Determination of nitrite in sea-water by ion-exchanger colorimetry

Summary A microdetermination method (at theg/l level for nitrite) has been developed, based on ion-exchanger colorimetry. The nitrite is reacted with sulphanilamide andN-(1-naphthyl)ethylenediamine to form an azo dye which is then sorbed on Dowex 50W-X2. The resin phase absorbance at 550 and 800 nm is measured directly. The relative detection limit is 0.27g/l and the distribution ratio is 2.6×10⁴. The method has been applied to determination of nitrite in 500-ml sea-water samples and compared with a conventional technique.

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Bestimmung von Nitrit in Meerwasser durch Ionenaustausch-Kolorimetrie

Zusammenfassung Eine Mikromethode zur Bestimmung von Mikrogramm Nitrit/Liter mit Hilfe der lonenaustausch-Kolorimetrie wurde ausgearbeitet. Zu diesem Zweck wird Nitrit mit Sulfanilamid und N-(1-Naphthyl)ethylendiamin zu einem Azofarbstoff umgesetzt, der an Dowex 50W-X2 adsorbiert wird. Die Absorbanz der Harzphase wird unmittelbar bei 550 und 800 nm gemessen. Die relative Nachweisgrenze beträgt 0,27g/l, das Verteilungsverhältnis 2,6×10⁴. Das Verfahren wurde zur Bestimmung von Nitrit in 500-ml-Proben Meerwasser verwendet und mit konventionellen Methoden verglichen.

     

Spectrophotometric extractive determination of iodide as tris(2-(phenyliminomethyl)pyridine) Fe(II) iodide

The iodide:tris(2-(phenyliminomethyl)pyridine) Fe(II) extraction system into nitrobenzene has been studied. The same method is proposed for the determination of iodide. The interference of foreign ions is also determined.     

Studies on the thermal decomposition of salicylhydroxamic acid and its metal complexes with Ni(II), Co(II), Fe(II), Mn(II) and Zn(II)

The thermal decomposition of salicylhydroxamic acid and its metal complexes with Ni(II), Co(II), Fe(II), Mn(II) and Zn(II) has been studied by TG, DTG, DTA and IR spectroscopy. All the compounds investigated decompose to yield intermediate N-hydroxylactams.Decomposition schemes have been proposed and reaction enthalpies and kinetic parameters have been calculated.     

Use of Optically Transparent Membranes for Preconcentration and Direct Phosphorimetric Determination of Pharmaceutical Flumequine

A preconcentration membrane for the retention and phosphorimetric determination of flumequine is proposed. The membrane has a circular zone adhering to the surface of a polyester strip, which constitutes the preconcentration area where the analyte is retained by absorption from a solution that contains it. The phosphorescence intensity emitted by the flumequine can be measured directly in the solid phase, at λ_exc = 358 nm and λ_em = 459 nm. The variables that influence the construction of the membrane have been studied, along with the experimental variables related to the fixation process of the analyte in the membrane. The calibration graph was linear over the range 0.1–2.0 mg/L with a detection limit of 0.03 mg/L and a precision of 0.5%. The method was applied to samples of human urine and cow's milk, with recovery percentages ranging between 100.0 and 102.8%.     

Spectrophotometric determination of vanadium in petroleum crudes and derivatives

The spectrophotometric study of the complexation reaction between 5,5′methylenedisalicylhydroxamic acid and V(V) shows that two complexes are formed, the 1:1 (? = 5100 liters mol^?1 cm^?1 at 490 nm, log K_est = 5.8 ± 0.1) and the 1:2 (L:V) (? = 6250 liters mol^?1 cm^?1 at 600 nm, log K_est = 6.1 ± 0.1). A spectrophotometric method is developed for the determination of vanadium (2–9 ppm) at 2 N HCl and 495 nm, which allows its determination in petroleum crude oils with a series of advantages over the ASTM D-1548-63 method.     

Determination of submicrogram amounts of gallium by ion-exchanger fluorimetry Determination of gallium in natural waters

A method for microdetermination of gallium at ng/ml level has been developed, based on ion-exchanger fluorimetry. The gallium reacts with salicylidene-o-aminophenol to give a highly fluorescent complex, which is fixed on a dextran-type cationic resin. The fluorescence of the resin, packed in a 1-mm silica cell, is measured directly with a solid-surface attachment. The range of concentration of the method is 2.0-10.0 ng/ml, the RSD 1.3% and the detection limit 0.3 ng/ml. The method has been applied to the determination of gallium in natural waters. The gallium content found in tap water was higher than that in raw water. This is related to the use of commercial aluminium salts in the water-treatment plant.     

Study of the GC–MS determination of the palmitic–stearic acid ratio for the characterisation of drying oil in painting: La Encarnación by Alonso Cano as a case study

The correct identification of drying oils plays an essential role in providing an understanding of the conservation and deterioration of artistic materials in works of art. To this end, this work proposes the use of peak area ratios from fatty acids after ensuring that the linear responses of the detector are tested. A GC-MS method, previously reported in the literature, was revisited to its developed and validated in order to identify and quantify of eight fatty acids that are widely used as markers for drying oils in paintings, namely myristic acid (C_14:0), palmitic acid (C_16:0), stearic acid (C_18:0), oleic acid (C_18:1), linoleic acid (C_18:2), suberic acid (2C₈), azelaic acid, (2C₉) and sebacic acid (2C₁₀). The quaternary ammonium reagent m-(trifluoromethyl)phenyltrimethylammonium hydroxide (TMTFAH) was used for derivatization prior to GC-MS analysis of the oils. MS spectra were obtained for each methyl ester derivative of the fatty acids and the characteristic fragments were identified. The method was validated in terms of calibration functions, detection and quantification limits and reproducibility using the signal recorded in SIR mode, since two of the methyl derivatives were not totally separated in the chromatographic run. The proposed method was successfully applied to identify and characterise the most widely used drying oils (linseed oil, poppy seed oil and walnut oil) in the painting La Encarnación. This 17th century easel painting is located in the main chapel of the cathedral in Granada (Spain) and was painted by the well-known artist of the Spanish Golden Age, Alonso Cano (1601-1667).