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.

Preliminary Comparison of Methods for Determining Sodium in Fertilizers

1980 ◽  
Vol 63 (3) ◽  
pp. 551-553
Author(s):  
Luis F Corominas ◽  
Victor M Boy ◽  
Manuel Guijosa
Keyword(s):  
Atomic Absorption ◽  
Experimental Work ◽  
Check Sample ◽  
Comparison Of Methods ◽  
Selective Electrode ◽  
Flame Emission ◽  
Aoac Method ◽  
Aoac Official ◽  
Aas Method

Abstract The AOAC official first action method 2.147–2.150 for the flame emission spectrophotometric (FES) determination of sodium in fertilizers was compared with the atomic absorption spectrophotometric (AAS) method and the sodium selective electrode (SSE) method. Two synthetic NPK samples, 3 commercial samples (urea, DAP, and superphosphate), 2 Magruder NPK check samples, and one Magruder muriate check sample were used for the study. Statistically significant differences were obtained in both averages and standard deviations for all samples. In general, the precision for all methods was acceptable; the AAS method seems to be the more accurate; the AOAC method needs to be revised; and the SSE method has the tendency to give higher values. Additional experimental work is necessary to define which method is the most convenient.

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.

Collaborative Study of Ion Selective Electrode Method for the Direct Determination of Fluoride in Feeds

1975 ◽  
Vol 58 (3) ◽  
pp. 477-481 ◽  
Author(s):  
Laszlo Torma
Keyword(s):  
Standard Deviation ◽  
Collaborative Study ◽  
Direct Determination ◽  
Ion Selective Electrode ◽  
Official Method ◽  
Selective Electrode ◽  
Standard Curve ◽  
Electrode Method ◽  
Aoac Method

Abstract A rapid and precise method for the determination of fluoride in feeds employs HC1 extraction of the sample. Acetate buffer and sodium citrate are added to control pH and ionic strength. The amount of fluoride is calculated from a standard curve after measuring the potentials of standard and sample solutions. Eight collaborators participated in the study of the method. Statistical values on 3 pairs of samples were calculated. The standard deviation, precision, coefficient of variation, and bias, respectively, were: Pair 1, 0.005071, 0.001763, 3.09, 0.0034; Pair 2, 0.037122, 0.006475, 1.82, 0.0258; Pair 3, 0.034587, 0.013021, 2.63, 0.0227. The results from the proposed method agreed favorably with the values obtained by using the official final action AOAC method, 7.089. The average and standard deviation, respectively, for individual samples by the proposed method were: Sample 3, 0.049, 0.0029; Sample 4, 0.059, 0.0021; Sample 5, 0.334, 0.0114; Sample 6, 0.341, 0.0101; Sample 7, 0.511, 0.0219; Sample 8, 0.492, 0.0237. By the official method the values were: Sample 3, 0.049, 0.0041; Sample 4, 0.058, 0.0029; Sample 5, 0.334, 0.0055; Sample 6, 0.331, 0.0082; Sample 7, 0.517, 0.0183; Sample 8, 0.499, 0.0175. The ion selective electrode method has been adopted as official first action.

Collaborative Study of Accuracy and Precision of Rapid Determination of Fat in Meat and Meat Products by Foss-Let Method

1977 ◽  
Vol 60 (4) ◽  
pp. 853-858 ◽  
Author(s):  
Julio D Pettinati ◽  
Clifton E Swift
Keyword(s):  
Food Industry ◽  
Rapid Determination ◽  
Collaborative Study ◽  
Meat Products ◽  
T Test ◽  
Laboratory Sample ◽  
Accuracy And Precision ◽  
Aoac Method ◽  
Better Than

Abstract Collaborators in 12 meat and food industry laboratories performed 4 fat determinations each on 7 samples of meat and meat products by the rapid (7–10 min) Foss-Let method and compared the results with those obtained by AOAC method 24.005(a) or 24.005(b). From the overall mean of results on all samples, determinations by the Foss-Let method averaged 0.11% fat higher than by the AOAC method. This difference was not significant by the t-test (P = 0.05), which indicated agreement between the compared methods in determining fat content. Precision of the Foss-Let method was equivalent to and generally slightly better than that of the AOAC method. Standard deviations with the Foss-Let method were 0.2 % fat for between-duplicates and for within-laboratory repeatability; 0.4% fat for between-laboratories, including variation due to laboratory-sample interaction; and 0.5% fat for reproducibility between analysts in different laboratories. The Foss-Let method has been adopted as official first action.

