Spectrophotometry Determination of Copper and Palladium Using Some 1,3,5-Triphenylformazans

A new rapid and accurate method for the spectrophotometric microdetermination of Cu(II) and Pd(II) using some 1,3,5-triphenylformazans (I) is given. The optimum conditions for the formation of the complexes are extensively investigated. The ligands form 1:1 and 1:2 (M:L) complexes with Cu and Pd ions, Beer's law is obeyed up to 3.8 and 6.5 ppm Cu and Pd respectively. The influence of foreign ions is investigated. The ligands were used successfully as indicators in spectrophotometric titration of Cu and Pd ions with EDTA and CDTA.     

Über die Phosphidierung des Nickels durch Phosphortrichlorid

On the Phosphidation of Nickel by Phosphorus Trichloride The phosphidation of nickel sheets by phosphorus trichloride vapor of 30 and 50 Torr has been studied kinetically by gravimetric means in the temperature range of 400–650°C in hydrogen atmosphere. The phosphidation proceeded generally according to the parabolic rate law. The parabolic rate constant increased with an increase of temperature, and its temperature dependence yielded the activation energies of about 33 and 47 kcal/mole for 400–550 and 550–650°C, respectively. X-ray and electron microprobe analyses showed that surfaces of the specimens phosphidized are made up of mixtures of Ni₂P and Ni₆P₅, and that at the phosphide/metal interface the compound Ni₂P is formed. The experiments using argon as carrier gas resulted in the formation of both the phosphides and the chlorides, and this fact could be explained in terms of thermodynamics.     

Formation of pyrazine derivatives from D-glucosamine and their deoxyribonucleic acid (DNA) strand breakage activity

Two pyrazine derivatives [fructosazine (3) and deoxyfructosazine (6)] were simultaneously formed in a solution of D-glucosamine hydrochloride under various conditions. They showed deoxyribonucleic acid (DNA) strand breakage activity in plasmid pBR322 comparable to that of D-glucosamine. The DNA strand breakage by fructosazine (3) was stimulated by Cu2+.     

Prospective study to assess the clinical efficacy of bone scintigraphy--some analyses of clinical data

The value of preoperative bone scans in patients with primary breast and prostate cancer was evaluated prospectively. Of 414 patients with breast cancer, clinical stage I is 14, II is 219, IIIA is 59, IIIB is 39 and IV is 14. Of 88 patients with prostate cancer, clinical stage I is 14, II is 15, III is 18 and IV is 41. 11 percent of patients with breast cancer and 54 percent of patients with prostate cancer had bone metastases. Clavicle, ribs, thoracic spine, lumbar spine and pelvis metastasized most frequently. The incidences of bone metastases were 18.4% with Scirrhous carcinoma, 15.4% with Medullary tubular carcinoma and 3.8% with Papillotubular carcinoma. The methodology and results of ROC analysis were described in our other papers. Some results of data analysis were described in this paper.     

Determination of phenol and catechol concentrations with oxygen probes coated with immobilized enzymes or immobilized cells

The enzyme phenol 2-hydroxylase was immobilized on Sepharose and used in conjunction with an O₂ electrode for quantitating phenol. Similarly, catechol 1,2-oxygenase was used for quantitating catechol. A third probe was prepared by immobilization ofTrichosporon cutaneum cells rather than purified phenol 2-hydroxylase for phenol quantitation. The whole cell system gave results comparable to the immobilized enzyme system.     

A Study of the Silylation of 1,8-Dihydroxynaphthalene

Twelve compounds each having a six membered Si-contained heterocycle, have been successfully synthesized. Of these eleven compounds have never been reported in the literature. The structures were confirmed by Spectral analysis and elementary analysis. The stability and properties of these compounds is also discussed.     

