Hydrogen elemental analysis

Measurement of percentage of acidic hydrogens by nmr was calculated from the relative area of the carbonyl carbon (169 ppm) to the total carbon atoms and from the carbon hydrogen elemental analysis (equation 2). 

Elemental analysis was performed on various coals, pitches, and blends. Table 7 reports the elemental composition of products from WVGS 13407. Compared to the raw coal, the NMP-soluble extract (EXT) contams essentially the same amount of carbon, though there is slightly more hydrogen as mdicated by a... 

For the most part, the elemental analysis data for the blends are consistent with a weighted average of the individual components. Also shown is the elemental analysis for some of the soluble products form WVGS 13423 in Table 10 As was observed for the WVGS 13421 products, hydrogenation increased the total hydrogen content and decreased the atomic C/H ratio. 

ADMET polymers are easily characterized using common analysis techniques, including nuclear magnetic resonance ( H and 13C NMR), infrared (IR) spectra, elemental analysis, gel permeation chromatography (GPC), vapor pressure osmometry (VPO), membrane osmometry (MO), thermal gravimetric analysis (TGA), and differential scanning calorimetry (DSC). The preparation of poly(l-octenylene) (10) via the metathesis of 1,9-decadiene (9) is an excellent model polymerization to study ADMET, since the monomer is readily available and the polymer is well known.21 The NMR characterization data (Fig. 8.9) for the hydrogenated versions of poly(l-octenylene) illustrate the clean and selective nature of ADMET. 

An elemental analysis of epinephrine resulted in the following composition 59.0% carbon, 26.2% oxygen, 7.15% hydrogen, and 7.65% nitrogen by mass. When 0.64 g of epinephrine was dissolved in 36.0 g of benzene, the freezing point decreased by 0.50°C. (a) Determine the empirical formula of epinephrine, (b) What is the molar mass of epinephrine ... 

The scanning transmission electron microscope (STEM) was used to directly observe nm size crystallites of supported platinum, palladium and first row transition metals. The objective of these studies was to determine the uniformity of size and mass of these crystallites and when feasible structural features. STEM analysis and temperature programmed desorption (TPD) of hydrogen Indicate that the 2 nm platinum crystallites supported on alumina are uniform In size and mass while platinum crystallites 3 to 4 nm in size vary by a factor of three-fold In mass. Analysis by STEM of platinum-palladium dn alumina established the segregation of platinum and palladium for the majority of crystallites analyzed even after exposure to elevated temperatures. Direct observation of nickel, cobalt, or iron crystallites on alumina was very difficult, however, the use of direct elemental analysis of 4-6 nm areas and real time Imaging capabilities of up to 20 Mx enabled direct analyses of these transition metals to be made. Additional analyses by TPD of hydrogen and photoacoustic spectroscopy (PAS) were made to support the STEM observations. 

The number of surface atoms can be determined by chemisorption of probe molecules (H2, O2...), knowing the stoichiometry of the adsorbed species. As an example, in the case of Pt, the stoichiometry of irreversibly adsorbed hydrogen (H/Pts) and oxygen (0/Pts) at room temperature are both close to 1/1 [108-111]. Knowing the total number of atoms (elemental analysis) and the number of irreversibly adsorbed H and O, the dispersion of the particles (D = Pts/Pt) is then easily obtained. Note that the dispersion of these particles decreases when their size increases (Fig. 5). 

Compounds 24a,b were reduced to the corresponding amino pyrazolones 25a-c by catalytic hydrogenation over 5% Pd - C in methanol. These amino pyrazolones were isolated as hydrochlorides because the free bases were decomposed in air with red coloring. The structural assignments of 24a,b and 25a-c were based on elemental analysis and spectral data. 

The tetradentate ligands (340) and (341) form 1 1 metakligand complexes with [IrCl(cod)]2.548 The complexes were tested in the asymmetric hydrogenation of prochiral olefins, providing enantioselectivities up to 36%. The multitopic ligands L, (342) and (343), bind to Ir1 to form [IrL] species which have been characterized by elemental analysis, mass spectrometry, IR and NMR spectroscopy.549 The complexes show enantioselectivities of up to 30% for the hydrogenation of prochiral olefins under mild reaction conditions. 

Elemental analysis shows that the polymer generally contains four monomer units per dopant ion [20], and that there is also more hydrogen than would be expected (cf. polypyrrole) [20, 395], although this may vary depending on the starting material [409,410,414], Even in the neutral form, the polymer contains a small quantity of anions (0.5-1%) [19], although Waltman et al. [400] found that the extent to which the counter ion is incorporated into the polymer on polymerisation depends strongly on the nature of the /J-substituent (if present). 

If the sample is pure (this can generally be checked by thin layer chromatography or gas chromatography) then the elemental analysis values for carbon, hydrogen and nitrogen can be used to obtain element ratios, provided that C, H, N and 0 are the only elements present. 

Elemental analysis of the oils was carried out as follows carbon and hydrogen by micro combustion using a Perkin-Elmer 240 Elemental Analyzer sulphur by X-ray fluorescence using a Telsec Lab X-100 apparatus nitrogen by chemiluminescence using a Dohrmann DN-10 apparatus. 

These complexes anchored to a solid via a ligand have been tested for a number of reactions including the hydrogenation, hydroformylation, hydrosilylation, isomerization, dimerization, oligomerization, and polymerization of olefins carbonylation of methanol the water gas shift reaction and various oxidation and hydrolysis reactions (see later for some examples). In most cases, the characterization of the supported entities is very limited the surface reactions are often described on the basis of well-known chemistry, confirmed in some cases by spectroscopic data and elemental analysis. 

Elimination of hydrogen halides from dihalogenoorganylboranes by reaction with ferrocene-1,1 -dithiol resulted in l,3-dithia-2-boryl[3]ferrocenophanes.170 These borylferrocenophanes were air sensitive, but were characterized by NMR, MS, and elemental analysis.170 A series of l,3-dibora-2-X-[3]fer-rocenophanes (X=S, Se, Te) were prepared and characterized and the crystal structure of [Se N Pr2)BC5Fl4 2Fe] has been reported.171... 

Ion induced nuclear reactions for light element analysis in general and hydrogen analysis in particular have been extensively discussed in the literature. Only a few ion-induced nuclear reactions have cross sections large enough to be useful for materials analysis, and these are listed in published compilations (Amsel et al., 1971 Mayer and Rimini, 1977). 

The above TGA and elemental analysis studies are consistent with Van Krevelen s two step model for polymer charring (2) in which a polymer first rapidly decomposes at 500°C to fuel gases and a primary char residue characterized by modestly high hydrogen content. On further heating above 550°C, this primary char is slowly converted in a second step to a nearly pure carbon residue by the loss of this hydrogen. 

Two methods were examined for digestion of biological samples prior to trace element analysis. In the first one a nitric acid-hydrogen peroxide-hydrofluoric acid mixture was used in an open system, and in the second one nitric acid in a closed Teflon bomb. The latter method was superior for Ge determination, however, germanium was lost whenever hydrogen fluoride had to be added for disolving sihcious material. End analysis by ICP-AES was used for Ge concentrations in the Xg/g range13. 

---