Mercury-Free Raney Catalyst Method for Total Nitrogen in Fertilizers

1974 ◽  
Vol 57 (1) ◽  
pp. 10-13
Author(s):  
Frank J Johnson ◽  
Terry C Woodis ◽  
James M Cummings
Keyword(s):  
Total Nitrogen ◽  
Digestion Time ◽  
Sulfate Sulfur ◽  
Powder Method ◽  
Modified Method ◽  
Catalyst Powder ◽  
Considerable Range

Abstract The original Raney catalyst powder method for total nitrogen was shown not to be applicable to nitric phosphates containing non-sulfate sulfur. Interference by the non-sulfate sulfur was eliminated by the addition of morin, a mordant dye, before the reduction. The method was modified further by omitting HgO, a possible pollutant, from the digestion and by shortening the digestion time. The modified method is highly rugged for a considerable range of fertilizer materials.

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.

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.

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.

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.

scholarly journals Relationship between Applied Fertilizer and Accumulated Levels of Nitrogen and Sulfur in a Soilless Mix

HortScience ◽  
1996 ◽  
Vol 31 (4) ◽  
pp. 584a-584
Author(s):  
Ellen T. Paparozzi ◽  
M. Elizabeth Conley ◽  
Walter W. Stroup
Keyword(s):  
Experimental Design ◽  
Total Nitrogen ◽  
Nitrate Nitrogen ◽  
Commercial Production ◽  
Production Schedule ◽  
Total N ◽  
Sulfate Sulfur ◽  
Nitrate N ◽  
Split Plot

Three cultivars of poinsettia, Freedom Red, Lilo and Red Sails, were grown in a peat:perlite:vermiculite mix according to a commercial production schedule. Twelve selected nitrogen–sulfur fertilizer combinations were applied (125, 150, 175 ppm N with either 12.5, 25, or 37.5 ppm S, 225 and 275 ppm N with either 37.5 or 75 ppm S). The experimental design was a split plot with cultivars as the whole plot and fertilizer levels as the split-plot factor. Mix samples were taken initially, at production week 7 and at the end of the experiment. Nitrate-nitrogen, sulfate-sulfur and total nitrogen were determined. Data were analyzed using SAS PROC MIXED. Visually all cultivars responded similarly to all treatments and were salable. Thus, levels of N as low as 125 or 150 with 12.5 ppm S produced quality plants. Sulfate-S tended to accumulate in the mix while nitrate-N and total N did not. Both nitrate-N and sulfate-S concentrations were affected by an interaction between the cultivar and the amount of S applied with `Freedom' better able to utilize available sulfur. `Lilo' removed more nitrate-N and total N from the mix than `Freedom' which removed more than `Red Sails', but only at specific levels of sulfur. There was no cultivar by nitrogen interaction for any variable measured.

A New Approach to the Raney Catalyst Powder Method for Total Nitrogen in Fertilizers

1969 ◽  
Vol 52 (1) ◽  
pp. 23-30 ◽  
Author(s):  
J A Brabson ◽  
T C Woodis
Keyword(s):  
Sulfuric Acid ◽  
Refractory Compound ◽  
Potassium Sulfate ◽  
Dilute Solution ◽  
Commercial Alloy ◽  
New Approach ◽  
Powder Method ◽  
Catalyst Powder ◽  
Time Required

Abstract Further study of the Raney catalyst powder method for the determination of nitrogen in fertilizers established conditions in which the commercial alloy containing 50% Ni and 50% Al was a more efficient reductant for nitrates than an experimental alloy that contained 10% Co. Errors in measurement were decreased, accuracy was increased, and time was saved by adding all the sulfuric acid and part of the potassium sulfate as a single dilute solution and heating the mixture immediately to promote the reduction. Changes in the amounts of reagents, including use of the contents of a Kcl-Pak without the polyethylene envelope, resulted in smoother and more effective Kjeldahl digestions. The method is “rugged” and is equally applicable to the refractory compound nicotinic acid, mixtures of nitrates and organic materials, and the simplest inorganic fertilizers. The time required for an analysis can be further shortened by using “Autopettes” for dispensing the standard acid and a “Titralyzer” for back titrations.

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.

Modification of the Official Fluorometric Method for Selenium in Plants

1975 ◽  
Vol 58 (1) ◽  
pp. 117-121 ◽  
Author(s):  
Oscar E Olson ◽  
Ivan S Palmer ◽  
Earle E Cary
Keyword(s):  
Perchloric Acid ◽  
Ground Glass ◽  
Official Method ◽  
Complete Oxidation ◽  
Digestion Time ◽  
Fluorometric Method ◽  
Special Equipment ◽  
Modified Method ◽  
Wide Range ◽  
Fluorometric Analysis

Abstract The official first action AOAC fluorometric method for selenium in plants, 3.074–3.078, has been modified to simplify the method and to make it more accurate. The digestion time has been increased from 15 to 30 min past the appearance of perchloric acid fumes to better assure complete oxidation of all forms of selenium to selenite. Preparation of the 2,3-diaminonaphthalene solution, the reagent used for fluorometric analysis, has been changed so that the reagent is stable for several weeks; in the previous writeup, this solution had to be prepared daily. Special equipment (micro-Kjeldahl flasks with ground glass joints) has been eliminated and cyclohexane has been substituted for decahydronaphthalene. The modified method is convenient and applicable to a wide range of materials; it yields results comparable to those from the official method.

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