Kinetic determination of thiocyanate on the basis of its catalytic effect on the oxidation of methylene blue with potassium bromate.

This study reports a sensitive kinetic spectrophotometric method for the determination of trace amounts of thiocyanate. In acidic solution, Methylene Blue (MB) is oxidized by bromate to form a colorless compound. The reaction is accelerated by trace amounts of thiocyanate and can be followed by measuring the absorbance at 664 nm. The absorbance of the reaction decreased with an increase in the reaction time. Under the optimum experimental conditions (0.56 M of sulfuric acid, 3.9 x 10(-5) M of MB, 3.0 x 10(-3) M of bromate, 180 s, 25 degrees C), thiocyanate can be determined in the range 5.0 - 180 ng/ml. The relative standard deviations (n = 8) are 2.81 and 1.43% for 10.0 and 150 ng/ml thiocyanate, respectively. The detection limit of this method is (3sigma) 3.8 ng/ml. This method was successfully applied to the determination of thiocyanate in real samples.     

A kinetic method for the determination of copper(II) by its catalytic effect on the oxidation of 3-methyl-2-benzothiazolinone hydrazone with hydrogen peroxide: a mechanistic study.

A catalytic spectrophotometric method for the determination of traces of copper(II) is proposed. 3-Methyl-2-benzothiazolinone hydrazone (MBTH) is oxidized by hydrogen peroxide to form a yellowish-brown compound. The reaction is accelerated by trace amounts of copper(II), and can be followed by measuring the increase in the absorbance at 390 nm. Since the absorbance at 40 min from the reaction start increases with an increase in the copper(II) concentration, the absorbance value is used as a parameter for copper(II) determination. Under the optimum experimental conditions (8.4 x 10(-3) mol dm(-3) MBTH, 0.7 mol dm(-3) hydrogen peroxide, pH 5.2, 35 degrees C), copper(II) can be determined in the range 0-50 microg dm(-3). The relative standard deviations are 6.9, 3.5, 2.7% for 2, 20 and 40 microg dm(-3), respectively. The detection limit of this method (3sigma) is 0.27 microg dm(-3). It was successfully applied to a determination of copper(II) in river water, tap water and ground-water samples. According to the results of a kinetic study, a mechanism is proposed which leads to the following rate equation: R0(cat) = kK1K2[MBTH][H2O2][Cu(II)]0/{(1 + K2[H2O2])[H+]}.     

Spectrophotometric determination of trace nitrite based on catalytic oxidation of thionine by potassium bromate

A kinetic method for the determination of trace nitrite (7 × 10^?9–1.2 × 10^?6 M) based on its catalytic effect on the reaction between potassium bromate and thionine in strongly acidic media is reported. The reaction is monitored spectrophotometrically by measuring the decreasing colour of thionine at 602 nm by the fixed-time method. At a given time of 5 min at 30°C, the detection limit is 2 × 10^?9 M (0.001 absorbance ratio, b = 1 cm) and the relative standard deviation for 1 × 10^?6 M nitrite is 2.6% (n = 6). The method is free from most interferences, especially from large amounts of nitrate. The procedure was successfully applied to the determination of trace nitrite in natural water and sausage samples without preconcentration and separation.     

Ion chromatographic determination of trace iodate, chlorite, chlorate, bromide, bromate and nitrite in drinking water using suppressed conductivity detection and visible detection

