Molybdenum, colorimetric method

Matrix effects in the analysis of nutrients in seawater are caused by differences in background electrolyte composition and concentration (salinity) between the standard solutions and samples. This effect causes several methodological difficulties. First, the effect of ionic strength on the kinetics of colorimetric reactions results in color intensity changes with matrix composition and electrolyte concentration. In practice, analytical sensitivity depends upon the actual sample matrix. This effect is most serious in silicate analysis using the molybdenum blue method. Second, matrix differences can also cause refractive index interference in automated continuous flow analysis, the most popular technique for routine nutrient measurement. To deal with these matrix effects, seawater of... 

In the measurement of nitrqgen dioxide with this technique, it is thermochemically converted to nitric oxide by reaction with molybdenum at about 200 C. The extent of possible interferences at various monitoring sites from nitrogen compounds other than amhionia, which does not interfere unless the temperature is considerably higher than 2(X) C, remains to be assessed. The instrumentation of this procedure is inherently more reliable than the original colorimetric analyzers. Unfortunately, the mutual equivalence in monitoring situations of data obtained by these two techniques has not yet been evaluated. This is particularly important for the data from California, where the colorimetric method has been used for more than 20 yr. 

Fresh water UV lamp 900 W, a few drops of 30% H202 and 0.004 M H2S04, t = 1.5-2 h P Colorimetric determination by molybdenum blue method 6... 

Colorimetric methods Silicon is determined by the molybdenum blue spectrophotometric method after solubilization in H2O, in alkaline solutions or in concentrated HF. A flow analysis procedure for the measurement of soluble silicon with respect to the total Si concentration is used. The proposed method is applied to samples of rain water and of aerosols on filters [45]. Simultaneous determination of orthophosphate and silicate in brackish water is performed by the same technique. Molybdate/ antimony, ascorbic acid, and oxalic acid reagents are added to the samples and spectra are recorded in the wavelength range 410-820 nm after a total reaction time of 30 min [46]. 

Colorimetric Method.—Molybdenum may be detected quantitatively by means of the xanthic acid test already described (p. 178). The red product is extracted with a mixture of ether and light petroleum (65 35) and the extract diluted with another mixture of ether and light petroleum (30 70) for comparison with the standard solution. If pure ether is used, decomposition takes place. 

Heath, Ghem. Trade J., 1920, 66, 629 Travers, Oompt. rend., 1918, 166, 416. Fora colorimetric method of estimating small quantities of molybdenum in tungsten, see King, Ind. Eng. Chem., 1923, 15, 350. 

Although most of the elements have been determined by XRF (21), some other methods were used. The fluorometric method for selenium uses diaminonaphthalene (32). The colorimetric method for molybdenum uses potassium thiocyanate (33). The uranium analyses were done by delayed neutron activation analysis (34). For the XRF analyses of the oil and water, a blank value implies that there were no x-rays above background for that element. Two elements conspicuously missing from Table IV are cadmium and mercury. Preliminary analyses for these two elements have not yielded reproducible results. Further work is needed before we can make definitive statements about cadmium and mercury. 

Phosphorus content in oil %) Colorimetric method (% transmittance 650 nm) for total phosphorus based on conversion to molybdenum blue Ca 12-55... 

Biological fluids such as serum or plasma, red blood cells, and urine are particularly diflBcult to analyze. The low molybdenum concentrations found in normal human samples are below the detection limit of the thiocyanate colorimetric method (100 ng) and much below conventional flame absorption spectroscopy (1 /xg). Normal blood levels of molybdenum are about 10 /xg/L and sample volume is usually < 1 mL. The low concentration and limited sample size preclude direct analysis or sample preconcentration for analysis by the conventional analytical methods. 

For humic substances which normally are expected to contain small amounts of phosphorus, the molybdenum blue colorimetric method (Ma and Rittner, 1979) is recommended. The blue color provides a high sensitivity, allowing relatively small samples to be used for the determination. 

Standard methods for phosphates, polyphosphates, and organic phosphates in environmental samples are predominantly nonchromatographic methods, which are based upon the molybdenum blue method. Within this colorimetric method ammonium molybdate and antimony potassium tartrate react under acidic conditions with dilute solution of phosphorous to form an antimony-phospho-molybdate complex which is then reduced to an intensely blue-colored complex by ascorbic acid. U.S. EPA Methods 365.1 to 365.4 are based upon this chemistry. 

Mineral elements except phosphorus and molybdenum in the tobacco fiber were analyzed by use of Varlan AA-6 Atomic Absorption Spectrophotometer. Samples were wet-ashed in nitric and perchloric acids (9 1, v/v) until completely digested. After evaporation to dryness, the ashes were solubllzed in IN HCl for analyses. Quantitation of phosphorus was a colorimetric method using a Technlcon Autoanalyzer and the color reaction of Fiske and Subbarow (IJ.). Molybdenum was quantitated by the method of Eivazi et al (12) which determines, with good reproducibility, a quantity as low as 0.02 ppm in plant materials. 

