Antimony, Analytical Procedures

According to Weingarten (Ref 11), metallic antimony is not used in any current US military pyrotechnic compns, but the US Military Specification MIL-A-1084IB, 10 Sept 1958, deals with Antimony, Technical, intended for use in pyrotechnics (See Antimony, Analytical Procedure... 

Antimony, Analytical Procedures. Various qualitative and quantitative procedures for detn of Sb including its detection in air are given in Refs 1,2 3. Specification requirements for refined antimony are given in Ref 4 and the US Military Specification requirements for technical antimony are given... 

Antigrisou (Explosifs) A466-R Antimony, Metal A467 R Antimony, Analytical Procedures A469 to A470... 

Certain volatile elements must be analyzed by special analytical procedures as irreproducible losses may occur during sample preparation and atomization. Arsenic, antimony, selenium, and tellurium are determined via the generation of their covalent hydrides by reaction with sodium borohydride. The resulting volatile hydrides are trapped in a liquid nitrogen trap and then passed into an electrically heated silica tube. This tube thermally decomposes these compounds into atoms that can be quantified by AAS. Mercury is determined via the cold-vapor... 

Zhang S, Meyer B, Moh GH, Scholz F (1995) Development of analytical procedures based on abrasive stripping coulometry and voltammetry for solid state phase microanalysis of natural and synthetic tin-, arsenic-, and antimony-bearing sulfosalts and sulfides of thalhum, tin, lead, and silver. Electroanalysis 7 319-328. 

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... 

Although it appears in Table I that the percent of analyses rejected and qualified is low, the problems are concentrated within a few species. Both laboratories appeared to have difficulty analyzing these selected parameters. The most difficult parameters appeared to be selenium in water samples (70 to 100 percent qualified) and antimony in solid samples (46 to 75 percent qualified). Other difficult parameters include silver, tin, and thallium. These parameters were not important in terms of risk at the CC/CC site. If these elements are important at other sites, special, instead of routine, analytical procedures should be requested to obtain better results. For example, for tin, thallium, and silver, furnace atomic absorption maybe more accurate and for antimony and selenium, cold vapor atomic absorption may be the method of choice. 

Wang et al. [475] have proposed a similar analytical method as that for bismuth for antimony determination based on Sb UPD on gold electrode. In the proposed procedure, Sb was accumulated at the gold surface, and this step was followed by anodic stripping. A detection limit 2.1 X 10 M was reported for a 120 s electrochemical deposition. 

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