Evaluation of Agreement Among Routine Methods for Determination of Fluoride in Vegetation: Interlaboratory Collaborative Study

1982 ◽  
Vol 65 (5) ◽  
pp. 1150-1154
Author(s):  
Jay S Jacobson ◽  
John J Troiano ◽  
Christina C Cosentini ◽  
John Evans
Keyword(s):  
Significant Interaction ◽  
Collaborative Study ◽  
Considerable Improvement ◽  
The Other ◽  
Mean Values ◽  
Potentiometric Analysis ◽  
Aoac Official ◽  
Vegetation Samples ◽  
Action Methods

Abstract An interlaboratory collaborative study was conducted to evaluate the performance of methods and laboratories for the measurement of fluoride in vegetation. Samples of 8 plant species containing about 5-200 ppm fluoride were distributed to 40 participants who were instructed to use their routine methods of analysis. Methods which had sufficient participants to allow the inclusion of results in statistical analyses were classified into 3 categories: (1) Willard-Winter method (similar to the AOAC official final action method); (2) semiautomated and potentiometric methods (similar to the 2 AOAC official first action methods); and (3) potentiometric analysis with prior ashing, fusion, and/or distillation (not an approved method). There was a significant interaction of methods with samples caused by 3 of the 8 samples. In the other 5 samples, the Willard-Winter and semiautomated methods gave higher mean values for fluoride content than did the 2 potentiometric methods. Despite considerable improvement in speed and simplicity of fluoride analyses during the last decade, agreement between laboratories has not improved because of the variety of methods and techniques in use, the inherent differences between methods, and, apparently, poor laboratory quality control.

Colorimetric Determination of Hydroxyproline as Measure of Collagen Content in Meat and Meat Products: NMKL Collaborative Study

1990 ◽  
Vol 73 (1) ◽  
pp. 54-57 ◽  
Author(s):  
Kurt Kolar
Keyword(s):  
Collaborative Study ◽  
Colorimetric Method ◽  
Meat Products ◽  
Acid Oxidation ◽  
Colorimetric Determination ◽  
Mean Values ◽  
Collaborative Studies ◽  
Freeze Dried ◽  
Analytical Result

Abstract A colorimetric method for the determination of hydroxyproline as a measure of collagen in meat and meat products has been collaboratively studied in 18 laboratories. The method includes hydrolysis with sulfuric acid, oxidation with chloramine- T, and formation of a reddish purple complex with 4- dimethylaminobenzaldehyde. Five frozen and 3 freeze-dried samples were tested, ranging in content from 0.11 to 0.88% and from 0.39 to 4.0% hydroxyproline, respectively. The mean values of 2 identical samples were 0.245 and 0.251 %. The average recovery from a spiked sample was 96.1 %. The hydroxyproline content of a known sample (a mixture of 2 samples in the ratio 5:2) was calculated to 1.42%, which agrees well with the analytical result, 1.40%. In comparison with other collaborative studies, based on the ISO analytical method, the repeatability and reproducibility of this method agree well with the other results. This method was accepted as an official NMKL method by all national Committees, and has been adopted official first action by AOAC as an NMKLAOAC method.

Pleasingness vs Interestingness of Visual Stimuli with Controlled Complexity: Their Relationship to Looking Time as a Function of Exposure Time

1975 ◽  
Vol 40 (1) ◽  
pp. 3-7 ◽  
Author(s):  
Gerda Smets
Keyword(s):  
Exposure Time ◽  
Binocular Rivalry ◽  
Stimulus Pair ◽  
Significant Interaction ◽  
Visual Stimuli ◽  
The Other ◽  
Stimulus Complexity

Ss take more time to perceive interesting/displeasing stimuli than uninteresting/pleasing ones. This is consistent with the results of former experiments. However we used a different operationalization of looking time, based on binocular rivalry. Each of six stimulus pairs was presented in a stereoscope. One member of each pair was interesting but displeasing in comparison to the other member. Stimulus complexity was under control. Due to binocular rivalry Ss perceived only one pattern a time. 20 Ss were asked to indicate which pattern they actually saw by pushing two buttons. For each stimulus pair was registered how long each button was pushed during each of six successive minutes. Unlike other operationalizations this one is less dependent on S's determination of what stimulus will be looked at or for how long. It has the advantage that it is bound up more exclusively with relations of similarity and dissimilarity between stimulus elements. It allows manipulation of exposure time in a systematic and continuous way. There is no significant interaction between looking and exposure time.

