PAN-6S作络合指示剂连续滴定测定汞和铅的研究

试验研究了pH3.0和pH5.4的介质中,以1 (2 吡啶偶氮) 2 萘酚 6 磺酸(PAN 6S)作为指示剂,以EDTA为滴定剂连续滴定汞和铅,其终点颜色变化敏锐,准确度高。     

Spectrophotometric determination of gallium with 1-(2,4-dihydroxyphenylazo)-2-naphthol-4-sulfonic acid

A new spectrophotometric method for the determination of gallium is described using 1-(2,4-dihydroxyphenylazo) -2-naphthol-4-sulfonic acid (DHPAN) as a reagent. The color reaction has a sensitivity of 0.013 μg Ga per cm² for log 1₀/1=0.005 at 500 mμ and obeys Beer's law up to 2.8 p.p.m. The effects of pH, time, order of addition of the reagents, temperature and diverse ions were investigated. Gallium is separated from interfering ions by solvent extraction.     

Titration of L-cysteine hydrochloride with standard nickel sulphate solution employing 1-(pyridyl-2′-azo)-naphthol-(2) as indicator

The estimation of cysteine hydrochloride can be carried out quantitatively against standard nickel sulphate solution using 1-(pyridyl-2′-azo)-naphthol-(2) in carbonate-bicarbonate buffer medium of pH 10.0. Other natural amino acids have no interference with the titration.     

新显色剂1-(2-咪唑偶氮)-2-萘酚-4-磺酸作为络合滴定指示剂的研究

本文报道了新显色剂1-(2-咪唑偶氮)-2-萘酚-4-磺酸(IANS)的物理性质、酸离解常数,并对该试剂作为EDTA络合滴定Cu~(2+)、Zn~(2+)、Pb~(2+)、Cd~(2+)、和Hg~(2+)的指示剂进行了研究,结果与二甲酚橙比较令人满意。     

Reactions of nickel ions with nitroso-naphthols—IV formation kinetics of nickel (1-nitroso-2-naphthol-6-sulphonate)

The formation kinetics of Ni(1-nitroso-2-naphthol-6-sulphonate) are reported in the temperature range 20-30°C at an ionic strength of 0.1 M. Both the acidic (HL^?) and basic (L^2? forms of the ligand react with nickel ions, the latter at a much higher rate. The rate constants are similar in magnitude to those observed with 1-nitroso-2-naphthol-3, 6-disulphonate and variation of rate constant with respect to temperature is reproduced by the equation.     

Diphenylcarbazone as an internal indicator in mercurimetric analysis: The determination of cerium by potassium thiocyanate

Summary The quantitative oxidation of thiocyanate by ceric sulphate has been studied and the method utilised for the determination of small quantities of cerium by back titrating the excess (unreacted) KSCN against standard mercuric nitrate with diphenylcarbazone as the internal indicator. Accurate results are obtained under the specified experimental conditions and the procedure is more simple and direct than that adopted during earlier studies of the above redox reaction.Grateful thanks of the author are due to Professor S. S. Joshi for facilities during the work and to the National Institute of Sciences of India for award of a Research Fellowship.     

Separation and determination of metals as complexes of 1-nitroso-2-naphthol-6-sulphonic and 2-nitroso-1-naphthol-6-sulphonic acids

A sensitive ion-pair liquid-liquid extraction-spectrophotometric method has been developed for the determination of copper, palladium, iron and cobalt, based on the formation of metal complexes with 1-nitroso-2-naphthol-6-sulphonic acid or 2-nitroso-1-naphthol-6-sulphonic acid as primary ligand, and zephiramine as counter-ion. The coloured metal complexes obtained over different pH ranges are easily and quantitatively extracted into dichloromethane. The method has been tested with samples containing known amounts of copper, palladium, iron and cobalt in ultrapure water. The reagents provide a sensitive spectrophotometric method for determining these metals.     

The colorimetric determination of thorium using 1-(o-arsonophenylazo)-2-naphthol-3:6-disulphonic acid

A method is described for tin; determination of thorium in milligram quantities using 1-(o arsunophenylazo)-2-naplithol-3:6-disulphonic acid (APANS) with a precision of 0.5%. An account. of the interferences to be expected from some common ions is given and the method is employed in the determination of thorium in monazite following an oxalate seperation.     

4-(3,5-dichloro-2-pyridylazo)-1,3-diaminobenzene as a metallochromic indicator for the complexometric determination of Cu(II) with EDTA

In slightly acid solutions Cu(II) and 4-(3,5-dichloro-2-pyridylazo)-1,3-diaminobenzene (3,5-C12PADAB) form a red-purple complex( = 5.0 x 10(4)1.mole(-). cm(-1) at 547 nm). The complex is readily broken by EDTA, with a sharp change of colour to the yellow of the free reagent (Deltalambda(max) = 110 nm at pH 3.5). This colour contrast and the reversibility of the formation reaction, together with the solubility of the complex in water, make the pyridylazo reagent useful as a metallochromic indicator for copper titration, at pH 2.7-5.5. The Cu(II)-3,5-C12PADAB indicator system has been satisfactorily applied to the determination of sulphur in cast iron, "useful oxides" (Al(2)O(3) + Fe(2)O(3)) in samples of commercial aluminium sulphate, and total phosphorus in a synthetic mixed fertilizer.     

Cylindrospermopsin determination using 2-[4-(2-hydroxyethyl)-1-piperazinyl]ethanesulfonic acid (HEPES) as the internal standard

Cylindrospermopsin (CYN) was determined by liquid chromatography/electrospray ionization-mass spectrometry (LC/ESI-MS) using 2-[4-(2-hydroxyethyl)-1-piperazinyl]ethanesulfonic acid (HEPES) as the internal standard. In the selected ion monitoring of LC/ESI-MS, m/z 414 for CYN and 237 for HEPES were monitored using the negative mode; the retention times of CYN and HEPES were 12.41 and 14.21 min, respectively. CYN was determined from peak area ratios of m/z 414/237. By the treatment of an anion exchange cartridge using a buffer at pH 10.5, CYN was isolated and condensed. No interfering peak was observed. Linearity of this method was observed at the range of 0.10-31.12 ng. Total coefficients of variation were 5.1 and 2.9% at 104 and 1038 μg CYN L⁻¹. The quantitative limit at a signal-to-noise (S/N) ratio of 10 was 0.16 ng.CYN concentration in natural waters is low. CYN in waters should be condensed for determination. This method including the treatment for isolation and condensation of CYN is useful for determination of CYN in environmental and/or drinking waters.     

Evaluation of 1-(2-thiazolylazo)-2-hydroxy-3-naphthoic acid as a metallochromic indicator

The acid dissociation constants of 1-(2-thiazolylazo)-2-hydroxy-3-naphthoic acid (TAHN) and the formation constants of Cu(II), Ni(II) and Zn(II) chelates of this dye have been determined spectrophotometrically at 25 degrees in a 5% v/v mixture of dioxan and water. The formation constants of the 1:2 chelates are smaller than those of other o-hydroxythiazolylazo compound chelates. TAHN is a satisfactory indicator for the titrations of Cu(II) and Ni(II) with EDTA.     

2-[2-(5-Chloropyridyl)azo]-5-dimethylaminophenol as indicator for the complexometric determination of zinc

2-[2-(5-Chloropyridyl)azo]-5-dimethylaminophenol (C1DMPAP) is proposed as a metallochromic indicator for zinc. The end-point colour change is from the violet-red of the zinc complex to the brownish-yellow of the indicator. The colour contrast is markedly greater than that for Erio-T.