Ion chromatographic determination of cyanate in saline gold processing samples.

An ion chromatographic method was developed for the determination of cyanate (CNO-) in saline gold processing samples. The method is based on the use of a very weak-eluting buffer (5 mM sodium borate) and a Dionex AS4A-SC anion-exchange column. This weak-eluting buffer facilitates the wide chromatographic separation of chloride (Cl-) from CNO-. After CNO- has been eluted, the switch to 1.8 mM Na2CO3-1.7 mM NaHCO3 buffer allows the fast elution of other major inorganic and organic anions. Validation of this method, including identification of interferences, has shown that this method is reliable, accurate, sensitive (detection limit, 0.1 mg/l CNO-) and reproducible.     

Ion chromatographic determination of transition metals in irradiated nuclear reactor surveillance samples

The determination of transition metal ions in radioactive (+/-25 microCi/g) low-alloy steels (nuclear reactor surveillance samples) by ion chromatography (IC) is described. The analysis has been done directly without prior separation of the iron matrix. The eluted metal ions have been detected with a UV-visible spectrophotometric detector after post-column complexation with 4-(2-pyridylazo)resorcinol. The results are in a good agreement with the certified values for the standard reference material used. The method was applied to nuclear reactor surveillance samples for the determination of Cu, Mn, Co and Ni.     

Ion chromatographic determination of transition metals in irradiated nuclear reactor surveillance samples

The determination of transition metal ions in radioactive (±25 Ci/g) low-alloy steels (nuclear reactor surveillance samples) by ion chromatography (IC) is described. The analysis has been done directly without prior separation of the iron matrix. The eluted metal ions have been detected with a UV-visible spectrophotometric detector after post-column complexation with 4-(2-pyridylazo)resorcinol. The results are in a good agreement with the certified values for the standard reference material used. The method was applied to nuclear reactor surveillance samples for the determination of Cu, Mn, Co and Ni.     

Fast chromatographic determination of polycyclic aromatic hydrocarbons in aerosol samples from sugar cane burning

The influence of the pH on the complexation equilibria between (S)- or (R)-alprenolol and the cellulase Cel7A was investigated by isothermal titration calorimetry. The results obtained agree with those of previous, similar studies of the same equilibria in which the protein was immobilized on silica particles, packed in a chromatographic column. The association constant and the complexation enthalpy and entropy of the (S)-enantiomer increase with increasing pH. For (R)-alprenolol, the binding is endothermic at all pH values. Thus, for both enantiomers in the pH range 5.5-6.8, the binding is an entropically driven process.     

Ion chromatographic determination of organic acids in food samples using a permanent coating graphite carbon column

From the viewpoint of a graphite carbon column with excellent durability, it was applied to the ion chromatography (IC) of several organic acids. The carbon column was permanently coated with the cetyltrimethylammonium (CTMA) ion, and the elution behaviors of several organic acids (acetic acid, lactic acid, succinic acid, malic acid, tartaric acid, citric acid) and inorganic anions (Cl⁻, NO₂⁻, NO₃⁻, SO₄²⁻) were examined according to a non-suppressed IC coupled with conductivity detector, when an ion-exchange ability was given to the graphite carbon column. When salicylic acid and sodium salicylate were used as a mobile phase, each organic acid are analyzed approximately 10 min. But the separation of malic acid, chloride and nitrite was difficult. When benzoic acid and 2-amino-2-hydroxymethyl-1,3-puropanediol (tris aminomethane) were used as a mobile phase, tartaric acid and citric acid, etc. with large valency showed tendency to which the width of each peaks extended and retention time increased. However, it was possible to separate excellently for the analytes detected within 10 min. The developed method was then applied to the determination of organic acids in several food samples.     

Ion chromatographic determination of platinum in biotic materials

A method for the determination of platinum is presented. The procedure consists of a high-pressure digestion of the sample followed by an ion Chromatographic separation. Then the platinum chloro complex is detected by UV-absorption.     