An ion chromatography method for the simultaneous determination of trace iodate, chlorite, chlorate, bromide, bromate and nitrite in drinking water has been developed using an anion-exchange column and the suppressed conductivity detector, followed by post-column addition of reagent to enhance visible absorbance detection of ions. A high capacity anion exchange Ion Pac9-HC column (250 mm x 4 mm I.D.) was used. Eight millimole per liter sodium carbonate was used as eluent, an auto-suppression external water mode was selected, 0.5 g/l o-dianisidine.2HCl (ODA)+4.5 g/l KBr+25% methanel+5.6% nitric acid was used as post-column reagent. The post-column reaction (PCR) temperature was at 60 degrees C, and the visible absorbance detected wavelength at 450 nm. The sample's pH and coexist anions had no influence on determination. The method enjoyed a wide linear range and a good linear correlation coefficient (r>0.999). The method detection limits were between 0.023 and 2.0 microg/l. The average recoveries ranged from 87.5 to 110.0%, and the relative standard deviations (RSD) were in the range of 1.1-4.6%. The analytical results by the method of post-column addition of reagent to enhance visible absorbance detection of anions was compared with that of the suppressed conductivity detection, and the former was proved to be better in sensitivity and selectivity. The results showed that this method was accurate, sensitive and might be good for application and suitable for trace analysis at the level of mug/l.     

Spectrophotometric determination of platinum in glass after extraction with polyurethane foam

A spectrophotometric method has been developed for determination of trace amounts of platinum in glass. The method is based on the extraction of platinum(II) from 1M hydrochloric acid containing 0.2M stannous chloride and 4 x 10(-4)M dithizone onto polyurethane foam, elution with acetone (containing 3% v/v concentrated hydrochloric acid) and measurement of the absorbance of the eluate at 530 nm. Beer's law is obeyed up to 10.0 microg/ml Pt. The minimum platinum level in the eluate that can be determined by this method is 0.1 microg/ml.     

Flame atomic absorption spectrometric determination of trace amounts of nickel after extraction and preconcentration onto natural modified analcime zeolite loaded with 2-(5-bromo-2-pyridylazo)-5-diethylaminophenol

Nickel is a moderately toxic element compared with other transition metals. However, inhalation of nickel and its compounds leads to serious problems, including cancer of the respiratory system and a skin disorder, nickel-eczema. Thus, attention has focused on the toxicity of nickel at low concentrations, and the development of reliable, analytical approaches for the determination of trace amounts of nickel is needed. This paper describes a simple, rapid, and sensitive flame atomic absorption spectrometric method for the determination of trace amounts of nickel in various samples after adsorption of its 2-(5-bromo-2-pyridylazo)-5-diethylaminophenol complex on a modified Analcime column in the pH range of 7.5-10.5. The retained analyte on the Analcime is recovered with 5.0 mL 2 M nitric acid and determined by flame atomic absorption spectrometry. The detection limit is 20 ng/mL, and the calibration curve is linear for analyte concentrations in the range of 0.1-8 microg/mL final solution, with a correlation coefficient of 0.9993. Eight replicate determinations of nickel at 2 microg/mL in the final solution gave an absorbance of 0.1222, with a relative standard deviation (RSD) of +/-1.2%. The interference of a large number of anions and cations was studied, and the proposed method was used for the determination of nickel in various standard reference samples. The accuracy of the proposed method was evaluated by analyzing standard reference samples, and the results were satisfactory (recoveries of >96%; RSD of <3.5%).     

Kinetic spectrophotometric determination of low levels of nitrite by catalytic reaction between pyrogallol red and bromate

A kinetic spectrophotometric method for the determination of trace nitrite (0.003-1.000 microg/ml) based on its catalytic effect on the reaction between potassium bromate and pyrogallol red in acidic media is described. The reaction is monitored spectrophotometrically by measuring the decreasing colour of pyrogallol red at 467 nm by the fixed-time method. At a given time of 3.0 min at 30 degrees, the detection limit is 0.001 microg/ml and the relative standard deviation for 0.010 microg/ml nitrite is 1.8% (n = 8). The method is free from most interferences, especially from large amounts of nitrate and ammonium. The procedure was successfully applied to the determination of trace nitrite in natural water without preconcentration.     

