D. Thorburn Burns

Aqueous size-exclusion chromatography

Part I. Separation Mechanisms. Size exclusion parameters (M.E. Himmel, P.G. Squire). Partitioning: Hydrophobic interactions (M. Janado). Electrostatic effects (P.L. Dubin). Exclusion chromatography of inorganic compounds (M. Shibukawa, N. Ohta). II. Characterization of Stationary Phases. Pore size distributions (L. Hagel). Structural analysis of porous materials by measurement of size exclusion (S. Kuga). Column efficiency (S. Mori). III. New Packings. Native and bonded silicas in aqueous SEC (K.K. Unger, J.N. Kinkel). Rigid polymer gels for SEC and their application to biopolymers (K. Makino, H. Hatano). IV. Biopolymers. Biopolymers. I. Protein chromatography in denaturing and non-denaturing solvents (R.C. Montelaro). Biopolymers. II. Serum lipoproteins (M. Okazaki, I. Hara). Application of SEC/LALLS to biopolymer assemblies (K. Konishi). V. Associating Systems. Measurement of equilibrium constants by exclusion methods (T.K. Korpela, J.-P. Himanen). 14. Frontal boundary analysis in size exclusion chromatography of self-associating proteins (G.W. Becker). 15. Exclusion chromatography of micelles (K.S. Birdi). Subject Index.

Quantitative analysis using chromatographic techniques

Introduction to the Chromatographic Process Detection in Quantitative Liquid Chromatography Quantitative Analysis by Liquid Chromatography Detection in Quantitative Gas Chromatography Quantitative Analysis by Gas Chromatography Quantitative Thin-Layer Chromatography Chromatography as a Quantitative Tool in Pharmaceutical Analysis Is Automation the Future of Quantitative Chromatography? Physico-Chemical Information from Peak Shape and Width in Liquid Chromatography.

Investigation of the determination of tin tetraalkyls and alkyltin chlorides by atomic-absorption spectrometry after separation by gas-liquid or high-performance liquid-liquid chromatography

A variety of sample presentation and atomisation methods have been examined to obtain sufficient sensitivity for the trace determination of tin tetraalkyls and alkyltin chlorides (RnSnCl4–n; R = methyl or ethyl; n= 1–4) after their separation by gas-liquid or by high-performance liquid-liquid chromatography. Detection limits range from 10–20 µg (flame atomisation) to 1 µg (direct pyrolysis) and 2–20 pg (hydride reduction followed by direct pyrolysis). The construction of systems including an automated hydride generator is described.

Use of basic dyes in the determination of anions, particularly as a means of determining antimony, thallium, and gallium.

The use of xanthene, triphenylmethane and other basic dye cations as reagents for the determination of anions is reviewed. Elements and anions determined include Sb, Tl, Ga, Au, Te, In, Zn, Ta, Hg, Re, Sn, U, Os, B, Cr, Ag, ClO(4)(-), PO(4)(-), SO(4)(2-) and NO(3)(-). Difficulties encountered in developing satisfactory procedures involving basic dyes are discussed. Procedures for the purification and analysis of basic dye samples are outlined.

Pyrolysis gas chromatography as an aid to the identification of Penicillium species

Using pyrolysis gas chromatography it was possible to identify each of a series of eleven Penicillium species and the related species Aspergillus niger CMI 31821 and Neurospora crassa CMI 75723, based on relative peak heights and retention times of the most reproducible peaks in each pyrogram.

Analytical aspects of organo-P, As, Sb, S, Se, Te and Sn(IV) (onium) cations

Reactions and the analytical applications of tetraphenyl-phosphonium, -arsonium and -stibonium, triphenylmethylarsonium, triphenyl-sulphonium, -selenonium and -telluronium and triphenyltin cations with oxy-anions, and halo- and thiocyanato-anionic complexes are surveyed.

A critical study of Brilliant green as a spectrophotometric reagent: extraction of chloro-complexes of antimony, thallium, gallium and indium, and of tetrabromoindate(III), and improved procedures for the determination of antimony and thallium

Use of cerium(IV), instead of nitrite, to oxidise antimony(III) improves the procedure for the determination of antimony with Brilliant green. Antimony(III) is oxidised in 6 M hydrochloric acid solution, the excess of oxidant being reduced with hydroxylammonium chloride. Brilliant green hexachloroantimonate(V) is extracted from 2 M hydrochloric acid solution with two 10-ml portions of toluene, the Brilliant green reagent solution being added to the aqueous solution immediately before each extraction. When a pure sample of dye is used, and the extraction is made rapidly after the addition of Brilliant green, complete recovery of antimony is effected. The recommended procedure is precise and reliable.A similar procedure based on the extraction of tetrachlorothallate(III) ions gives complete recoveries of thallium and is an improvement on existing procedures. Tetrachlorogallate(III) and tetrachloroindate(III) ions are not completely extracted by toluene, and procedures based on such extractions cannot be recommended.

A critical study of Brilliant green as a spectrophotometric reagent: the determination of perrhenate and gold

The spectrophotometric methods for determining rhenium and gold with Brilliant green have been re-examined in an investigation of the effects of purity of reagent and acidity on the precision and accuracy of results. The perrhenate-Brilliant green ion-association complex is extracted from a solution at pH 6, and is unaffected by reagent purity. The extraction of the tetrachloroaurate(III)-Brilliant green ion-association complex is carried out from 0·5 M hydrochloric acid solution, however, and an impure reagent gives low recoveries. Procedures are recommended for the determination of rhenium and gold, and the purification of the reagent is discussed.

The luminescence properties of some anti-inflammatory and antipyretic drugs

Twenty anti-inflammatory and antipyretic drugs have been examined for their fluorescence and phosphorescence characteristics, and conditions established for detection of fourteen of them at trace levels.

Spectrophotometric determination of molybdenum in steel with thiocyanate and tetraphenyl-arsonium chloride

An alternative procedure is described for the colorimetric determination of molybdenum in steel. Molybdenum(VI) is reduced to molybdenum(V) with ascorbic acid and titanium(III) before being caused to react with thiocyanate and extracting it with tetraphenylarsonium chloride into chloroform that contains quinol. The procedure is sensitive (Iµmax.= 17 400 l mol–1 cm–1 at 470 nm) and precise. A forty-fold excess of tungsten over molybdenum can be tolerated. Results for a series of low-alloy and tungsten tool steels are reported.