The oil is charred in the presence of magnesium carbonate and then ashed. The ash is dissolved in dilute hydrochloric acid and phosphorus is determined colorimetrically in the resulting solution by a molybdenum blue method. 

Various modifications of the colorimetric determination of phosphorus by the molybdenum blue method are available. The method described above has proved to be the most suitable. 

Phosphate and other salts may be measured by various titrimetric and colorimetric methods. Phosphate is measured titrimetrically by precipitation of quinoline phosphomolybdate that is collected and dissolved in a small known excess of alkali and then back-titrated with standard acid. A colorimetric method based on the reaction of the phosphate with ammonium molybdate followed by partial reduction to give molybdenum blue has been developed for use in auto-analyzers. 

In addition to the iodometiic determination, direct precipitation as barium sulfate before and after treatment with bromine was suggested for both quantitative and qualitative test for sulfur dioxide in wine (see Monier-Williams, 1927). Precipitation of SO2 after oxidation with H2O1 as the benzidine sulfate was proposed by Rothen-fusser (1929) reduction of the molybdenum in phosphomolybdic acid by the sulfite ion present in an aqueous solution of the food was proposed by Sasaki (1928) as a colorimetric method formation of a blue color from a solution of 1% methylene blue and 5% iodine in potassium iodide was proposed by Svershkov (1939). Mathers (1949) proposed a turbidimetric method based on the distillation of wine into a dilute solution of lead acetate to form a colloidal suspension of lead sulfite whose spectral transmittance in the range of 400 to 700 mn could be used as a measure of sulfur dioxide. This is similar to turbidimetric methods based on turbidity produced by adding BaCfii to a... 

The authors then analysed the mixed acetate esters by gas chromatography. It would also be possible to determine the phosphoric acid in the water washings, after suitable dilution, by a colorimetric method. There are many published methods, e.g. [30] (see also section 2.5.4), which depend on the formation of molybdophosphoric acid and its subsequent reduction to molybdenum blue. 

Another example is a fully computerized MSFIA system for the spectrophotometric determination of available phosphorus in soil extracts. The molybdenum blue method is chosen for the colorimetric determination, using ascorbic acid as reducing agent, antimony to accelerate the reduction to the blue complex and applying the Egner-Riehm method to extract phosphorus from soil samples. It presents a hnear calibration curve between 0.75 and 15 mg/1. A determination frequency of 15/h may be achieved, with good repeatability for 12 consecutive injections of soil extracts (RSD <1.7%). Results obtained from 12 soil samples were statistically comparable to those attained by the usual batch method [102]. 

M.D. Hurtado, S. Carmona, A. Delgado, Automated modification of the molybdenum blue colorimetric method for phosphorus determination in soil extracts, Commun. Soil Sci. Plant Anal. 39 (2008) 2250-2257. 

Discussion. Molybdenum may be determined colorimetrically by the thiocyanate-tin(II) chloride method (for details, see Section 6.14) or by the dithiol method described here. 

Deans [192] have proposed a method for the colorimetric determination of traces of phosphorus with molybdenum blue, making use of the laser-induced thermal lensing effect. The procedure is described, and the results obtained on samples of sea water and lake water are presented. 

For a number of years, phenolic substances were dosed by colorimetric techniques, based on redox reactions usually known as Folin Ciocalteau methods, even if a number of adjustments were developed to fit different matrix characteristics. The Folin Cioalteau reagent is a mixture of phosphomolybdic and phosphotingstic acids, with molybdenum in the 6+ oxidation state and, when the reaction takes place, it is reduced to form a complex called molybdenum blue and tungsten blue. In this complex, the mean oxidation state is between 5 and 6 and the formed complex is blue so it can be read spectrophotometrically at 750 nm. 

This method for determining arsenic is particularly useful in biological and toxicological studies.8 The material under test is oxidised with a mixture of sulphuric and nitric acids and perhydrol, the arsenic is precipitated as sulphide, which is then oxidised and the arsenic determined colorimetrically after addition of sodium molybdate and stannous chloride. The formation of the molybdenum blue compound is also applied to the micro-determination of arsenic in soil extracts.9... 

Another method34 involves fusion of the organosilicon with magnesium to produce magnesium silicide. This is then decomposed to produce gaseous silicon hydrides by addition of dil. sulphuric acid. The hydrides are absorbed in bromine water and thus hydrolysed to silicic acid. The latter is converted into molybdosilicic acid and determined colorimetrically as molybdenum blue. The error is 0.73 to 0.54% over the range 10.53 to 37.8% of silicon. After removal of silicon hydrides, the elementary carbon which separates is deactivated with ferric or aluminium salts and filtered off, when halogens can be determined in the filtrate by Volhard s method. 

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