scholarly journals Comparison of Babcock and Ether Extraction Methods for Determination of Fat Content of Cream: Collaborative Study

1996 ◽  
Vol 79 (4) ◽  
pp. 907-916 ◽  
Author(s):  
Joanna M Lynch ◽  
David M Barbano ◽  
J Richard Fleming
Keyword(s):  
Extraction Method ◽  
Collaborative Study ◽  
Extraction Methods ◽  
Fat Content ◽  
Official Method ◽  
Ether Extraction ◽  
Aoac Official ◽  
The Difference ◽  
Aoac Official Method

Abstract A modified Mojonnier ether extraction method for determination of the fat content of cream was developed based on the method for milk (AOAC Official Method 989.05). The cream Babcock method (AOAC Official Method 920.111 B-C) was modified to harmonize with the milk Babcock method (AOAC Official Method 989.04) and to clarify procedural details. Using the AOAC collaborative study format, 10 laboratories tested 9 pairs of blind duplicate heat-treated cream samples with a fat range of 30-45% using both methods. The statistical performance (invalid and outlier data removed) was as follows: mean % fat = 37.932, sr = 0.125, sR = 0.151, RSDr = 0.330, RSDR = 0.398, r = 0.354, and R = 0.427 for the ether extraction method. For the Babcock method, mean % fat = 38.209, sr = 0.209, SR = 0.272, RSDr = 0.548, RSDR = 0.712, r = 0.592, and R = 0.769. Average test results for fat from the Babcock method were 0.277% (absolute fat) greater than for the Mojonnier ether extraction method. The difference between methods, as a percentage of the average fat content of the samples, was 0.73%. This agrees with differences observed between the 2 methods for milk when 10 to 17 laboratories tested 7 milk samples in blind duplicate at bimonthly intervals over a 4-year period (average difference 0.029% fat, 0.78% as a percentage of average fat content). The Mojonnier ether extraction and Babcock methods for fat in cream have been adopted by AOAC INTERNATIONAL. The new Babcock method replaced the AOAC Official Method 920.111 B-C.

Potassium Interferences in Flame Emission Method for Determining Sodium in Fertilizers

1984 ◽  
Vol 67 (5) ◽  
pp. 888-889
Author(s):  
Luis F Corominas ◽  
Roberto A Navarro ◽  
Ruben J Lopez
Keyword(s):  
Analysis Of Variance ◽  
Calibration Curve ◽  
Collaborative Study ◽  
Potassium Content ◽  
Emission Method ◽  
Average Recovery ◽  
Flame Emission ◽  
Aoac Official ◽  
Preliminary Determination

Abstract Several sodium concentrations ranging from 5.2 to 20 ppm at K:Na ratios ranging from 0 to 40 were studied to determine potassium interferences in the AOAC official first action method, 2.147-2.150, for flame emission spectrophotometric (FES) determination of sodium in fertilizers. According to an analysis of variance performed with recoveries of sodium in solution, potassium interference is the same at low (5.2 ppm) or high (20 ppm) sodium concentrations but is different when the K:Na ratio is changed. A Duncan test showed that potassium interference is equivalent only in the adjacent ratios studied (0, 1, 2, 5, 10, 20, 40) and not for larger ranges. We obtained an average recovery of 98.8% using a calibration curve for a K:Na ratio from a preliminary determination with a calibration curve without potassium content. It is essential to know the potassium content of the sample to enable preparation of a calibration curve for correction. We recommend a collaborative study of NPK samples to determine whether to modify the FES method.

