Extractive radiometric procedure for the estimation of fluoride

A radiochemical method for the determination of fluoride has been developed. The effect of fluoride on the extraction of the Fe/III/ thiocyanate complex into TBP in nitrobenzene has been utilized. Microgram quantities of F^– have been determined. Effect of diverse ions has also been reported. The method is applied for the determination of F^– in a natural sample of apetite.     

A new fundamental parameter based calibration procedure for micro X-ray fluorescence spectrometers

Fundamental parameter based quantification of X-ray fluorescence (XRF) measurement data requires an accurate knowledge of the spectrometer parameters, including the spectral distribution of the excitation radiation. In case of micro-XRF where a polycapillary optic is utilized in the excitation channel this distribution is changed due to the transmission properties of the lens. A new calibration procedure, based on fluorescence data of thin standard samples, was developed to determine the excitation spectrum, i.e., the product of the X-ray tube spectrum and the transmission of the used X-ray optic of a micro-XRF setup. The calibration result was validated by the quantitative analyses of certified multi-element reference standards and shows uncertainties in the order of 2% for main components, 10% for minor elements and 25% for trace elements. The influence of secondary order effects like Coster-Kronig transitions and cascade effects is analyzed and the accuracy of fundamental parameters in common databases is discussed.     

A rapid procedure for the determination of the tellurium content of organotellurium compounds

A rapid micro-analytical procedure for the analysis of tellurium in organotellurium compounds is described. The compounds are decomposed using the conventional oxygen flask method followed by treatment with aqueous hydrogen peroxide/hydrochloric acid solution. The tellurium content of the resulting solution is determined by atomic absorption spectrophotometry. If the analyses are carried out batch wise i.e. 6–8 samples with each standardisation of the instrument, the total analysis time is about $\text{1}\text{2}$ hour per sample.     

A micro liquid column chromatography procedure for twelve anticonvulsants and some of their metabolites

Solvent extracts of 50 microliter volumes of serum were sufficient for the determination of twelve anticonvulsant drugs. The liquid chromatography procedure utilized a C-18 reversed-phase column and isocratic elution with 15% acetonitrile in water. No derivatization was required. Eluted anticonvulsants were detected by UV absorption at 195 nm and quantitated by drug--internal standard peak area ratios. The procedure provided linear working curves over the concentration range from 1 to 100 mg/l of drug in the serum. The procedure for serum provided recoveries of the drugs from 92 to 101%. Within-day precision was about 4% and day-to-day precision was about 6.5%. The procedures has been applied to urine samples to facilitate bioavailability studies. Data are also given for several metabolites. There is a discussion of many practical aspects of the procedure to improve the reliability of the results.     

Determination of phosphorus in organic compounds: A new micro procedure

Summary A new micro procedure for the determination of phosphorus in organic compounds has been developed. It is based on the yellow complex produced by mixing ammonium vanadate, molybdate, and phosphate. The procedure is rapid, simple, and suited for series determinations; the reagents and the colored compounds are stable. A precision of ± 0.2% phosphorus is obtained with samples of 3 to 10 mg weight.

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Zusammenfassung Das beschriebene Mikroverfahren für die Phosphorbestimmung in organischen Substanzen beruht auf der photometrischen Auswertung des gelben Komplexes mit Vanadat und Molybdat. Es ist einfach, schnell, und für Serienbestimmungen geeignet. Die dafür nötigen Reagenzien sind gut haltbar, die gefärbte Verbindung ist beständig. Eine Genauigkeit von ± 0.2% Phosphor wird mit Probemengen von 3 bis 10 mg erhalten.

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Résumé On présente un micro-procédé de dosage du phosphore dans des composés organiques. Il repose sur le complexe jaune produit en mélangeant des vanadate, molybdate et phosphate d'ammonium. Le procédé est rapide, simple et convenable pour les dosages en série. Les réactifs et les composés colorés sont stables. Une précision de ± 0,2% sur le phosphore est obtenue avec des échantillons allant de 3 à 10 mg.

     

A new screening procedure for the estimation of oxidizable organic compounds in water samples

Summary Immobilized lead dioxide (supported on SiO₂) has been used as the packing material in a solid phase reactor for the oxidation of organic compounds in water samples by flow injection analysis (FIA). On-line oxidation takes place in a FIA-system; this allows the detection of mobilized Pb²⁺ either photometrically, after complex formation with 4-(2-pyridylazo)-recorcinol (PAR), or directly with flame-AAS. The oxidation yield is quite different (0–100%) for a variety of organic compounds; however, calibration was possible in all cases investigated. Thus the systems can be used for the screening of polluted waters and as a post-column chemical-reaction detector (e.g. after HPLC-separation of organic compounds). After modification the FIA determination of COD equivalent values should be possible.     

