Molybdenum analysis

Main group element analysis was carried out with a Perkin-Elmer CHN elemental analyzer, while molybdenum analysis was performed using atomic absorption spectroscopy. The content of Mo and O on the surface of the catalysts was obtained by X-ray photoelectron spectroscopy (XPS) using a Shimazu ESCA-850 spectrometer with monochromatic MgKa. Since Mo 3p3/2 spectra overlapped with the N Is spectra for the nitrided catalysts, the degree of nitriding (N IsfMo 3d ratio) had to be obtained from a combination of elemental analysis and XPS. 

Arsenic analysis by atomic absorption selenium analysis by fluorimetry molybdenum analysis by colorimetry. 

The graphite furnace technique for atomic absorption spectrophotometry permits molybdenum determination at the ng level with small sample volumes. This technique is, however, prone to matrix interferences when used for molybdenum analysis. The boiling point of molybdenum is about 4600°C, about 1800°C above the maximum temperature obtained in the graphite furnace. Therefore, molybdenum atomization can only take place by a mechanism which includes the formation of a compound that is volatile at 2800°C. Molybdenum atoms will only be produced if the volatile molybdenum compound dissociates at this temperature. Any ions or compounds which affect the complicated atomization mechanism will alter the sensitivity of the method. This crucial fact is the primary reason for the extreme matrix sensivity of the method. 

A Jarrell-Ash Model 82-532 MV spectrophotometer equipped with a Perkin Elmer nebulization system and a Leeds-Northrup Type W calibrated AZAR Recorder was used for the molybdenum analysis. The 3133 primary molybdenum absorption wavelength coupled with an acetylene-nitrous oxide flame were the basic parameters of the instrument. The recorder was set for a 5-fold signal expansion along with the amplifier at 3/4 damped position. 

This experiment uses the molybdenum-blue method to determine the concentration of phosphate in a phosphate/sodium chloride mixture. Elow-injection analysis is used to increase the speed of analysis, allowing students to... 

Description of Method. The FIA determination of phosphate is an adaptation of a standard spectrophotometric analysis for phosphate. In the presence of add, phosphate reacts with molybdate to form a yellow-colored complex in which molybdenum is present as Mo(VI). 

Micronutrients. Attention to meeting the micronutrient needs of crops has greatiy increased as evidenced in an analysis undertaken by TVA and the Soil Science Society in 1972 (99). The micronutrient elements most often found wanting in soil—crop situations are boron, copper, iron, manganese, molybdenum, and zinc. Some of these essential micronutrients can be harmful to plants when used in excess. 

Analytical Methods. Molybdenum contents in ore concentrates and technical oxide are most accurately deterrnined gravimetricaHy by precipitating lead molybdate. Molybdenum content is usually not determined on pure compounds or metal. Instead, spectrographic methods are used to measure impurity elements that must be controlled. Carbon and oxygen in metal products are measured by standard gas analysis methods. 

Molybdenum is classified among the elements for which the state of art of analysis is still unsatisfactory. The modest number of referenced materials available with certified value for Mo seems to confirm this. 

Samples were tested on in a melt of salts (75% Na SO, 25% NaCl) at 950°C in an air atmosphere for 24 hours. Micro X-rays spectrum by the analysis found that the chemical composition of carbides of an alloy of the ZMI-3C and test alloys differs noticeably. In the monocarbide of phase composition of an alloy of the ZMI-3C there increased concentration of titanium and tungsten is observed in comparison with test alloys containing chemical composition tantalum. The concentration of more than 2% of tantalum in test alloys has allowed mostly to deduce tungsten from a mono carbide phase (MC) into solid solution. Thus resistance of test alloys LCD has been increased essentially, as carbide phase is mostly sensitive aggressive environments influence. The critical value of total molybdenum and tungsten concentration in MC should not exceed 15%. 

Such significant increase of accuracy may be explained on the base of analysis of the numerical values of the theoretical correction coefficients and calculated for 1, , and for analytical pai ameter lQ.j,yipj.j,jj- Changing from lines intensities for the ratios of analytical element line intensity to the intensity of the line most effecting the result of analytical element (chromium in this case) measurement enables the decreases of the error 5 or even 10 times practically to the level of statistics of the count rate. In case of chromium the influencing elements will be titanium, tungsten or molybdenum. 

Samples Analyzed by Inductively Coupled Plasma (ICP) Metals — Where two or more of the following analytes are requested on the same filter, an ICP analysis may be conducted. However, the Industrial Hygienist should specify the metals of interest in the event samples cannot be analyzed by the ICP method. A computer print-out of the following 13 analytes may be typically reported Antimony, Beryllium, Cadmium, Chromium, Cobalt, Copper, Iron, Lead, Manganese, Molybdenum, Nickel, Vanadium, Zinc. Arsenic — Lead, cadmium, copper, and iron can be analyzed on the same filter with arsenic. 

Apparent indicator constant 264, 267 Apparent stability constant 59 Aqua regia 111 Arc alternating current, 764 direct current, 763, 771 sensitivities of elements, (T), 766 Aromatic hydrocarbons analysis of binary mixtures, 715 Arsenates, D. of (ti) 357 Arsenic, D. of as silver arsenate, (ti) 357 as trisulphide, (g) 448 by iodine, (am) 634, (ti) 397 by molybdenum blue method, (s) 681 by potassium bromate, (ti) 406 by potassium iodate, (ti) 401 in presence of antimony, (s) 724 Arsenic(III) oxide as primary standard, 261... 

