On line pre-concentration for simultaneous determination of low molecular weight organic acids and inorganic anions in Amazonian river water samples employing ion chromatography with conductivity detection

An ion chromatography procedure, employing an IonPac AC15 concentrator column was used to investigate on line preconcentration for the simultaneous determination of inorganic anions and organic acids in river water. Twelve organic acids and nine inorganic anions were separated without any interference from other compounds and carry-over problems between samples. The injection loop was replaced by a Dionex AC15 concentrator column. The proposed procedure employed an auto-sampler that injected 1.5 ml of sample into a KOH mobile phase, generated by an Eluent Generator, at 1.5 mL min-1, which carried the sample to the chromatographic columns (one guard column, model AG-15, and one analytical column, model AS15, with 250 x 4mm i.d.). The gradient elution concentrations consisted of a 10.0 mmol l-1 KOH solution from 0 to 6.5 min, gradually increased to 45.0 mmol l-1 KOH at 21 min., and immediatelly returned and maintained at the initial concentrations until 24 min. of total run. The compounds were eluted and transported to an electro-conductivity detection cell that was attached to an electrochemical detector. The advantage of using concentrator column was the capability of performing routine simultaneous determinations for ions from 0.01 to 1.0 mg l-1 organic acids (acetate, propionic acid, formic acid, butyric acid, glycolic acid, pyruvate, tartaric acid, phthalic acid, methanesulfonic acid, valeric acid, maleic acid, oxalic acid, chlorate and citric acid) and 0.01 to 5.0 mg l-1 inorganic anions (fluoride, chloride, nitrite, nitrate, bromide, sulfate and phosphate), without extensive sample pretreatment and with an analysis time of only 24 minutes.

Determination of nitrate in lettuce by ion chromatography after microwave water extraction

Lettuce is worldwide known as the most important vegetable. In this context, most farmers are searching new techniques for best quality products including hydropony. However, nitrate is of great concern, since it has a negative impact on human metabolism. The main objective of the present work was to evaluate the nitrate content of lettuce produced by conventional and hydroponic systems. The determination was conducted by ion chromatography and a new method of extraction was tested using microwave oven digestion. The results indicated that nitrate level produced in the conventional system was lower than in the hydroponic system.

Internal standard versus external standard calibration: an uncertainty case study of a liquid chromatography analysis

Traditionally, in the cigarettes industry, the determination of ammonium ion in the mainstream smoke is performed by ion chromatography. This work studies this determination and compares the results of this technique with the use of external and internal standard calibration. A reference cigarette sample presented measurement uncertainty of 2.0 μg/cigarette and 1.5 μg/cigarette, with external and internal standard, respectively. It is observed that the greatest source of uncertainty is the bias correction factor and that it is even more significant when using external standard, confirming thus the importance of internal standardization for this correction.

Phloem mobility of Boron in two eucalypt clones

Boron deficiency causes large productivity losses in eucalypt stands in extensive areas of the Brazilian Cerrado region, thus understanding B mobility is a key step in selecting genetic materials that will better withstand B limitation. Thus, in this study B mobility was evaluated in two eucalypt clones (68 and 129), under B sufficiency or B deficiency, after foliar application of the 10B isotope tracer to a single mature leaf. Samples of young tissue, mature leaves and roots were collected 0, 1, 5, 12 and 17 days after 10B application. The 10B:11B isotope ratio was determined by HR-ICP-MS. Samples of leaves and xylem sap were collected for the determination of soluble sugars and polyalcohols by ion chromatography. Boron was translocated within eucalypt. Translocation of foliar-applied 10B to the young tissues, mature leaves and roots was higher in clone 129 than in 68. Seventeen days after 10B application to a single mature leaf, between 14 and 18 % of B in the young tissue was originated from foliar B application. In plants with adequate B supply the element was not translocated out of the labeled leaf.

Validação do método de determinação simultânea dos íons brometo e bromato por cromatografia iônica em águas de consumo humano

European Directive (98/83/CE), compulsory after 2008, states that bromate in drinking water must be controlled at levels below 10 mg L-1. Supporting implementation of the Directive, the European Comission has established project SMT4-CT96 2134, in collaboration with various european institutions, aiming at the identification of the interferents to the current analytical method (Ionic Chromatography with Conductimetric Detection - IC/CD), their removal and the automation of pre-treatment and injection steps, as well as the development of alternative methods. EPAL, responsible for the water supply to a great deal of Portuguese regions, has taken steps to meet these requirements. Although not part of such project, this work (the result of a project conducted under a protocol of collaboration between EPAL SA and FCUL - Faculty of Sciences, University of Lisbon), reports on studies of usefulness to laboratories planning to monitor bromate in ozone treated waters, in conditions different from those described in EPA 300.1. Simultaneous determination of bromide is justified by its role as bromate precursor.

Análise química de sais de cobre fabricados entre 1877 e 1995

Samples of copper compounds covering all of the XXth century and the end of the XIXth century were submitted to classical and instrumental quantitative analysis. The amount of impurities greatly decreased with time, reaching a constant level since the 1960's. The gravimetric method was suitable for the determination of copper although other procedures also gave good or reasonable results. However, for metal contaminants, atomic absorption spectrometry was the best choice because of its lower detection limits, being able to determine several elements in the oldest samples. Ion chromatography detected several anions in copper salts manufactured before the 1950's. An increasing quality of raw materials and a better sensitivity of analytical methods led to quality improvement of copper compounds with time.