Report of Ad Hoc Committee on Vitamin D Methodology, AOAC

1975 ◽  
Vol 58 (2) ◽  
pp. 330-332
Author(s):  
Forrest W Quackenbush ◽  
Daniel Banes ◽  
Philip H Derse
Keyword(s):  
Maleic Anhydride ◽  
Chemical Method ◽  
Ad Hoc ◽  
Collaborative Study ◽  
Mean Values ◽  
Biological Tests ◽  
Aoac Official ◽  
The Mean ◽  
Biological Methods ◽  
Good Agreement

Abstract In a collaborative study 6 samples of vitamin D3 resins were analyzed chemically by 9 laboratories and tested biologically by 3 laboratories to determine whether there exists a discrepancy between chemical and biological methods of measuring potency of these materials. The chemical methods employed saponification with and without subsequent maleic anhydride treatment. The biological method was the AOAC official final action rat assay, 39.149–39.162. The results showed good agreement between laboratories in the chemical analysis and relatively poor agreement in the biological tests. However, based upon the mean values as reported by the different laboratories, the chemical method employing saponification alone consistently overestimated biopotency, whereas the chemical method including maleic anhydride treatment gave results which averaged much closer to the mean biopotency values. There was no evidence that maleic anhydride treatment reduced values significantly below biopotency values.

scholarly journals Determination of Cholecalciferol (Vitamin D3) in Selected Foods by Liquid Chromatography: NMKL Collaborative Study

2003 ◽  
Vol 86 (2) ◽  
pp. 400-406 ◽  
Author(s):  
Anders Staffas ◽  
Arne Nyman ◽  
K Ask ◽  
E Hermansson ◽  
J S Jacobsen ◽  
...  
Keyword(s):  
Liquid Chromatography ◽  
Standard Deviation ◽  
Fish Oil ◽  
Vitamin D3 ◽  
Collaborative Study ◽  
The Other ◽  
Vitamin D2 ◽  
Cooking Oil ◽  
Relative Standard

Abstract Results are presented from an NMKL (Nordic Committee on Food Analysis) collaborative study of a method for the determination of cholecalciferol (vitamin D3) in foods. The method is based on the addition of an internal standard (vitamin D2), followed by saponification and extraction with n-heptane. The fraction that contains vitamin D2/D3 is separated by preparative normal-phase liquid chromatography (LC), and the analytes are determined by reversed-phase LC with UV detection at 265 nm. The method was tested by 8 participating laboratories. In this study 6 different matrixes were analyzed for cholecalciferol content: milk, liquid infant formula (gruel), cooking oil, margarine, infant formula, and fish oil. The contents varied from 0.4 to 12 μg/100 g. Three matrixes (milk, gruel, and margarine) were fortified with vitamin D3. In the other matrixes, vitamin D3 was added at 3 different levels at the Swedish National Food Administration. The milk was analyzed as a blind duplicate, whereas the other matrixes were analyzed as split-level pairs. The recoveries from the samples with vitamin D3 added varied from 93 to 102%. The repeatability relative standard deviation (RSDr) values for accepted results varied between 2.2% (fish oil) and 7.4% (cooking oil), whereas the reproducibility relative standard deviation (RSDR) values varied between 6.8% (margarine) and 24% (cooking oil).

Comparison of Methods for Determining Sodium in Fertilizers

1981 ◽  
Vol 64 (3) ◽  
pp. 704-708
Author(s):  
Luis F Corominas ◽  
Víctor M Boy ◽  
Pedro Rojas
Keyword(s):  
Phosphate Rock ◽  
Collaborative Study ◽  
Ammonium Oxalate ◽  
Selective Electrode ◽  
Accuracy And Precision ◽  
Flame Emission ◽  
Aoac Method ◽  
Aoac Official ◽  
Aas Method

Abstract The AOAC official first action method, 2.147-2.150, for flame emission spectrophotometry (FES) determination of sodium in fertilizers was compared with the atomic absorption spectrophotometric (AAS) method and the sodium selective electrode (SSE) method. Ammonium oxalate, which was previously compared with water, H2SO4, HC1, and HNO3, was used to extract the sample for all 3 methods. Three synthetic NPK samples, 3 commercial samples (urea, normal superphosphate, and neutrophos), 1 phosphate rock, and 2 Magruder check samples were used for the study. Statistically significant differences were obtained in averages for most of the samples, but few differences were found in standard deviations. The AAS method showed the best accuracy and precision. Accuracy of the AOAC method is acceptable. The SSE method showed the highest deviations from the theoretical values. A collaborative study is recommended to compare the AOAC with the AAS method.

