scholarly journals Use of Flow InjectionMultisite Detection as a Novel Approach for Blank Signal Correction in a Spectrophotometric Determination

2005 ◽  
Vol 88 (5) ◽  
pp. 1511-1515
Author(s):  
Teresa A C Oliveira ◽  
Raquel B R Mesquita ◽  
José L F C Lima ◽  
António O S S Rangel

Abstract A flow injection multisite detection system was developed for correction of the sample blank in a colorimetric determination. By using detector relocation, a single spectrophotometer is used for the sequential reading of the sample blank and of the colored product; the sample crosses the flow cell to measure intrinsic absorption, the color reagent is subsequently added, and the flow cell is relocated to provide the reading of the resulting plug. The subsequent detector relocation immediately after peak maximum increases the determination frequency. This strategy was tested in the colorimetric determination of iron in soil samples based on the reaction of Fe (II) with 1,10-phenanthroline after reduction of Fe (III) to Fe (II) by ascorbic acid. The results obtained for 15 soil extracts were in good agreement with those obtained by the reference procedure. Relative standard deviations better than 4% were obtained, with a sampling rate of 30/h.

2009 ◽  
Vol 2009 ◽  
pp. 1-8 ◽  
Author(s):  
Ibrahim A. Darwish ◽  
Heba H. Abdine ◽  
Sawsan M. Amer ◽  
Lama I. Al-Rayes

Simple and rapid spectrophotometric method has been developed and validated for the determination of paroxetine (PRX) in tablets. The proposed method was based on nucleophilic substitution reaction of PRX with 1,2-naphthoquinone-4-sulphonate (NQS) in an alkaline medium to form an orange-colored product of maximum absorption peak () at 488 nm. The stoichiometry and kinetics of the reaction were studied, and the reaction mechanism was postulated. Under the optimized reaction conditions, Beer's law correlating the absorbance (A) with PRX concentration (C) was obeyed in the range of 1–8 g . The regression equation for the calibration data was: A = 0.0031 + 0.1609 C, with good correlation coefficients (0.9992). The molar absorptivity () was L  1 . The limits of detection and quantitation were 0.3 and 0.8 g , respectively. The precision of the method was satisfactory; the values of relative standard deviations did not exceed 2%. The proposed method was successfully applied to the determination of PRX in its pharmaceutical tablets with good accuracy and precisions; the label claim percentage was %. The results obtained by the proposed method were comparable with those obtained by the official method.


2013 ◽  
Vol 295-298 ◽  
pp. 950-953 ◽  
Author(s):  
Dong Yuan ◽  
Da You Fu ◽  
Wen Yuan Tan

A rapid spectrophotometric method for flow injection determination of sulfite in tan wastewater is described. The proposed method was based on the addition reaction of sulfite with fuchsin in Na2B4O7-NaOH medium. The optimum conditions allow a linear calibration range of 0.01-1.20 μg ml-1 SO32-. The detection limit is 0.0023μg ml-1 (S/N=3), and the relative standard deviation for night replicate measurements is 1.1% for 0.5μg ml-1 of sulfite. The sampling rate is 60 samples h-1. The procedure has been applied to the determination of sulfite in tan wastewater. The results were in good agreement with those obtained by pararosaniline method.


1991 ◽  
Vol 74 (1) ◽  
pp. 22-26 ◽  
Author(s):  
David K Christians ◽  
Thomas G Aspelund ◽  
Scott V Brayton ◽  
Larry L Roberts

Abstract Seven laboratories participated In a collaborative study of a method for determination of phosphorus in meat and meat products. Samples are digested In sulfuric acid and hydrogen peroxide; digestion Is complete In approximately 10 mln. Phosphorus Is determined by colorimetric analysis of a dilute aliquot of the sample digest. The collaborators analyzed 3 sets of blind duplicate samples from each of 6 classes of meat (U.S. Department of Agriculture classifications): smoked ham, water-added ham, canned ham, pork sausage, cooked sausage, and hamburger. The calibration curve was linear over the range of standard solutions prepared (phosphorus levels from 0.05 to 1.00%); levels in the collaborative study samples ranged from 0.10 to 0.30%. Standard deviations for repeatability (sr) and reproducibility (sR) ranged from 0.004 to 0.012 and 0.007 to 0.014, respectively. Corresponding relative standard deviations (RSDr and RSDR, respectively) ranged from 1.70 to 7.28% and 3.50 to 9.87%. Six laboratories analyzed samples by both the proposed method and AOAC method 24.016 (14th Ed.). One laboratory reported results by the proposed method only. Statistical evaluations Indicated no significant difference between the 2 methods. The method has been adopted official first action by AOAC.


