Determination of methyldibromoglutaronitrile in cosmetic products by high-performance liquid chromatography with electrochemical detection. Method validation

An increased frequency of contact allergy to methyldibromoglutaronitrile (MDBGN), a commonly used preservative in cosmetics and other consumer products, has been reported in recent years. A high-performance liquid chromatography (HPLC) method for the determination of MDBGN in cosmetic products has been validated in the present study. The identification is performed by reductive electrochemical detection of the bromine present in the molecule. The method is suitable for compliance testing of cosmetic products as well as for the research to support clinical and epidemiological studies.     

Phase shifting interferometry using a robust parameter estimation method

The paper proposes a maximum-likelihood (ML) method based on spectral estimation theory for the estimation of phase distribution in interferometry in the presence of nonsinusoidal waveforms, noise, and the miscalibration of the piezoelectric device. The proposed method also allows the use of arbitrary phase steps. ML estimators are asymptotically efficient for large number of data samples. The method is complemented well by the incorporation of global search algorithm known as Probabilistic Global Search Lausanne for minimizing the ML function. The performance of the proposed method is studied in the presence of noise.     

Kinetics and mechanism of solid-state reaction between bismuth(III) oxide and molybdenum(VI) oxide

The mechanism of the following solid-state reactions between bismuth(III) oxide and molybdenum(VI) oxide was investigated within the temperature range 400–650°C.

$\text{(i)}\text{Bi}{}_2\text{O}{}_3\text{+ MoO}{}_3\text{→ Bi}{}_2\text{MoO}{}_6\text{, (ii)}\text{Bi}{}_2\text{O}{}_3\text{+ 2MoO}{}_3\text{→ Bi}{}_2\text{MO}{}_2\text{O}{}_9\text{, (iii)}\text{Bi}{}_2\text{O}{}_3\text{+ 3MoO}{}_3\text{→ Bi}{}_2\text{(MOO}{}_4\text{)}{}_3\text{, (iv)}\text{Bi}{}_2\text{MoO}{}_6\text{+ MoO}{}_3\text{→ Bi}{}_2\text{MO}{}_2\text{O}{}_9\text{, (v)}\text{Bi}{}_2\text{Mo}{}_2\text{O}{}_9\text{+ MoO}{}_3\text{→ Bi}{}_2\text{(MoO}{}_{\mathrm{2)3}}\text{.}$

Two types of experiments, capillary and particle size, were performed to ascertain whether MoO₃ diffuses into Bi₂O₃ or vice versa. These show that molybdenum trioxide diffuses into bismuth oxide grains. If α is the fraction of molybdenum trioxide reacted, the kinetics in all five cases are found to be governed by the equation αⁿ = kt throughout the temperature range, where n and k are constants at a given temperature and t is the time. Both n and k are temperature dependent. The characteristic feature of these reactions is that they proceed to completion. Results are also fitted by the relation $\text{α = k}{}_2\text{t}{}^{\mathrm{<mtext>1</mtext><mtext>2</mtext>}}\text{? k}{}_3\text{t}$, where k₂ and k₃ are constants, which shows that the reactions occur by bulk diffusion through grain boundary contacts. The number of grain boundary contact points decreases with time in the course of reaction.     

Vibrational spectra, normal coordinate analysis and thermodynamics of 2, 5-difluorobenzonitrile

The FTIR spectrum of 2, 5-difluorobenzonitrile has been recorded in the region 200–4000 cm⁻¹ (in liquid phase). The laser Raman spectrum in the range of 0–3500 cm⁻¹ (in liquid phase) has also been recorded. The spectra have been analyzed assuming C _s point group symmetry for the molecule. A zero-order normal coordinate analysis has been made for the molecule using force constants derived earlier. On the basis of potential energy distributions and eigen vectors unambiguous vibrational assignments have been made for all the fundamentals of the molecule. Thermodynamic functions have also been computed in the temperature range 200–1000 K by utilizing the observed fundamental frequencies assuming rigid-rotor harmonic oscillator approximation.     

Paal knorr reaction for novel pyrrolo[2,3‐d]pyrimidines

An expeditious and convenient solid supported synthesis of 1,3,7‐triaryl‐6‐phenyl‐2‐thioxo‐1,2,3,7‐tetrahydropyrrolo [2,3‐d]pyrimidin‐4‐one derivatives from readily accessible N,N‐disubstituted thiobarbituric acids under microwaves utilising Paal Knorr reaction is described.     

Synthesis and biological evaluation of aromatic analogues of conduritol F, L-chiro-inositol, and dihydroconduritol F structurally related to the amaryllidaceae anticancer constituents

Pancratistatin is a potent anticancer natural product, whose clinical evaluation is hampered by the limited natural abundance and the stereochemically complex structure undermining practical chemical preparation. Fifteen aromatic analogues of conduritol F, l-chiro-inositol, and dihydroconduritol F that possess four of the six pancratistatin stereocenters have been synthesized and evaluated for anticancer activity. These compounds serve as truncated pancratistatin analogues lacking the lactam ring B, but retaining the crucial C10a-C10b bond with the correct stereochemistry. The lack of activity of these compounds provides further insight into pancratistatin's minimum structural requirements for cytotoxicity, particularly the criticality of the intact phenanthridone skeleton. Significantly, these series provide rare examples of simple aromatic conduritol and inositol analogues and, therefore, this study expands the chemistry and biology of these important classes of compounds.     

Chirp estimation in phase-shifting interferometry

We propose a new approach for estimating the phase in the presence of a nonlinear response of a phase-shifting device: a piezoelectric transducer (PZT). The method is complemented well by the high resolution and the maximum likelihood estimation techniques in the estimation of the phase step and the nonlinear coefficient. The advantage of the proposed method is that it can be extended to the extraction of multiple phases in configurations involving multiple PZTs in the presence of nonlinearity. Symmetricity in the phase steps is not required in this method. Hence hysteresis of the PZT does not have any influence on the accuracy of the phase estimation. The effectiveness of the method is shown by experimental results.     

Peak effect studies in single crystals CeRu2 and 2H-NbS2

We have studied the peak effect (PE) phenomenon in single crystals of weakly pinned superconductors CeRu₂ and 2H-NbS₂. 2H-NbS₂ is iso-structural and iso-electronic to 2H-NbSe₂, whose similarity with CeRu₂ as regards the PE representing the order-to-disorder transformation of the flux line lattice was claimed some time ago. We report on the step change in equilibrium magnetization across the peak effect in CeRu₂. We also present the vortex phase diagram of 2H-NbS₂ obtained from the magnetization data, and compare the PE phenomenon in 2H-NbS₂ and 2H-NbSe₂.