Direct determination of gentamicin components by capillary electrophoresis with potential gradient detection

A simple and fast method was developed to determine non-UV active compounds directly without derivatization. The usefulness of the method was demonstrated by detecting the major components in aminoglycoside antibiotic mixtures using capillary zone electrophoresis with potential gradient detection. Under optimized separation conditions (0.2 mM cetyltrimethylammonium bromide (CTAB), 1 mM ammonium citrate, pH 3.5), gentamicin was separated into three major peaks (C1, C1a, and C2+C2a) within 15 min. This method showed better sensitivity than other capillary electrophoresis (CE) methods for determining underivatized gentamicin. The linear range was from 10 to 500 ppm. Because of its good repeatability and simplicity, this new method could be a good alternative for the current assays given by US Pharmacopoeia and European Pharmacopoeia.     

Gas-chromatographic determination of ultramicro amounts of selenium in pure sulphuric acid

Ultramicro amounts of selenium in pure sulphuric acid are converted into selenous acid with a bromine-bromide redox buffer solution. The selenous acid reacts quantitatively with 4-nitro-o-phenyl-enediamine to form 5-nitropiaselenol which can be extracted into toluene. The extract is very sensitive to electron-capture detection in gas chromatography, and the sensitivity is higher than that of 5-chloro-or 4, 5-dichloro-piaselenol. The calibration curve (peak heights) is linear up to 0.15 mug of selenium in 1 ml of toluene. Pure sulphuric acid, commercially available, contains 10(-6)$ 10(-5) % selenium.     

Studies on antimony oxides: Part I

Thermogravimetry (TG), differential thermal analysis (DTA) and X-ray diffraction studies of antimony(III) oxide, (Sb₂O₃), in air, nitrogen and argon atmospheres have been made. In air Sb₂O₃ becomes oxidized to Sb₂O₄ above 510°. The oxidation reaction proceeds in two stages as revealed by the TG and DTA curves. The behaviour of Sb₂O₃ is similar in both N₂ and Ar. Sb₂O₃ remains unaffected up to 430°, above which there is a slow, and continuous mass loss up to 550°. Above 550° Sb₂O₃ volatilizes resulting in an enormous weight loss. X-ray studies of the sublimate and the residue indicate the former to be the cubic form of Sb₂O₃ (Senarmontite) while the residue is the orthorhombic (Valentinite) structure. From the DTA curves in air, N₂ and Ar, the transition temperature for the cubic to the orthorhombic modification has been estimated to be around 610°.     

Luminarin 9: A new fluorescent reagent for the precolumn derivatizatioin of main volatile and non-volatile N-nitrosamines in RP-HPLC

Summary A sensitive precolumn fluorescence derivatization method for low level detection of the, volatile (N-nitrosodimethylamine and N-nitrosopyrrolidine) and non-volatile N-nitrosamines (N-nitrosoproline and N-nitrosodiethanolamine) an high-performance liquid chromatography was developed. This method is based on the denitrosation of the compounds of interest by a mixture of hydrobromic acid and acetic acid to produce the corresponding secondary amines. These are, then, able to react with, a quinolizinocoumarin derivative (luminarin 9^®) to form highly fluorescent labelled N-nitrosamine derivatives. The structural elucidation of the luminarin 9^® derivatives of N-nitrosoproline and N-nitrosodimethylamine by way of example, were established by liquid chromatography-mass spectrometry (LC-MS) and by direct chemical ionization-mass spectrometry (CI-MS). The separation, derivatization and detection conditioins were optimized for all the studied compounds. The detection limits (signal to noise ratio=3) were between 0.4 and 1.0 pmol injected depending on the compound. The calibration graphs were linear for derivatized amounts in the range of 0.5–40 nmol for N-nitrosodimethylamine and N-nitrosopyrrolidine, 0.4–2- nmol for N-nitrosoproline and 1.0–40 nmol for N-nitrosodiethanolamine. The repeatability (RSD less than 3.5%, n=6) and reproducibility (RSD less than 4.8%, n-6) were satisfactory.