C Analysis

C. Analysis of Two-Electron, Two-Orbital, Single-Bond Formation... 

Acrolein is produced according to the specifications in Table 3. Acetaldehyde and acetone are the principal carbonyl impurities in freshly distilled acrolein. Acrolein dimer accumulates at 0.50% in 30 days at 25°C. Analysis by two gas chromatographic methods with thermal conductivity detectors can determine all significant impurities in acrolein. The analysis with Porapak Q, 175—300 p.m (50—80 mesh), programmed from 60 to 250°C at 10°C/min, does not separate acetone, propionaldehyde, and propylene oxide from acrolein. These separations are made with 20% Tergitol E-35 on 250—350 p.m (45—60 mesh) Chromosorb W, kept at 40°C until acrolein elutes and then programmed rapidly to 190°C to elute the remaining components. 

Fig. 5. Various current transients obtained by a time-of-fligbt method (a) nondispersive transport (b) dispersive transport and (c) analysis of disperse...

Choline Bitartrate. This substance [87-67-2] is a white crystalline material possessing an acid taste. It melts at 149—I53°C. Analysis by cobaltous chloride shows more than 99% as the bitartrate. Free ethylene glycol is less than 0.25%, with free alkaU at 0.0%. 

A long evolving use of PSA was for Anticipated Transients without Scram (ATWS) which extended over 15 years to culminate in NUREG-0460 which was upset by the Salem failure-to-scram incident and the subsequent SECY Letter 83-28. Other special studies have been (a) value-impact analysis (VIA.) studies of alternative containment concepts (e.g., vented containment, NUREG/CR-0165), (b) auxiliary feedwater studies, (c) analysis of DC power requirements, (d) station blackout (NUREG/CR-3220), and (e) precursors to potential core-damage accident.s (NUREG/CR-2497), to name a few of the NRC sponsored studies. 

Methylpiperidino)-propyl p-cyclohexyloxybenzoate hydrochloride thus prepared melted at about 178° to 180°C. Analysis showed the presence of 8.88% chlorine as compared with the calculated value of 8,96%. 

N-(a-methylhomoveratryl)-3-methoxy-4-ethoxyphenylacetamide thus prepared melted at about 135°-136°C. Analysis showed the presence of 68.05% carbon and 7.62% of hydrogen compared with the calculated amount of 68.19% carbon and 7.54% hydrogen. 

Dimethoxy-3-methyl-T(3 -methoxy-4 -ethoxybenzylisoquinoline thus prepared melted at 124°-125°C. Analysis showed the presence of 71.68% carbon and 7.07% hydrogen as compared with the calculated amount of 71.91% carbon and 6.85% hydrogen. 

To make the hydrochloride salt, the bisacetamide or, by another name, 1,11-diphenyl-2,2,3,9,10,10-hexamethyl-4 3hydroxy ethyl )-3,6,9-triazaundecane is dissolved In n-butanol. The solution is chilled and then dry hydrogen chloride gas is passed into the solution causing an oil to separate. To the heavy oil ether is added and then stirred causing crystallization to occur. MP146°Cto 147°C. Analysis for nitrogen calc. 8.3%, found 8.2%. 

To make the acetate salt, the bisacetamide (4.7 g) (0.01 mol) is dissolved in ethyl acetate to vuhich is added glacial acetic acid (OB g) (OjOI mol). Ether is added to precipitate the acetate as a gum vuhich is vuashed vuith hexane, and finally added to dry ether. Allovu to stand for crystallization. MP 141 °C. Analysis for nitrogen calc. 8.0% found 8.2%. 

The only known instance of ring-opening polymerization with these compounds is also the only report on the successful polymerization of 2,5-dihydrofuran74 in which this compound was cationically copolymerized with epichlorhydrin (rx 0, r2 0), propylene oxide (r, 0, r2 0) and 3,3-bischloromethyl oxacyclobutane (/ ] 0, r2 = 1.6). It was shown that all the copolymers obtained possessed a certain degree of unsaturation which was attributed to the presence of open units from 2,5-dihydrofuran. Thus, for example the alternating copolymer with epichlorhydrin had the following structure (IR spectra, Cl content. C=C analysis) ... 

The TBDMS ether was dissolved in MeCN containing 5-30% of aqueous HF (40%), and the course of the reaction monitored by direct t.l.c. analysis. When deprotection was complete, chloroform and water were added. Normal isolation procedures then gave the free alcohol. 