Ion chromatographic behaviour and determination of perbromates

Ion chromatographic behaviour of perbromates in aqueous solutions was studied, using ion suppressed conductimetric detection (Dionex DX-100 ion chromatograph with ASRS-I suppressor). Various eluents (sodium hydroxide, carbonate and phenate solutions) were examined using the AS-14  mm anion-exchange column and an optimization study concerning pH and total eluate concentration of mobile phase was carried out. Phenate buffer (20.0 mM, pH 11.0) at 1.18 ml/min flow rate, gave the best results. Calibration curve was linear in the range of 1.5-200 ppm, with a limit of detection of 0.46 ppm and R.S.D. 1.8% (100 ppm standard). Perbromates were separated with good resolution from potentially interfering anions (bromides, bromates, iodides, perchlorates). Selectivity coefficients were determined for perbromates, perchlorates and iodides, from linear plots of retention volume versus the reciprocal of eluent concentration. The new method was used to monitor the perbromate reactions with lactic acid, iodide and citric acid in the absence and presence of Fe(II) acting as an inducer. Furthermore, it was confirmed the inability of various common strong oxidative media to oxidize bromate to perbromate.     

Ion chromatographic determination of selected ions in antarctic ice

Ion chromatography is used to measure the concentrations of chloride, nitrate, sulphate, ammonium and sodium ions at the μg l^?1 level in Antarctic ice and to investigate the occurrence of methanesulphonate, fluoride, formate, acetate and nitrite. Of the latter group of ions, only methanesulphonate was found in measurable concentrations.     

Gas chromatographic determination of dimethylarsinic acid in aqueous samples

Procedures are described for the determination of dimethylarsinic acid in aqueous samples by gas chromatography of iododimethylarsine. Dimethylarsinic acid is converted into iododimethylarsine rapidly and quantitatively by treatment with hypophosphorous acid and potassium iodide, the resulting iododimethylarsine is extracted with toluene and determined with a gas chromatograph equipped with an electron-capture detector. The detection limit is 0.005 ppm as As. Recoveries from urine are over 95%. Other arsenicals do not give any response in the chromatography. The method has been applied to the determination of dimethylarsinic acid in urine and in water extracts of sea-weeds.     

Ion-paired high-performance liquid chromatographic determination of mitoxantrone in physiological fluids

Mitoxantrone is one of the newer anthracenedione derivatives which has already been studied in phase I and II trials, where it has shown significant antitumor activity against a variety of human tumours. To determine the prolonged terminal half-life of mitoxantrone, we developed a sensitive high-performance liquid chromatographic method, providing a detection limit of 1 ng/ml of extracted serum. This system uses a C18 reversed-phase column. The mobile phase consists of a mixture of acetonitrile (30%, v/v) and an ammonium formate buffer (70%, v/v) with a pH of 2.7. Hexane sulphonic acid is added as an ion-pair former. Detection at a wavelength of 658 nm provides a highly selective system, showing no interfering peaks. Ametantrone, another anthracenedione derivative, is used as an internal standard. The extraction procedure for serum also uses hexane sulphonic acid in an ion-paired system. Because of the highly selective detection wavelength, urine samples can be injected without a sample clean-up procedure. This very sensitive method, combined with high selectivity and a fast and inexpensive serum clean-up procedure, has allowed us to document the prolonged terminal plasma half-life of mitoxantrone (levels of 2-5 ng/ml of plasma can still be detected six days after an intravenous infusion of 15 mg/m2 over 30 min). In urine an as yet unidentified metabolite was discovered.     

Ion chromatographic determination of trace level phosphorus in purified quartz

Trace levels of phosphorus in purified quartz are determined by ion chromatography. In situ reagent purification, matrix digestion and oxidation of phosphorus to orthophosphate ion are carried out simultaneously in a vapour phase digestion (VPD) assembly using a mixture of HF, HNO3 and H2O2. A drastic reduction (475 times) in phosphate blank from reagents (HF/H2O2) was achieved in the VPD through in situ purification of the reagent. The residues remaining after volatilisation (solvent/matrix), mostly consisting of insoluble phosphate/fluoride salts of divalent and trivalent cations, were solubilised by ion-exchange dissolution. Phosphate was analysed on the IonPac AS17 column with suppressed conductivity detection. The results of the ion chromatography (IC) method were compared with a spectrophotometric method. Accuracy was evaluated by analysing a certified reference material (silicon, NIST 57a). The method detection limit was 0.05 microg g(-1).     