Spectrophotometric Determination of Phosphorus in Certifiable Straight Color Additives: Collaborative Study

1981 ◽  
Vol 64 (4) ◽  
pp. 808-813
Author(s):  
Wallace S Brammell ◽  
◽  
C Arozarena ◽  
J Hunter ◽  
H G Kiernan ◽  
...  
Keyword(s):  
Total Phosphorus ◽  
Phosphorus Content ◽  
Collaborative Study ◽  
Mean Values ◽  
Total Phosphorus Content ◽  
Standard Curve ◽  
Coefficients Of Variation ◽  
Molybdovanadophosphoric Acid ◽  
Acid Reagent

Abstract A simple and rapid spectrophotometric method was developed for determining the total phosphorus content of certifiable straight color additives. The dye sample is mixed with a cellulose powder and MgO mixture, and ashed at 500°C in a small Pyrex beaker in a muffle furnace. The ash is dissolved in vanadomolybdic acid reagent and filtered through glass wool, and the absorbance of the resulting yellow molybdovanadophosphoric acid solution is measured at 400 nm. The total phosphorus content of the sample, expressed as percent Na3PO4, is determined from a standard curve. Recovery of phosphorus added as KH2PO4 to 39 different dyes in amounts equivalent to 0.300% Na3PO4 ranged from 95.3 to 106.8%, averaging 100.6%. In the collaborative study, 7 laboratories successfully performed duplicate analyses of 6 different dyes (D&C Orange No. 5, D&C Yellow No. 8, FD&C Blue No. 2, FD&C Red No. 3, FD&C Red No. 40, and FD&C Green No. 3). The mean values found ranged from 0.325 to 6.86% Na3PO4. In general, the accuracy and reproducibility of the method were satisfactory, with single determination coefficients of variation ranging from 3.76 to 9.60%. The method was adopted official first action.

Gas Chromatographic Methods for Determination of γ-BHC in Technical Emulsifiable Concentrates and Water-Dispersible Powder Formulations and in Lindane Shampoo and Lotion: Collaborative Study

1984 ◽  
Vol 67 (4) ◽  
pp. 834-837
Author(s):  
James W Miles ◽  
Dwight L Mount ◽  
◽  
T J Beckmann ◽  
S K Carrigan ◽  
...  
Keyword(s):  
Coefficient Of Variation ◽  
Collaborative Study ◽  
Internal Standard ◽  
The Other ◽  
Water Dispersible ◽  
Coefficients Of Variation ◽  
Aoac Method ◽  
Liquid Chromatographic ◽  
Gas Chromatographic Separation

Abstract Although the gas chromatographic separation of the isomers of BHC was demonstrated two decades ago, the present AOAC method of analysis of BHC for gamma-isomer (lindane) content is based on a separation carried out on a liquid chromatographic partition column. A method of analysis has been developed that uses an OV-210 column for separation of the gamma-isomer from the other isomers and impurities in technical BHC. Di-n-propyl phthalate was chosen as an internal standard. The same system allows quantitation of lindane in lotion and shampoo after these products are extracted with ethyl acetate-isooctane (1 + 4). The analytical methods were subjected to a collaborative trial with 10 laboratories. The coefficient of variation for technical BHC was 2.83%. For the water-dispersible powder and emulsifiable concentrate, the coefficients of variation were 2.89% and 4.62%, respectively. Coefficients of variation for 1% lindane lotion and shampoo were 4.36% and 11.92%, respectively. The method has been adopted official first action.

Gas Chromatographic Determination of Phenolic Compounds in Drug Preparations: Collaborative Study

1972 ◽  
Vol 55 (3) ◽  
pp. 610-612 ◽  
Author(s):  
Carol C Douglas
Keyword(s):  
Phenolic Compounds ◽  
Methyl Salicylate ◽  
Chromatographic Method ◽  
Collaborative Study ◽  
Chromatographic Determination ◽  
The Other ◽  
Gas Chromatographic Method

Abstract A gas chromatographic method for the determination of phenol, methyl salicylate, menthol , and camphor in drug preparations was studied collaboratively by 9 laboratories. Mean recoveries were: phenol 98.2, 106.0, a n d 103.6%; methyl salicylate 103.9, 102.0, and 101.9%; menthol 102.9 and 100.9%; and camphor 101.9 and 100.9%. The method has been adopted as official first action for camphor-containing drugs. Additional study will be done to improve recoveries for the other 3 compounds.

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