The reaction is quenched by the addition of 1.28 g (2.94 mmol) of molybdenum pentoxidc/pyridinc/UMPA, and the yellow slurry is stirred initially at OX (30 min), then for 45 min at 25 X. The mixture is added to 1 N sodium hydroxide and extracted with diethyl ether. The ethereal solution is washed with brine, dried over Na,S04 and concentrated in vacuo to give 0.705 g (100%) of an oily, light-yellow solid. Analysis of the crude aldol adduct by 1 C NMR and analytical HPLO (Waters, Radial Pak, 8 mm x 10 cm, silica gel, ethyl acetate/hexane, 15 85) indicates only one. un-diastereomer (2X3S ) accompanied by approximately 10% of the two ethyl acetate/hexane affords fine white needles yield 0.359 g (57%) mp 155.5 156.5X (a]u -92.5 (c = 0.0294, CHCfi). 

Tungsten ores often contain traces of molybdenum that need to be determined before the ore is processed. When the tungsten content is known, as it usually is, that element can serve as a built-in standard for the determination of molybdenum. In the work to be described, the intensity ratio was measured for molybdenum Ka and tungsten Lyl. The general approach thus resembles that of Eddy and Laby to the analysis of brass (7.10), but conditions are less favorable in the present instance. The background corrections necessary were somewhat involved, and they will be discussed in Chapter 8. See Figure 8-1 c. 

Seven coordination in molybdenum chemistry analysis of oligonuclear structures. M. Melnik and P. Sharrock, Coord. Chem. Rev., 1985, 65, 49 (91). 

Complexes of molybdenum in the lower valence-states of -t 2 and + 3 have been produced only in the past two years. For the Mo(II) species, the usual starting-material is Mo2(acetate>4. Reaction of this with KS2COEt in THF gives two products, a green complex tentatively assigned as [Mo2(Etxant>4], which solvates to form the red complex [Mo2(Etxant)4(THF)2]. The structure of the latter complex was elucidated by X-ray analysis 169). Steele and Stephenson 170) were also able to synthesize a red, crystalline solid (methanol solution), which they formulated as [Mo(Etxant)2]2 (XI), and reacted this with Lewis bases, e.g., pyridine, to form [Mo(Etxant)2L]2- Thus, there appears to be a difference between the two compounds formulated as [Mo2(Et-xant)2]2 that... 

Just as, in Group VB, niobium, so, in this Group, molybdenum provides most of the examples of the chalcogenide halides. The occurrence and preparation of such compounds are described in numerous publications. In most cases, they have been obtained as powders, with the composition based on chemical analyses only. The presence of defined, homogeneous phases is, therefore, in many cases doubtful. In addition, some published results are contradictory. A decision is possible where a complete structure analysis has been made. As will be shown later, the formation of metal-metal bonds (so-called clusters), as in the case of niobium, is the most characteristic building-principle. Such clusters... 

Heated in molybdenum, nickel or niobium containers for times varying from 1 to 100 h before analysis. 

A second unusual EPR spectrum was observed in the oxidized (as-isolated) protein (Fig. 3). This spectrum, which was assigned to an S = z system, was not reminiscent of any Fe-S cluster. Indeed, with g-values of 1.968, 1.953, and 1.903, it looked more like a molybdenum or tungsten spectrum. However, chemical analysis ruled out the possibility that this EPR spectrum arose from Mo or W, and the spectrum was assigned to an Fe-S center instead. The spin concentration, however, was sub stoichiometric and sample-dependent. Furthermore, when the as-isolated protein was oxidized with ferricyanide, it became EPR silent. This, together with the iron determination and the fingerprint of the reduced protein, led Hagen and colleagues to the... 

The Mo/Al ratio measured by XPS always decreased upon sulfiding. Bulk analysis showed no change in molybdenum concentration upon sulfiding, indicating that no molybdenum was lost during sulfiding. 

A cationic molybdenum sulfide cluster [Mo3S4(H20)9] " with incomplete cubane-type structure and a cationic nickel-molybdenum mixed sulfide cluster [Mo3NiS4Cl(H20)9p " with complete cubane-type structure were introduced into zeolites NaY, HUSY and KL by ion exchange. Stoichiometry of the ion exchange was well established by elemental analyses. The UV-visible spectra and EXAFS analysis data exhibited that the structure of the molybdenum cluster remained virtually intact after ion exchange. MoNi/NaY catalyst prepared using the molybdenum-nickel sulfide cluster was found to be active and selective for benzothiophene hydrodesulfurization. 

This paper describes the successful incorporation of molybdenum and molybdenum-nickel clusters into zeolites with 12-membered ring by aqueous ion exchange and application of the resulting materials to HDS reaction of benzothiophene. Stoichiometry of the ion exchange was examined by elemental analysis. UV-visible spectroscopy and EXAFS measurements were carried out to investigate the structure of molybdenum species loaded on zeolites. 

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