Copper chromatography

Pyrolysis gas chromatograms (PGC) were obtained on a model AIOOC Wilkens Aerograph gas chromatograph equipped with a Leeds and Northrup Speedomax G Recorder. The copper chromatography column was packed with acid washed chromosorb W and 20% SE-20. Pyrolysis was accomplished by placing a small, dry sample of polymer on a Rh-W, code 13-002, Gow-Mac coil and pyrolyzing for a predetermined time. 

Hydantoin itself can be detected ia small concentrations ia the presence of other NH-containing compounds by paper chromatography followed by detection with a mercury acetate—diphenylcarba2one spray reagent. A variety of analytical reactions has been developed for 5,5-disubstituted hydantoias, due to their medicinal iaterest. These reactions are best exemplified by reference to the assays used for 5,5-diphenylhydantoiQ (73—78), most of which are based on their cycHc ureide stmcture. Identity tests iaclude the foUowiag (/) the Zwikker reaction, consisting of the formation of a colored complex on treatment with cobalt(II) salts ia the presence of an amine (2) formation of colored copper complexes and (3) precipitation on addition of silver(I) species, due to formation of iasoluble salts at N. ... 

Acetylene has a low solubiHty in Hquid oxygen. Excessive concentrations can lead to separation of soHd acetylene and produce accumulations that, once initiated, can decompose violently, detonating other oxidizable materials. Acetylene is monitored routinely when individual hydrocarbons are determined by gas chromatography, but one of the wet classical methods may be more convenient. These use the unique reaction of acetylene with Ilosvay s reagent (monovalent copper solution). The resulting brick-red copper acetyHde may be estimated colorimetricaHy or volumetricaHy with good sensitivity (30). 

Total carbon in beryUium is determined by combustion of the sample, along with an accelerator mixture of tin, iron, and copper, in a stream of oxygen (15,16). The evolved carbon dioxide is usuaUy measured by infrared absorption spectrometry. BeryUium carbide can be determined without interference from graphitic carbon by dissolution of the sample in a strong base. BeryUium carbide is converted to methane, which can be determined directly by gas chromatography. Alternatively, the evolved methane can be oxidized to carbon dioxide, which is determined gravimetricaUy (16). 

A number of analytical methods have been developed for the determination of chlorotoluene mixtures by gas chromatography. These are used for determinations in environments such as air near industry (62) and soil (63). Liquid crystal stationary columns are more effective in separating m- and chlorotoluene than conventional columns (64). Prepacked columns are commercially available. ZeoHtes have been examined extensively as a means to separate chlorotoluene mixtures (see Molecularsieves). For example, a Y-type 2eohte containing sodium and copper has been used to separate y -chlorotoluene from its isomers by selective absorption (65). The presence of ben2ylic impurities in chlorotoluenes is determined by standard methods for hydroly2able chlorine. Proton (66) and carbon-13 chemical shifts, characteristic in absorption bands, and principal mass spectral peaks are available along with sources of reference spectra (67). 

In this work ion-exchange and gel-permeation chromatography coupled with membrane filtration, photochemical oxidation of organic metal complexes and CL detection were applied to the study of the speciation of cobalt, copper, iron and vanadium in water from the Dnieper reservoirs and some rivers of Ukraine. The role of various groups of organic matters in the complexation of metals is established. 

MeOH (copper-coloured prisms) or from diethyl ether by adding MeOH. Also purified by chromatography on columns of magnesia or calcium hydroxide, and crystd from CS2/EtOH. May be purified via the dipalmitate ester. Stored in the dark, in an inert atmosphere. 

EC 1.15.1.1]. Purified by DEAE-Sepharose and copper chelate affinity chromatography. The preparation was homogeneous by SDS-PAGE, analytical gel filtration chromatography and by isoelectric focusing [Weselake et al. Anal Biochem 155 193 1986 Fridovich J Biol Chem 244 6049 7969]. 

Pituitary Growth Factor (from human pituitary giand) [336096-71-0]. Purified by heparin and copper affinity chromatography, followed by chromatography on carboxymethyl cellulose (Whatman 52). [Rowe et al. Biochemistry 25 6421 1986.]... 

In contrast to the stability exhibited by tlie copper reagents contaimng an a-fluorine, the corresponding a-bromocopper reagent is not stable and decomposes to give an excellent yield of the triene (cumulene) product [254] (equation 167) The ( ) and (Z) cumulenes were separated by chromatography, and the structures were assigned by X ray analysis [254]... 

The product is analyzed by vapor phase chromatography using a 6-ft., f-in. O.D. copper tube, packed with 5% Bentone-34 (Wilkins Instrument Co.) and 0.5% XF-1150 (General Electric Silicone Products) on Diatoport-S (80-100 mesh) (F and M Co.) flow rate of helium 60 ml./min., oven temperature 85°. This column separates m-cymene (retention time 12 minutes) from />-cymene (retention time 10 minutes) but does not resolve the ortho isomer. The purity of the distilled w-cymene is above 98%. 

The Vilsmeier formylation of copper deuteroporphyrin dimethyl ester (6) in which unsubstituted /3-positions are present yields a complex mixture of mono- and disubstituted formylation products which can be partially separated by chromatography on neutral alumina.106... 

A similar rcgioselccti vity is observed in the Friedel-C rafts acylation of copper deuteroporphyrin dimethyl ester (6) which gives a mixture of two /Fmonoacylated products 9 when the reaction time and temperature are carefully controlled or diacylated products 10 on prolonged reaction time.85b-100 106 As with the four / -monoformylated deuteroporphyrin derivatives 7a. the acylated products can be separated by chromatography.100106... 

In contrast, transmetalation of the lithium enolate at —40 C by treatment with one equivalent of copper cyanide generated a species 10b (M = Cu ) that reacted with acetaldehyde to selectively provide a 25 75 mixture of diastereomers 11 and 12 (R = CH3) which are separable by chromatography on alumina. Other diastereomers were not observed. Similar transmetalation of 10a (M = Li0) with excess diethylaluminum chloride, followed by reaction with acetaldehyde, produced a mixture of the same two diastereomers, but with a reversed ratio (80 20). Similar results were obtained upon aldol additions to other aldehydes (see the following table)49. 

Usually, HPLC analysis resolves four peaks identified by co-chromatography with authentic standards as copper pheophorbide a, Cn(II) chlorin e6, Cn(II) chlorin e4, Cu rhodin g7, and their degradation products, but a sum of other colored components can also be found, for example, native chlorophylls, pheophytins, pheophor-bides, and rodochlorins (free carboxyl forms of pheophorbides) besides epimers, allomers, and degradation products that have been only tentatively identified. 

Inoue, H. et al., Determination of copper(II) chlorophyllin by reversed-phase high-performance liquid chromatography, J. Ghromatogr. A, 679, 99, 1994. 

The gases used were purchased premixed in aluminum cylinders to avoid carbonyl formation. The high purity gas mixture was further purified by a zeolite water trap and a copper carbonyl trap. The gas pressure in the reactor was measured with a capci-tance manometer and the fTow monitored with a mass fTow controT-ler. The typical gas flow rates were 15 cc/min (STP) and the maximum conversion was 1% based on integration of hydrocarbon products. The hydrocarbon products were analyzed by gas chromatography (temperature programmed chromosorb 102, FID). 

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