scholarly journals Development of Karl Fischer titration method using quality by design concept

2012 ◽  
Vol 66 (5) ◽  
pp. 659-665
Author(s):  
Biljana Jancic-Stojanovic ◽  
Ana Vemic ◽  
Tijana Rakic ◽  
Nadja Kostic ◽  
Andjelija Malenovic
Keyword(s):  
Water Content ◽  
Quality By Design ◽  
Fractional Factorial ◽  
Clindamycin Phosphate ◽  
Karl Fischer Titration ◽  
Water Determination ◽  
Karl Fischer ◽  
Robustness Testing ◽  
Validation Parameters

Modern trends in drug quality control are moving toward incorporating quality into the method during its development. That course is in accordance with Quality by Design (QbD) concept defined by ICH Q 8 (R2) guideline. This implies that the method development begins by defining the method goals and collecting the relevant data, i.e. analyzing the properties of a given active pharmaceutical ingredient and evaluating the optimal experimental conditions. It is followed by a risk assessment defined by systematic robustness testing with the application of experimental design, while the final confirmation of the method reliability is done through the complete validation tests. In this paper, development of Karl Fischer titration for water determination in active pharmaceutical substance clindamycin phosphate is presented. Karl Fischer titration (KFT) is a widely used method in the pharmaceutical industry for determination of water content. For the analyzed substance, the European Pharmacopoeia suggests a relatively large amount of samples for the determination of water, so the objective of this study is to confirm the applicability of the developed method for the determination of water in small amount of samples applying QbD approach. According to QbD rules, detail development of coulometric Karl Fischer titration for water determination in clindamycin phosphate was done. For robustness testing fractional factorial design 24-1 was successful applied and confirmed that method was robust. Robustness was evaluated using statistical and graphical methods. Also, design space was defined so the region, in which factors could be changed without significant changes in water content, was defined. At the end, other validation parameters were determined and it was proved that analytical test system was capable of providing useful and valid analytical data.

Determination of total water content in inulin using the volumetric Karl Fischer titration

Talanta ◽  
2006 ◽  
Vol 70 (5) ◽  
pp. 1006-1010 ◽  
Author(s):  
Sébastien N. Ronkart ◽  
Michel Paquot ◽  
Christian Fougnies ◽  
Claude Deroanne ◽  
Jean-Claude Van Herck ◽  
...  
Keyword(s):  
Water Content ◽  
Total Water Content ◽  
Total Water ◽  
Karl Fischer Titration ◽  
Karl Fischer

Determination of water content in bee’s pollen samples by Karl Fischer titration

Food Control ◽  
2006 ◽  
Vol 17 (3) ◽  
pp. 176-179 ◽  
Author(s):  
Iosif Gergen ◽  
Florina Radu ◽  
Despina Bordean ◽  
Heinz-Dieter Isengard
Keyword(s):  
Water Content ◽  
Karl Fischer Titration ◽  
Karl Fischer

scholarly journals Simple Modification of Karl-Fischer Titration Method for Determination of Water Content in Colored Samples

2012 ◽  
Vol 2012 ◽  
pp. 1-6 ◽  
Author(s):  
Eva Tavčar ◽  
Erika Turk ◽  
Samo Kreft
Keyword(s):  
Water Content ◽  
Visual Detection ◽  
Moisture Determination ◽  
Spectrophotometric Detection ◽  
Karl Fischer Titration ◽  
Simple Modification ◽  
Karl Fischer ◽  
Titration Endpoint ◽  
Specialized Equipment

The most commonly used technique for water content determination is Karl-Fischer titration with electrometric detection, requiring specialized equipment. When appropriate equipment is not available, the method can be performed through visual detection of a titration endpoint, which does not enable an analysis of colored samples. Here, we developed a method with spectrophotometric detection of a titration endpoint, appropriate for moisture determination of colored samples. The reaction takes place in a sealed 4 ml cuvette. Detection is performed at 520 nm. Titration endpoint is determined from the graph of absorbance plotted against titration volume. The method has appropriate reproducibility (), accuracy, and linearity ().

scholarly journals Headspace Volumetric Karl Fischer Titration for the Determination of Water Content in Finished Tobacco Products

