Molybdenum colorimetric

Phosphate. Phosphoms occurs in water primarily as a result of natural weathering, municipal sewage, and agricultural mnoff The most common form in water is the phosphate ion. A sample containing phosphate can react with ammonium molybdate to form molybdophosphoric acid (H2P(Mo202q)4). This compound is reduced with stannous chloride in sulfuric acid to form a colored molybdenum-blue complex, which can be measured colorimetrically. SiUca and arsenic are the chief interferences. 

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. 

Toluene-3,4-dithiol, usually called dithioP, yields a slightly soluble, dark-green complex, (CH3.C6H3.S2)3Mo(VI), with molybdenum(VI) in a mineral acid medium, which can be extracted by organic solvents. The resulting green solution is used for the colorimetric determination of molybdenum. 

Discussion. Small quantities of dissolved silicic acid react with a solution of a molybdate in an acid medium to give an intense yellow coloration, due probably to the complex molybdosilicic acid H4[SiMo12O40]. The latter may be employed as a basis for the colorimetric determination of silicate (absorbance measurements at 400 nm). It is usually better to reduce the complex acid to molybdenum blue (the composition is uncertain) a solution of a mixture of l-amino-2-naphthol-4-sulphonic acid and sodium hydrogensulphite solution is a satisfactory reducing agent. 

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. 

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. 

Colorimetric field tests for TATP and HMTD were described in Section 5 dealing with peroxide-based explosives. This group contains Keinan s PEX [85] (E. Keinan, Personal Communication, February 2006) and the kit developed by Schulte-Ladbeck et al., which involves also a preliminary stage to avoid falsepositive responses by non-explosive peroxides [86]. The color change of molybdenum hydrogen bronze suspension upon reaction with TATP was recommended also as a field test. Exposure of filter paper strips which were soaked in butanol suspension of the molybdenum compound to TATP or hydrogen peroxide vapors rapidly bleaches the blue color [87, 88]. 

Ammonium molybdates are used to prepare high purity grade molybdenum metal powder, sheet, or wire for colorimetric analysis of phosphates and arse-... 

Under acid conditions, molybdate reacts with orthophosphate, P04 to form a blue heteropoly acid, molybdophosphoric acid. A similar reaction occurs with arsenate ion, As04. In the presence of vanadium, the product is yellow vanadomolybdophosphoric acid. These reactions are used for colorimetric analyses of phosphate, arsenate, and many other substances. Colloidal molybdenum blue has limited apphcations such as dyeing silk. It readily absorbs onto surface-active materials. 

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. 

If a drop of 0-02N aqueous sodium sulphide is added to a drop of a solution containing arsenate or phosphate on a filter paper and a drop of aqueous ammonium molybdate acidified with sulphuric acid also added, a blue colour develops 2 ferro- and ferri-cyanides and thiocyanate should be absent. The formation of molybdenum blue is used in the colorimetric estimation of arsenic (see p. 321). 

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... 

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... 

The decomposition products were separated by eluting with potassium chloride solution on a column packed with anion-exchange resin, Dowex 1x4 in chloride form. During the elution the concentration of potassium chloride in the eluent was increased exponentially. The phosphorus contents in effluent fractions were determined colorimetrically with a molybdenum(V)-molybdenum(VI) reagent (4J. 

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. 

Use Colorimetric reagent for iron, manganese, titanium, molybdenum. 

Use Colorimetric determination of ferric iron, titanium, or molybdenum. 

Claisse Fusion Device. The detailed procedure is described by Botto (10). This isan automated device which simultaneously fuses six samples. In this procedure, the finely powdered sample was mixed with ten times its weight of lithium metaborate in a platinum crucible and heated at 950°C for 15 minutes. The melt was dissolved in either dilute HC1 or HNO and the elements of interest were then determined by AAS or ICPES. Phosphorus was determined from the same solution by a separate molybdenum blue colorimetric procedure. 

Phosphate Colorimetric determination as molybdenum until 2005 0.02 mmol/m ... 

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. 

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