Product oils elemental analysis

Results from the liquefaction experiments with the five molst-blomass feedstocks are given In Table III. The oil yield Is based on the combined mass of acetone- and methylenechlorlde-soluble oils as a percent of the mass of dried feedstock calculated to an ashfree basis. The product oil elemental analysis Is the calculated composite analysis for the combined acetone- and methylene chloride-soluble oils. 

The product from Step 1 was dissolved in 50 ml toluene, tri-n-butyltin-hydride (9.7 mmol) added followed by azobisisobutyronitrile (30 mg). The mixture was heated to 95 °C 5 hours, cooled, concentrated, purified by chromatography on silica gel using EtOAc/hexane, (1 1), and the product isolated in 60.8% yield as an oil. Elemental analysis data supplied. 

The product from Step 2 (0.38 mmol) was dissolved in 15 ml chloroform at ambient temperature and 0.1 M iodine dissolved in chloroform added dropwise until a brown color persisted. Thereafter, the reaction was stirred 24 hours and then quenched with 2 ml 1 M KF dissolved in methyl alcohol and 2 ml 5% aqueous sodium bisulfite. The layers were separated, the aqueous layer extracted 3 times with 20 ml chloroform, washed, dried, concentrated, and the product isolated in 84.3% yield as a slightly yellow oil. Elemental analysis data supplied. 

Solid sodium nitrite (0.97 g) was added at room temperature with stirring over a period of one hour to a solution of 2-chloro-9-(2-hydroxyethoxymethyl)adenine (0.5 g) in glacial acetic acid (10 ml). The reaction mixture was stirred for an additional A A hours. The white solid was removed by filtration, washed with cold acetic acid and then well triturated with cold water to remove the sodium acetate present. The solid product was retained. The combined acetic acid filtrate and wash was evaporated at reduced pressure and 40°C bath temperature and the residual oil triturated with cold water. The resulting solid material was combined with the previously isolated solid and the combined solids dried and recrystallized from ethanol to give 2chloro-9-(2-hydroxyethoxymethyl)+iypoxanthine (0.25 g), MP>310°C. Elemental analysis and NMR spectrum were consistent with this structure. 

The material balance is consistent with the results obtained by OSA (S2+S4 in g/100 g). For oil A, the coke zone is very narrow and the coke content is very low (Table III). On the contrary, for all the other oils, the coke content reaches higher values such as 4.3 g/ 100 g (oil B), 2.3 g/ioo g (oil C), 2.5 g/ioo g (oil D), 2.4/100 g (oil E). These organic residues have been studied by infrared spectroscopy and elemental analysis to compare their compositions. The areas of the bands characteristic of C-H bands (3000-2720 cm-1), C=C bands (1820-1500 cm j have been measured. Examples of results are given in Fig. 4 and 5 for oils A and B. An increase of the temperature in the porous medium induces a decrease in the atomic H/C ratio, which is always lower than 1.1, whatever the oil (Table III). Similar values have been obtained in pyrolysis studies (4) Simultaneously to the H/C ratio decrease, the bands characteristics of CH and CH- groups progressively disappear. The absorbance of the aromatic C-n bands also decreases. This reflects the transformation by pyrolysis of the heavy residue into an aromatic product which becomes more and more condensed. Depending on the oxygen consumption at the combustion front, the atomic 0/C ratio may be comprised between 0.1 and 0.3 ... 

One gram (0.0054 mol) of dithiomaleonitrile disodium salts was mixed with 1.65 mL (0.0108 mol) of 3-Phenylpropylbromide in 30 mL of acetone refluxed a 60°C for about 20 hours. The reaction time was controlled by TLC. When acetone was evaporated, the remain which was oil like product treated with CHCl to remove insoluble salts by decantation. The CHClj phase was extracted several times with Na SO. The crude oil product obtained by evaporation of the solvent was chromatographed on a silica column (eluent Chloroform). Yield 2.1 g (89%) Mw 378 g/mol (determined by GC-MS) The product is good soluble in CHCl, acetone and hexane. Elemental analysis results for Calculated C 69.80, H 5.86, N 7.40, S 16.94, Experimental 69.27, H 5.8, N 7.33, S 16.32%. 

Elemental analysis of fuel oil often plays a more major role that it may appear to do in lower-boiling products. Aromaticity (through the atomic hydrogen/carbon ratio), sulfur content, nitrogen content, oxygen content, and metals content are all important features that can influence the use of residual fuel oil. 

In two cases submitters have observed that the residue separated into two layers. The upper layer consists of a heavy oil apparently because of incomplete washing of the lithium suspension used in manufacturing methyl 1 ithium. When this happens it is necessary to remove the oil with a pipette prior to distillation. Failure to do so gives a product which appears pure by TLC, but which is substantially impure according to elemental analysis (IX high in carbon). ... 

