre liquid std’ by pressing the ‘Mode’ from the main menu, then
do the titration to determine the concentration (mg/mL) of the titer with the water
standard;
4. Select the method of ‘sample titration’ by pressing the ‘Mode’ from the main menu,
then do the titration to determine the water concentration in the sample;
Parameter Setting
1. Type of reagent: two component system
2. Volume/Weight: Weight manual for both ‘sample titration’ and ‘Titer water std.’
method
3. Result Formula: F, F2 and F3 are all equal to 1.000 for ‘Sample titration’ method;
F equals to 10.00 for ‘Titre water standard’ method but it may not be this value (refer to
your standard);
4. Result unit: %
Result decimals: 3
Result statistics: 03
5. Documentation: Short
6. The pretitration volume [mL]: 0.0;
7. The extraction time [s]: 10 [10-600];
8. The drift stop [uL/min] or [ug/min]: 10 [3-30];
9. The switch-off time [s]: 10 [0-10];
10. The switch-off current [uA]: 20 [10-30];
11. The pole voltage [mV]: 100 [20-150];
12. Min. titration duration [s]: 0 [0-9999];
13. Max. titration duration [s]: 0 [0-600];
14. Dose volume: 10%=2mL;
15. Filling time [s]: 30;
16. Optimum pH range: 6-7;
Be sure to notify the responsible user when you plan to change the parameter setting and
change it back to this standard setting after you complete your titration!!!
Process of titer determination:
1. Fill some solvent into the titration vessel;
2. Open one ampoule of water standard and use it to rinse the one-way syringe;
3. Draw 2-2.5mL water standard into the syringe (proceed carefully and slowly to avoid air
into the syringe) and put the needle protector on if necessary;
4. Place the syringe in a beaker glass on a weighting-balance and press the tara-weight key;
5. Start the ‘Titre liquid std’ with the ‘Start’ key;
6. Wait for the conditioning process to be done;
7. Press the ‘Start’ key again;
8. Inject the water standard into the titration cell using a syringe through a septum;
9. Put the syringe with the needle protector back to the weighting balance, read off the
value in terms of grams without sign;
10. Input the weight of sample into the system;
11. Confirm the weight input, then the actual titration will start;
12. The results will be indicated on the display at the end of the titration;
13. Press the ‘Start’ key to trigger the next titration;
14. A triple determination is required is required for this method;
Process of Sample Titration
1. Fill some solvent into the titration vessel;
2. Draw 50-250mg sample into the syringe (refer to manual for weight range of different water
content);
3. Place the syringe in a beaker glass on a weighting-balance and press the tara-weight key;
4. Start the selected method with the ‘Start’ key;
5. Wait for the conditioning process to be done;
6. Press the ‘Start’ key again;
7. Inject the sample into the titration cell using syringe through a septum or the opening (if the
sample has high viscosity);
8. Put the syringe with the needle protector back to the weighting balance, read off the value in
terms of grams without sign;
9. Input the weight and ID of the sample into the system;
10. Wait for 10s of extraction time;
11. Follow the extraction time, the actual titration will start;
12. The results will be indicated on the display at the end of the titration;
13. Press the ‘Start’ key to start next titration which could for different sample or the parallel
sample.
Caution: Do not immerse the needle in to the solvent when injecting the sample or water
standard!!! Be highly sensitive to the leaking of the titration cell.
Maintance:
1. Once per month the dosing unit has to be visually checked for damage;
2. Once a year the inspection according to DIN 12 650 or 7 or to ISO DIS 8655 Part 3 should
be carried out;
3. Once per quarter the electrical contacts (plugs, stirrer, manual key button) have to be
checked for corrosion;
4. Check whether there is moisture below the dosing unit;
5. Check the hoses, screwed connections and seals for visible damage, contamination and
leakage, assembly of the screwed connection;
6. Check the electrical plug connections for corrosion and physical damage;
7. If the TitroLine KF titrator is not used for more than one week, the liquids contained in
the system should removed, and the Titroline K titrator is to be rinsed with alcohol;
8. In no case must the liquid penetrate into the interior of the titrator;
Supplies
Item
One way Syringe OMNIFIX
Needle
One way Syringe OMNIFIX
One way Syringe OMNIFIX
HYDRANAL – Solvent E
HYDRANAL – Titrant 5 E
HYDRANAL – Water Standard 10.0
Supplier
B Braun
Sigma
Catalog No.
4610303-02
4665600-02
4617053V-02
4617100V-02
34730
34732
34849
Price
Call for
the price
59.5
60.6
73.2
Specification
3mL
5mL
23G*2-3/8’’
10mL
1L
1L
80mL
For ordering from B Braun, please call 1-800-2272862; the order must be more than $200,
otherwise, we will be charged $40 for handing.