Kinetic Method for the Determination of 2,4-Dinitrophenol

2008 ◽  
Vol 59 (7) ◽  
Author(s):  
S. S. Mitic ◽  
V. V. Zivanovic ◽  
G. Z. Miletic ◽  
D. A. Kostic ◽  
I. D. Rasic

A kinetic method for the determination of dinitrophenol is proposed. The method is based on the inhibiting effect of 2,4-dinitrophenol on the Mn(II) catalysis of the oxidation of malachite green with potassium periodate. The reaction was monitored spectrophotometrically at 615 nm. Kinetic expressions for the reaction are postulated. The optimal experimental conditions for the determination of 2,4-dinitrophenol were established and 2,4-dinitrophenol was determined in concentrations from 0.092-0.92 mg . mL-1 with relative standard error of 5.9 %. Detection limit is 0.014 mg . mL-1. The selectivity of the method is appropriate. The method was applied for the determination of dinitrophenol in urine and river water.

2002 ◽  
Vol 67 (10) ◽  
pp. 661-667 ◽  
Author(s):  
Snezana Mitic ◽  
Valentina Zivanovic

Akinetic method for the determination of phenol is proposed. The method is based on the inhibiting effect of phenol on the Mn(II) catalysis of the oxidation of malachite green with potassium periodate. The reaction rate was followed spectrophotometrically at 615 nm. Kinetic expression for the reaction in the presence and absence of phenol are postulated. The optimal experimental conditions for the determination of phenol were established and phenol was determined in concentrations from 30.0 to 188.0 ng/cm3 with a relative standard deviation of 5.5%. The lower detecton limit is 7.8 ng/cm3. The effects of certain foreign ions upon the reaction rate were determined for the assessment of the selectivity of the method. The method was applied for the determination of phenol in tap and river water.


2012 ◽  
Vol 554-556 ◽  
pp. 1999-2005
Author(s):  
Zhi Rong Zhou ◽  
Qun Wang ◽  
Shu Yuan Zhang

A spectrophotometric method for the determination of ruthenium (III) is described, based on its catalytic effect on the oxidation reaction of 2-[(3,5-dibromo-2-pyridy)azo]-5-diethylaminophenol (3,5-diBr-PADAP) with potassium periodate in 0.008 mol/L sodium hydroxide medium and in the presence of OP emulsifier (p-iso-octyl phenoxy polyethoxy ethanol) at 100 °C. The above reaction is followed spectrophotometrically by measuring the decrease in the absorbance at 530 nm for the catalytic reaction of 3,5-diBr-PADAP. The calibration curve for the recommended method was linear in the concentration range over 0.04 µg/L–1.0 µg/L and the detection limit of the method for Ru (III) is 0.012 µg/L. The influence of the factors such as acidity, concentration of reactants, reaction time, temperature and co-existing ions on the reaction is discussed. The optimum conditions of reaction are established and some kinetic parameters are determined. The apparent activation energy of catalytic reaction is 100.48 kJ/mol. The relative standard deviation for the determination of ruthenium (III) at the concentration of 0.02 µg/25mL is calculated to be 2.30 % (n=11). In combination with distilled separation, the method has been successfully applied for the determination of trace ruthenium (III) in some ores and metallurgy products with the relative standard deviations (RSD) over 1.8 %–2.9 % and the recovery over 98.1 %–103.1 %.


2000 ◽  
Vol 65 (8) ◽  
pp. 595-601
Author(s):  
S.S. Mitic ◽  
J.I. Vucetic ◽  
S.M. Miletic ◽  
D.A. Kostic

A kinetic method is described for the determination of Se(IV) based on its inhibiting effect on the Fe(III) catalysis of the oxidation of C6H5COONa with hydrogen peroxide. The detection limit is 0.06 pg cmT The relative error ranges between 2.1 and 9.5 % for the concentration interval 0.26 to 2.6 ?g cm-3. Kinetic equations are proposed for the investigated process. The effects of certain foreign ions upon the reaction rate were determined in order to assess the selectivity of the method. The method was applied for the determination of Se(IV) in pharmaceutical samples.


