How Rugged Are Our Nitrogen Methods?

1965 ◽  
Vol 48 (3) ◽  
pp. 501-507
Author(s):  
W G Burgh ◽  
J A Brabson
Keyword(s):  
Salicylic Acid ◽  
Standard Deviation ◽  
Total Nitrogen ◽  
Reduction Method ◽  
Official Method ◽  
Powder Method ◽  
Catalyst Powder ◽  
Time Of Reaction

Abstract Youden’s ruggedness test was made of two official methods and four more recent methods for the determination of total nitrogen in fertilizers containing nitrates. Among the variables tested were amounts of nitrogen and reductant, effect of chloride, and time of reaction of reductant. Official method 2.039 (reduced-iron) failed the test. In order of increasing standard deviation, the five methods that passed the test were the chromous reduction method, Raney-catalyst-powder method, official method 2.037 (salicylic acid), improved reduced-iron method, and the chromiumpowder method.

An Unforeseen Problem in the Use of Kel-Paks

1968 ◽  
Vol 51 (6) ◽  
pp. 1290-1295
Author(s):  
T C Woodis ◽  
J A Brabson ◽  
W G Burch
Keyword(s):  
Salicylic Acid ◽  
Nicotinic Acid ◽  
Organic Compounds ◽  
Total Nitrogen ◽  
Ammoniacal Nitrogen ◽  
Powder Method ◽  
Catalyst Powder ◽  
Possible Cause ◽  
Digestion Step

Abstract In Kjeldahl methods for the determination of nitrogen in fertilizers, the digestion temperature must be above 370°C to mineralize the nitrogen in refractory organic compounds such as nicotinic acid. In total nitrogen determinations by the Raney catalyst powder method, temperatures during the digestion step were investigated as a possible cause of occasional low results. Decomposition of the polyethylene envelopes of Kel-Paks in the presence of salts of metallic reductants caused rapid fluctuations and excessive rise in temperature with consequent loss of ammoniacal nitrogen. Complete Kel-Paks can be used without difficulty in methods such as 2.044 (for nitrate-free samples) or 2.045 (salicylic acid) that do not use metallic reductants, but only the contents of the Kel-Paks without the envelopes should be used when Raney catalyst or chromium powders have been used to reduce nitrates.

Determination of Total Nitrogen in Fertilizers

1965 ◽  
Vol 48 (2) ◽  
pp. 401-406
Author(s):  
H A Davis ◽  
W E Urban
Keyword(s):  
Nickel Catalyst ◽  
Raney Nickel ◽  
Total Nitrogen ◽  
Official Method ◽  
Chromium Powder ◽  
Powder Method ◽  
Raney Nickel Catalyst ◽  
Catalyst Powder ◽  
Iron Chromium

Abstract Five methods, AOAC 2.037, 2.039, modified reduced iron, chromium powder, and Raney nickel catalyst powder for the determination of total nitrogen in fertilizers, were submitted to collaborators for study. Twelve laboratories participated and completed the work. No one method was “best.” The modified reduced iron, chromium powder, and Raney nickel catalyst powder methods gave essentially equal results, but the chromium powder method is favored for case of operation and time required. However, if considerable organic matter and nitrate are present in a sample, satisfactory results may not be obtained. The analyst should select the official method best suited to the makeup of the sample. It is recommended that the chromium powder method he adopted as official, first action, and that study be continued with the modified reduced iron and Raney nickel catalyst methods, including helpful proposals in developing a method that may be applicable to all fertilizers.

An Improved Raney Catalyst Powder Method for Determination of Nitrogen in Fertilizers

1965 ◽  
Vol 48 (6) ◽  
pp. 1111-1115
Author(s):  
W G Burch ◽  
J A Brabson
Keyword(s):  
Sulfuric Acid ◽  
Total Nitrogen ◽  
Organic Nitrogen ◽  
Nitrogen Compounds ◽  
Test Results ◽  
Powder Method ◽  
Catalyst Powder ◽  
Good Agreement

Abstract With a Raney catalyst powder containing 10% Co, 40%; Ni, and 50% Al, nitrates are reduced to ammonia in 8N sulfuric acid in 10 minutes. Neither chlorides nor organic nitrogen compounds interfere with the reduction, and the reduction passed Youden’s ruggedness test. Results of analyses of fertilizers for total nitrogen that included reduction with the powder were in good agreement with those of accepted methods.

Total Nitrogen in Fertilizers

1968 ◽  
Vol 51 (4) ◽  
pp. 851-857
Author(s):  
Paul R Rexroad ◽  
Gary F Krause
Keyword(s):  
Total Nitrogen ◽  
Collaborative Study ◽  
New Method ◽  
Official Method ◽  
Powder Method ◽  
Catalyst Powder

Abstract A three-laboratory collaborative study was made of the comprehensive nitrogen method and the new Raney catalyst powder method for total nitrogen in fertilizers. Both methods worked quite well and, with minor modifications, they should provide the basis for a broader collaborative stvidy to provide an official method for total nitrogen in fertilizer applicable to all samples. The limitations of method 2.045 are reviewed and a rephrasing of the official applications of the method is recommended. Further work is recommended toward adoption of a new method and possible deletions or change of status in current official methods.

