THE DETERMINATION OF NUCLEOTIDE PHOSPHORUS WITH A STANNOUS CHLORIDE - HYDRAZINE SULPHATE REAGENT

1964 ◽  
Vol 42 (2) ◽  
pp. 287-292 ◽  
Author(s):  
R. O. Hurst

Stabilization of stannous chloride as reducing agent for the analysis of phosphorus by the molybdenum blue method has been achieved by combining it with hydrazine sulphate. Application of the procedure to the determination of inorganic and nucleotide phosphorus is described. Colorimetric measurement of light absorption is made at 700 mμ, permitting a highly sensitive and accurate estimation of phosphorus.

1939 ◽  
Vol 17b (6) ◽  
pp. 178-191 ◽  
Author(s):  
G. R. Smith ◽  
W. J. Dyer ◽  
C. L. Wrenshall ◽  
W. A. De Long

A study of factors affecting the ceruleomolybdate reaction for phosphate is reported. The concentrations of stannous and stannic ions, the presence of extraneous salts, and temperature are important factors affecting the intensity and stability of the blue colour.The stannous chloride reagent should be preserved from oxidation by storing it under hydrogen.The interference by ferric iron is due largely to its reaction with the reducing agent, and may be avoided by diluting the sample to contain 0.1 p.p.m. of phosphorus and using two or three times the usual quantity of stannous chloride.


2009 ◽  
Vol 63 (1) ◽  
Author(s):  
Aneta Jastrzębska

AbstractSpectrophotometric determination of total phosphorus in meat samples was modified using the molybdenum blue reaction with the following reducing agents: ascorbic acid (AA), hydrazine sulphate (HS), and mixture of hydroquinone and hydrazine sulphate (HHS). Proposed methods were validated by evaluation of statistical parameters such as: linearity, sensitivity, limits of detection (DL) and quantification (QL), precision, and accuracy, against the standard and malachite green (MG) modified procedures and by applying food certified materials. The values of within-day and between-days precision in meat samples for all tested reducing agents were better than 3.4 % and 4.2 %, respectively. The recoveries for CRMs analyses were between 92 % and 102.3 %. Obtained results suggest usefulness of the hydroquinone and hydrazine sulphate mixture in the determination of phosphorus ions.


1954 ◽  
Vol 26 (1) ◽  
pp. 159-168
Author(s):  
Armi Kaila

The interference of ferric and ferrous iron in the determination of phosphate by the molybdenum blue method has been studied. It was found that the presence of ferric iron in the solutions could cause either an increase or a decrease in the colour intensity depending on the amount of stannous chloride applied and on the acid and molybdate concentrations in the reagent. Also the phosphorus concentration exerted its effect upon the course of the errors. If the original modification of Truog and Meyer was employed, generally, the most convenient way for the elimination of the interference of ferric iron was to dilute the solution. An increase in the amount of stannous chloride largely helped to prevent the fading effect of ferric iron, provided the phosphorus concentration was not lower than 0.25 ppm. When the effect of ferric iron upon the development of molybdenum blue at various concentrations of sulphuric acid and ammonium molybdate was studied, the observation was made that at each acidity there could be found a concentration of molybdate in which the effect of even fairly high amounts of ferric iron was almost negligible. In lower molybdate concentrations the presence of ferric iron caused an increase in the colour intensity, in higher molybdate concentrations the fading effect of ferric iron was marked. This most suitable level of the molybdate concentration depended to a certain degree on the phosphorus concentration of the solution and on the amount of stannous chloride applied. Fairly good results could be obtained, if the ratio of molybdate (expressed as mg/ml) to acid (expressed as normality) in the solution to be reduced was five times as high as the acidity of the solution to be reduced (expressed as its normality), e.g. 4 in 0.8 N acid, 3.5 in 0.7 N acid, 3 in 0.6 N acid etc. Although it seemed to be fairly possible to avoid the interference of ferric iron by a proper choice of the concentrations of acid and molybdate and of the amount of stannous chloride applied, the fading effect of ferrous iron could not be prevented, if only sulphuric acid was used in the reagents. But the substitution of sulphuric acid by hydrochloric acid totally prevented the fading effect of ferrous iron. On the contrary, a slight increase in the colour intensity was demonstrated. This was true also when only one half of the acid present was hydrochloric acid. It was found that this mixture of sulphuric acid and hydrochloric acid in the molybdate reagent offers an available way for the elimination of the disturbing effect of iron.


