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1.
Composite diazotization-coupling reagents containing sulfanilamide (SAM), sulfapyridine (SP) or sulfathiazole (ST) as the diazotizable aromatic amines and sodium 1-naphthol-4-sulfonate (NS) as the coupling agent using column preconcentration on naphthalene-tetradecyldimethylbenzylammonium(TDBA)-iodide adsorbent have been used for the spectrometric determination of trace nitrate and nitrite in soil and water samples. Nitrite ion reacts with SAM in the pH range 2.0–5.0, SP in the pH range 2.0–2.5 and ST in the pH range 2.0–3.3 in HCl medium to form water-soluble colourless diazonium cations. These cations were coupled with NS in the pH range 9.0–12.0 for the SAM system, 9.6–12.0 for the SP system and 8.5–12.0 for the ST system to be retained on naphthalene-TDBA-I material packed in a column. The solid mass is dissolved from the column with 5 ml of dimethylformamide and the absorbance is measured spectrometerically at 543 nm for SAM-NS, 533 nm for SP-NS and 535 nm for ST-NS. Nitrate is reduced to nitrite by a copper-coated cadmium reductor column and the nitrite is then treated with the diazotization-coupling reagent by column preconcentration. The absorbance due to the sum of nitrate and nitrite is measured and nitrate is determined by difference. The calibration graph was linear over the range 2–40 ng NO2-N ml−1 and 1.5–30 ng NO3-N ml−1 in aqueous samples for the SAM and ST systems and 2–48 ng NO2-N ml−1 and 1.5–36 ng NO3-N ml−1 in aqueous samples for the SP system, respectively. The sensitivity, accuracy and precision of the systems decreased in the order STSAMSP. The detection limits were 1.4 ng NO2-N ml−1 and 1.1 ng NO3-N ml−1 for SAM, 1.6 ng NO2-N ml−1 and 1.2 ng NO3-N ml−1 for SP, and 1.0 ng NO2-N ml−1 and 0.75 ng NO3-N ml−1 for ST, respectively. The preconcentration factors are 8, 5 and 6 for SAM-NS, SP-NS and ST-NS, respectively. Interferences from various foreign ions have been studied and the methods have been applied to the determination of ng ml−1 levels of nitrite and nitrate in soil and water samples. The mean recovery was 95–102% for all three systems.  相似文献   

2.
Tirumalesh K 《Talanta》2008,74(5):1428-1434
This study describes a new ion chromatography method using a low-capacity anion exchange column with amperometric and absorbance detection for rapid and simultaneous determination of Br and NO3 in contaminated waters where one of these ions is present in excess compared to other. The use of two detectors overcomes the problem of baseline separation for Br and NO3 for accurate quantification, which was commonly encountered when using a low-capacity anion exchange column and suppressed conductivity detection mode. The method achieved accurate quantification of these two ions without requirement of baseline separation. The accuracy of 2.8% for NO3 was determined using a quality control sample obtained from UN GEMS/Water PE Study No. 6. The detection limits for Br and NO3 were 20 and 6 μg l−1 (25 μl sample), respectively. Linearity of these two ions was over three orders of magnitude with a correlation coefficient >0.998. The influence of potential interfering ions was also studied followed by the determination of Br and NO3 in seawater, unsaturated zone water, soil extract and groundwater.  相似文献   

3.
A simple and sensitive method for the determination of nitrite and nitrate in water using solid phase spectrophotometry is described. The method utilizes the quantitative and rapid sorption of the dye formed from nitrite, using the Griess reaction, into a thin layer of polyurethane foam (PUF) where a preconcentration factor of >140 has been achieved. Nitrate is pre-reduced using a cadmium reductor before applying the Griess reaction. The direct spectrophotometric measurement of the dye enriched in the solid foam phase has allowed the detection of as little as 5 and 40 ng ml−1 nitrite and nitrate, respectively. Optimization of the parameters affecting the quantitative formation and sorption of the dye into PUF has been considered. Analysis of natural water samples has been performed.  相似文献   

4.
Ruengsitagoon W 《Talanta》2008,74(5):1236-1241
A simple reversed flow injection colourimetric procedure for determining iron(III) was proposed. It is based on the reaction between iron(III) with chlortetracycline, resulting in an intense yellow complex with a suitable absorption at 435 nm. A 200 μl chlortetracycline reagent solution was injected into the phosphate buffer stream (flow rate 2.0 ml min−1) which was then merged with iron(III) standard or sample in dilute nitric acid stream (flow rate 1.5 ml min−1). Optimum conditions for determining iron(III) were investigated by univariate method. Under the optimum conditions, a linear calibration graph was obtained over the range 0.5–20.0 μg ml−1. The detection limit (3σ) and the quantification limit (10σ) were 0.10 and 0.82 μg ml−1, respectively. The relatives standard deviation of the proposed method calculated from 12 replicate injections of 2.0 and 10.0 μg ml−1 iron(III) were 0.43 and 0.59%, respectively. The sample throughput was 60 h−1. The proposed method has been satisfactorily applied to the determination of iron(III) in natural waters.  相似文献   