2011 ◽  
Vol 236-238 ◽  
pp. 2729-2732
Author(s):  
Pi Xue Gong ◽  
Wei Hua Liu ◽  
Wen Wen Liu ◽  
Kang Du ◽  
Kang Liu ◽  
...  

A simple, sensitive and rapid method for flow injection with chemiluminescence analysis has been developed for the determination of prednisone acetate at trace level. This method is based on the luminescent properties of the tris(1,10-phenanthroline) ruthenium(II)-potassium permanganate -prednisone acetate in acidic medium sensitized by Na2SO3. The optimized experimental conditions are evaluated. Under the optimum experimental conditions, the linear ranges of prednisone acetate are: 4.0×10-10~4.0×10-8g·mL-1and 4.0×10-8~2.0×10-7g·mL-1with a low detection limit is 4.5×10-11g·mL-1and the relative standard deviation for 1.0×10-8g·mL-1sample is 1.04% (n=11). The proposed method has been successfully applied to the determination of prednisone acetate in tablets.


2009 ◽  
Vol 63 (4) ◽  
Author(s):  
Zenovia Moldovan

AbstractA simple, selective and sensitive kinetic method for the determination of nitrite in water was developed. The method is based on the catalytic effect of nitrite on the oxidation of methylene blue (MB) with bromate in a sulfuric acid medium. During the oxidation process, absorbance of the reaction mixture decreases with the increasing time, inversely proportional to the nitrite concentration. The reaction rate was monitored spectrophotometrically at λ = 666 nm within 30 s of mixing. Linear calibration graph was obtained in the range of 0.005–0.5 μg mL−1 with a relative standard deviation of 2.09 % for six measurements at 0.5 μg mL−1. The detection limit was found to be 0.0015 μg mL−1. The effect of different factors such as acidity, time, bromate concentration, MB concentration, ionic strength, and order of reactants additions is reported. Interference of the most common foreign ions was also investigated. The optimum experimental conditions were: 0.38 mol L−1 H2SO4, 5 × 10.4 mol L−1 KBrO3, 1.25 × 10.5 mol L−1 MB, 0.3 mol L−1 sodium nitrate, and 25°C. The proposed method was conveniently applied for the determination of nitrite in spiked drinking water samples.


Molecules ◽  
2019 ◽  
Vol 24 (7) ◽  
pp. 1265 ◽  
Author(s):  
Qingkui Fang ◽  
Quan Zu ◽  
Xiude Hua ◽  
Pei Lv ◽  
Wanwen Lin ◽  
...  

A sensitive biotinylated indirect competitive enzyme-linked immunosorbent assay (Bic-ELISA) was developed to detect acetamiprid pesticides in pollen, based on the heterogeneous coating antigen and biotinylated anti-acetamiprid monoclonal antibody. Under optimized experimental conditions, the detection limit for the Bic-ELISA was 0.17 ng/mL and the linear range was 0.25–25 ng/mL. The cross-reactivities could be regarded as negligible for the biotinylated antibodies with their analogues except for thiacloprid (1.66%). Analyte recoveries for extracts of spiked pollen (camellia pollen, lotus pollen, rape pollen) ranged from 81.1% to 108.0%, with intra-day relative standard deviations (RSDs) of 4.8% to 10.9%, and the average reproducibility was 85.4% to 110.9% with inter-assay and inter-assay RSDs of 6.1% to 11.7%. The results of Bic-ELISA methods for the Taobao’s website samples were largely consistent with HPLC-MS/MS. Therefore, the established Bic-ELISA methods would be conducive to the monitoring of acetamiprid in pollen.