1991 ◽  
Vol 74 (2) ◽  
pp. 346-350 ◽  
Author(s):  
Matthieu Tubino ◽  
Flavio G Barros

Abstract Recent methods for determination of the volatile acidity of vinegars are relatively slow (about 40 mln) and involve techniques subject to a variety of errors (ca 2.5%). The present paper describes a method that provides results in a shorter time (ca 2 mln, Including dilution), with a smaller relative error rate (ca 1%). Conductometric analysis consists of the Injection of the sample In a deionlzed water stream that then flows past a PTFE membrane separator. Acetic acid diffuses through the membrane to another deionlzed water stream that passes through a conductivity cell. Colorimetric analysis also consists of sample injection into a deionlzed water stream that passes through the same PTFE membrane separator. However, the acetic acid diffuses into a bromocresol purple solution stream at pH 7. This solution passes through a flow cell In a spectrophotometer set at 540 nm. Before injection, samples were treated with hydrogen peroxide to ensure complete oxidation of sulfite to sulfate. Results of the proposed method were also compared with another similar method. At a 95% confidence level, the statistical t-test Indicates no significant difference between them. Typical estimates of the relative standard deviations obtained with the new methods are ca 1%. Analyses were performed with red and white wine vinegars.


1991 ◽  
Vol 74 (4) ◽  
pp. 671-673 ◽  
Author(s):  
Thomas C Mueller ◽  
Thomas B Moorman

Abstract A rapid, sensitive method Is described for the determination of fluometuron and Its soil metabolites In 4 soil types. The method consists of extraction of moist soil samples with methanol, filtration, liquid chromatographic separation of methanol-soluble components using a C18 column, and fluorescence detection with excitation at 292 nm and emission measured at 345 nm. Fluometuron recoveries from fortified soils were >90% from the Dundee, Okalona, Cecil, and Ships soils. Recoveries from a Dundee silt loam for desmethyl fluometuron, 3-(trlfluoromethyl)phenyl urea, and 3- (trifluoromethyl)anillne were 77, 77, and 35%, respectively. Average percent relative standard deviations of Dundee soil extracts were 5.3% for fluometuron and <8.0% for each metabolite. The limit of detection for fluometuron and each of its soil metabolites was 25 ng/g soil.


2018 ◽  
Vol 34 (2) ◽  
pp. 67
Author(s):  
Orlando Fatibello-Filho ◽  
Heberth Juliano Vieira

A spectrophotometric flow injection method for the determination of Zn(II) in ophthalmic formulations was developed. In this work, Zn(II) ion was complexed with Alizarin red S in borate buffer solution (pH 9.0) and the chromophore produced was monitored at 520 nm. The analytical curve was linear in the Zn(II) concentration range from 6.05 x 10-6 to 1.50 x 10-4 mol L-1 with a detection limit of 3.60 x 10-6 mol L-1. Recoveries ranged from 96.3 to 105 % and a relative standard deviation of 1.2 % (n = 10) for 5.5x10-5 mol L-1 Zn(II) reference solution were obtained. The sampling rate was 60 h-1 and the results obtained of Zn(II) in ophthalmic products using this procedure are in close agreement with those obtained using a comparative spectrophotometric procedure at 95 % confidence level.


PLoS ONE ◽  
2021 ◽  
Vol 16 (11) ◽  
pp. e0258508
Author(s):  
Sihua Peng ◽  
Aqiang Wang ◽  
Yuyang Lian ◽  
Xi Zhang ◽  
Bei Zeng ◽  
...  

In order to achieve rapid detection of thiamethoxam residues in mango, cowpea and water, this study modified the screen printed carbon electrode (SPCE) to make a specific molecular imprinting sensor (Thiamethoxam-MIP/Au/rGO/SPCE) for thiamethoxam. An integrated smartphone platform was also built for thiamethoxam residue analysis. The performance of the complete system was analyzed by cyclic voltammetry (CV) and differential pulse voltammetry (DPV). The system was then applied for the rapid determination of thiamethoxam residues in water, mango and cowpea samples. The results showed that the molecular sensor showed good linearity in the range 0.5–3.0 μmol/L of thiamethoxam. The detection limit of thiamethoxam was 0.5 μmol/L. Moreover, the sensor had good reproducibility and anti-interference performance. The average recovery rates of the pesticide residues in water, mango and cowpea samples were in the range of 90–110% with relative standard deviations < 5%. The rapid detection system for thiamethoxam residue constructed in this study was simple, reliable, reproducible and had strong anti-interference. It has broad application prospects in the field detection of thiamethoxam residue, and serves as a valuable reference for the further development of rapid detection technology of pesticide residues in the field of environment and food safety.


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