Carbon compounds, identification elements

Both solid and liquid samples can be analyzed by XRF as described earlier in the chapter. Very flat surfaces are required for quantitative analysis, as discussed subsequently. Liquids flow into flat surfaces, but cannot be run under vacuum. The best solvents are H2O, HNO3, hydrocarbons, and oxygenated carbon compounds, because these compounds contain only low atomic number elements. Solvents such as HCl, H2SO4, CS2, and CCLt are undesirable because they contain elements with higher atomic numbers they may reabsorb the fluorescence from lower-Z elements and will also give characteristic lines for Cl or S. This will preclude identification of these elements in the sample. Organic solvents must not dissolve or react with the film used to cover the sample. 

The carbon compounds individuated and identified in carbon chemistry—the remaining stoichiometric plant and animal substances and the pure carbon compounds isolated from coal tar, as well as the artificial carbon compounds created in the laboratory—were nested in extended networks of experiments and work on paper. In the late 1840s, when the culture of carbon chemistry was firmly established, the individuation and identification of carbon compounds required quantitative elemental analysis, control of stoichiometric purity by studies of the chemical properties and reactions of a substance, experimental examination of their proximate components or constitution (later structure ), and work on paper with chemical formulae to demarcate the substances and to model their constitution and chemical reactions. Analysis of composition (qualitative and quantitative), control of purity, studies of reactions, and modeling on paper allowed chemists to draw ever more sophisticated... 

A significant advantage of the PLM is in the differentiation and recognition of various forms of the same chemical substance polymorphic forms, eg, brookite, mtile, and anatase, three forms of titanium dioxide calcite, aragonite and vaterite, all forms of calcium carbonate Eorms I, II, III, and IV of HMX (a high explosive), etc. This is an important appHcation because most elements and compounds possess different crystal forms with very different physical properties. PLM is the only instmment mandated by the U.S. Environmental Protection Agency (EPA) for the detection and identification of the six forms of asbestos (qv) and other fibers in bulk samples. 

Comparative x-ray absorption measurements were used in the identification of various new compounds that could contain at most the following elements carbon, hydrogen, fluorine, and chlorine. The presumed composition of each compound, known in advance, was duplicated by properly blending carbon tetrachloride, benzotrifluoride, heptane, and benzene the latter also was used as solvent for the unknown. Under conditions intended to be identical, the amount of unknown... 

Elemental composition C 15.77%, S 84.23% carbon disulfide. It may be analyzed by GC using a sulfur chemiluminescence detector or by GC/MS. A concentration of 1 ppm in the air may be measured by mass spectrometry. The primary characteristic ionic mass for identification of this compound by mass spectrometry is 76. Many GC columns are available commercially. 

Elemental composition Pb 77.54%, C 4.49%, O 17.96%. The compound is digested with nitric acid, diluted and analyzed for lead by various instrumental techniques (See Lead). Carbonate may be tested by treating the compound with dilute HCl. It will effervesce, the evolved CO2 gas will turn hmewater milky. Also, liberated CO2 can be identified using a GC-equipped with a TCD or by GC/MS. The characteristic mass ion for GC/MS identification of CO2 is 44. 

Elemental composition Os 74.82%, 0 25.18%. The compound can be identified by its physical properties, such as, odor, color, density, melting-, and boiling points. Its acrid odor is perceptible at concentrations of 0.02 mg/hter in air. The oxide also produces an orange color when a small amount of the compound or its aqueous solution is mixed with an aqueous solution of ammonia in KOH (see Reactions). Aqueous solution of the tetroxide may be analyzed for osmium by AA or ICP spectrometry (see Osmium). Vapors of the tetroxide may be purged from an aqueous solution by helium, adsorbed over a trap, and desorbed thermally by helium onto a GC. Alternatively, a benzene or carbon tetrachloride solution may be injected onto the GC and the compound peak identified by mass spectrometry. The characteristic mass ions for its identification should be 190 and 254. 

Elemental composition Zn 52.14%, C 9.58%, O 38.28%. Zinc carbonate is identified by effervescence produced upon adding dilute HCl. CO2 evolved is identified by the lime water test or by GC or GC/MS. Characteristic mass for identification of CO2 is 44. Zinc may be analyzed in an acid solution by AA, ICP, and other methods to measure zinc content of the compound. 

The feedstocks (straight-mn naphtha (SRN) and a blend of SRN and hydrocracked naphtha) and hydrotreated products were analysed by ASTM methods for density, carbon, hydrogen, hydrocarbon and boiling point distribution. Total sulfur was determined by ASTM D-4045 method, mercaptan sulfur by the potentiometric method (ASTM D-3227 and UOP-212), disulfides by the UOP-202 method, polysulfides by polarography [1], and elemental sulfur by the UOP-286 method. The Perkin-Elmer gas chromatograph (Model 8700), equipped with a flame photometric detector (GC/FPD) and a DB-1 fused silica capillary column (30 m x 0.53 mm), was used for identification of individual sulfur compounds [2-6]. The sensitivity of the GC/FPD technique was maximized by optimizing the gas flow rates and temperature programming as presented elsewhere [1]. 

Often, one of the the first steps in the identification of an unknown organic compound is to submit the compound for quantitative elemental analysis. This type of analysis will determine the percentage by mass of the elements present in the compound. From the results of the analysis, the empirical formula of the compound can be calculated. To find out the relative amounts of carbon and hydrogen in a hydrocarbon, a weighed sample of the hydrocarbon is passed through a tube packed with copper(ll) oxide at a temperature of about 700°C. The copper(ll) oxide oxidizes the carbon in the hydrocarbon to carbon dioxide and the hydrogen to steam ... 

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