Flow-injection catalytic spectrophotometric determination of nitrite using the redox reaction between naphthol green B and potassium bromate

A flow injection catalytic spectrophotometric method is proposed for the determination of nitrite based on its catalytic effect on the redox reaction between naphthol green B and potassium bromate in phosphoric acid medium. The reaction is monitored spectrophotometrically by measuring the decrease in absorbance of naphthol green B at the maximum absorption wavelength of 722 nm. The detection limit is 0.5 ng cm(-3) in a sample volume of 90 mm(3). Up to 50 samples can be analyzed per hour with a relative precision of ca. 2%. The method is free from most interferences, especially from large amounts of nitrate. The procedure was successfully applied to the determination of trace nitrite in natural waters.     

Kinetic Spectrophotometric Determination of Trace Amounts of Nitrite Ion Using Its Reaction With Neutral Red

Abstract

A rapid, simple, sensetive and selective method for the determination of trace amounts of nitrite ion(30-800 ng/ml) is developed. It depends on the reaction of nitrite with Neutral Red. The reaction is monitored spectrophotometrically by measuring the decrease in absorbance at 530 nm by a fixed time method. The limit of detection is 14 ng/ml. The method is used for the determination of nitrite ion in waste water.     

Spectrophotometric determination of nitrite and nitrate using phosphomolybdenum blue complex

A method for spectrophotometric determination of nitrite and nitrate is described. This method is based on the reduction of phosphomolybdic acid to phosphomolybdenum blue complex by sodium sulfide. The obtained phosphomolybdenum blue complex is oxidized by the addition of nitrite and this causes a reduction in intensity of the blue color. The absolute decrease in the absorbance of the blue color or the rate of its decrease is found to be directly proportional to the amount of nitrite added. The absorbance of the phosphomolybdenum blue complex is monitored spectrophotometrically at 814 nm and related to the concentration of nitrite present. The effect of different factors such as acidity, stability of the complex, time, temperature, phosphate concentration, molybdenum concentration, sodium sulfide concentration and the tolerance amount of other ions have been reported. Maximum absorbance is at 814 nm. The range of linearity using the conventional method is 0.5-2.0 ppm with molar absorptivity of 1.1 x 10(4) l mol(-1) cm(-1). and a relative standard deviation of 2.6% for five measurements. The range of linearity using the reaction rate method is 0.2-3.6 ppm with a relative standard deviation of 2.4% for five measurements. The method is applied for determination of nitrite and nitrate in water, meat products and vegetables.     

Indirect kinetic spectrophotometric determination of hydroxylamine based on its reaction with iodate.

A simple, precise and accurate method is proposed for rapid determination of trace amounts of hydroxylamine based on the reaction of hydroxylamine with iodate in acidic media. The reaction of neutral red by the produced nitrite ion was used to monitor the reaction spectrophotometrically at 525 nm by a fixed time method. Hydroxylamine in the range of 0.0400-1.200 microg mL(-1) could be determined. The relative standard deviation for 10 determinations of 0.500 microg mL(-1) hydroxylamine was 1.81% and the limit of detection was 0.010 microg mL(-1). The proposed method was applied to the determination of hydroxylamine in water samples with satisfactory results.     

Spectrophotometric determination of nitrite based on its catalytic effect on the oxidation of carminic acid by bromate

A highly sensitive and selective method is described for the determination of trace amounts of nitrite based on its effect on the oxidation of carminic acid with bromate. The reaction was monitored spectrophotometrically by measuring the decrease in absorbance of carminic acid at 490 nm after 3 min of mixing the reagents. The optimum reaction conditions were 1.8×10⁻¹ mol l⁻¹ H₂SO₄, 3.8×10⁻³ mol l⁻¹ KBrO₃, and 1.2×10⁻⁴ mol l⁻¹ carminic acid at 30°C. By using the recommended procedure, the calibration graph was linear from 0.2 to 14 ng ml⁻¹ of nitrite; the detection limit was 0.04 ng ml⁻¹; the R.S.D. for six replicate determinations of 6 ng ml⁻¹ was 1.7%. The method is mostly free from interference, especially from large amounts of nitrate and ammonium ions. The proposed method was applied to the determination of nitrite in rain and river water.     