Liquid chromatographic determination of sugar alcohols in beverages and foods after nitrobenzoylation

Use of p-nitrobenzoyl chloride (PNBC) to form an ultraviolet-absorbing derivative was attempted to determine the sugar alcohols meso-erythritol, xylitol, D-sorbitol, and D-mannitol by liquid chromatography (LC). LC determination of derivatives was performed on an ODS column with acetonitrile-water (65 + 35) as mobile phase. Calibration curves were linear in the concentration range 0.01-100 micrograms/mL. Method sensitivity is 10 to 1000 times higher than that of LC with refractive index detection and gas chromatography with flame ionization detection. Recoveries of sugars added to various foods at 0.1 and 1% ranged from 91 to 102% for meso-erythritol, 75 to 115% for xylitol, 81 to 105% for D-sorbitol, and 81 to 108% for D-mannitol.     

Ion chromatographic determination of N-nitrosoglyphosate in a glyphosate matrix

The use of high-performance ion chromatography (HPIC) for the determination of N-nitrosoglyphosate [N-nitroso-N-(phosphonomethyl)glycine] is reported. NMR, spectrophotometric and electroanalytical measurements showed that two conformers of N-nitrosoglyphosate in slow equilibrium are always present. Separation of these conformers is achieved by using appropriate chromatographic conditions. The conductimetric detection of N-nitrosoglyphosate and glyphosate and application to the determination of traces of N-nitrosoglyphosate in complex matrices are also reported.     

Fluorimetric and high-performance liquid chromatographic determination of D-lactate in biological samples

D-Lactate in biological samples was converted into a strongly fluorescent substance in a one-vial reaction. It was first converted into the pyruvate hydrazone in the presence of D-lactate dehydrogenase, an NADH-reoxidation system using diaphorase, D,L-6,8-thioctamide and hydrazine. This hydrazone was then converted into 2-hydroxy-6,7-dimethoxy-3-methylquinoxaline by 1,2-diamino-4,5-dimethoxybenzene in 1 M hydrochloric acid, and the quinoxaline was extracted and measured fluorimetrically at 432 nm (excitation at 365 nm). The calibration curve for D-lactate was linear up to at least 100 nmol/ml of the assay mixture, with a determination limit of 2 nmol/ml. The quinoxaline was also analysed by high-performance liquid chromatography with fluorimetric detection. The calibration curve for D-lactate was linear from 500 fmol to 75 nmol in the reaction mixture. This method was 4000 times more sensitive than the fluorimetric method, and could determine D-lactate in blood plasma volumes of less than 1 microliter.     

Ion chromatographic determination of phosphorus soluble in different extracting media in fertilizers

A new method based on ion chromatography (IC) was developed for the determination of phosphorus in fertilizers. Fertilizers were extracted with water, mineral acids, and 2% formic acid, 2% citric acid, and neutral ammonium citrate solutions according to European Regulation No. 2003/2003 of the European Parliament and the Council of October 13, 2003, or the Decree of the Italian Agriculture Minister of June 17, 2002; the extracts were analyzed by direct injection, after simple filtration, by IC on an IonPac AS19 (250 x 4 mm id) column, using a KOH (21-50-21 mM) gradient and suppressed conductivity detection. The calibration plot was linear over the range of 5-50 mg/L (r(2) of >0.999). The method was evaluated by comparison with a gravimetric method according to established norms. Associated uncertainty at the 95% confidence level was established as 0.47% for the determination of 3-46% P2O5 by IC. A good chromatographic separation of phosphorus forms such as phosphates and phosphites, and some other important anions like nitrates, chlorides, and sulfates present in many commercial fertilizers was also possible, with a linear response over the range of 5-50 mg/L. After a more complete validation, this IC determination of phosphorus could replace more tedious methods such as those using gravimetric determinations.     

High-performance liquid chromatographic determination of formate as benzimidazole in biological samples

Formate was determined as benzimidazole by high-performance liquid chromatography after reaction with o-phenylenediamine at 130 degrees C for 2 h in 1 M perchloric acid. The useful concentration range was 1.6-40 mumol/l and the determination limit was 20 pmol. The recoveries from rat liver homogenate and human urine were 90.3 +/- 2.9 and 89.4 +/- 2.5%, respectively. Using this method, the activity of formaldehyde dehydrogenase in biological samples could be measured, and also the formate concentration in the liver and urine of rats to which methanol had been administered.