Ammonia-Selective Electrode Determination of Nitrogen in Fertilizers

1981 ◽  
Vol 64 (5) ◽  
pp. 1096-1099
Author(s):  
Victor M Boy ◽  
Manuel Guijosa
Keyword(s):  
Magnesium Oxide ◽  
Total Nitrogen ◽  
Ammoniacal Nitrogen ◽  
Selective Electrode ◽  
Nitrogen Determination ◽  
Accuracy And Precision ◽  
Routine Work ◽  
Electrode Method ◽  
Aoac Official

Abstract The official AOAC magnesium oxide method (MOM), 2.065, for determining ammoniacal nitrogen in fertilizers not containing urea was compared with an alternative ammonia-selective electrode method (ASEM-1). Likewise, the official AOAC Raney powder method (RPM), 2.063-2.064, for determining total nitrogen in fertilizers, except nitric phosphates containing nonsulfate S, was compared with an ammonia- selective electrode method (ASEM-2). Each comparison included 6 samples. For ammoniacal nitrogen determination, MOM and ASEM-1 showed equivalent precision, although significant statistical differences were obtained in average values for the majority of samples. For total nitrogen determination, RPM and ASEM-2 showed equivalent precision, although significant statistical differences were obtained in 3 samples. The AOAC official methods showed better accuracy than ASEM-1 and ASEM-2. However, the accuracy and precision of ASEM-1 for ammoniacal nitrogen is suitable for routine work.

Determination of Biuret in Urea and Mixed Fertilizers by Cupric Ion Selective Electrode

1986 ◽  
Vol 69 (1) ◽  
pp. 119-122
Author(s):  
Luis F Corominas ◽  
Roberto A Navarro ◽  
Pedro Rojas ◽  
José L Cruz
Keyword(s):  
Atomic Absorption ◽  
Copper Complex ◽  
Confidence Level ◽  
Collaborative Study ◽  
Ion Selective Electrode ◽  
Selective Electrode ◽  
Cupric Ion ◽  
Excess Copper ◽  
Aas Method

Abstract A method for determining biuret in urea and mixed fertilizers by using a cupric ion selective electrode (CISE) has been developed to take advantage of the simplicity of the apparatus. The method is based on the same principle as the atomic absorption spectrophotometric (AAS) method, 2.091-2.093: formation of a biuret-copper complex, elimination of excess copper, and determination of complexed copper. However, some changes were needed to eliminate starch and alcohol interferences. The method was tested for ruggedness and then compared with the AAS method for 4 fertilizer samples. Averages and variances were equivalent at the 99% confidence level according to t- and F-tests. A collaborative study is recommended to compare behavior of both methods in different laboratories.

Allyl Isothiocyanate in Mustard Seed

1970 ◽  
Vol 53 (1) ◽  
pp. 1-3 ◽  
Author(s):  
Donald L Andersen
Keyword(s):  
Allyl Isothiocyanate ◽  
Mustard Seed ◽  
Official Method ◽  
Average Recovery ◽  
Aoac Method ◽  
Aoac Official ◽  
Mustard Seeds ◽  
Column Preparation ◽  
Aoac Official Method

Abstract A new GLC method for the determination of allyl isothiocyanate in mustard seed was compared to a method of the Midwest Research Institute and to a combination of the AOAC official method and the proposed method. Twelve collaborators compared the AOAC method and the GLC method, using whole mustard seeds. Each collaborator assayed three seed portions by both methods. The range, standard deviation, and coefficient of variation are less for each seed portion by the proposed than by the official method. The average recovery value of allyl isothiocyanate in the prepared standard solutions is lower, using the proposed GLC procedure, but seed assay values are significantly and consistently higher for each seed portion when compared with the results for the AOAC method. Reports from the collaborators also indicate that the proposed method is rugged, as the GLC column preparation was subjected to many changes. It is recommended that the GLC method be adopted as official first action.

