scholarly journals Youden Analysis of Karl Fischer Titration Data from an Interlaboratory Study Determining Water in Animal Feed, Grain, and Forage

2005 ◽  
Vol 88 (6) ◽  
pp. 1840-1841 ◽  
Author(s):  
Frank E Jones
Keyword(s):  
Animal Feed ◽  
Systematic Errors ◽  
Interlaboratory Study ◽  
Matched Pairs ◽  
Karl Fischer Titration ◽  
Karl Fischer ◽  
Collaborative Studies ◽  
Titration Data ◽  
Repeatability And Reproducibility

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.

scholarly journals Liquid Chromatographic Determination of Deoxynivalenol in Baby Food and Animal Feed: Interlaboratory Study

2006 ◽  
Vol 89 (4) ◽  
pp. 1012-1020 ◽  
Author(s):  
Joerg Stroka ◽  
Michelle Derbyshire ◽  
Carsten Mischke ◽  
Massimo Ambrosio ◽  
Katy Kroeger ◽  
...  
Keyword(s):  
Standard Deviation ◽  
Relative Standard Deviation ◽  
High Performance ◽  
Animal Feed ◽  
Chromatographic Determination ◽  
Baby Food ◽  
Interlaboratory Study ◽  
Relative Standard ◽  
Liquid Chromatographic

Abstract An interlaboratory study was conducted for the determination of deoxynivalenol in baby food and animal feed by high-performance liquid chromatography with UV detection. The study included 14 participants representing a cross section of industry, official food control, and research facilities. Mean recoveries reported ranged from 89% (at 120 g/kg) to 85% (at 240 g/kg) for baby food and from 100% (at 200 g/kg) to 93% (at 400 g/kg) for animal feed. On the basis of the results for spiked samples (blind duplicates at 2 levels), as well as those for naturally contaminated samples (blind duplicates at 3 levels), the relative standard deviation for repeatability (RSDr) in analyses of baby food ranged from 6.4 to 14.0% and in analyses of animal feed, from 6.1 to 16.5%. The relative standard deviation for reproducibility (RSDR) in analyses of baby food ranged from 9.4 to 19.5% and in analyses of animal feed, from 10.5 to 25.2%. The HorRat values ranged from 0.4 to 1.0 and from 0.7 to 1.3, for baby food and animal feed, respectively. The method showed acceptable performance for within-laboratory and between-laboratory precision for each matrix, as required by European legislation.

Automatic Karl Fischer Titration of Moisture in Grain

1981 ◽  
Vol 64 (6) ◽  
pp. 1277-1283
Author(s):  
Frank E Jones ◽  
Carroll S Brickenkamp
Keyword(s):  
Standard Deviation ◽  
Moisture Content ◽  
Systematic Uncertainty ◽  
Reference Method ◽  
Titration Method ◽  
Karl Fischer Titration ◽  
Karl Fischer ◽  
Moisture Content Level ◽  
Primary Reference

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.

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

Gas-Liquid Chromatographic Determination of Mirex and Photomirex in the Presence of Poly chlorinated Biphenyls: Interlaboratory Study

1980 ◽  
Vol 63 (1) ◽  
pp. 37-42 ◽  
Author(s):  
Ross J Norstrom ◽  
Henry T Won ◽  
Micheline Van Hove Holdrinet ◽  
Patrick G Calway ◽  
Caroline D Naftel
Keyword(s):  
Chromatographic Determination ◽  
Interlaboratory Study ◽  
Gas Liquid Chromatography ◽  
Coefficients Of Variation ◽  
Fuming Nitric Acid ◽  
Liquid Chromatographic Determination ◽  
Repeatability And Reproducibility ◽  
Concentrated Sulfuric Acid ◽  
Liquid Chromatographic

Abstract Mirex and photomirex (8-monohydromirex) were separated from polychlorinated biphenyls (PCBs) and other aromatic compounds by nitration with fuming nitric acid-concentrated sulfuric acid and removal of nitro-PCBs on an alumina microcolumn; the compounds were then determined by gas-liquid chromatography. Recoveries of Mirex and photomirex were 102±8 and 104±5%, respectively, from standard solutions which had a PCB-to-Mirex and photomirex ratio of 1000. Recoveries from fortified, uncontaminated samples of sediment, fish, and eggs averaged 93±7 and 92±3% for Mirex and photomirex, respectively. The coefficients of variation for repeatability and reproducibility averaged 8 and 15%, respectively, in an interlaboratory study conducted by 4 laboratories using extracts of naturally contaminated substrates (sediment, carp, eel, and gull egg). Levels of Mirex in the samples ranged from 0.1 to 8 mg/kg, and levels of PCB ranged from 0.5 to 166 mg/kg.