A simplified HPTLC screening method for the estimation of the PAH content in soil samples

Based on a highly significant correlation between the visual fluorescing fraction of PAH on the one hand and the total EPA-PAH16 content in mineral soils on the other hand, a deliberately incomplete RP-TLC separation of these compounds into a few fingerprint-like compressed bands within a determined "PAH window" has been achieved. The resulting band-pattern does not interfere normally with the more or less non-polar phenolic compounds which are associated with natural soil humic substances. The extraction step has been extremely simplified with regard to the quantity of the soil sample and of the extractant. The accuracy of this procedure has been ascertained by means of recovery experiments with an artificial soil enriched with PAH. A single spot application mode and an evaluation scheme allow the estimation of EPA-PAH16 contents of soil samples in relation to threshold values (1 or 5 or 10 mg/kg). This HPTLC screening method has been compared against standard HPLC methods. The simplified extraction step and the separation by HPTLC minimizes the actual costs and the time spent per sample.     

A simplified HPTLC screening method for the estimation of the PAH content in soil samples

Based on a highly significant correlation between the visual fluorescing fraction of PAH on the one hand and the total EPA-PAH₁₆ content in mineral soils on the other hand, a deliberately incomplete RP-TLC separation of these compounds into a few fingerprint-like compressed bands within a determined “PAH window” has been achieved. The resulting band-pattern does not interfere normally with the more or less non-polar phenolic compounds which are associated with natural soil humic substances. The extraction step has been extremely simplified with regard to the quantity of the soil sample and of the extractant. The accuracy of this procedure has been ascertained by means of recovery experiments with an artificial soil enriched with PAH. A single spot application mode and an evaluation scheme allow the estimation of EPA-PAH₁₆ contents of soil samples in relation to threshold values ¶(1 or 5 or 10 mg/kg). This HPTLC screening method has been compared against standard HPLC methods. The simplified extraction step and the separation by HPTLC minimizes the actual costs and the time spent per sample.     

A colorimetric method for the estimation of glutamic acid in protein hydrolyzates

On heating with hydroxylamine and on subsequent treatment with ferric chloride, pyrrolidonecarboxylic acid gives a colour reaction. This reaction can be used for the quantitative estimation of glutamic acid in protein hydrolyzates since this acid is almost completely converted into pyrrohdonecarboxylic acid at 125° and pH 3–4.     

A selective procedure for the gravimetric estimation of uranium as oxinate using complexone as masking agent

The existing method. for the estimation of U in hexavalent condition as oxinate has been slightly modified and the scope of complexone (disodium salt of ethylenediaminetetraacetic acid) as a masking agent to develop a selective method for its estimation in presence of interfering elements has been studied. It has been found that at pH ranges from 5-9 complexone exerts no influence on the complete precipitation of uranium and that uranium can be quantitatively separated from Th, R.E., Zr, Fe⁺³, Al, Cu, Co, Ni, Zn, Cd, Pb, Bi, Mn and P₂O₅ by precipitation with oxine in a solution buffered with acetic acid and ammonium acetate (pH approximately 5.3) and also from V₂O₅, MoO₃ and WO₃ in ammoniacal medium (pH approximately 8.4).     

A general procedure for building the transmembrane domains of G‐protein coupled receptors

The only results available at present about the structural features of G‐protein coupled receptors are the low resolution electron projection maps obtained from microscopy studies carried out on two‐dimensional crystals of rhodopsin. These studies support previous suggestions that these integral proteins are constituted by seven transmembrane domains. The low resolution electron density map of rhodopsin can be used to extract information about helix relative positions and tilt. This information, together with a reliable procedure to assess the residues involved in each of the transmembrane regions, can be used to construct a model of rhodopsin at atomic resolution. We have developed an algorithm that can be used to generate such a model in a completely automated fashion. The steps involved are: (i) locate the centers of the helices according to the low resolution electron density map; (ii) compute the tilt of each helix based on the elliptical shape observed by each helix in the map; (iii) define a local coordinate system for each of the helices; (iv) bring them together in an antiparallel orientation; (v) rotate each helix through the helical axis in such a way that its hydrophobic moment points in the same direction as the bisector formed between three consecutive helices in the bundle; (vi) rotate each helix through an axis perpendicular to the helical one to assign a proper tilt; (vii) translate each of the helix to its center deduced from the projection map. A major advantage of the procedure presented is its generality and consequently can be used to obtain a model of any G‐protein coupled receptor with the only assumption that the shape of the bundle is the same as found in rhodopsin. This avoids uncertainties found in other procedures that construct models of G‐protein coupled receptors based on sequence homology using rhodopsin as template. This revised version was published online in July 2006 with corrections to the Cover Date.     

