Determination antimony

Lead, arsenic, and antimony—determined in the solution obtained by boiling 10 g of the titanium dioxide for 15 min in 50 mL of 0.5 Nhydrochloric acid In addition to individual specifications, general specifications have been written for provisionally Hsted certifiable colors ... 

Angstrom unit (A), definition, 307 Antimony, determination by x-ray emission spectrography, 328 in silicate, determination by absorption-edge method, 140 in solution, determination by absorption-edge method, 140 Aperture, relative, of x-ray optical system, 113... 

Sturgeon et al. [59] have described a hydride generation atomic absorption spectrometry method for the determination of antimony in seawater. The method uses formation of stibene using sodium borohydride. Stibine gas was trapped on the surface of a pyrolytic graphite coated tube at 250 °C and antimony determined by atomic absorption spectrometry. An absolute detection limit of 0.2 ng was obtained and a concentration detection limit of 0.04 pg/1 obtained for 5 ml sample volumes. 

Hydrogen sulfide gas interfered in the determination of antimony since, after the addition of hydrogen sulfide, a peak comes a few seconds after the antimony peak. It was found that either degassing the sample for 300 s or placing lead acetate in the line eliminated the problem without interfering with the antimony determination. 

The acid digestion procedure described above for biological tissues. Crock and Lichte [135] recently described a similar procedure, involving hydrofluoric as well as nitric, perchloric and sulphuric acids, for dissolution of geological materials prior to arsenic and antimony determination by atomic absorption spectrometry. 

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. 

The antimony determination is carried out by pipetting 200-p.L aliquots of the decomposition solution into four reaction vessels of the hydride system, adding 10 mL 3% HCl, 1 mL 40% KI, 0.5 mL 20% NH OH, and 0.5 mL antifoam emulsion. The total volumes of Sb standard and... 

In our work with antimony determination in natural waters, we have not experienced serious contamination problems. We have used Niskin and Teflon-coated Go-Flo samplers (General Oceanics) and polycarbonate COC and TPN samplers (Hydrobios) for the collection of seawater samples without evidence of contamination resulting from any of these sampler types (see also Chapter 1). 

The same procedures as described in Section 12.2.3.1 for arsenic can be applied to the antimony determination, using the corresponding antimony species at concentrations of 1.0 nmol/L. As mentioned above, more problems were encountered with the stability of antimony(///) standards than with those for arsenic(///). If little or no peak is obtained using an antimony(///) solution, this problem can be isolated by running the same solution through the antimony(F) procedure. 

Anodic stripping voltammetry at a mercury film electrode can be used to determine whether an individual has recently fired a gun by looking for traces of antimony in residue collected from the individual s hands, fn a typical analysis a sample is collected with a cotton-tipped swab that had been wetted with 5% v/v HNO3. When returned to the lab, the swab is placed in a vial containing 5.00 mb of 4 M HCl that is 0.02 M in hydrazine sulfate. After allowing the swab to soak overnight,... 

A rapid method to determine the calcium content of lead alloys is a Hquid-metal titration using lead—antimony (1%) (9). The end point is indicated by a gray oxide film pattern on the surface of a sohdifted sample of the metal when observed at a 45° angle to a light source. The basis for the titration is the reaction between calcium and antimony. The percentage of calcium in the sample can be calculated from the amount of antimony used. If additional calcium is needed in the alloy, the melt is sweetened with a lead—calcium (1 wt %) master alloy. 

Silver diethyldithiocarbamate [1470-61-7] is a reagent commonly used for the spectrophotometric measurement of arsenic in aqueous samples (51) and for the analysis of antimony (52). Silver iodate is used in the determination of chloride in biological samples such as blood (53). 

Analysis of zinc solutions at the purification stage before electrolysis is critical and several metals present in low concentrations are monitored carefully. Methods vary from plant to plant but are highly specific and usually capable of detecting 0.1 ppm or less. Colorimetric process-control methods are used for cobalt, antimony, and germanium, turbidimetric methods for cadmium and copper. Alternatively, cadmium, cobalt, and copper are determined polarographicaHy, arsenic and antimony by a modified Gutzeit test, and nickel with a dimethylglyoxime spot test. 

High purity stibiae is used as an -type, gas-phase dopant for Si in semiconductors (14). Low temperature distillation of stibiae at <53.3 kPa (400 torr) yields a product that on decomposition gives metallic antimony having less than 8 x lO " % impurity (18). A method for determining quantities of stibiae in the neighborhood of 0.1 mg/m in air has been reported (19). 

This method is used for the determination of total chromium (Cr), cadmium (Cd), arsenic (As), nickel (Ni), manganese (Mn), beiylhum (Be), copper (Cu), zinc (Zn), lead (Pb), selenium (Se), phosphorus (P), thalhum (Tl), silver (Ag), antimony (Sb), barium (Ba), and mer-cuiy (Hg) stack emissions from stationaiy sources. This method may also be used for the determination of particulate emissions fohowing the procedures and precautions described. However, modifications to the sample recoveiy and analysis procedures described in the method for the purpose of determining particulate emissions may potentially impacl the front-half mercury determination. 

Spectrophotometric methods based on an enhancement of the blue color produced on reduction of 12-molybdophosphate (arsenate) in the presence of antimony(III) are widely used for the determination of phosphoms(V) or arsenic(V). However, nature of heteropoly blue, their spectra, mechanism of the reaction are obscure. In addition, mixed POMs were shown as very efficient analytical forms for the determination of P(V) and As(V). 

APPLICATION OF SURFACE ELECTROCHEMICAL PASSIVATION OF LEAD-ANTIMONY ALLOY FOR A SIMPLE AND RAPID ELECTROCHEMICAL DETERMINATION OF ANTIMONY CONTENT OF ITS ALLOYS... 

A simple, rapid and seleetive eleetroehemieal method is proposed as a novel and powerful analytieal teehnique for the solid phase determination of less than 4% antimony in lead-antimony alloys without any separation and ehemieal pretreatment. The proposed method is based on the surfaee antimony oxidation of Pb/Sb alloy to Sb(III) at the thin oxide layer of PbSOyPbO that is formed by oxidation of Pb and using linear sweep voltammetrie (LSV) teehnique. Determination was earried out in eoneentrate H SO solution. The influenee of reagent eoneentration and variable parameters was studied. The method has deteetion limit of 0.056% and maximum relative standard deviation of 4.26%. This method was applied for the determination of Sb in lead/aeid battery grids satisfaetory. 

The phase diagram for the copper-antimony system is shown on the next page. The phase diagram contains the intermetallic compound marked "X" on the diagram. Determine the chemical formula of this compound. The atomic weights of copper and antimony are 63.54 and 121.75 respectively. 

The long-wavelength limit which depends on the cathode material is ca. 2 = 650 nm m the red region of the spectrum. If this does not suffice for the determination an antimony-alkaline metal alloy is employed as the cathode material [56—58]. 

Arsenites may also be determined by this procedure but must first be oxidised by treatment with nitric acid. Small amounts of antimony and tin do not interfere, but chromates, phosphates, molybdates, tungstates, and vanadates, which precipitate as the silver salts, should be absent. An excessive amount of ammonium salts has a solvent action on the silver arsenate. 

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