The ‘Horwitz ratio’—a study of the ratio between reproducibility and repeatability precisions in the analysis of foodstuffs

2015 ◽  
Vol 7 (1) ◽  
pp. 375-379 ◽  
Author(s):  
Michael Thompson ◽  
Roger Wood
Keyword(s):  
Standard Deviation ◽  
Detection Capability ◽  
Reproducibility Standard Deviation ◽  
Repeatability Standard Deviation

In the analysis of food, the ratio of reproducibility standard deviation to repeatability standard deviation is usually close to 2.0. This has implications in estimating uncertainty and detection capability.

Mass Loss on Drying for Instant Coffee: Collaborative Study

1980 ◽  
Vol 63 (2) ◽  
pp. 178-179
Author(s):  
William P Clinton ◽  
Paul H Manni ◽  
John M Ferry
Keyword(s):  
Standard Deviation ◽  
Mass Loss ◽  
Coefficient Of Variation ◽  
Collaborative Study ◽  
Instant Coffee ◽  
Reproducibility Standard Deviation ◽  
Repeatability Standard Deviation ◽  
Working Method

Abstract A collaborative study was undertaken to define an acceptable routine working method for determination of mass loss in instant coffee. Fourteen laboratories of 24 invited to participate submitted results. The repeatability standard deviation and coefficient of variation were 0.026 and 0.7%, respectively. The reproducibility standard deviation and coefficient of variation were 0.153 and 3.8%, respectively. The method has been adopted as official first action.

Microdiffusion and Fluoride-Specific Electrode Determination of Fluoride in Infant Foods: Collaborative Study

1981 ◽  
Vol 64 (4) ◽  
pp. 1021-1026
Author(s):  
Robert W Dabeka ◽  
Arthur D Mckenzie ◽  
◽  
R A Baetz ◽  
D W Bingham ◽  
...  
Keyword(s):  
Standard Deviation ◽  
Collaborative Study ◽  
Variance Analysis ◽  
Infant Foods ◽  
Reproducibility Standard Deviation ◽  
Coefficients Of Variation ◽  
Repeatability Standard Deviation

Abstract Twelve laboratories analyzed (1 replicate) 12 samples of infant foods – milk, pears, and peas – containing 0.2-5 ppm F. There was one laboratory outlier. Mean coefficients of variation were 7.06% for intralaboratory determination of 3 sets of blind duplicates and 21.6% for interlaboratory determination of 12 samples. Variance analysis for all samples yielded a reproducibility standard deviation of 0.41 ppm; for 3 sets of blind duplicates, repeatability standard deviation was 0.26 ppm and reproducibility standard deviation was 0.32 ppm.

scholarly journals Liquid Chromatographic Determination of Maleic Hydrazide in Technical and Formulated Products: Collaborative Study

2006 ◽  
Vol 89 (4) ◽  
pp. 929-936 ◽  
Author(s):  
James L Mertz ◽  
Dora Y Lau ◽  
David M Borth ◽  
E D Ausan ◽  
O Bennett ◽  
...  
Keyword(s):  
Data Analysis ◽  
Standard Deviation ◽  
Potassium Salt ◽  
Maleic Hydrazide ◽  
Collaborative Study ◽  
Laboratory Data ◽  
Internal Standard ◽  
Reversed Phase ◽  
Reproducibility Standard Deviation ◽  
Repeatability Standard Deviation

Abstract Fourteen collaborating laboratories assayed maleic hydrazide (MH), 6-hydroxypyridazin-3(2H)-one, in technical and formulated products by reversed-phase liquid chromatography (LC) with sulfanilic acid as an internal standard. The active MH in the samples (6 lots) ranged from 16% (expressed as the potassium salt) to 98% (MH in the technical). A small amount of 1 M KOH was added to the technical MH and analytical standards to create the potassium salt of the analyte which is soluble in water. Test samples and standards were extracted with water containing the internal standard before analysis by LC on a C8 column with an ion-pairing eluting solution and UV detection at 254 nm. The concentration of MH was calculated by comparing the peak area response ratios of the analyte and the internal standard with those in the analytical standard solution. Eleven laboratories weighed each test sample twice with single analysis. Three laboratories weighed each sample once and made duplicate injections on the LC system. The data were analyzed using the 11 laboratories' results. A second data analysis was done including all laboratory results using a Youden pair approach, selecting one of 2 duplicate assay values randomly for each laboratory and sample. In the first data analysis, the repeatability standard deviation ranged from 0.07 to 1.39%; reproducibility standard deviation ranged from 0.22 to 1.39%. In the second data analysis (using all laboratory data), repeatability standard deviation ranged from 0.09 to 0.86%; reproducibility standard deviation ranged from 0.22 to 1.31%.

scholarly journals Determination of Selenium in Feeds and Premixes: Collaborative Study