Total Nitrogen Methods—Applicable to All Fertilizer Samples

1970 ◽  
Vol 53 (3) ◽  
pp. 450-456
Author(s):  
Paul R Rexroad ◽  
Gary F Krause
Keyword(s):  
Salicylic Acid ◽  
Total Nitrogen ◽  
Collaborative Study ◽  
Official Method ◽  
Chromium Powder ◽  
Powder Method ◽  
New Methods

Abstract An extensive collaborative study was conducted to evaluate a comprehensive nitrogen method and a Raney powder method for acceptance as official methods. Twenty-nine laboratories participated; 10 samples were used and the new methods were compared to the official method, 2.045 (sulfuric-salicylic acid). Evaluation of the data and overall consideration lead to the recommendation that both new methods be adopted as official. It is recommended that 2.047 (reduced iron) and 2.049 (chromium powder) be deleted as official methods.

Total Nitrogen in Fertilizer: Collaborative Study

1978 ◽  
Vol 61 (2) ◽  
pp. 299-306
Author(s):  
Paul R Rexroad ◽  
Gary F Krause
Keyword(s):  
Total Nitrogen ◽  
Collaborative Study ◽  
Oxidation Catalyst ◽  
Official Method ◽  
Probability Level ◽  
Sulfate Sulfur ◽  
Powder Method ◽  
Modified Method ◽  
Accuracy And Precision ◽  
Cent Nitrogen

Abstract A modified comprehensive nitrogen method, using 0.4 g C11SO4 as catalyst, is presented. This method plus a modified Raney powder method (mercury-free) with no metallic oxidation catalyst are compared with the AOAC comprehensive nitrogen method. Results from 19 collaborating laboratories for 11 samples are evaluated. The modified Raney method gave significantly low results on 2 samples: 21-7-14 (nitric phosphates-non-sulfate sulfur) and tryptophan. The results for the average per cent nitrogen for 11 samples from the modified comprehensive nitrogen method were comparable to those from the official method at the 95 % probability level; the overall pooled standard deviations were also similar. In this collaborative study, the modified method (with copper) was equal in accuracy and precision to the official method (with mercury). The modified comprehensive nitrogen method has been adopted as official first action.

Determination of Maleic Hydrazide Residues in Tobacco and Vegetables

1973 ◽  
Vol 56 (5) ◽  
pp. 1164-1172
Author(s):  
Milan Ihnat ◽  
Robert J Westerby ◽  
Israel Hoffman
Keyword(s):  
Standard Deviation ◽  
Present Method ◽  
Maleic Hydrazide ◽  
Collaborative Study ◽  
Official Method ◽  
Sample Weight ◽  
Relative Standard ◽  
The Mean ◽  
Pipe Tobacco

Abstract The distillation-spectrophotometric method of Hoffman for determining maleic hydrazide has been modified to include a double distillation and was applied to the determination of 1–30 ppm maleic hydrazide residues in tobacco and vegetables. Recoveries of 1–23 μg added maleic hydrazide were independent of weight of maleic hydrazide, but did depend on sample and sample weight. The following recoveries were obtained from 0.5 g sample: pipe tobacco, 84%; commercially dehydrated potato, 83%; cigar tobacco, 81%; dried potato, 76%; fluecured tobacco, 73%; dried carrot, 71%. In the absence of sample, the recovery was 82%. When appropriate standard curves were used, maleic hydrazide levels determined in tobacco samples were essentially independent of sample weight in the range 0.1–3 g. The mean relative standard deviation for a variety of field-treated and fortified tobacco samples containing 1–28 ppm maleic hydrazide was 3%. The precision and sensitivity of this procedure seem to be substantial improvements over official method 29.111–29.117. It is recommended that the present method be subjected to a collaborative study.

scholarly journals Simultaneous Determination of Free Carnitine and Total Choline by Liquid Chromatography/Mass Spectrometry in Infant Formula and Health-Care Products: Single-Laboratory Validation

2008 ◽  
Vol 91 (4) ◽  
pp. 777-785 ◽  
Author(s):  
Pierre Andrieux ◽  
Tamara Kilinc ◽  
Christian Perrin ◽  
Esther Campos-Giménez
Keyword(s):  
Health Care ◽  
Standard Deviation ◽  
Simultaneous Determination ◽  
Relative Standard Deviation ◽  
Infant Formula ◽  
Free Carnitine ◽  
Official Method ◽  
Relative Standard ◽  
Single Laboratory

