Search results for "STANDARD"
showing 10 items of 3299 documents
Flow injection Fourier transform infrared determination of caffeine in coffee
1999
Abstract A fully automatized procedure has been developed for the Fourier transform infrared (FT-IR) spectroscopic determination of caffeine in coffee samples. The method involves the on-line extraction of caffeine with CHCl3. Samples, weighed inside empty PTFE cartridges of 0.5 cm internal diameter (i.d.) and 1.5 ml volume, were humidified with four drops of 0.25 M NH3. The cartridge was installed in a flow manifold, in which samples were extracted in a closed-flow system with 1 ml CHCl3 during 6 min. Four hundred microliters of the extract were introduced in a microflow cell and absorbance measured as a function of time at 1659 cm−1, with a baseline established between 1900 and 830 cm−1, …
Simultaneous determination of hydride and non-hydride forming elements by inductively coupled plasma optical emission spectrometry
2011
e percentagens de recuperacao entre 97 e 103%. A aplicabilidade do sistema foi demonstrada na determinacao simultânea de Ca, Cd, Co, Cr, Cu, Fe, Mg, Mn, Mo, Ni, Zn, As, Bi, Sb, Se e Te em amostras certificadas para elementos tracos, NIST 1549 (leite em po desnatado), NIST 1570a (folhas de espinafre), DORM-2 (musculo de cacao) e TORT-2 (hepatopâncreas de lagosta). Os resultados obtidos foram concordantes com os teores certificados. The operating characteristics of a dual nebulization system were studied including instrumental and chemical conditions for the hydride generation and analytical figures of merit for both, hydride and non hydride forming elements. Analytical performance of the neb…
Determination of titanium by adsorption voltammetry with 4-(2-pyridylazo) resorcinol
1990
Titanium (IV) forms a complex with 4-(2-pyridylazo) resorcinol (PAR) in weakly acidic solutions. This complex can be used to determine titanium by adsorption voltammetry at a stationary Hg-electrode. The experimental conditions for the determination are described. The current-concentration curve is linear from 0.15–4.8 ng/g. Ti at a deposition time of 3 min, the detection limit lies at 0.1 ng/g. The influence of foreign ions was investigated. The determination can be carried out in the presence of a 1000-fold excess of iron by the standard addition method, albeit with decreased sensitivity.
Multi-element trace determinations in pure alkaline earth fluoride powders by high-resolution ICP-MS using wet-chemical sample preparation and laser …
2003
Four alternative analytical procedures for the determination of ten important trace impurities (Mg, Cr, Fe, Cu, Zn, Sr, Zr, Cd, Ba, and Pb) in pure alkaline earth fluoride powders were applied using high-resolution inductively coupled plasma mass spectrometry (ICP-MS). Two procedures are based on a wet-chemical microwave digestion with boric acid and quantification by the standard addition technique and isotope dilution mass spectrometry (IDMS), respectively. In addition, analyses are also performed by laser ablation as a direct solid sampling technique applying matrix-matched external calibration as well as isotope dilution of the powdered sample. For most elements good agreement between t…
Calibration of LA-ICP-MS via standard addition using dried picoliter droplets
2020
A novel microanalytical calibration approach for quantitative spatially resolved analysis of thin layered materials with laser ablation-inductively coupled plasma-mass spectrometry (LA-ICP-MS) is presented. This method relies on standard addition via the generation of dried pL-droplet residues. Therefore, a drop on demand dosing device based on a modified commercial ink cartridge and a dosing interface, both accessible via a self-constructed microcontroller, were developed. This dosing device enables the precise deposition of pL-droplets onto solid samples for the generation of residues with dimensions in the low μm-range. The LA-ICP-MS analysis of such residues allows calibration over at l…
Non-chromatographic speciation of mercury in mushrooms
2016
A fast, sensitive and cheap procedure has been developed for the determination of inorganic mercury (i-Hg) and organic mercury (o-Hg) in mushroom samples. The procedure is based on the use of cold vapour atomic fluorescence spectrometry (CV-AFS). The method involves the extraction of total mercury (t-Hg) with diluted HCl, followed by measurements of the corresponding Hg vapour under two different conditions: (i) directly to determine i-Hg, and (ii) after oxidation with a mixture KBr/KBrO3 to determine t-Hg. o-Hg was estimated from the difference between t-Hg and i-Hg. Previous studies were focused on the assessment of different reagents for mercury extraction and breakdown of organomercury …
Automated determination of amisulpride by liquid chromatography with column switching and spectrophotometric detection.
2003
A fully automated chromatographic method including on-line blood serum or plasma clean-up, isocratic high-performance liquid chromatography (HPLC) and spectrophotometric detection was developed for quantitative analysis of the new antipsychotic drug amisulpride. After injection of serum or plasma onto the HPLC system and clean-up on a pre-column (10x4.0 mm I.D.) filled with Silica CN 20 micrometer (pore size 10 nm) by an eluent consisting of 8% acetonitrile in deionized water, the chromatographic separation was performed on Lichrospher CN (5 micrometer; 250x4.6 mm I.D.) by an eluent consisting of 50% acetonitrile and 50% aqueous potassium phosphate buffer (0.008 M, pH 6.4). The UV detector …
Vanadium and molybdenum concentrations in particulate from Palermo (Italy): analytical methods using voltammetry
2014
The main purpose of this work was to develop a reliable method for the determination of vanadium (V) and molybdenum (Mo) in atmosphere particles or aerosols because they can not be readily measured using conventional techniques. For this research, 30 particulate samples were collected from five different stations located at Palermo, Italy. We used the catalytic adsorptive stripping voltammetry and differential pulsed voltammetry to measure Vand Mo in atmospheric particulate, respectively. The represented method includes advantages of high sensitivity, high selectivity, simplicity, reproducibility, speed and low costs. The quantification limits for V and Mo are, respectively, 0.57 and 0.80 n…
Multi-pumping mechanised determination of selenium in natural waters by light emitting diode (LED) spectrometry
2009
It has been developed a fully mechanised procedure for the determination of selenium in waters employing a LED based spectrometer and solenoid multi-pumps as solution propelling devices. The proposed method is based on the reaction of selenium with potassium iodide in an acidic medium to liberate iodine, which oxidizes Variamine Blue to form a violet-colour species which absorb at 530 nm. The system was mechanised using the multicommutation process and a stopped flow strategy in the final step reaction. The analytical curve was linear between 0.010 and 0.500 mg L-1, with an equation ΔA = 0.501 (± 0.004) C and r = 0.999. The limit of detection (3σ/S) obtained for the proposed method was 0.00…
Micropumping multicommutation turbidimetric analysis of waters
2007
Abstract A micropumping multicommutation manifold to perform turbidity determinations in waters is described. The procedure is based on the use of a combination of hydrazine sulfate and hexamethylenetetramine, to obtain an external standard of nephelometric turbidity units (NTU), which could compare the absorbance measurements at high wavelengths for samples with a calibration line obtained from a concentrated formazine standard diluted on-line. To minimize sample and reagent consumption and waste generation, the flow system was designed with two solenoid micro-pumps, one of them for the alternative introduction of the formazine standard and samples and the other one for the water carrier. …