1997 ◽  
Vol 80 (3) ◽  
pp. 469-480 ◽  
Author(s):  
Ivan S Palmer ◽  
Nancy Thiex ◽  
R Allen ◽  
E Alley ◽  
N Anderson ◽  
...  
Keyword(s):  
Statistical Analysis ◽  
Standard Deviation ◽  
Atomic Absorption ◽  
Collaborative Study ◽  
Hydride Generation ◽  
Poor Agreement ◽  
Reproducibility Standard Deviation ◽  
Repeatability Standard Deviation ◽  
Fluorometric Study

Abstract A total of 17 laboratories participated in a collaborative study for the determination of selenium in feeds and premixes using either a fluorometric or a continuous hydride generation atomic absorption (HGAA) method. Each collaborator analyzed 16 blind duplicate samples of feed and premixes from various feed manufacturers. The amount of Se in these materials ranged from 0.2 to 5500 μg/g. Six laboratories used only the fluorometric procedure, 8 laboratories used only the hydride generation atomic absorption procedure, and 3 laboratories used both procedures. One laboratory in the fluorometric study and 3 laboratories in the HGAA study were initially excluded because of invalid data. Poor agreement between the blind duplicates indicated probable sample interchange and/or dilution error. The data from 8 laboratories were submitted to statistical analysis, including data from 2 laboratories participating in both studies. The repeatability standard deviation (RSDr) for samples analyzed by the fluorometric procedure ranged from 5.9 to 33%, and the reproducibility standard deviation (RSDR) ranged from 12 to 33%. RSDf for samples analyzed by HGAA ranged from 2.8 to 18%, and RSDR ranged from 4.0 to 36%. Both fluorometric and continuous hydride generation atomic absorption methods for the determination of Se in feeds and premixes have been adopted first action by AOAC INTERNATIONAL.

scholarly journals Fructans in Foods and Food Products, Ion-Exchange Chromatographic Method: Collaborative Study

1997 ◽  
Vol 80 (5) ◽  
pp. 1029-1039 ◽  
Author(s):  
Hubert Hoebregs ◽  
P Balis ◽  
J De Vries ◽  
J v Eekelen ◽  
P Farnell ◽  
...  
Keyword(s):  
Standard Deviation ◽  
Ion Exchange ◽  
Chromatographic Method ◽  
Collaborative Study ◽  
Food Products ◽  
Food Samples ◽  
Exchange Chromatography ◽  
Reproducibility Standard Deviation ◽  
Repeatability Standard Deviation

Abstract Nine collaborating laboratories assayed 6 blind duplicate pairs of food samples containing the fructans inulin or oligofructose. The 6 sample pairs ranged from low (4%) to high levels (40%). Following the proposed method, the samples were treated with amyloglucosidase and inulinase enzymes and the released sugars were determined byion exchange chromatography. Repeatability standard deviation ranged from 2.9 to 5.8%; reproducibility standard deviation ranged from 4.7 to 11.1%. The ion-exchange chromatographic method for determinationof fructans in food and food products has been adopted first action by AOAC INTERNATIONAL (997.08)

Cylinder Plate Assay for Determining Bacitracin in Premix Feeds and Finished Feeds: Collaborative Study

1982 ◽  
Vol 65 (5) ◽  
pp. 1168-1177
Author(s):  
John B Gallagher ◽  
Linda L Knotts ◽  
◽  
D Brennecke ◽  
H H Bryant ◽  
...  
Keyword(s):  
Standard Deviation ◽  
Collaborative Study ◽  
Reverse Phase ◽  
Average Recovery ◽  
Plate Assay ◽  
The Poor ◽  
Reproducibility Standard Deviation ◽  
Assay Procedure ◽  
Acceptable Method ◽  
Repeatability Standard Deviation

Abstract A cylinder plate assay procedure was studied by 10 laboratories. For premix feeds, 3 samples of bacitracin methylene disalicylic acid and 3 samples of bacitracin zinc premixes covering the range of 10 to 50 g/lb were used. The repeatability standard deviation was 2.11, and the reproducibility standard deviation was 2.13. The average recovery of bacitracin was 101.5%. The method has been adopted official first action. For finished feeds, 6 samples of bacitracin methylene disalicylic acid and 6 samples of bacitracin zinc covering the range of 10 to 800 g/ton were used in the study. The procedure included a sample cleanup step using disposable reverse phase columns. This step appears to be the cause of the poor results reported by most collaborators. Continued study is needed to develop an acceptable method for finished feeds.

scholarly journals Sample Sizes Needed for Specified Margins of Relative Error in the Estimates of the Repeatability and Reproducibility Standard Deviations

2005 ◽  
Vol 88 (5) ◽  
pp. 1503-1510 ◽  
Author(s):  
Foster D McClure ◽  
Jung K Lee
Keyword(s):  
Standard Deviation ◽  
Sample Size ◽  
Relative Error ◽  
Analytical Method ◽  
Actual Error ◽  
Repeatability Standard Deviation ◽  
Repeatability And Reproducibility ◽  
Standard Deviations ◽  
True Values ◽  
Addition Formulas

