Studies with an inorganic ion-exchange membrane exhibiting selectivity for Pb(II) ions

A solid membrane electrode made with titanium arsenate as membrane material and "Araldite" as binder has been used to measure the activity of lead in the concentration range from 0.1 M to 5 x 10(-6)M. The electrode is unaffected by many cations, nitrate and acetate. The response time is 40-60 sec over the whole concentration range (in a static system) and the electrode has a working life of at least four months. The electrode can work in the pH range 2-5 and is tolerant of ethanol up to a content of 30% v v . It has been successfully used for end-point indication in potentiometric titration of lead. A membrane treated with cationic surfactant exhibits better selectivity.     

Iron(III) complexes of 2-acetylpyridine-4-phenyl-3-thiosemicarbazones: Magnetic,E.s.r. and spectral studies

Summary Iron(III) complexes of 2-acetylpyridine-4-phenyl-3-thiosemicarbazone (LH) with the general formulae FeLX₂ (X = Cl, Br, NO₃ or SCN) and FeLSO₄ have been prepared and characterised by elemental analysis and by magnetic measurements in the polycrystalline state in the 77–298 K range and by electronic, i.r. and e.s.r. spectra. The FeLX₂ species (X = Cl, NCS or NO₃) are square pyramidal of intermediate spin-state (S=3/2) with an⁴ A ₂ ground state. The magnetic behaviour of FeLSO₄ is commensurate with high order effects coupled with antiferromagnetic exchange interactions. FeLBr₂ is a spin-free dimer involving bromine bridging between two FeLBr₂ square pyramids. However, the low-spin species [FeL(DMF)₃]²⁺ exists in dimethylformamide solution.     

Polarographic reduction of some guanylpyrazoline nitrates and the effect of double layer structure on E1/2 values

Polarographic reduction of 4-arylhydrazono-1-guanylnitrate-3-methyl-2-pyrazoline-5-ones takes place in a single 4-electron transfer, giving a diffusion controlled irreversible wave in B.R. buffers of pH range 2.0–10.0. The reduction in these compounds takes place at the ?NH?N=C-bond. Effect of various cations, anions and solvent percentage on the reduction has been discussed. The effect of substituents and its correlation with the Hammett substituent constant (δ) have also been studied.     

High energy muon-nucleon inelastic scattering at lowq 2

The inelastic interactions of 150 GeV positive muons produced at Fermi Laboratory have been studied in nuclear emulsion. Secondary particles produced in these interactions have been identified, the energy spectra and angular distributions for pions and protons are given. The inclusive pionproduction reaction is studied and the relative shape ofp _t ² distribution is discussed. The average charged multiplicity relations are determined as a function of different parameters and are compared with the multiplicities produced in pure hadronic interactions. The integral cross sections have been measured and are compared with the first and second powers of 1/(1+q ²/m _p ² ) forσ _exp(q ²,v), the quantity commonly called the “virtualphoton-nucleon total cross section”. The values of the structure function νW ₂ are calculated for 0.02≤q ²≤0.5. The present data are compared with other muon data at the same energy.     

Lattice instability in Hf1-x Ta x V2 compounds

The temperature dependence of the electric quadrupole interaction frequency _l ^o , experienced by the¹⁸¹Ta probe occupying Hf site in the compounds Hf_1-xTa_xV₂ has been measured for x=0.06, 0.10 and 0.20 in the temperature region between 8.5 K to 296 K. The measurements show lattice transformation in all the three compounds below 120 K.     

Development and Validation of a Liquid Chromatographic Method for Determination of Efavirenz in Human Plasma

A simple, rapid, and sensitive high-performance liquid chromatographic method for estimation of efavirenz in human plasma has been developed and validated. Chromatography was performed with C₁₈ analytical column and 50:50 acetonitrile–phosphate buffer (pH 3.5) as mobile phase. Compounds were monitored by UV detection at 247 nm. The retention time for efavirenz was 6.45 min and that for the internal standard, nelfinavir, was 2.042 min. Response was a linear over the concentration range of 0.1 μg–10 μg mL⁻¹ in human plasma. The method was simple, specific, precise and accurate and was useful for bioequivalence and pharmacokinetic studies of efavirenz.     

Ammonia chemical ionization tandem mass spectrometry in structural determination of alkaloids. II. Tetraponerines from pseudomyrmecine ants

Chemical ionization tandem mass spectrometry (CI-MS/MS) of alkaloids with ammonia reagent gas and collision-activated dissociation as well as EI-MS/MS were applied to the tetraponerine alkaloids in extracts from six pseudomyrmecine ants of the genus Tetraponera. The MS/MS techniques along with gas chromatography Fourier transform infrared (GC/FTIR) spectra allowed identification in two extracts of seven of the eight known tetraponerines. The EI-MS/MS fragmentations proved diagnostic for the ring system and the CI-MS/MS patterns for the C-8 or C-9 substitution, while the Bohlmann bands in FTIR spectra were diagnostic for the C-8 or C-9 configurations. An Indian ant (T. allaborans) had T-2, T-4 and T-8, while a Chinese ant (T. binghami) had T-5, T-6, T-7 and T-8. Four other ants, T. rufonigra (India), T. penzigi (Africa), T. clypeata (Africa) and T. sp. cf. emeryi (Africa), had no tetraponerines.     

The biosynthesis of the alkaloids of croton sparsiflorus morong

Incorporation of tyrosine, dopa, dopamine, 4-hydroxyphenylpyruvic acid, (±)-, norcoclaurine-1-carboxylic acid, -norcoclaurine, -coclaurine, and -N-methylcoclaurine into N-methylcrotsparine, N-methylcrotsparinine and N-methylsparsiflorine in Croton sparsiflorus Morong has been studied. The evidence supports the direct oxidative coupling of (+)-, and (-)-N-methylcoclaurines to give N-methylcrotsparine and N-methylcrotsparinine respectively. Tracer experiment show that N-methylcrotsparine undergoes dienone-phenol rearrangement to give N-methylsparsiflorine. A double labelling experiment with (±)-N[¹⁴C]methyl[1-³H]coclaurine demonstrated that the H atom at the asymmetric centre in the 1-benzylisoquinoline precursor is retained in the bioconversion. The intermediacy of norcoclaurine-1-carboxylic acid and specific incorporation of dehydro-N-methylcoclaurinium salt into the bases have been demonstrated.