Purity of product

The plutonium extracted by the Purex process usually has been in the form of a concentrated nitrate solution or symp, which must be converted to anhydrous PuF [13842-83-6] or PuF, which are charge materials for metal production. The nitrate solution is sufficientiy pure for the processing to be conducted in gloveboxes without P- or y-shielding (130). The Pu is first precipitated as plutonium(IV) peroxide [12412-68-9], plutonium(Ill) oxalate [56609-10-0], plutonium(IV) oxalate [13278-81-4], or plutonium(Ill) fluoride. These precipitates are converted to anhydrous PuF or PuF. The precipitation process used depends on numerous factors, eg, derived purity of product, safety considerations, ease of recovering wastes, and required process equipment. The peroxide precipitation yields the purest product and generally is the preferred route (131). The peroxide precipitate is converted to PuF by HF—O2 gas or to PuF by HF—H2 gas (31,132). 

Preparation of Plutonium Metal from Fluorides. Plutonium fluoride, PuF or PuF, is reduced to the metal with calcium (31). Although the reactions of Ca with both fluorides are exothermic, iodine is added to provide additional heat. The thermodynamics of the process have been described (133). The purity of production-grade Pu metal by this method is ca 99.87 wt % (134). Metal of greater than 99.99 wt % purity can be produced by electrorefining, which is appHcable for Pu alloys as well as to purify Pu metal. The electrorefining has been conducted at 740°C in a NaCl—KCl electrolyte containing PuCl [13569-62-5], PuF, or PuF. Processing was done routinely on a 4-kg Pu batch basis (135). 

The rate of darkening is related to the temperature of the solution and, if warm potassium hydroxide solution is used, the color will de velop somewhat more rapidly. Differences in the rate of darkening do not appear to affect the yield or purity of product. 

An alternative preparation of deuterio-Raney nickel is described using a more elaborate purification procedure. There is no evidence however, that the use of this nickel results in a better yield or higher isotopic purity of products from the desulfurization reactions. 

The heterogeneous catalytic systems have some advantages over homogeneous re Chemical transformations under heterogeneous conditions can occur v/ith better efficiencies, higher purity of products, and easier work-up Balliniandcoworkers have found that commercial amberlyst A-27 is the best choice for the Michael addition of nittoalkanes v/ith fi-subsdnited alkene acceptors fEq 4111 The reacdon is also carried out by potassium carbonate in the presence of Aliquat 336 under idttasonic irradiadon fEq 4 112 ... 

Chemical purity of product, t Corrosion control of vessel. tD s diameter. H = height. 

For off-bead analysis, coupling between chromatographic separation and mass spectrometric detection has proven especially powerful. The combination between high performance liquid chromatography (HPLC) and electrospray ionisation mass spectrometry has the advantage that purity of product mixtures can be coupled on-line with the product identification. 

HPLC is limited to relatively low molar mass compounds, Le. below 3000. In practice this tends to restrict the technique to dendrons rather than fully formed dendrimers, but it is nonetheless a useful technique, given the importance of establishing high analytical purity of products at each step in a dendrimer synthesis. 

The focus is on the primary formation of bonds, not on subsequent reactions of the products to form other bonds. These latter reactions are covered at the places where the formation of those bonds is described. Reactions in which atoms merely change their oxidation states are not included, nor are reactions in which the same pairs of elements come together again in the product (for example, in metatheses or redistributions). Physical and spectroscopic properties or structural details of the products are not covered by the reaction volumes which are concerned with synthetic utility based on yield, economy of ingredients, purity of product, specificity, etc. The preparation of short-lived transient species is not described. 

The DKRs of (J-azido alcohols and p-hydroxy nitriles were also accomplished hy employing 1 and CALB with PCPA as the acyl donor. The DKRs of p-azido alcohols were performed at 60°C while those of (3-hydroxy nitriles required higher temperature (100°C) primarily to enhance the racemization rate. The optical purities of products were satisfactory in all cases. In the case of p-hydroxy nitriles, dehydrogenation lowered the yield. 

Model cycling of the first column in the purification stream (this usually is subjected to the harshest cleaning conditions and sees the dirtiest feedstocks), process monitoring of production columns (yield and purity of product, HETP measurements, pressure-vs.-flow tests)... 

The 1,3-dipole is often very unstable, its formation requires high temperatures and the subsequent cycloadditions require often long reaction times. Both of these conditions result in a decrease in yields and purity of products. The rapid heating induced by microwave irradiation avoids the harsh reaction conditions associated with classical heating and facilitates 1,3-dipolar cycloadditions that are very difficult (or impossible) to achieve with classical energy sources. 

