Ketones, methyl with nitric acid

Molybdenum may be identified at trace concentrations by flame atomic absorption spectrometry using nitrous oxide-acetylene flame. The metal is digested with nitric acid, diluted and analyzed. Aqueous solution of its compounds alternatively may be chelated with 8—hydroxyquinobne, extracted with methyl isobutyl ketone, and analyzed as above. The metal in solution may also be analyzed by ICP/AES at wavelengths 202.03 or 203.84 nm. Other instrumental techniques to measure molybdenum at trace concentrations include x-ray fluorescence, x-ray diffraction, neutron activation, and ICP-mass spectrometry, this last being most sensitive. 

The first examples of the conversion of nitroalkanes to carbonyl compounds were described in 1893 by Konovaloff, who was examining the reactivity of nitroalkanes obtained from nitration of alkanes with nitric acid.1 Konovaloff reported that treatment of 2-nitrohexane (3) with strong soda (NaOH) followed by reaction with Zn/HOAc afforded a mixture of methyl butyl ketone (4) and 2-aminohexane (5). Additionally, the reaction of the potassium salt of 2-phenylnitroethane with dilute aqueous acid provided mixtures of acetophenone and 2-phenylnitroethane. 

First studies of the aqueous phase chemistry of element 105 were conducted by Gregorich et al. (1988). Like Nb and Ta, Db was adsorbed on glass surfaces upon fuming with nitric acid. In 801 manually performed experiments, 24 a events due to the decay of 34 s Db or its 3.9 s Lr daughter including five aoc mother-daughter correlations were observed. In an attempt to study the extraction of the dubnium fluoride complex from 3.8 M HNO3/I.I M HF into methyl isobutyl ketone (MIBK), no decays attributable to Db could be observed. 

Only few data are available in the literature that deal with the measurement of Gd in biological fluids and tissues. Some workers used atomic emission spectrometry (AES) for the determination of Gd in tissues [4] after digesting samples with nitric acid. Others used radiolabeled Gd to study the biodistribution of the element [14]. ICP-MS has been used for the determination of Gd in serum and urine. With this method samples are simply diluted in water [16]. To our knowledge the method described by the group of D Haese [28] is the only report that exists on the determination of Gd in biological fluids and tissues by electrothermal AAS (ETAAS). With this procedure the element can be accurately determined in serum, urine, blood, bone, and tissues after extraction into methyl isobutyl ketone followed by reextraction in hydrochloric acid. Atomization of the element for AAS determination is performed from a tantalum boat. 

A number of workers have described methods for the determination of mercury in which the mercury is first reduced to the element or collected as the sulfide on a cadmium sulfide pad. It is then volatilized into a chamber for measurement. These techniques are extremely sensitive. Thillez108) recently described a procedure for urinary mercury in which the mercury is collected on platinum and then volatilized into an air stream. Rathje109) treated 2 ml of urine with 5 ml of nitric acid for 3 min, diluted to 50 ml, and added stannuous chloride to reduce the mercury to the element. A drop of Antifoam 60 was added and nitrogen was blown through the solution to carry the mercury vapor into a quartz end cell where it is measured. Six nanograms of mercury can be detected. Willis 93) employed more conventional methods to determine 0.04 ppm of mercury in urine by extracting it with APDC into methyl-n-amyl ketone. Berman n°) extracted mercury with APDC into MIBK to determine 0.01 ppm. 

Aznarez et al. [2] have described a Spectrophotometric method using curcumin as chromopore for the determination of boron in soil. Boron is extracted from the soil into methyl isobutyl ketone with 2-methylpentane-2,4-diol. In this method 0.2-lg of finely ground soil is digested with 5ml concentrated nitric-perchloric acid (3 + 1) in a polytetrafluoroethylene lined pressure pump for 2h at 150°C. The filtrate is neutralized with 6M sodium hydroxide and diluted to 100ml with hydrochloric acid 1+l.This solution is triple extracted with 10ml of methyl isobutyl ketone to remove iron interference. This solution is then extracted with 10ml 2-methyl pentane-2,4 diol and this extract dried over anhydrous sodium sulphate. 

Note Polar solvent soluble in water, ketones, organic halides, alcohols, ether, and many oils highly flammable narcotic by inhalation incompatible with strong oxidizers, nitrates, nitric acid, reducing agents. Synonyms ethyl methyl ketone, 2-butanone, MEK, methyl acetone. 

Nitrolic acids, which can be isolated from sources such as nitroalkanes and aldoximes, are also probable intermediates in a wide variety of furoxan preparations involving nitric and nitrous acid, and nitrogen oxides. Diacylfuroxans have been synthesized via nitrosation of methyl ketones for example acetone reacts with anhydrous dinitrogen tetroxide or nitric acid/sodium nitrite to give diacetylfuroxan. 

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