Analysis of antimony compounds

The compound is cautiously dissolved in nitric acid and the solution is appropriately diluted for the analysis of antimony by AA spectrophotometry or ICP emission spectrophotometry and fluoride ion is determined by ion—selective electrode or ion chromatography. 

Gas chromatography has, of course, been used extensively in the analysis of many types of organic compounds with boiling points up to about 250°C, also to the analysis of organic compounds of lead, mercury, selenium, tin, manganese and silicon. Derivitisation of these compounds to produce compounds sufficiently volatile to be amenable to gas chromatography is frequently practised. Gas chromatography has also been applied to the determination of arsenic, antimony, selenium, tin, beryllium and aluminium and the common anions such as sulphate, nitrate, phosphate, sulphide, cyanide and thiocyanate. 

X-Ray crystallographic analysis of antimony containing four-membered ring compounds is still unknown to the best of our knowledge. 

The analysis of these compounds is effected by boiling them with a rmxture of concentrated sulphuric acid and nitric acid (density 1-49) and subsequent treatment of the-solution with ammonium sulphate until all the residual nitric acid has been destroyed. The arsenic and antimony are then estimated in the usual manner,... 

Na[Sb(OH)g], respectively. The latter compound is one of the least soluble sodium salts known and is useful in sodium analysis. Numerous polyantimonate(V) derivatives are prepared by heat treatment of mixtures of antimony trioxide and other metal oxides or carbonates. Of these, K Sb O [12056-59-6] and K Sb O [52015-49-3] have been characterized by x-ray. These consist of three-dimensional networks of SbO in which corners and edges are shared with K" ions located in tunnels through the network (23). Simple species such as SbO and Sb20 2, analogous to orthophosphate and pyrophosphate, apparendy do not exist. 

All of the organohalogen compounds studied were commercial products obtained from various manufacturers and used as received. Only the DBDPO was purified further by recrystallization for some of the chromatography and thermal analysis experiments. Samples of antimony trioxide and antimony pentoxide were also obtained from commercial sources. The ultrapure antimony trioxide, bismuth trioxide, bismuth metal, antimony metal, dibenzofuran and diphenyl ether were all obtained from Aldrich Chemicals. The poly(propylene) (PP) resin was 0.7 mfi, food grade from Novamont and the poly(ethylene) was unstabilized, high molecular weight, HDPE from American Hoechst. 

When Lemery was received into the Academy of Sciences in 1699, he decided to make a thorough analysis of the mineral known as antimony [stibnite] in a search for useful medicaments. After reading his paper in instalments to the Academy, he finally published it in 1707 as the Treatise on Antimony. When I resolved to study antimony thoroughly in all its aspects, said he, I believed it proper to begin with some reflections on the nature of this compound and the places where it occurs on the names which were applied to it, and their diversity on how to select it and on its medicinal virtues (41). 

Since 1960, it has been demonstrated by various analytical procedures that high concentrations of arsenic were present in Napoleon s hair.88 Multi-element analysis of two specimens of Napoleon s hair by ICP-MS after mineralization in concentrated nitric acid resulted in arsenic concentrations (42.1 and 37.4(xgg-1) about 40 times higher than normal values, confirming the hypothesis of a significant exposure to arsenic. However, mercury (3.3. and 4.7(xgg 1), antimony (2.1 and 1.8(xgg 1) and lead (229 and 112p,gg-1) were also detected at elevated levels. The elevated concentrations of Sb and Hg are in agreement with the data already known about the therapeutic treatments given to Napoleon (calomel and tartar emetic are compounds of mercury and antimony, respectively).88... 

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