1989 ◽  
Vol 54 (3) ◽  
pp. 616-621 ◽  
Author(s):  
Záviš Holzbecher

It has been found that phosphoric acid decreases the first excitation maximum of Ce(III) at 256 nm, increases the second excitation maximum at 297 nm and shifts the fluorescence maximum from 350 to 346 nm. Under optimum conditions, with λexc = 297 nm and λem = 346 nm, Ce(III) can be determined fluorimetrically with a detection limit of 1.2 ng ml-1 in 12M-H3PO4 medium. No interference was observed from a 20-200 fold excess of HCl, H2SO4, Na, K, NH4+, Al and the rare earth elements. HNO3 interferes and Ce(IV) and Fe(III) interfere strongly. It follows from the stereofluorograms of Ce and Tb that the spectra of the two elements are practically independent. The detection limit for Tb(III) in 0.02-2.5M-H2SO4 medium for λexc = 222 nm and λem = 494 nm is 33 ng ml-1. No interference was observed from a 5-20 fold excess of Al3+ and the other rare earth elements. The determination is slightly less sensitive in H3PO4 or HCl medium. The relative standard deviation of the measurement for 10 ng ml-1 Ce(III) or 50 ng ml-1 Tb(III) is about 3%.


2010 ◽  
Vol 8 (3) ◽  
pp. 617-625 ◽  
Author(s):  
Hossein Abdolmohammad-Zadeh ◽  
Elnaz Ebrahimzadeh

AbstractA rapid dispersive liquid-liquid micro-extraction (DLLME) methodology based on the application of 1-hexylpyridinium hexafluorophosphate [C6py][PF6] ionic liquid (IL) as an extractant solvent was applied for the pre-concentration of trace levels of cobalt prior to determination by flame atomic absorption spectrometry (FAAS). 1-Phenyl-3-methyl-4-benzoyl-5-pyrazolone (PMBP) was employed as a chelator forming a Co-PMBP complex to extract cobalt ions from aqueous solution into the fine droplets of [C6py][PF6]. Some effective factors that influence the micro-extraction efficiency include the pH, the PMBP concentration, the amount of ionic liquid, the ionic strength, the temperature and the centrifugation time which were investigated and optimized. In the optimum experimental conditions, the limit of detection (3s) and the enrichment factor were 0.70 µg L−1 and 60, respectively. The relative standard deviation (RSD) for six replicate determinations of 50 µg L−1 Co was 2.36%. The calibration graph using the pre-concentration system was linear at levels 2–166 µg L−1 with a correlation coefficient of 0.9982. The applicability of the proposed method was evaluated by the determination of trace amounts of cobalt in several water samples.


2018 ◽  
Vol 33 (2) ◽  
pp. 47
Author(s):  
Orlando Fatibello-Filho ◽  
Heberth Juliano Vieira

A spectrophotometric flow injection method for the determination of paracetamol in pharmaceutical formulations is proposed. The procedure was based on the oxidation of paracetamol by sodium hypochloride and the determination of the excess of this oxidant using o-tolidine dichloride as chromogenic reagent at 430 nm. The analytical curve was linear in the paracetamol concentration range from 8.50 x 10-6 to 2.51 x 10-4 mol L-1 with a detection limit of 5.0 x 10-6 mol L-1. The relative standard deviation was smaller than 1.2% for 1.20 x 10-4 mol L-1 paracetamol solution (n = 10). The results obtained for paracetamol in pharmaceutical formulations using the proposed flow injection method and those obtained using a USP Pharmacopoeia method are in agreement at the 95% confidence level.


2001 ◽  
Vol 84 (1) ◽  
pp. 59-64 ◽  
Author(s):  
Inês P A Morais ◽  
António O S S Rangel ◽  
M Renata S Souto

Abstract A turbidimetric flow-injection system was developed for the determination of sulfate in natural and residual water samples, with no previous treatment, using spectrophotometric detection. The precipitating agent, 7.0% (w/v) barium chloride solution prepared in 0.10% (w/v) polyvinyl alcohol, was added by using the merging-zones approach. A 100 mg/L sulfate solution in 0.07M nitric acid was mixed with the sample before it entered the injection loop to improve the detection limit, provide in-line pH adjustment, and prevent the interference of some anionic species. The relative standard deviations of the results were between 1.4 and 3.0% and were in agreement with results obtained by the reference method. Samples within a linear concentration range of 10–120 mg SO42−/L can be analyzed at a rate of 40/h. The detection limit is 5 mg SO42−/L.


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