Complexometric estimation of copper

Summary Copper(II) or Copper(II) and iron(III) in a mixture are determined by titration with EDTA (disodium salt) solution as complexometric reagent at p_H 4.0 using potassium thiocyanate-p-anisidine as an indicator.Fe^III is estimated in the mixture by titration with EDTA (disodium salt) solution using potassium thiocyanate-ether as an indicator.Cu^II present in the mixture is, therefore, equivalent to the difference in amounts of the EDTA (disodium salt) used for the two sets of titrations of the mixture using potassium thiocyanate-p-anisidine and potassium thiocyanate-ether as indicators respectively.Strontium, magnesium, manganese, calcium, barium and mercuric ions do not interfere in these estimations.

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Zusammenfassung Kupfer(II) oder Kupfer(II) und Eisen(III) zusammen werden komplexometrisch mit ÄDTA-Lösung bei p_H 4,0 unter Verwendung von Kaliumthiocyanat-p-Anisidin als Indicator titriert. Eisen(III) wird in dem Gemisch durch komplexometrische Titration gegen Kaliumthiocyanat-Äther als Indicator bestimmt. Der Kupfer(II)-gehalt ergibt sich aus der Differenz der beiden Titrationen. Strontium, Magnesium, Mangan, Calcium, Barium und Quecksilber(II) stören nicht.

     

Chromatographic study of anionic complexes

Summary In this paper we have reported our results on the attempted separation of copper(II), nickel(II), cobalt(II) and iron(III) in mixtures by filter paper strip chromatography, using aqueous ethanol as solvent. The effect of the presence of varying concentrations of citrate ion as a complexing agent in the mixtures has been studied. The complexing agent has been added in the metal solution, and not in the solvent as usually done by previous workers.     

Photochemical and thermal transformations of carboxylic dithiocarbamic anhydrides and acyl xanthates

The reaction of diphenylchloroacetyl chloride with different dithiocarbamates gave the corresponding dithiocarbamic anhydrides. Under analogous conditions, dithiocarbamyl phenylacetic acids and dithiocarbamyl acetic acids were formed from the reaction of dithiocarbamates with phenylchloroacetyl chloride and chloroacetyl chloride, respectively. O-Ethyl S-acyl xanthates were formed from the reaction of potassium O-ethyl xanthate with diphenylacetyl chloride, diphenylchloroacetyl chloride, cyclopentylphenylacetyl chloride and triphenylacetyl chloride. Photolysis of dithiocarbamic anhydrides gave a mixture of products consisting of 1,2-dichlorotetraphenylethane, carbon monoxide and the corresponding thiocarbamoyl sulfides. Acyl xanthates, on the other hand, gave carbon monoxide and the corresponding substituted ethane derivatives. When dithiocarbamic anhydrides were refluxed in hydroxylic solvents such as methanol, ethanol and n-propanol, the corresponding dithiocarbamyl acetates were formed. Thermal decomposition of acyl xanthates gave carbon disulfide and the corresponding esters.     

Thiotropolone as a chromogenic reagent for the simultaneous determination of cobalt(II) and nickel(II)

Thiotropolone forms chloroform-soluble reddish-brown and violet complexes with cobalt(II) and nickel(II), in the pH range 7.0-8.5 and 6.0-9.0 respectively. Based on this, a sensitive and rapid method for the spectrophotometric determination of traces of cobalt and nickel in metals and alloys has been developed. The two metals can be determined accurately in the range 0.6-2.6 ppm of cobalt and 0.75-4.57 ppm of nickel, simultaneously.     

Beta galactosidase enzyme fragment complementation as a novel technology for high throughput screening

In this review, the applications of beta galactosidase complementation are described. alpha Complementation is a naturally occurring process in bacteria and in engineered cells, and can also occur in eukaryotic cells. Two forms of alpha complementation have been used in high throughput screening (HTS), in which interacting fragments complement with either low or high affinity. Low affinity complementation is used to monitor protein protein interactions, such as those occurring in homodimerization of the epidermal growth factor receptor (EGFR), and provides a robust screen for detection of EGFR inhibitors. High affinity complementation provides the basis for several HTS assays, in which analytes, such as cAMP or IP(3), are detected in crude cell lysates. A development of the latter approach is protein labeling, providing for measurement of cell protein expression and trafficking. Collectively, the use of beta galactosidase complementation provides a novel and flexible technology for highly sensitive, homogeneous HTS assay development.     