The reflux ratio = 3, the slope of the fractionating line = 1.4, the purity of product = 99 per cent, and the concentration of carbon disulphide in the waste liquors = 1 per cent. What is the minimum slope of the rectifying line in this case ... 

The synthesis of disperse dyes derived from 1-indanylidenemalononitrile has been performed and the purity of products was checked by TLC. The synthesis scheme is shown in Fig. 3.13. The substituents of the new disperse dyes are listed in Table 3.9. 

Although gradient elution is generally required for RPLC separations of proteins, isocratic elution can be successful in some instances. For example, isocratic elution has been used for the determination of purity of production batches of biosynthetic human growth hormone (HGH).42 The method was used to... 

These macromolecule-based purification methods isolate polymer-bound products from soluble impurities, but do not generally purify the product from other polymer-bound byproducts. Such byproducts arise from incomplete reactions or side reactions and in classical solution chemistry, similar byproducts are removed during product purification at each step of a multi-step synthesis. Support-based methodologies, while removing the multiple, laborious purification steps of a classical synthesis, generally do not provide a method for the purification of intermediates. Instead, these methodologies demand that reaction conditions be optimized such that reactions are driven to completion to avoid a complicated final mixture of products. However, some developed liquid-phase methods achieve high purity of products without quantitative reaction yields [21-26]. 

This is a key finding in understanding why solvent extraction is widely adopted in industrial practice. It is possible to achieve a higher purity of product than would be indicated by the separation between species when they are extracted individually. Clean separations between species with very similar extractabilities such as rare earth ions have proved practical by relying on saturation effects more than on the inherent separability of the species. 

Alkaline nitration with alkoxide bases and nitrate esters was first explored by Endres and Wislicenus who synthesized phenylnitromethane by treating ethyl phenylacetate with potassium ethoxide in ethanol, followed by addition of ethyl nitrate and hydrolysis-decarboxylation of the resulting a-nitroester with aqueous acid. Phenylnitromethane is synthesized in a similar way via alkaline nitration of benzyl cyanide, followed by treatment of the resulting a -nitronitrile with aqueous base. ° Wieland and co-workers used alkali metal alkoxides and nitrate esters for the nitration of cyclic ketones but the yields and purity of product are often poor. ° ... 

The efficiency of the van Arkel-De Boer process (Section II,D) for refining thorium and protactinium metals can be increased by repeating the process to achieve higher purity of product metal. 

The highest yield of perchloryl fluoride (97%) was achieved with a mixture of fluorosulfonic acid and SbFj as fluorinating medium. Potassium, sodium, lithium, magnesium, barium, calcium, and silver perchlorates and perchloric acid itself undergo the reaction. Commercial reagents are used and their additional puriflcation is not necessary unlike all the previous methods the preparation of perchloryl fluoride by this method can be carried out at room temperature. At high temperature (100°-135°C) the reaction time is 1-10 min in all, which allows the process to be carried out continuously in a packed column. The purity of product obtained after the usual puriflcation reaches 98% and over air and carbon dioxide are present as trace impurities 23). 

The starting material for the synthesis of the 4-substituted derivatives 176 was the tautomeric 4(7)-nitrobenzo-triazole 173, which upon methylation with dimethyl sulfate in aq NaOH afforded the 4-nitro-2-methylbenzotriazole 174. The H NMR spectrum of the purified reaction mtKture after methylation showed the existence of all three triazole ring iV-methylated isomers in equal amounts. Compound 174 was isolated by virtue of its insolubility in cone HCl. Purity of products was confirmed by gas liquid chromatography (GLC). 

Gross and Rys (81) investigated correlations between optical purity of product and the degree (%) of conversion in the enantio-differentiating hydrogenation of MAA with TA-MRNis prepared from various kinds of RNi. The degree (%) of conversion at which the highest OY was obtained was found to depend on the sort of RNi as shown in Fig. 35. 

According to White [38a], nitrosation involving the use of dinitrogen tetroxide ( nitrogen tetroxide ) represents the most general method of nitrosating amides. The method is quite rapid, yields are high, and purity of products is excellent. Since nitric acid is a coproduct of the reaction, the normal procedure involves the use of an excess of anhydrous sodium acetate as a base. If the base is not added, dinitrosation takes place. 

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