2012 ◽  
Vol 25 (1) ◽  
pp. 350-359
Author(s):  
N Aydin ◽  
F Chardonnens ◽  
M Rotach
Keyword(s):  
Sample Size ◽  
Water Content ◽  
Karl Fischer Titration ◽  
Intermediate Precision ◽  
Time Saving ◽  
Tobacco Products ◽  
Karl Fischer ◽  
Highly Sensitive ◽  
Good Repeatability

AbstractBecause many physicochemical properties of tobacco are highly sensitive to its moisture content, the determination of water level is an important parameter for tobacco characterization. A headspace volumetric Karl Fischer titration (HS-V-KFT) method is presented for the quantification of water content in different finished tobacco materials. The parameters affecting the extraction of water from the tobacco materials were the sample size and the oven temperature which have been optimized. The extraction of water from the samples was achieved within a reasonable time (<25 min) with a sample size of 200 mg and an optimum temperature of between 90 °C and 100 °C. The results of the water determination by HS-V-KFT at the optimized parameters were in good agreement with those obtained by standard volumetric Karl Fischer titration. HS-V-KFT showed very good repeatability (RSDr 0.9%) and intermediate precision (RSDiR 1.1%). With respect to a considerable time saving, solvent consumption reduction, precision and accuracy, HS-V-KFT can therefore be suggested as the method of choice to determine water amount in finished tobacco products.

scholarly journals Elaboration of near infrared spectroscopy model for determination of water content in freeze-dried immunological veterinary medicinal products

2016 ◽  
Author(s):  
Krzysztof Bulenger ◽  
Dorota Marta Krasucka ◽  
Bogumił Biernacki ◽  
Jakub Szumiło ◽  
Beata Cuvelier
Keyword(s):  
Infrared Spectroscopy ◽  
Water Content ◽  
Near Infrared Spectroscopy ◽  
Near Infrared ◽  
Residual Water ◽  
Medicinal Products ◽  
Karl Fischer Titration ◽  
Karl Fischer ◽  
Veterinary Medicinal Products

Residual water is a critical parameter in assessing the quality of immunological veterinary medicinal products (IVMPs). In majority of the laboratories the Karl Fischer titration (KFT) is used for the determination of water content in IVMPs. However, the transfer of IVMP into titration cell without affecting the baseline drift and repeatability seems to be the main problem when using this method. In turn, Near Infrared Spectroscopy (NIRS) allows measurement of closed vials, therefore eliminating the impact of atmospheric conditions on the sample. The aim of the study was to create a calibration model based on the reference method (Karl Fischer titration) and its optimization. Five different IVMPs designated for two animal species (dogs and rabbits) were used. The model was constructed on the basis of 49 samples tested, each in triplicate (n=147). The spectra were divided in two sets: calibration and validation. Proper selection of samples and their processing allowed to obtain a model of high quality (Q-value>0.6).

scholarly journals DETERMINATION OF WATER CONTENT IN PYROLYTIC TARS USING COULOMETRIC KARL-FISHER TITRATION

2017 ◽  
Vol 57 (1) ◽  
pp. 8-13
Author(s):  
Lenka Jílková ◽  
Tomáš Hlinčík ◽  
Karel Ciahotný
Keyword(s):  
Water Content ◽  
High Energy ◽  
Residual Water ◽  
Karl Fischer Titration ◽  
Water Separation ◽  
Water Determination ◽  
Karl Fischer ◽  
Energy Value ◽  
Content Determination ◽  
Coulometric Karl Fischer Titration

The liquid organic fraction of pyrolytic tar has a high energy value which makes possible its utilization as an energy source. However, before utilization, it is crucial to remove water from the liquid fraction. The presence of water reduces the energy value of pyrolytic tars. Water separation from the organic tar fraction is a complex process, since an emulsion can be readily formed. Therefore, after phase separation, it is important to know the residual water content in the organic phase and whether it is necessary to further dry it. The results presented in this manuscript focus on a water determination in liquid products from coal and biomass pyrolysis by a coulometric Karl‑Fischer titration. The Coulometric Karl‑Fischer titration is often used for a water content determination in gaseous, liquid and solid samples. However, to date, this titration method has not been used for a water determination in tars. A new water determination method, which has been tested on different types of tar, has been developed. The Coulometric Karl‑Fischer titration is suitable for tar samples with a water content not greater than 5 wt. %. The obtained experimental results indicate that the new introduced method can be used with a very good repeatability for a water content determination in tars.

Sign in / Sign up

Export Citation Format

Share Document