An aqueous solution of HF (40%, 2eq.) was added to a solution of the substrate in MeCN at either 0°C or at ambient temperature. When the reaction was complete by t.l.c. analysis (ca. 30min), excess sodium hydrogen carbonate solution (8%) was added, and the product was extracted with ether. The product was purified by flash chromatography on silica gel. 

A solution of Pd(OAc)2 (0.05 mmol) and bis(diphenylphosphino)ethane (0.05 mmol) in acetonitrile (1 ml) was heated gently to reflux, at which time a solution of the silyl enol ether (1 mmol) and diallyl carbonate (2 mmol) in MeCN (4 ml) was added in one portion. The mixture was heated under reflux for 1-3 h, the course of reaction being monitored by t.l.c. or g.l.c. analysis. On completion, the cooled reaction solution was filtered through fluorosil. The pure a/ -unsaturated compound was isolated by column chromatography on silica gel (70-95%). 

HF-induced elimination (5). To a solution of aqueous HF (4 drops, 50%) in MeCN (8 ml) was added a solution of the /3-hydroxysilane (lmmol) in MeCN (2ml), and the mixture was stirred at room temperature until t.l.c. analysis indicated completion (5-20min). The reaction mixture was then partitioned between pentane (50 ml) and saturated sodium hydrogen carbonate solution (10ml). The aqueous layer was extracted thoroughly with pentane (3 x 50 ml), and the combined organic extracts were washed with brine and dried. Concentration followed by chromatographic purification gave the product alkenes. 

To a solution of 4-t-butylcyclohexanone (lmmol), tris(triphenylphos-phine)ruthenium(n) chloride (0.05 mmol) and silver trifluoroacetate (0.05 mmol) in toluene (5 ml) was added triethylsilane (1.5 mmol). The mixture was heated under reflux for 20 h, and concentrated under reduced pressure. The residue was diluted with hexane (3 ml), filtered and distilled to give a mixture of triethylsilyl ethers (0.96mmol, 96%), b.p. 70°CI 0.1 mmHg. G.l.c. analysis shows an axial (cis) equatorial (trans) ratio of 5 95—a result comparable to the best LAH results. 

West, A. C. Analysis of Mass Transfer and Fluid Flow for Electrochemical Processes 32... 

Disconnecting one of the C-N bonds around the tertiary amine will help (a) is not possible, (b) would be possible after FGl to the amide but (c) separates the two nitrogens and requires the easily synthesised (16) as intermediate. We shall follow (c). Analysis... 

Preparation of F-2DFG through the reaction of tri-C>-acetyl-D-glucal (61) and Xe F2 has been reported - (see Section 11,5). In 1985, a question was raised concerning the purity of the synthetic F-2DFG thus far reported. Thus, van Rijn and coworkers " clarified, by t.l.c. (NaH2P04-impregnated silica plates) and h.p.l.c. analysis, that the addition reactions of AcOF to... 

Bridle, R and Garcia-Viguera, C., Analysis of anthocyanins in strawberries and elderberries a comparison of capiUary-1 electrophoresis and HRLC, Food Ghent., 59, 299, 1997. 

Rastogi, S. C., Analysis of diisocyanate monomers in chemical products containing polyurethanes by high pressure liquid chromatography, Chro-matographia, 28, 15, 1989. 

Kim, Y. J. Freas, A. Fenselau, C. Analysis of viral glycoproteins by MALDI-TOF mass spectrometry. Anal. Chem. 2001, 73,1544—1548. 

Phosphorylation of the GABAA receptor by cAMP-dependent protein kinase and by protein kinase C analysis of the substrate domain. Neurochem. Res. 18, 95-100. 

The fractions from elution chromatography were studied by a number of spectroscopic methods, n.m.r., i.r., u.v., fluorescence and phosphorescence spectroscopy. Equivalent fractions from chromatographic separation of the various oils showed no significant differences in their spectra and it appears that the composition of the fractions was independent of the catalyst concentration used to produce the oil. Though, as previously mentioned the amounts of the various fractions especially the polar fractions differ with the catalyst concentration. G.1.C. analysis of the saturate fractions also indicated no changes with different catalyst concentrations. 

Compositional analysis shows a decrease in the percentage of polar compounds in the oils with increasing residence time (see Table II). The decrease in polar content is substantiated by a lower sulphur content and results in a lower viscosity (see Table II). The oil becomes more aromatic, as shown by n.m.r. spectroscopy (see Table II), with increasing time at temperature, while the molecular weights showed little change. G.l.c. analysis of the saturate hydrocarbon fractions from elution chromatography indicated little change in the saturates with residence time. 

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