Water determination of peroxide derivatives by Karl Fischer titration at low temperatures

1991 ◽  
Vol 340 (2) ◽  
pp. 71-72 ◽  
Author(s):  
Eugen Scholz
2012 ◽  
Vol 66 (5) ◽  
pp. 659-665
Author(s):  
Biljana Jancic-Stojanovic ◽  
Ana Vemic ◽  
Tijana Rakic ◽  
Nadja Kostic ◽  
Andjelija Malenovic

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.


2022 ◽  
Vol 7 (2) ◽  
Author(s):  
Olga B. Radchenko ◽  
Dmytro S. Radchenko ◽  
Angelika I. Konovets ◽  
Oleksandr O. Grygorenko

2005 ◽  
Vol 88 (6) ◽  
pp. 1840-1841 ◽  
Author(s):  
Frank E Jones

Abstract Data from a recent interlaboratory study of the determination of water (moisture) in animal feed, grain, and forage (plant tissue) by Karl Fischer titration were re-analyzed using Youden plots. The purpose was to show the unique ability these plots possess of separating random and systematic errors visually while providing numerical estimates of the precision and the systematic error of the method. Furthermore, the usefulness of the technique is underscored because AOAC INTERNATIONAL allows the use of matched pairs in collaborative studies to obtain estimates of repeatability and reproducibility.


1981 ◽  
Vol 64 (6) ◽  
pp. 1277-1283
Author(s):  
Frank E Jones ◽  
Carroll S Brickenkamp

Abstract Automatic Karl Fischer titrators of the motor-driven buret type and the coulometric generation type were applied to the determination of moisture in grain. Techniques were developed to optimize the performance of the Karl Fischer titration method and to overcome disadvantages attributed to it. The imprecision (1 standard deviation) of a determination is typically 0.06% moisture content at a moisture content of 15%; the systematic uncertainty from known sources is estimated to be ±0.05% moisture content at a moisture content level of 15%. It is suggested that the method be designated as the primary reference method for grain in general and for corn and soybeans in particular.


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

1971 ◽  
Vol 54 (5) ◽  
pp. 1231-1235
Author(s):  
Boris Kviesitis

Abstract Successful use of the method depends on several factors, one of which is the size of the sample because it affects the result of the titration. In this study, 2 sizes of cane molasses samples were tested and the results were compared with those from the vacuum oven method. The use of larger samples with or without the addition of surfactant increased the precision of the analysis. It is recommended that the Karl Fischer method for water determination in molasses and sugar sirups be subjected to collaborative study.


2014 ◽  
Vol 32 (5) ◽  
pp. 602-609 ◽  
Author(s):  
L. Carbognani ◽  
L. C. Roa-Fuentes ◽  
L. Diaz ◽  
J. Berezinski ◽  
L. Carbognani-Arambarri ◽  
...  

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