A modified protein precipitation procedure for efficient removal of albumin from serum

Proteomic analysis of sera and the quest for identifying serum proteins as disease markers have often been hampered by the predominance of several highly abundant proteins including albumin and immunoglobulins. Prior albumin depletion so as to enrich for otherwise undetectable serum components is therefore a prerequisite in mining the serum proteome. In the course of evaluating several available methods and commercial kits, we have been able to refine the albumin depletion protocols and establish a modified albumin removal method using trichloroacetic acid (TCA)/acetone. Changes in major protein bands were monitored by one-dimensional sodium dodecyl sulfate-polyacrylamide gel electrophoresis (1-D SDS-PAGE) and used as the first screening strategy to evaluate and optimize for the precipitation experimental conditions. Our method showed better performance in efficiency, specificity, and costs in comparison with two commercially available albumin removal kits, and provides a simple pre-fractionation step for the proteomic analysis of serum biomarkers. Albumin isolated by the modified method is in the native state. Our method may offer a rapid method for purifying serum albumin in large scale.     

A reactive analytical approach for the estimation of olefinic content in gasoline-range hydrocarbons by gas chromatography

The estimation of olefinic content in conversion processes such as the etherification of olefins in fluid catalytic cracking (FCC) gasoline is essentially required. Gas chromatography (GC) is the well-established method for the quantitative analysis of olefins in etherification processes. The current state-of-the-art GC methods employing highly specific long single capillary columns such as Petrocol-DH are being used for the analysis of gasoline-range hydrocarbons. However, the method needs many standard reference samples of respective components in a complex mixture of hydrocarbons, which limits the scope of the analytical method. The alternative approach followed by this investigation is based on the reactive method of the analysis of olefins in FCC light gasoline by subjecting them to hydrogenation and estimating the olefinic content by GC comparing the gas chromatograms of the original feed and hydrogenated product using a Petrocol-DH column. A decrease in the quantity and disappearances of the peaks are assumed as olefins, and their number and total composition is calculated. In this study the bromine number method is used to estimate the olefinic content for a comparison of results with the adopted proposed methodology. The adopted methodology quantitates olefinic content in FCC light gasoline, which is comparable with reported literature values and the bromine number method. With the availability of standard reference samples of some important major reactive olefins, the adopted methodology can also give component-wise analysis as well as total olefinic content in a single step in processes such as etherification. The methodology can be also useful in reactions in which the conversion of total olefinic content is needed such as hydration, esterification, and alkylation of olefins in a complex mixture of hydrocarbons apart from the etherification of olefins in FCC gasoline.     

A micro method for the determination of protein and screening of added water in meat and meat products

Summary The automatic Dumas method is feasible for determining the protein and screening for added water in meats and meat products. It is rapid, convenient, and requires less laboratory space and cost for routine operation. Homogeniety of the meat sample is important. Samples identified as positive for added water should be confirmed and quantified by the official macro-Kjeldahl method.

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Zusammenfassung Die automatisierte Dumas-Methode eignet sich für die Proteinbestimmung in Fleisch und Fleischwaren zwecks Ermittlung von Wasserzusätzen. Das Verfahren ist rasch durchzuführen, beansprucht wenig Platz im Labor und verursacht im Routinebetrieb nur geringe Kosten. Die Fleischproben müssen homogen sein. Gegebenenfalls festgestellter Wasserzusatz soll mit der offiziellen Makro-Kjeldahlmethode verifiziert werden.

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This paper was persented at the Sixth Middle Atlantic Regional Meeting of the American Chemical Society, February 3–5, 1971, Baltimore, Md.     

An automated neutron activation procedure for screening PCB content of oil

An analytical procedure for rapidly screening large numbers of oils for polychlorinated biphenyl (PCB) content has been developed and is now in routine use. Pontential levels of PCBs are inferred from chlorine concentrations as determined using the automated neutron activation analysis (NAA) facility at the Los Alamos National Laboratory Omega West Reactor. The technique is designed to screen up to 200 oil samples per eight hour working day, using a sample volume of approximately 1 milliliter. Because of the automated nature of the analysis, elements in addition to chlorine are determined, when present. These include fluorine, bromine, iodine and sulfur. U.S. National Bureau of Standards (NBS) and U. S. Environmental Protection Agency (EPA) Standard Reference Materials are routinely analyzed for quality assurance purposes. The results of our analyses of these materials for certified elements is discussed as well as results for other non-certified elements observed in the standard materials.