Elements materials data

Gladney ES, O Malley BT, Roeiandts I, and Gills TE (1987,1993 update) Standard Reference Materials Compilation of Elemental Concentration Data for NBS Chemical, Biological Geological and Environmental SRMs. NBS Spec Pub 260-111, NIST, Gaithersburg, MD. 

Widespread medicinal use of colloidal bismuth subcitrate (CBS) has prompted extensive studies of bismuth compounds involving the citrate anion. Bismuth citrate is essentially insoluble in water, but a dramatic increase in solubility with increasing pH has been exploited as a bio-ready source of soluble bismuth, a material referred to as CBS. Formulation of these solutions is complicated by the variability of the bismuth anion stoichiometry, the presence of potassium and/ or ammonium cations, the susceptibility of bismuth to oxygenation to Bi=0, and the incorporation of water in isolated solids. Consequently, a variety of formulas are classified in the literature as CBS. Solids isolated from various, often ill-defined combinations of bismuth citrate, citric acid, potassium hydroxide, or ammonium hydroxide have been assigned formulas on the basis of elemental analysis data or by determination of water and ammonia content, but are of low significance in the absence of complementary data other than thermal analysis (163), infrared spectroscopy (163), or NMR spectroscopy (164). In this context, the Merck index lists the chemical formula of CBS as KgfNHJaBieOafOHMCeHsCbh in the 11th edition (165), but in the most recent edition provides a less precise name, tripotassium dicitrato bismuthate (166). 

The PSM Standard requires that the following information be contained within the PSI element-physical data, reactivity data, corrosivity data, thermal and chemical stability data, and hazardous effects of potential inadvertent mixing of different materials. The standard does not specifically define what is to be included in any of these data categories, the level of detail required, or the method of compilation.41 It does, however, stipulate that an MSDS can be used to compile the data to the extent that it contains the information required. In 1996, OSHA issued a Hazard Information Bulletin cautioning that MSDSs do not always contain information about hazards from mixing or blending chemicals (OSHA, 1996). 

To further characterize the effect of the ammonia hydrothermal treatment, we compared elemental analysis data and 1R spectra before and after ammonia hydrothermal treatment to quantitatively disclose the role of counterion between the silica framework and surfactants. In Table 2, the N/C molar ratio of the mesoporous materials prior to the ammonia hydrothermal treatment is nearly twice of that after the treatment. Moreover, the IR band at 1383 cm 1, which arises from the N03 stretch bending mode, completely disappears after ammonia hydrothermal treatment [20], These results verify that the existence of nitrate counterion (the nitrate/surfactant 1) between surfactant molecules and silica framework in the acid-made mesoporous materials. The bridging counterion N03 was completely removed after ammonia hydrothermal treatment. 

E. S. Gladney, C. E. Burns, D. R. Perrin, I. Roelandts, T. E. Gill, 1982 Compilation of Elemental Concentration Data for NBS Biological, Geological, and Environmental Standard Reference Materials, NBS Special Publication, 1984, 260-288. 

The product from Step 1 (3.2mmol) was dissolved in 50ml CH2CI2 and treated with 1,T-carbonyldiimidazole (3.6 mmol) and aniline (4.4 mmol), stirred 18 hours, concentrated, and purified by chromatography on silica gel using diisopropyl ether/diethyl ether. Thereafter, the product was dissolved in 10 ml hot propan-2-ol and the solution acidified with ethereal HCl. The material crystallized upon trituration with ether and 0.897 g product isolated as dihydrochloride quarter hydrate, mp = 250-255 °C (dec.). Elemental analysis data supplied. 

To the crude product from Step 1 (6.96 g) dissolved in 30 ml triethylamine and 6 ml dimethylformamide at ambient temperature was added 3 ml trimethylsilylacetylene, Cul (150 mg) and bis(triphenyl-phosphine)palladium(II)chloride (300 mg). The mixture was heated 1 hour to 50-60°C, an additional 0.3 ml trimethylsilylacetylene added, and heating continued 30 minutes. The cooled mixture was diluted with 250 ml water, extracted with 250 ml diethyl ether, separated, dried, and concentrated. The material was purified by chromatography on silica gel using CH2Cl2/hexane, 1 1, re-crystallized from diethyl ether/hexane, and the product isolated, mp = 181-182°C. H-NMR, MS, and elemental analysis data supplied. 

Free base N-guanylurea was prepared by dissolving N-guanylurea sulfate hydrate (0.5 mmol) in 3 ml water and neutralizing with aqueous NaOH (1 mmol). This material was added to a stirred suspension of the product from Step 3 dissolved in 3 ml of water, stirred 2 hours at 25 °C, further cooled to 5 °C, filtered, and the product isolated in 96% yield, mp >300°C (dec). H- and C-NMR and elemental analysis data supplied. 

In Table III are reported elemental analyses of the original sample (toluene-soluble and toluene-insoluble fractions), of the bases obtained from them, and of the unprecipitated remainder. The preasphaltenes, though defined as tetrahydrofuran-soluble, toluene-insoluble materials, are sufficiently soluble in toluene (approximately 1 g/100 mL) to be used in these precipitation experiments. The elemental analysis data suggest that no significant fractionation has taken place in this dissolution step. 

To provide a clear idea of the accuracy that can be expected in the analysis of a complex material, data on the determination of four elements in a variety of materials are presented in Tables 34-1 to 34-4. These data were taken from a much larger set of results collected by W. F. Hillebrand and G. E. F. Lundell of the National Bureau of Standards and published in the first edition of their classical book on inorganic analysis.-... 

Gladney, E. S. "Compilation of Elemental Concentration Data for NBS biological and Environmental Standard Reference Materials" LA-8438MS Informal Report, July 1980, pp. 14-20. 

The NMR spectrum of the polysiloxane-immobilized diethylpropyl-amine system in Fig. 25.5C shows signals at 12.6, 21.8 (shoulder at 27.2), 47.8 and 57.0 ppm. The shoulder at 27.2 ppm may come from C(2 ) of residual, unreacted 3-chloropropyl groups, due to incomplete reaction of 3-chloropro-pylpolysiloxane with diethylamine. The C(T) and C(3 ) peaks of the residual precursor ((S)-CH2CH2CH2C1) are overlapped with the C(l) and C(4) peaks of the product, polysiloxane-immobilized diethylpropylamine system. This interpretation of the 27.2 ppm shoulder is in agreement with the elemental analysis data, which show that unreacted polysiloxane-immobilized 3-chloropropyl material remained in the product. 

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