Kinetic-spectrophotometric determination of palladium in hydrogenation catalyst by its catalytic effect on the oxidation of pyrogallol red by hydrogen peroxide

A new kinetic-spectrophotometric method is described for the determination of ultra trace amounts of Pd(II). The methods based on catalytic action of Pd(II) on the oxidation of pyrogallol red (PGR) with hydrogen peroxide at pH 9.7. The reaction was monitored spectrophotometrically by measuring the decrease in absorbance of the PGR at 540 nm, for the first 4.5 min from initiation of the reaction. Calibration curve was linear in the range of 0.02-1.00 microg ml(-1) Pd(II). The limit of detection is 0.017 microg ml(-1) Pd(II). The relative standard deviation (R.S.D.) for ten replicate analyses of 0.03 and 0.60 microg ml(-1) Pd(II) was 1.5 and 0.9%, respectively. The influence of more than 40 potential interfering ions was studied for the selectivity. The proposed method was used for the determination of palladium in catalytic material.     

A fluorescence quenching method for the determination of nitrite with Rhodamine 110

A simple and sensitive fluorescence quenching method for the determination of trace nitrite has been developed. The method is based on the reaction of Rhodamine 110 with nitrite in acidic medium to form a new compound, which has much lower fluorescence. The optimum experimental conditions were studied. The linear range was obtained at a nitrite concentration of 1.0 x 10(-8)-3.0 x 10(-7)mol l(-1) with a detection limit of 7.0 x 10(-10) mol l(-1) (S/N=3). The proposed method has been successfully applied to the determination of nitrite in tap water and lake water without extraction.     

Kinetic spectrofluorimetric determination of trace ascorbic acid based on its inhibition on the oxidation of pyronine Y by nitrite

A highly sensitive spectrofluorimetric method is proposed for the determination of trace amount of ascorbic acid using a new indication. The method is based on the inhibition of ascorbic acid on the oxidation of pyronine Y (PRY) by nitrite. The detection limit for ascorbic acid is 0.012 microg ml(-1), the linear range of the determination is 0.02-0.36 microg ml(-1). Analytical parameters, such as reagent concentration, pH, reaction temperature and time, were optimized. The relative standard deviations of eleven replication determinations of 0.12 and 0.24 microg ml(-1) ascorbic acid were 1.4 and 0.72%, respectively. This method has been used to determine ascorbic acid in pharmaceuticals, vegetables, fruits and soft drink with satisfactory results.     

Elimination of the interferences of anions in the kinetic spectrophotometric determination of vanadium (V) solution

Accurate determination of vanadium (V) in industrial waste water is of great importance in environmental, biological and toxicological studies. Most of kinetic spectrophotometric methods based on the catalytic effect of vanadium (V), when applied to real samples for determination of trace levels of vanadium (V) lack the satisfactory sensitivity and selectivity. This may be attributed to the serious interferences of various anions which are common pollutants in industrial waste water. The oxidation of gallic acid by ammonium persulphate, catalysed by vanadium (V) was chosen for our study. The effect of the serious interferences of various anions such as chloride, bromate, bromide, chromate, iodide, iodate, molybdate, carbonate and sulphate on the net absorbance given by 4 microg l(-1) of vanadium (V) solution were studied. The minimum concentrations of citric acid, EDTA, ascorbic acid and oxalic acid as leveling off agents required to level off interfering effects due to the aforementioned anions in the kinetic determination of vanadium (V) were 50, 70, 80 and 120 microg ml(-1), respectively. In the presence of optimum concentrations of effective leveling off agents, the dynamic range can be extended and sensitivity increased as compared with the proposed method without levelling off agents. The proposed method is a rapid, sensitive and selective method for the determination of ultra trace amounts of vanadium (V) in real samples with satisfactory results.     