Fluctuating boundary layers in combined convection flows along a vertical surface

The effect of buoyancy force on laminar boundary layer in two dimensional flow and heat transfer along a semi-infinite vertical surface, when the velocity of the on-coming stream oscillates in magnitude about a steady mean, is analysed. Two separate solutions valid for low and high frequency ranges are developed. It is found that for low frequency oscillations the phase angles of oscillatory components of skin friction and the rate of heat transfer increase as the Grashof number increases. For very high frequencies, the velocity field is of shear-wave type unaffected by the mean flow; the phase lead in the skin friction is, then, /4 and the rate of heat transfer fluctuation indicates a phase lag of /2 over that of the free stream oscillations.The authors are thankful to referee for many useful suggestions.     

Teaching Operational Research Technique

Good technique, i.e. competence in carrying out operational research, is as vital for the practitioner to acquire as competence in the traditional ‘techniques’. It is suggested that universities should teach students how to conduct simple projects prior to alerting them to more sophisticated methodological issues.As an aid to this task, the traditional five or six parts of an operational research project are broken down and extended into 39 steps, and regrouped into three phases. Also, five skills are identified as being conceptually essential to "good" operational research, which students can develop through tackling suitable case studies.     

Amperometric ascorbimetric determination of cerium(IV) and Iron(III) with two polarized electrodes

Summary Amperometric ascorbimetric determinations of cerium(IV) and ferric iron have been carried out at 50°C with two polarized electrodes at 200 and 100 mV respectively. The results obtained are fairly accurate and precise within ±1.0 per cent. A simple method for successive determination of cerium and iron has been developed; and conditions for such estimations have been established. At an acidity of 2.5 M with respect to sulphuric acid, it is possible to ward off the reduction of ferric iron and thereby cerium(IV) is successfully titrated with ascorbic acid in this medium. After completion of the reaction and then lowering the acid concentration to p_H 1.5 with aid of ammonium hydroxide, Fe^III is titrated with standard ascorbic acid yielding good results.     

Rotational relaxation of neutral red in alkanes: effect of solvent size on probe rotation

Rotational reorientation times of a polar molecule neutral red (NR) have been measured in n-alkanes using steady-state fluorescence depolarization technique. The rotational dynamics of NR in alkanes is described by the Stokes-Einstein-Debye hydrodynamic theory with slip boundary condition. However, we have observed that as the size of the solvent molecule becomes bigger than the size of the solute molecule, the probe molecule experiences reduced friction and the experimentally measured reorientation times are shorter than those predicted by the hydrodynamic theory. These size effects have been analyzed using quasihydrodynamic theories.     

Electrophilic fluorinating reagent mediated synthesis of fluorinated alpha-keto Ethers,benzil, and 6,6'-dialkoxy-2,2'-bipyridines

Interactions of various fluorinated and nonfluorinated alcohols with trans-stilbene in the presence of electrophilic reagents were studied. Under neat conditions, reactions of trans-stilbene (1) with fluorinated alcohols, R(f)OH (R(f) = CF3CH2-, CFH2CH2-, CF3CF2CH2-, CF2H(CF2)3CH2-, (CF3)2CH-, (CF3)3C- (2a-f) in the presence of an electrophilic reagent, 1-(chloromethyl)-4-fluoro-1,4-diazoniabicyclo[2.2.2]octane bis(tetrafluoroborate) (Selectfluor) or N,N-difluoro-2,2'-bipyridinium bis(tetrafluoroborate) (MEC-31), gave alpha-keto ethers (3a-f) and benzil (4) in good to moderate yields. alpha-Keto ether and benzil formation was very much dependent on the reaction time, the degree of fluorination of the alcohols, and whether a solvent such as CH3CN, DMF or DMA was utilized. In solution, alpha-keto ethers and benzil did not form. Interestingly, under neat conditions, nonfluorinated alcohols, ROH (R = CH3-, CH3CH2-, CH3CH2CH2-, CH3CH2CH2CH2-, CH3CH2CH2CH2CH2CH2-) (5g-k) did not react with trans-stilbene in the presence of MEC-31 but gave 6,6'-dialkoxy-2,2'-bipyridines (6g-k), regioselectively, in excellent isolated yields. On the other hand, fluorinated alcohols did not react with MEC-31. Reaction of MEC-31 with an excess of diethylene glycol (7) gave the bipyridine derivative (8) in 88% isolated yield. Reaction of 8 either with diethylaminosulfur trifluoride (DAST) or bis(2-methoxyethyl)aminosulfur trifluoride (Deoxofluor) readily produced the corresponding difluoro derivative (9) in 85% isolated yield. All new compounds have been characterized by spectroscopic and elemental analysis.