Abstract Sample size formulas are developed to estimate the repeatability and reproducibility standard deviations (sr and sR) such that the actual error in (sr and sR) relative to their respective true values, σr and σR, are at predefined levels. The statistical consequences associated with AOAC INTERNATIONAL required sample size to validate an analytical method are discussed. In addition, formulas to estimate the uncertainties of (sr and sR) were derived and are provided as supporting documentation.Formula for the Number of Replicates Required for a Specified Margin of Relative Error in the Estimate of the Repeatability Standard Deviation

Colorimetric Method for Carbadox in Feeds: Collaborative Study

1977 ◽  
Vol 60 (5) ◽  
pp. 1059-1063
Author(s):  
John T Goras
Keyword(s):  
Standard Deviation ◽  
Stannous Chloride ◽  
Collaborative Study ◽  
Colorimetric Method ◽  
Feed Supplement ◽  
Colored Complex ◽  
Feed Supplements ◽  
Repeatability Standard Deviation ◽  
Standard Additions ◽  
The Mean

Abstract A colorimetric method for determining carbadox in complete swine feeds and feed supplements was collaboratively studied. Carbadox is separated from feed with CHCl3-methanol (3+1) and then separated from interfering materials by a series of solvent-solvent extractions. The drug is isolated as a dry residue, reconstituted, and reacted with stannous chloride to form a colored complex that is measured at 520 nm. The method of standard additions is used to compensate for a feed or feed supplement matrix effect. Twenty-seven laboratories assayed feeds containing 0.0013, 0.0053, and 0.0242% carbadox. The repeatability standard deviation (σ0) and reproducibility standard deviation (σx) were σ0 = 0.00014%, σx = 0.00035% (29% of grand mean) for 0.0013% carbadox in feed; σ0 = 0.00025%, σx = 0.00037% (6.7% of grand mean) for 0.0053% carbadox in feed; and σ0 = 0.0019%, σx = 0.0024% (9.6% of grand mean) for 0.0242% carbadox in feed. The between-laboratory variance ratio was not significant for feeds containing 0.0013 and 0.0053% carbadox, but was significant for feeds containing 0.0242% carbadox. The mean recovery values for feeds containing 0.0013, 0.0053, and 0.0242% carbadox were 92, 104, and 103%, respectively. The method was adopted as official first action for feeds having a guaranteed potency of 0.0055% carbadox or higher.

Experimental Designs for Interlaboratory Precision Experiments: Comparison of ISO 5725 with Draft NEN 6303

1989 ◽  
Vol 72 (1) ◽  
pp. 34-37 ◽  
Author(s):  
J Zaalberg
Keyword(s):  
Standard Deviation ◽  
Edible Oils ◽  
Collaborative Study ◽  
Experimental Designs ◽  
Interlaboratory Experiments ◽  
Interlaboratory Studies ◽  
Repeatability Standard Deviation ◽  
Level Design ◽  
Iso 5725

Abstract To determine the precision of standardized analytical methods, interlaboratory experiments are carried out in which several laboratories analyze identical samples from well homogenized batches of material. From the test results, estimates of the standard deviations under repeatability as well as under reproducibility conditions are calculated. In the present work, the experimental designs recommended in the International Standard ISO 5725 have been compared with a design proposed in the draft Netherlands Standard NEN 6303. This has been done by comparing their mathematical models as well as by applying them to the results of a recent collaborative study on the determination of heavy metals in edible oils and fats. The reproducibility standard deviation is estimated equally well with both Standards, but it appeared that the designs given in ISO 5725 can lead to serious underestimation (uniform-level design) or overestimation (split-level design) of the repeatability standard deviation. By using the design proposed in NEN 6303, these biases can be avoided. Hence, it is recommended that interlaboratory studies be organized according to the design of NEN 6303.

Modified Method for Carbadox in Feeds: Collaborative Study

1979 ◽  
Vol 62 (5) ◽  
pp. 982-984
Author(s):  
John T Goras
Keyword(s):  
Standard Deviation ◽  
Room Temperature ◽  
Collaborative Study ◽  
Variance Ratio ◽  
Modified Method ◽  
Repeatability Standard Deviation ◽  
Standard Solution ◽  
The Mean ◽  
Optimum Working ◽  
Statistical Results

Abstract The official first action method for carbadox in swine feed, 42.C01-42.C04, was modified in 2 respects. First, the samples were leached overnight at room temperature instead of boiled for 1 hr. This change avoided problems with overheating and excessive evaporation. Second, the dilution scheme for samples spiked with carbadox standard solution was changed to give absorbance values that were within the optimum working range of all types of spectrophotometers. The modified procedure was collaboratively studied by 21 laboratories. The repeatability standard deviation (σo) and reproducibility standard deviation (σo) were σ0 = 0.00029% and σx = 0.00056% (8.9% of grand mean) for feeds containing 0.00617% carbadox; and σo = 0.0012% and σx = 0.0019% (9.3% of grand mean) for feeds containing 0.0198% carbadox. The between-laboratory variance ratio was significant for feeds containing 0.0198% carbadox. The mean per cent of intent values for feeds containing 0.00617% carbadox and 0.0198% carbadox were 102% and 104%, respectively. In general, the statistical results were comparable to those previously obtained for the official first action method. Consequently, the modified procedure is not recommended as a replacement for the official first action method.

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