Multiresidue Gas Chromatographic Method for Determining Organochlorine Pesticides in Poultry Fat: Collaborative Study

1984 ◽  
Vol 67 (2) ◽  
pp. 284-289 ◽  
Author(s):  
James A Ault ◽  
Tim E Spurgeon ◽  
◽  
M M Anderson ◽  
R Bowers ◽  
...  
Keyword(s):  
Chromatographic Method ◽  
Collaborative Study ◽  
Gel Permeation Chromatography ◽  
Accuracy And Precision ◽  
Coefficients Of Variation ◽  
Poultry Fat ◽  
Gel Permeation ◽  
Detector Method ◽  
Gas Chromatographic Method

Abstract A gas chromatographic electron capture detector method is described for the quantitative determination of organochlorine pesticide residues in poultry fat. The samples are rendered and cleaned up using automated gel permeation chromatography. The collaborative samples consisted of 10 fortified samples and one incurred residue sample, all in duplicate. Fortification levels ranged from 0.15 to 1.0 ppm for a-BHC, lindane, cis- and frans-chlordane, octachlor epoxide, o,p' and p,p'-DDT, p,p'-DDE, p,p'-TDE, hexachlorobenzene, heptachlor epoxide, dieldrin, endrin, methoxychlor, mirex, and toxaphene. The average recovery was 91.9% with a range of 81-102%. The ranges of coefficients of variation were: CVo = 3.39-14.79%; CVL = 0-16.6%; and CVx = 5.82-19.0%. The results indicate accuracy and precision comparable to other official methodology. The method has been adopted official first action.

scholarly journals Comparison of Vitros Dry Slide Technology for Determination of Lithium Ions with Other Methods

2006 ◽  
Vol 6 (2) ◽  
pp. 32-36
Author(s):  
Nafija Serdarević ◽  
Ivan Malešić ◽  
Franc Kozjek
Keyword(s):  
Reference Method ◽  
Absorption Spectrometry ◽  
Lithium Carbonate ◽  
T Test ◽  
Selective Electrode ◽  
Lithium Ions ◽  
Control Precision ◽  
Aas Method ◽  
Sera Samples

The lithium ions concentration in human serum was determined using Dry-slide technology Vitros 250 Analyser (Ortho Clinical Diagnostic), atomic absorption spectrometry (AAS) method Perkin Elmer 403 and ion-selective electrode (ISE) potentiometry AVL 9181. We compared lithium ions results in sample sera between these methods. Our reference method was AAS. We analyzed lithium ions concentration in 23 sera samples of patients after oral administration of lithium carbonate (3x 300mg) Jadran, Galen Laboratory Rijeka, by dry-slide technology, AAS and ISE methods. The quality control, precision, reproducibility and accuracy for Vitros dry slide technology were assessed. We established that the main difference between AAS method and dry slide technology was not statistically significant at p< 0.05 according to Student t-test. Therefore, the dry slide technology may be a useful alternative or it may even replace other methods, such as AAS. The main difference between dry slide technology and ISE methods was statistically significant at p<0.05 using Student t-test. By ISE method, we obtained considerably higher results, which may be explained by the presence of electrolytes or medicaments interfering with lithium ions.

Collaborative Study of the Quantitative Gas-Liquid Chromatographic Determination of Fusel Oil and Other Components in Whisky

1972 ◽  
Vol 55 (3) ◽  
pp. 549-556
Author(s):  
J H Kahn ◽  
E T Blessinger
Keyword(s):  
Ethyl Acetate ◽  
Collaborative Study ◽  
Chromatographic Determination ◽  
Official Method ◽  
Fusel Oil ◽  
Fusel Alcohols ◽  
Aoac Method ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic

Abstract Fifteen chemists participated in a collaborative study for the quantitative pas-liquid chromatographic determination of the individual fusel alcohols and ethyl acetate in whisky. Two levels of congeners represented by 4 coded samples of whisky were analyzed by using t h e proposed method, employing a glycerol-1,2,6-hexanetriol column, and the official AOAC method, 9.063-9.065. Since isobutyl and the atnyl alcohols comprise by far the greatest part of fusel oil, their determination is of major importance to the total fusel oil content . Statistical analyses show that the proposed method is superior to the AOAC method for the determination of these alcohols, whereas the official method is superior for the determination of ethyl acetate and n-propyl alcohol. In general, collaborators employing modern instrumentation preferred the proposed method over the AOAC method. The former method also separates and permits the quantitative measurement of active amyl and isoamyl alcohols. The proposed method has been adopted as official first action as an alternative to 9.063–9.065 for the determination of higher alcohols and ethyl acetate in whisky.

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