Spectrophotometric determination of osmium based on its catalytic effect on the oxidation of carminic acid by hydrogen peroxide

A highly sensitive spectrophotometric method is described for the determination of trace amounts of osmium(VIII), based on its catalytic effect on the oxidation of carminic acid by hydrogen peroxide. The reaction was monitored spectrophotometrically by measuring the decrease in absorbance of carminic acid at 540 nm after 3 min of mixing the reagents. The optimum reaction conditions were 1x10(-4) mol l(-1) carminic acid, 0.013 mol l(-1) hydrogen peroxide and pH 10 at 25 degrees C. By using the recommended procedure, the calibration graph was linear from 0.1 to 1.5 ng ml(-1) of osmium; the detection limit was 0.02 ng ml(-1); the RSD for five replicate determinations of 0.2-1.4 ng ml(-1) was in the range of 1.8-4.7%. The influence of several foreign ions on osmium determination were studied and the effect of interfering ions were removed by extracting osmium into isobuthyl methyl ketone and back extracting into sodium hydroxide solution.     

Preconcentration of gallium by coprecipitation with synthetic zeolites prior to determination by electrothermal atomic absorption spectrometry.

Synthetic zeolites were dissolved in nitric acid, and the resulting solution used as a coprecipitant for the preconcentration of trace amounts of gallium in water samples prior to determination by electrothermal atomic absorption spectrometry (ETAAS). The gallium preconcentration conditions and the ETAAS measurement conditions were optimized. Gallium was quantitatively concentrated with the zeolites coprecipitate from pH 6.0 to 8.0. The coprecipitate was easily dissolved in nitric acid, and an aliquot of the resulting solution was introduced directly into a tungsten metal furnace. The atomic absorbance of gallium in the resulting solution was measured by ETAAS. An ashing temperature of 400 degrees C and an atomizing temperature of 2600 degrees C were selected. The calibration curve was linear up to 3.0 microg of gallium and passed through the origin. The detection limit (S/N > or = 3) for gallium was 0.08 microg/100 cm3. The relative standard deviation at 1.0 microg/100 cm3 was 3.0% (n = 5). The proposed method has been successfully applied to trace gallium analysis in environmental water samples.     

催化褪色光度法测定痕量亚硝酸根

用吸收光谱法研究了在磷酸介质中,亚硝酸根催化甲基绿被溴酸钾氧化而褪色的反应。在紫外可见光谱区,甲基绿的三个吸收峰出现在632．6,421．4和313．4nm。根据亚硝酸根的催化褪色反应在632．6nm产生的吸光度差或在三个吸收峰产生的吸光度差的总和,与亚硝酸根的浓度呈线性关系,建立了催化褪色光度法测定痕量亚硝酸盐的方法。     

Differential determination of arsenic (III) and total arsenic with L-cysteine as prereductant using a flow injection non-dispersive atomic absorption device

Speciation of arsenic in environmental samples gains increasingly importance, as the toxic effects of arsenic are related to its oxidation state. A method was developed for the determination of trace amounts of arsenic (III) and total arsenic by flow injection hydride generation coupled with an in-house made non-dispersive AAS device. The total arsenic is determined after prereduction of arsenic (V) to arsenic (III) with L-cysteine in a low concentration of hydrochloric, acetic or nitric acid. The conditions for the prereduction, hydride generation and atomization were systematically investigated. A quartz tube temperature of 800 degrees C was found to be optimum in view of peak shape and baseline stability. Pb(II), Ni(II), Fe(III), Cu(II), Ag(I), Al(III), Ga(II), Se(IV), Bi(III) were checked for interfering with the 2 microg/L As(V) signal. A serious signal depression was only observed for Se(IV) and Bi(III) at a 150-fold excess. With the above system, arsenic was determined at a sampling frequency of about 1/min with a detection limit (3sigma) of 0.01 microg/L using a 0.5 mL sample. The reagent blank was 0.001+/-0.0003 absorbance units and the standard deviation of 10 measurements of the 2 microg/l As signal was found to be 1.2%. Results obtained for standard reference materials and water samples are in good agreement with the certified values and those obtained by ICP-MS