scholarly journals Determination of Atrazine in Water by Magnetic Particle Immunoassay: Collaborative Study

1996 ◽  
Vol 79 (2) ◽  
pp. 529-537 ◽  
Author(s):  
Mary C Hayes ◽  
Scott W Jourdan ◽  
David P Herzog ◽  
P Barnes ◽  
C Charan ◽  
...  
Keyword(s):  
Detection Limit ◽  
Water Sample ◽  
Magnetic Particle ◽  
Collaborative Study ◽  
Study Data ◽  
Collaborative Studies ◽  
Enzyme Conjugate ◽  
Repeatability And Reproducibility ◽  
The Mean

Abstract A collaborative study was performed to determine mean recovery and precision for analysis of atrazine in drinking and surface waters by immunoassay. The study design was based on the blind duplicate test plan for collaborative studies. Three blank waters (municipal drinking water, well water, and surface water) were spiked at 3 atrazine levels. Two water samples with naturally incurred atrazine loads were also spiked with atrazine at 3 levels. In the enzyme-linked immunoassay method, the water sample is mixed with a pesticide–enzyme conjugate and added to paramagnetic particles with triazine-specific antibodies attached. After separation of antibody-bound atrazine and atrazine–enzyme conjugate from free components, the bound enzyme conjugate catalyzes a reaction producing a colored end product. The color developed is inversely proportional to the original concentration of atrazine in the water sample. Fourteen laboratories participated in the collaborative study. Data were analyzed for repeatability and reproducibility, and average recoveries at the spike levels were calculated. Over the concentration range tested, the mean recovery of atrazine spiked into blank and pesticide-contaminated waters was 104%. Overall RSDRaveraged about 40% for atrazine concentrations near the method detection limit (0.05 μg/L) and about 15% at concentrations above 5 times the detection limit (0.25 μg/L). Corresponding single-analyst RSDr values were 24 and 10%. Recovery and precision for the 3 blank water matrixes and the waters that had been naturally contaminated with atrazine showed no significant differences. The magnetic particle immunoassay

Reliable Determination of Water Contents of Bitumen and Vacuum Residua via Coulometric Karl Fischer Titration Using Tetrahydrofuran

2014 ◽  
Vol 32 (5) ◽  
pp. 602-609 ◽  
Author(s):  
L. Carbognani ◽  
L. C. Roa-Fuentes ◽  
L. Diaz ◽  
J. Berezinski ◽  
L. Carbognani-Arambarri ◽  
...  
Keyword(s):  
Karl Fischer Titration ◽  
Reliable Determination ◽  
Karl Fischer ◽  
Coulometric Karl Fischer Titration ◽  
Water Contents

Determination of Nitrogen Content in Milk by the Kjeldahl Method Using Copper Sulfate: Interlaboratory Study

1988 ◽  
Vol 71 (5) ◽  
pp. 893-898 ◽  
Author(s):  
R Grappin ◽  
William Horwitz
Keyword(s):  
Quality Control ◽  
Nitrogen Content ◽  
Copper Sulfate ◽  
Interlaboratory Study ◽  
Internal Quality ◽  
Relative Standard ◽  
Nitrogen Concentrations ◽  
Kjeldahl Method ◽  
Repeatability And Reproducibility

Abstract Copper sulfate was substituted for mercury as the catalyst in the International Dairy Federation (IDF) Standard 20A:1986 method for the determination of nitrogen content in milk. The substitution was supported by results obtained in an interlaboratory study by 24 laboratories in 12 countries. Each laboratory analyzed 12 test samples of milk as blind duplicates in a double split level design with high, medium, and low nitrogen concentrations. The method protocol requires the concurrent analyses of an ammonium salt solution and a tryptophan solution as internal quality control standards with a minimum nitrogen recovery between 99 and 100% for the former and at least 98% for the latter. The repeatability and reproducibility relative standard deviations are 0.5 and 1%, respectively, for the range 0.35-0.70 g N/100 g. The performance of the laboratories that did not meet the required quality control specifications was clearly poorer than that of those that did meet the specifications.

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