Composição iônica majoritária de águas de chuva no centro da cidade de São Paulo

The chemical composition of rainwater samples collected from March 2002 to February 2003 in downtown São Paulo city (Universidade Presbiteriana Mackenzie) is presented. Potentiometric and conductimetric measurements were used to evaluate the [H+] and the total ionic content. Major anions and cations were determined by ion chromatography with conductivity detection. The rainwater was acidic with a mean pH of 4.99. The volume weighted means, VWM, of the anions nitrate, acetate and sulfate were, respectively, 21.2, 16.9 and 12.4 µmol L-1. Ammonium was the most abundant ion with a VWM of 37.6 µmol L-1. The contribution of each anion to the free acidity potential decreases in the following order: SO4(2-) (28.8%), CH3COO- (24.7%), NO3- (22.8%), Cl- (13.4%), HCOO- (7.7%) and C2O4(2-) (2.5%). The relative contribution of the weak organic acids to the free acidity was significant, 34.9%.

Analytical procedures for determining Pb and Sr isotopic compositions in water samples by ID-TIMS

Few articles deal with lead and strontium isotopic analysis of water samples. The aim of this study was to define the chemical procedures for Pb and Sr isotopic analyses of groundwater samples from an urban sedimentary aquifer. Thirty lead and fourteen strontium isotopic analyses were performed to test different analytical procedures. Pb and Sr isotopic ratios as well as Sr concentration did not vary using different chemical procedures. However, the Pb concentrations were very dependent on the different procedures. Therefore, the choice of the best analytical procedure was based on the Pb results, which indicated a higher reproducibility from samples that had been filtered and acidified before the evaporation, had their residues totally dissolved, and were purified by ion chromatography using the Biorad® column. Our results showed no changes in Pb ratios with the storage time.

Caracterização do MP10 e MP2,5 e distribuição por tamanho de cloreto, nitrato e sulfato em atmosfera urbana e rural de Londrina

Samplings of atmospheric particulate matter (PM) were carried out between the months of March and April of 2007, simultaneously in two areas of Londrina, an urban (Historical Museum) and other rural (Farm School-UEL). PM was collected using the cascade impactor consisting of four impaction stages (0.25 to 10 μm). The results indicated that the fine fraction (PM2.5) represented a significant portion of the mass of PM10 (70 and 67% in the urban and rural places, respectively). Cl-, NO3- and SO4(2-) were determined by ion chromatography and the size distribution is presented. Natural and anthropogenic sources were suggested to the ionic components in the fine and coarse mode of PM.

Degradação eletroquímica do cloranfenicol em reator de fluxo

This paper reports a study of electrochemical degradation of the chloramphenicol antibiotic in aqueous medium using a flow-by reactor with DSA® anode. The process efficiency was monitored by chloramphenicol concentration analysis with liquid chromatography (HPLC) during the experiments. Analysis of Total Organic Carbon (TOC) was performed to estimate the degradation degree and Ion Chromatography (IC) was performed to determinate inorganic ions formed during the eletrochemical degradation process. In electrochemical flow-by reactor, 52% of chloramphenicol was degraded, with 12% TOC reduction. IC analysis showed the production of chloride ions (25 mg L-1), nitrate ions (6 mg L-1) and nitrite ions (4.5 mg L-1).

Composição química da precipitação úmida da região metropolitana de Porto Alegre, Brasil, 2005- 2007

This work aims to quantify the wet precipitation the Metropolitan Area of Porto Alegre (MAPA), in southern Brazil, through the analysis of major ions (by ion chromatography) and metallic elements (ICP/AES). By principal components analysis and cluster analysis was possible to identify the influence of natural and anthropic sources in wet precipitation. The results indicated of the higher contribution to the ions NH4+, SO4(2-) and Ca2+. Thus it was possible to identify the contribution of anthropogenic sources in wet precipitation in the study area, such as power plants, oil refineries, steel and vehicle emissions.

Oxidação eletroquímica do herbicida tebutiuron utilizando eletrodo do tipo DSA

Tebuthiuron (TBH) is a herbicide widely used in different cultures and known for its toxic effects. Electrochemical methods are promising for removing pollutants such as pesticides. This study showed the degradation of TBH using a DSA® anode operated at current densities of 50 to 200 mA cm-2. Removal presented pseudo-first order kinetics while high-pressure liquid chromatography (UV detection) showed two peaks, ascribed to degradation intermediates. The maximum percentage of total organic carbon removed was 12.9%. Ion chromatography revealed that higher concentrations of nitrate and nitrite ions formed with increasing current density.

Solubility and Seeded Metastable Zone width of functional sugar L-arabinose

L-arabinose is widely used in food, medicine, chemistry, and biology fields; however, solubility and seeded metastable zone width (MSZW) of L-arabinose have not been reported in the literature. In this paper, solubility and MSZW of L-arabinose in aqueous solution were determined. Solubility of L-arabinose was measured in the range of 20-68 °C by a conventional equilibrium solubility method and quantitation was determined using the ion chromatography technique. Seeded MSZW was determined in the range of 51-73% by the calorimetric method. The effect of two salts (potassium chloride and calcium chloride) on the solubility and MSZW of L-arabinose were also evaluated. Results showed that both potassium chloride and calcium chloride increased the solubility of L-arabinose, and this increase was intensified with temperature rise. The MSZW of L-arabinose was not constant but a spread. Potassium chloride increased the MSZW of L-arabinose. However, the effect of calcium chloride on MSZW of L-arabinose was concentration dependent. Conclusion: the L-arabinose solubility increased with the increase in temperature, and both potassium chloride and calcium chloride increased the solubility of L-arabinose in aqueous solution. The seeded MSZW of L-arabinose is not a constant; it increases in the presence of potassium chloride and varies with the change in calcium chloride concentration.