Collaborative Study of Infrared Methods for Phorate in Formulations

1964 ◽  
Vol 47 (2) ◽  
pp. 245-247
Author(s):  
N Kobekt Pasarela

Abstract An infrared method for the determination of phorate in 5% and 10% granules was studied by 10 collaborators. In the method, the formulation is eluted from the carrier with acetonitrile, the solvent is removed by evaporation, and the residue is dissolved in cyclohexane. The absorbance of the solution is measured at 8.32 μ and the phorate content is determined by comparison with a sample of purified phorate treated in the same manner. Results show good agreement between replicates and laboratories. It is recommended that the method for phorate in granular formulations be adopted as official, first action.

1964 ◽  
Vol 47 (2) ◽  
pp. 283-286
Author(s):  
D P Johnson

Abstract Collaborative study of a method for Sevin insecticide residues was repeated with apples and lettuce as test crops. The method is based on alkaline hydrolysis of Sevin and colorimetric determination of the resulting 1-naphthol with p-nitrobenzenediazonium fluoborate as chromogenic agent. Data from 5 collaborators were in good agreement with an average recovery of 87.8% at 2 concentration levels. It is recommended that the method be adopted as official, first action.


1970 ◽  
Vol 53 (3) ◽  
pp. 575-578
Author(s):  
Ben Estrin ◽  
Frederick E Boland

Abstract A collaborative study was conducted to compare a spectrophotometric molybdovanadate method and the official gravimetric quinoline molybdate fertilizer method 2.025(b), slightly modified, with the official volumetric method 20.032. Six collaborating laboratories analyzed dilute acid solutions of the ash of 5 different kinds of fruit products and an aqueous solution containing only KH2PO4 by each of the 3 methods. Satisfactory agreement between laboratories and good agreement between methods were obtained. From the results of this collaborative study it appears that the quinoline molybdate and the molybdovanadate methods are more accurate and precise than the official volumetric method. It is recommended that both the spectrophotometric molybdovanadate method and the gravimetric quinoline molybdate method for the determination of phosphorus in fruits and fruit products be adopted as official first action.


1971 ◽  
Vol 54 (3) ◽  
pp. 725-727 ◽  
Author(s):  
Frederick E Boland ◽  
Dorothy D Paige

Abstract Dyer’s method for the determination of trimethylamine was collaboratively studied. Six samples of fish extract and one standard solution were sent to each of 9 collaborators. The results from one laboratory differed significantly from the remainder and were not included in the statistical analysis. The results from the remainder of the collaborators were generally in good agreement. Results clearly differentiate between the acceptable and decomposed samples which were used in this study. The method for determining trimethylamine nitrogen in fish has been adopted as official first action.


1972 ◽  
Vol 55 (5) ◽  
pp. 1027-1030 ◽  
Author(s):  
John L Iverson

Abstract A joint AOAC-OICC method for determining ash in cacao products, combining the best features of AOAC method 13.003 and OICC method 4a-E/1952 and with an ashing temperature of 600°C, has been developed. The results from an international collaborative study with 12 collaborators were in good agreement. The preferred method is pre-ashing of the sample under infrared lamps, followed by overnight ashing, thus eliminating reweighing at intervals to arrive at constant weight. The method for determining ash in cacao products has been adopted as official first action.


1970 ◽  
Vol 53 (3) ◽  
pp. 474-475
Author(s):  
John L Iverson

Abstract The sample is dispersed in hot water, filtered, and cooled and the pH of the filtrate is measured with a pH meter standardized against standard buffers. Results of a collaborative study show good agreement between samples and laboratories. It is recommended that the method be adopted as official first action.


1976 ◽  
Vol 59 (1) ◽  
pp. 141-147
Author(s):  
Rodney J Noel

Abstract An automated macro Kjeldahl instrument determines per cent protein at the rate of 20 samples/hr. The methodology involved is similar to the present official final action Kjeldahl method, sec. 7.016. The 2 methods were compared in a collaborative study. Sixteen animal feeds, 4 meats, tryptophan, ammonium dihydrogen phosphate NBS standard, and ammonium sulfate primary standard were analyzed by the participating laboratories. The data were treated statistically and the results showed good agreement between the 2 methods. The automated method has been adopted as official first action for the determination of crude protein in feeds, plants, and cereal foods.


1999 ◽  
Vol 82 (5) ◽  
pp. 1156-1162 ◽  
Author(s):  
Mark Laikhtman ◽  
Jeffrey S Rohrer

Abstract Choline was determined in infant formula by ion chromatography with suppressed conductivity detection. Samples were digested with 1M hydrochloric acid, filtered, diluted, and injected into the chromatographic system. Choline and the alkali and alkaline earth metals were separated on a high-resolution cation-exchange column and detected by suppressed conductivity. The method was linear between 2 and 200 mg/L (r2 = 0.9999), the concentration range of the diluted samples. This method accurately determined choline in powdered, concentrated, and ready-to-feed infant formulas. Recoveries of choline spikes into powdered infant formula at approximately 1, 0.8, 0.5, and 0.2 times the labeled value ranged from 85 to 114%. This method had good agreement for 8 blind duplicates. The values determined for these samples, which were used in an AOAC collaborative study of an enzymatic method, were consistent with the values determined by the enzymatic method.


1982 ◽  
Vol 65 (3) ◽  
pp. 696-700 ◽  
Author(s):  
Ole-Christian Bjarnø ◽  
◽  
W Arneth ◽  
W Noack ◽  
G Pfeiffer

Abstract A new method for rapid multicomponent analysis of meat products based on infrared transmission was tested in a collaborative study with 4 laboratories. A series consisting of 31 samples of different meats, cooked sausage, liver sausage, and fermented sausage was distributed and analyzed at all laboratories for protein, fat, and water by the present method and by well established reference methods. There was no significant difference between the infrared method and reference methods at the 95% confidence level for determination of protein, fat, and water in meat products. There is a great


1966 ◽  
Vol 49 (4) ◽  
pp. 726-730 ◽  
Author(s):  
Bobby R Eader

Abstract A collaborative study was conducted to compare the near-infrared spectrophotometric method and a Karl Fischer volumetric method with a vacuum oven method for the determination of moisture. Results by the near-infrared method were as accurate as and more rapid and specific than the vacuum oven method. Results by the Karl Fischer method were not as satisfactory; more study is needed to improve the precision of the method.


1971 ◽  
Vol 54 (3) ◽  
pp. 706-710
Author(s):  
Marshall Malina

Abstract A collaborative study was conducted on direct and indirect infrared methods of analysis for both dicamba-MCPA aqueous formulations and dicamba-2,4-D aqueous formulations. Twelve laboratories participated in this study, including 3 international CIPAC member laboratories. The indirect methods require acidification, followed by extraction of the formulation samples before quantitative measurement, which is performed by comparing the absorbance of the sample to that of a prepared reference standard. In the direct methods, the absorbances of solutions of the untreated sample are directly compared with those of the prepared reference standard. The results on both formulations from the 12 collaborating laboratories exhibit excellent precision and accuracy for the indirect infrared method, with the following coefficients of variation: dicamba-MCPA, 0.059 and 0.063, respectively; and dicamba-2,4-D, 0.057 and 0.091, respectively. The method has been adopted as official first action. Five laboratories participated in the study of the direct infrared methods and, although results indicate that these methods also exhibit excellent precision, the accuracy obtained is less than desirable.


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