ELECTROLAB

Your Quality Our Assurance

Moisture Content Determination in Volumetric

Karl Fischer Titration
ELECTROLAB
Your Quality Our Assurance

1. INTRODUCTION:

Karl Fischer is a titrimetric method used to calculate the % moisture content in

samples. This Application Bulletin provides information on the titer and moisture
content determination using volumetric Karl Fischer titration.

The titer determination of Karl Fischer titrants is a necessary task to assure

accuracy of measurements. The titer value is measured in mg/ml units. The value
determined in a titer determination corresponds to the milligrams of water which
react with one milliliter of titrant. The moisture determination in the sample is
measured in % w/w or in ppm.

Keywords:

Titration; Karl Fischer titration; volumetric; titer; titer determination; water

standard.

2. INSTRUMENTS:

 ezFiSCHR
 Analytical balance.

Electrodes:

Dual Platinum wire-electrode (indicator electrode for volumetric Karl Fischer

titration

3. REAGENTS:

Titrant Karl Fischer Reagent

Titrate Water in Solvent (specially dried methanol)

ELECTROLAB
Your Quality Our Assurance

4. PROCEDURE FOR TITER DETERMINATION:

Titer Value Determination:

1. Go to configuration and feed sample details in the sample data screen. Click
on set method and change the mode to titer for titer determination of Karl
Fischer reagent.
2. The potential (in millivolts) of the methanol (blank) in the titration vessel
should be within the range 600 to 650 mV to start the test. The Karl Fischer
(KF) reagent will be added automatically till the mV is between 600-650
mV.
3. Press run on the screen, the total weight window will appear on the display.
4. Take 10 microliters of water in the syringe and remove excess liquid from
the outside of the needle with a paper tissue. Tare the balance and place
the filled syringe on a balance. Weigh and note the total fill weight.
5. Add filled 10 microliter syringe weight into software (as total weight).
6. Add 10 microliters through the septum into the titration vessel. Take care
that the water is injected into the methanol in titration vessel and not at
the electrode or the wall of the titration vessel. This leads to irreproducible
results. After addition of water, press ok
7. Initially, the vessel contents are stirred for 30 seconds (pre-stir time) before
the addition of the KF agent.
8. On addition of water, the potential rises, KF reagent is added to the
titration vessel gradually & automatically. The test is completed when the
potential reaches back to 600 to 650 mV, which is identified by the beep
sound. The holder weight window will appear on the display.
ELECTROLAB
Your Quality Our Assurance

9. Place the syringe again on the balance, weigh and add the measured weight
into the software as holder weight. The results are calculated from the
formula set in the system automatically. To view the results, go to record
and click on the titer runs.
10.For the next determinations, follow the same above-mentioned steps and
find the titer value (mg/ml). The test has to be repeated (usually 2-3 times
till the titer value of the tests passes the limit (We recommended the RSD
limit of < 2 %).
11.Take the average of the titer readings and click on the option txt to burette
to transfer the average titer value to burette data.

Moisture determination:

12. For sample testing, go to home screen, click on configure and click on set
method, change the mode to sample on sample data screen.
13. Repeat steps 2-9 for sample moisture determination.
14. Click on records and click on sample runs to find the moisture % (in % w/w
or ppm. The test has to be repeated usually 2-3 times till the sample purity
of the sample passes the limit (We recommended the RSD limit of < 2 %).
Find the average by clicking on the multiple runs and note down the
average % of moisture (in % w/w or ppm) from the report.
 ELECTROLAB
Your Quality Our Assurance

Figure 1: ezFiSCHR

5. CALCULATION:

Table 1: Formula for calculating titer value and moisture content

Titer (in mg/ml) Moisture in sample (in % w/w)

Std. Purity X Std. Weight X 10 (Epml-Blank) X Titer

KF Titer = ------------------------------------ Moisture = -----------------------------

Epml Sample weight X 10

where, where,

Std. Purity is: 100 Blank is: 00 mL

Epml is: End point mL Epml is: End point mL

ELECTROLAB
Your Quality Our Assurance

6. RESULTS:

6.1 Titer Determination:

Table 2: Percent RSD of titer

Sr. Titer Value (mg/ml) Average S. D. % R.S.D

No. (mg/ml)
1. 4.79810
4.7869 0.0158 0.33
2. 4.80929

6.2 Moisture: (water is used as sample)

Table 3: Percent weight by weight of water

Sample No. Burette Reading (ml) Results (% w/w)

Sample 1 2.09836 100.68

Sample 2 2.07100 99.37
Average 100.025

7. CONCLUSION:

The moisture (%) in the sample was found to be 100.025% w/w using the
ezFiSCHR apparatus.