The oil described above was utilized directly in the condensation reaction with the epichlorohydrin. A mixture of 0.1 mole of methyl 3-(4-hydroxyphenyl)propionate, 0.2 mole potassium carbonate and 0.4 mole epichlorohydrin in 250 mL acetone was heated to reflux for 24 hours. The reaction medium was then filtered and evaporated. The residue was taken up in 100 mL toluene and washed with 100 mL 1.0 N NaOH and 100 mL water (2 times). The toluene phase was then dried over magnesium sulfate and evaporated to provide the crude product as an oil. Purification was effected by vacuum distillation (156°C/0.4 mm) and provided methyl 3-[4-(2,3-epoxypropoxy)phenyl]propionate. The NMR and IR spectra and elemental analysis data were consistent with the assigned structure. 

Purify of the crude residue by flash chromatography on silica gel using hexane ethyl acetate as eluent (gradient elution from 98 2 to 90 10). Pure 6-(dimethylphenylsilyl)-2,2-dimethyl-4-(2-phenylethyl)-5-hexyn-3-one (33) (0.141 g, 65%) as a clear oil. Characterize the product by 1H NMR, IR, MS spectroscopy, and elemental analysis. 

The oil was dissolved in 20 ml toluene/heptane, 1 1, and the product isolated by chro-matographyon silica gel with CH2CI2 in 50% yield. Elemental analysis data supplied. 

HCI. The product was extracted 3 times using 50 ml CH2CI2 and extracts combined, dried, and filtered. The solvent was removed and a brown oil obtained which slowly crystallized, was purified by flash chromatography using CH2Cl2/hexanes, 2 1, and the product isolated in 89% yield, mp = 116-117°C. and C-NMR and elemental analysis data supplied. 

NaBH4 (9.25 mmol) was added to a solution of the product from Step 2 (4.81 mmol) dissolved in 100 ml methyl alcohol at 0°C. After 3 hours, the solvent was removed and the residue acidified to pH 2 using 2 M HCl. The mixture was then neutralized with NaHCOj and the product extracted 3 times with 50 ml diethyl ether. The product was isolated as an oil, re-crystallized in hexane/chloroform, 3 1, and isolated in 96% yield as 1 1 trans/cis isomers, mp = 89-90°C. H- and F-NMR and elemental analysis data supplied. 

Table I. Elemental Analysis of Bitumen and Product Oils...

A total of 310.3 g of methyl ester were pyrolysed to yield 204.4 g of liquid product which corresponds to a 65.9% actual liquid yield. The theoretical yield based on a typical Cie, C composition of soybean oil, and the y-hydrogen transfer mechanism is approximately 76%. Therefore, the yield based on this limitation is approximately 87%. "niis shows that random cracking of the ester chain does not play a significant role in the reaction. The infrared spectrum shows no carbonyl peaks at 1720 cm. Peaks appearing at 907 cm" and 965 cm arc probably absorptions due to terminal alkenes and trans alkenes, otherwise the spectrum looks like that of a typical alkane. Consistent with these results, elemental analysis gave 83.7% carbon, 14.56%... 

Trace elemental analysis can also be used to indicate the level of contamination of middle distillate fuels, e.g. turbine fuels. Metal contamination can cause corrosion and deposition on turbine components at elevated temperatures. Some diesel fuels have specification limits to guard against engine deposits, however they sometimes employ Mo or Ni as a catalyst for the refining process which eventually ends up in the finished products. There are several sources of multi-elemental contamination in naval distillate fuels. Sea water is pumped into the diesel tanks as ballast to immerse ships and submarines. Some oil transport ships have dirty tanks and contamination and corrosive products can also come from piping, linings and heat exchangers. 

Test methods of interest for hydrocarbon analysis of residual fuel oil include tests that measure physical properties such as elemental analysis, density, refractive index, molecular weight, and boiling range. There may also be some emphasis on methods that are used to measure chemical composition and structural analysis, but these methods may not be as definitive as they are for other petroleum products. 

The ASTM International D02 Committee on Petroleum Products and Lubricants through its Subcommittee 3 on Elemental Analysis has played a large and crucial role in the last several decades in standardizing numerous elemental analysis methods used in the oil industry. Currently there are about 75 standard test methods under the jurisdiction of SC 3, and additionally at least 6 more are under active development and moving towards standard designations. I have no doubt that this activity will continue in the future. These standards comprise virtually ail known modem techniques for elemental analysis of petroleum products and lubricants. 

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