Abstract A single-laboratory validation study was conducted for a liquid chromatographic/mass spectrometric (LC/MS) method for the simultaneous determination of the free carnitine and total choline in milk-based infant formula and health-care products. The sample preparation used for both carnitine and choline was adapted from AOAC Official Method 999.14, with an acidic and enzymatic hydrolysis of esterified forms of choline. Carnitine and choline were quantified by ion-pair chromatography with single-quadrupole MS detection, using their respective deuterated internal standards. The repeatability relative standard deviation was 2.5 and 2.1, respectively, for carnitine and choline. The intermediate reproducibility relative standard deviation was <4.7 and 2.4, respectively, for carnitine and choline. The ranges of the average product-specific recoveries were 9298 and 94103, respectively, for carnitine and choline. Choline concentration determined in infant formula reference material SRM 1846 was in agreement with the reference value. The proposed method was compared with the enzymatic methods for a range of products; good correlation (r = 0.99) was obtained, although a significant bias was observed for both analytes. The method, with a short chromatographic run time (7 min), is convenient for routine analysis to enhance analytical throughput and is a good alternative to enzymatic assays.

scholarly journals Determination of Site-Specific (Deuterium/Hydrogen) Ratios in Vanillin by 2H-NuclearMagnetic Resonance Spectrometry: Collaborative Study

2007 ◽  
Vol 90 (1) ◽  
pp. 187-195 ◽  
Author(s):  
Eric Jamin ◽  
Frédérique Martin ◽  
Gilles G Martin ◽  
I Billault ◽  
A -I Blanch-Cortès ◽  
...  
Keyword(s):  
Standard Deviation ◽  
Collaborative Study ◽  
Official Method ◽  
Site Specific ◽  
Hydrogen Position ◽  
Nmr Spectrometry ◽  
Measuring Site ◽  
Commercial Sources

Abstract The results of collaborative study are reported for a method that determines the site-specific isotope ratios of deuterium/hydrogen (D/H)i in vanillin by deuterium-nuclear magnetic resonance (2H-NMR) spectrometry. This method allows characterization of all the main commercial sources of commercial vanillin and detection of undeclared mixtures. It is based on the fact that the amounts of deuterium at various positions in the vanillin molecule are significantly different from one source to another. Vanillin is dissolved in acetonitrile and analyzed with a high-field NMR spectrometer fitted with a deuterium probe and a fluorine lock. The proportions of isotopomers monodeuterated at each hydrogen position of the molecule are recorded, and the corresponding (D/H) ratios are determined by using a calibrated reference. Nine laboratories analyzed 5 materials supplied as blind duplicates (1 natural vanillin from vanilla beans, 2 synthetic vanillins from guaiacol, 1 semisynthetic vanillin from lignin, and a mixture of natural and synthetic vanillins). The precision of the method for measuring site-specific ratios was as follows: for (D/H)1 the within-laboratory standard deviation (sr) values ranged from 2.2 to 5.8 ppm, and the among-laboratories standard deviation (sR) values ranged from 3.6 to 5.1 ppm; for (D/H)3 the sr values ranged from 1.7 to 3.2 ppm, and the sR values ranged from 2.4 to 3.7 ppm; for (D/H)4 the sr values ranged from 2.3 to 6.2 ppm, and the sR values ranged from 2.4 to 6.4 ppm; for (D/H)5 the sr values ranged from 0.8 to 2.7 ppm, and the sR values ranged from 0.9 to 2.3 ppm. It was shown that these values allow a satisfactory discrimination between vanillin sources. Therefore, the Study Director recommends the method for adoption as a First Action Official Method by AOAC INTERNATIONAL.

scholarly journals A Simple Spectrophotometric Determination of Phosphate in Sugarcane Juices, Water and Detergent Samples

2007 ◽  
Vol 4 (4) ◽  
pp. 467-473 ◽  
Author(s):  
Mahadevaiah ◽  
M. S. Yogendra Kumar ◽  
Mansour S. Abdul Galil ◽  
M. S. Suresha ◽  
M. A. Sathish ◽  
...  
Keyword(s):  
Sulfuric Acid ◽  
Standard Deviation ◽  
Spectrophotometric Method ◽  
Molar Absorptivity ◽  
Official Method ◽  
Sodium Sulphide ◽  
Cane Juice ◽  
Sulfuric Acid Medium ◽  
Sugar Cane Juice

A simple spectrophotometric method is developed for the determination of phosphate in sugar cane juice, water and detergent samples. The method is based on the formation of phosphomolybdate with added molybdate followed by its reduction with sodium sulphide in aqueous sulfuric acid medium. The system obeys Lambert-Beer’s law at 715 nm in the concentration range 0.3-12.24 ppm. Molar absorptivity, correlation coefficient and Sandell’s sensitivity values were found to be 6.1x103mol-1cm-1, 0.999 and 0.0156 µg cm-2respectively. The results obtained were reproducible with acceptable standard deviation 3.7% and relative error 3.4%. For a comparison of the method phosphate present in various samples were also determined separately following an official method. The results of the developed method compare well with those of the official method.

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