Search results for "Standard addition"
showing 10 items of 72 documents
Systematic Study of Several Causes and Effects Due to Absorbent Blanks in Determinations of One Analyte
1999
A systematic study is performed about several factors involved in the measurements when a absorbent blank is used, as molar absorption coefficient of the formed complex, absorbance of the blank at the measured wavelength, and kind of spectrophotometer used (conventional double-beam or diode-array). It is proved that the usual methodology, measuring against reagent blank, produces less accurate measurements than those obtained against solvent blank. On the other hand, use of the H-Point standard additions method provides always equal or better results than the best ones obtained at single wavelengths by using measurements against solvent bank, at the maximum of the formed complex. To test th…
Solid sampling Fourier transform infrared determination of Mancozeb in pesticide formulations
2004
Abstract A series of approaches have been assayed for FTIR determination of Mancozeb in several solid commercial fungicides using different calibration strategies. The simplest procedure was based on the use of the ratio between the absorbance of a characteristic band of Mancozeb and that of a KSCN internal standard measured in the FTIR spectra obtained from KBr pellets. It was employed the quotient between peak height absorbance values at 1525 cm−1 for Mancozeb and 2070 cm−1 for KSCN. In these conditions a precision as relative standard deviation (RSD) of 0.6% and a relative accuracy error of 0.8% (w/w) were found. For complex formulations, containing other compounds with characteristic ab…
Creatinine determination in urine samples by batchwise kinetic procedure and flow injection analysis using the Jaffé reaction: chemometric study
2001
The classical Jaffé reaction for the determination of creatinine in urine samples is tested. A comparative study of the main analytical characteristics focussed to minimize the bias error and improve the precision, for the batchwise and flow injection (FI) methods is realized. Also, the effect of the albumin concentration in the determination of creatinine has been studied. Different analytical signals were studied. Absorbance increments at different times permit to estimate the creatinine concentration free from bias error in urine by the batchwise method using the calibration graph obtained with creatinine standards and no measurement of the blank solution is needed. The lineal interval w…
Fluorimetric determination of amphetamine in urine by flow injection with on-line liquid–liquid extraction
2001
Abstract Determination of amphetamine in urine was performed by batch and flow injection methodologies. The suitable experimental conditions for fluorimetric measurements were established. The liquid–liquid extraction was carried out at pH 13 using diethyl ether as extracting reagent. The measurement conditions were 260 nm and 277 nm for excitation and emission wavelengths, respectively. The method requires standard addition calibration and Youden blank correction. The influence of the main metabolites of amphetamine and metamphetamine were studied. The accuracy and precision of the proposed method was tested and the method is adapted to the flow injection procedure with on-line extraction.
Effectiveness of microwave based digestion procedures for the demineralization of human milk and infant formulas prior to fluorometric determination …
1996
The use of two types of microwave oven, one domestic (A) and the other specially designed for laboratory (B) for microwave-based digestion, to destroy the organic matter in milk and infant formulas prior to fluorometric determination of selenium is studied in order to check their applicability and reliability. In both systems the best results were obtained using the acid mixture HNO3—H2O2, and additional treatment with perchloric acid (60%) in a Thermoblock. The application of two different microwave-based digestion procedures to infant formulas was free of interferences. In the case of human milk, it was necessary to use the standard addition method. Values obtained for detection and quant…
New spectrophotometric procedure for determining cefotaxime based on derivatization with 1,2-naphthoquinone-4-sulphonate into solid-phase extraction …
1998
Cefotaxime was derivatised with 1,2-naphthoquinone-4-sulphonate (NQS), extracted into solid-phase cartridges (C18) and detected using a UV-visible detection system. Optimum conditions for this new procedure were: hydrogencarbonate-carbonate buffer, pH 10.5, 5-min reaction time at 25 degrees C and an NQS concentration of 7.1x10(-3) mol l(-1). The accuracy and the precision of the liquid-solid procedure were tested. The procedure was used to measure cefotaxime in pharmaceutical and urine samples. The results obtained were contrasted with those reported for a HPLC method for urine samples. The generalized H-point standard additions method was used to measure cefotaxime in urine samples.
The generalized H-point standard-additions method to determine analytes present in two different chemical forms in unknown matrix samples. Part II. C…
2000
The generalized H-point standard-additions method (GHPSAM) is used in order to obtain the total Cr(VI) and chromate concentration in water samples whose matrices are completely unknown. Moreover, a new methodology, which is a modification of the GHPSAM, is proposed for the simultaneous determination of the two major chemical forms of Cr(VI) present in the sample. The method is based on the location of spectral intervals where the behaviour of the interferent absorbance can be considered as linear. From these intervals, the analyte concentration free from bias error can be estimated. Spiked samples of dig and harbour water measured in the UV–visible spectral region have been tested to check …
Evaluation and elimination of the “blank bias error” using the H-point standard addition method
1992
Abstract The basis of the H-point standard addition method in the cases where the analyte determination requires the use of an absorbent reagent is considered. The method evaluates and eliminates the blank bias error present in such procedures by using the absorbance increment at two selected wavelengths as the analytical signal of the calibration graphs. Three different determinations were tested: the determination of proteins with the biuret method, thorium with thoron and of magnesium with Titan Yellow. These procedures are better described by the proposed method than by the traditional approach using absorbance values against reagent blank.
Principal component analysis for the selection of variables in the application of the H-point and generalised H-point standard addition method
2000
The present paper deals with the selection of variables for the H-point and generalised H-point standard additions methods (HPSAM and GHPSAM, respectively). Both methods are applied for the resolution of spectroscopic interfered signals in the UV-vis range. The HPSAM is a suitable method for the resolution of binary and ternary mixtures when the interferent is known. The GHPSAM is applied for the resolution of samples that contain unknown interferents. In this paper, a method based on the study of a principal components analysis (PCA) for the selection of variables for the HPSAM and GHPSAM is proposed. The PCA results show the isolation of the analyte signal from the sample signal, achieved…
Evaluation and elimination of the blank bias error using the H-point standard additions method (HPSAM) in the simultaneous spectrophotometric determi…
1997
Abstract The aim of this report is to demonstrate the usefulness of the HPSAM in all instances where the determination of two analytes requires the use of an absorbent reagent, particularly when it does not present a constant analytical signal because of its consumption. This problem can be treated as a ternary mixture by the HPSAM method and then, the fundamentals of the method for resolving these kind of mixtures can be applied. The method can calculate the concentration of one species from spectral data at two wavelengths where the two other species present the same absorbance relationship. These wavelength pairs are easily found, and can be selected to give the most precise results. The…