1981 ◽  
Vol 27 (3) ◽  
pp. 464-465 ◽  
Author(s):  
R J Wood ◽  
D G Williams

Abstract We present a sensitive colorimetric determination of 5'-nucleotidase based on the measurement of liberated phosphate by reaction with stannous chloride/molybdenum blue. No protein precipitation is required. The method is simple, sensitive, economical, and easy to use, and involves relatively stable reagents.


1994 ◽  
Vol 77 (6) ◽  
pp. 1557-1561 ◽  
Author(s):  
T Katrdna Pulliainen ◽  
Harriet C Wallin

Abstract A spectrophotometric method in which the sample is dry-ashed in the presence of zinc oxide, and total phosphorus content is measured colorimetrically as molybdenum blue was evaluated by 12 participating laboratories from the Nordic countries. The study included potato flour, sausage, cold ham, infant formula powder, cheese, and skimmed milk powder. The materials were presented to the participants as 12 randomly coded samples of 2 blind duplicates of each material. The phosphorus content of the materials varied between 0.076 and 0.96 g/100 g. The relative standard deviation for repeatability of the method varied from 1.1% for 0.96 g phosphorus/100 g to 5.4% for 0.29 g phosphorus/100 g. The relative standard deviation for reproducibility varied from 3.6% for 0.96 g phosphorus/100 g to 7.7% for 0.23 g phosphorus/100 g.


1967 ◽  
Vol 13 (12) ◽  
pp. 1071-1078 ◽  
Author(s):  
Bernard Klein ◽  
James H Kaufman ◽  
John Isaacs

Abstract A procedure is described for the automated simultaneous determination of serum calcium and phosphorus. Calcium is assayed fluorometrically; phosphorus is determined spectrophotometrically by the molybdenum blue reaction in an improved flow system with a more sensitive reducing agent.


1981 ◽  
Vol 64 (1) ◽  
pp. 9-13
Author(s):  
Amer El-Ahraf ◽  
W Van Willis ◽  
Dutt V Vinjamoori

Abstract The reduction of mercury in samples of dairy cattle and chicken feed rations and manures prepared by acid digestion for determination by flameless atomic absorption is rapidly, smoothly, and quantitatively effected by sodium hypophosphite. The reducing agent is air-stable, is effective over a wide range of mercury concentrations, and is useful in the presence of many mineral acids commonly used for wet digestion of these matrices. The accuracy and precision obtained in determinations with this reagent are equivalent to those obtained using stannous chloride at the same conditions. Recovery efficiencies for the total analytical procedure were studied using cattle manure and feed rations spiked to 0.6 ppm Hg as phenylmercuric nitrate; the range of recoveries varied from 93 to 102% (97% average). The absolute detection limit of the method is 10 ng Hg, and the precision varies in the range of 2.2-6% for samples containing 3 ppt-10 ppm Hg. The advantages of sodium hypophosphite lie in the elimination of premature reduction of mercury caused by traces of stannous chloride adhering to the walls of the reaction vessel, the elimination of several wash steps in the determination, and the long shelf life of the reagent.


1967 ◽  
Vol 13 (12) ◽  
pp. 1079-1087 ◽  
Author(s):  
Bernard Klein ◽  
James H Kaufman

Abstract A procedure is described for the automated simultaneous determination of serum calcium and phosphate. Calcium is assayed by atomic absorption spectrophotometry. Phosphate is determined by the molybdenum blue reaction in an improved flow system with a more sensitive reducing agent.


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