5.
A simple and rapid flow injection (FI) method is reported for the determination of phosphate (as molybdate reactive P) in freshwaters based on luminol chemiluminescence (CL) detection. The molybdophosphoric heteropoly acid formed by phosphate and ammonium molybdate in acidic conditions generated chemiluminescence emission via the oxidation of luminol. The detection limit (3× standard deviation of blank) was 0.03 μg P l−1 (1.0 nM), with a sample throughput of 180 h−1. The calibration graph was linear over the range 0.032–3.26 μg P l−1 (r2=0.9880) with relative standard deviations (n=4) in the range 1.2–4.7%. Interfering cations (Ca(II), Mg(II), Ni(II), Zn(II), Cu(II), Co(II), Fe(II) and Fe(III)) were removed by passing the sample through an in-line iminodiacetate chelating column. Silicate interference (at 5 mg Si l−1) was effectively masked by the addition of tartaric acid and other common anions (Cl, SO42−, HCO3, NO3 and NO2) did not interfere at their maximum admissible concentrations in freshwaters. The method was applied to freshwater samples and the results (26.1±1.1–62.0±0.4 μg P l−1) were not significantly different (P=0.05) from results obtained using a segmented flow analyser method with spectrophotometric detection (24.4±4.45–84.0±16.0 μg P l−1).  相似文献   

6.
A supported liquid membrane system has been developed for the extraction of vanillin from food samples. A porous PTFE membrane is impregnated with an organic solvent, which forms a barrier between two aqueous phases. The analyte is extracted from a donor phase into the hydrophobic membrane and then back extracted into a second aqueous solution, the acceptor. The determination (100–1400 μg ml−1 vanillin) was performed using a PVC-graphite composite electrode versus Ag/AgCl/3MKCl at +0.850 V placed in a wall-jet flow cell as amperometric detector. The solid sample is directly placed in the membrane unit without any treatment, and the analyte was extracted from the sample, passes through the membrane and conduced to the flow cell by the acceptor stream. The limit of detection (3σ) was 44 μg ml−1. The method was applied to the determination of vanillin (9–606 μg g−1) in food samples.  相似文献   

7.
Mousavi MF  Jabbari A  Nouroozi S 《Talanta》1998,45(6):1247-1253
A new sensitive colour reaction for nitrite determination is presented. In acidic medium, nitrite was reacted with safranine to form a diazonium salt which caused the reddish-orange dye colour of the solution to change to blue. The carrier stream, into which the sample solution was injected, was doubly distilled water. The reagent solution stream, which contained safranine dye, hydrochloric acid and potassium chloride, was mixed with the carrier in a 3-m length of silicon tubing (bore 0.5 mm) maintained at 30°C in a thermostatic bath. The absorbance intensity was measured at 520 nm. The detection limit was 20 ng ml−1 and the RSD% of 20 injections of 1 μg ml−1 of nitrite was 0.65%. Analysis can be done at a rate of up to 30 h−1. Under the optimum conditions in the concentration range of 30–4000 ng ml−1 of nitrite ion, a linear calibration graph was obtained (r=0.9999). The method was applied successfully to the determination of nitrite in sausages.  相似文献   

8.
Monser L  Sadok S  Greenway GM  Shah I  Uglow RF 《Talanta》2002,57(3):511-518
A direct spectrophotometric flow injection method for the simultaneous determination of nitrite and nitrate has been developed. The method is based on the oxidation of a phosphomolybdenum blue complex by the addition of nitrite and the decrease in absorbance of the blue complex is monitored at 820 nm. The injected sample is split into two segments. One of the streams was directly reacted with the above reagent and detected as nitrite. The other stream was passed through a copperised cadmium reductor column where reduction of nitrate to nitrite occurs, and the sample was then mixed with the reagent and passed through the cell of the spectrophotometer to be detected as nitrite plus nitrate. The conditions for the flow injection manifold parameters were optimised by experimental design and the concentration of nitrite and nitrate was determined in the linear range from 0.05 to 1.15 mug ml(-1) nitrite and 0.06 to 1.6 mug ml(-1) nitrate with a detection limit of 0.01 mug ml(-1) for nitrite and 0.025 mug ml(-1) for nitrate. The method is suitable for the simultaneous determination of nitrite and nitrate in fish and water samples with a sampling rate of 25+/-2 sample per hour.  相似文献   

9.
Matos RC  Coelho EO  Souza CF  Guedes FA  Matos MA 《Talanta》2006,69(5):1208-1214
The importance of atmospheric hydrogen peroxide (H2O2) in the oxidation of SO2 and other compounds has been well established. A spectrophotometric method for the determination of hydrogen peroxide in rainwater is proposed. This method is based on selective oxidation of hydrogen peroxide using an on-line tubular reactor containing peroxidase immobilized on Amberlite IRA-743 resin. The hydrogen peroxide in the presence of phenol, 4-aminoantipyrine and peroxidase, produces a red compound (λ = 505 nm). Beer's law is obeyed in a concentration range of 1–100 μmol l−1 hydrogen peroxide with an excellent correlation coefficient (r = 0.9991), at pH 7.0, with a relative standard deviation (R.S.D.) <2%. The detection limit of the method is 0.7 μmol l−1 (4.8 ng of H2O2 in a 200 μl sample). Measurements of hydrogen peroxide in rain samples were carried out over the period from November 2003 to January 2005, in the central area of the Juiz de Fora city, Brazil. The concentration of H2O2 varied from values lower than the detection limit to 92.5 μmol l−1. The effects of the presence of nonseasalt (NSS) SO42−, NO3 and H+ in the concentration of hydrogen peroxide in the rainwater had been evaluated. The average concentrations of H2O2, NO3, NSS SO42− and SO42− are 23.4, 18.9, 7.9 and 10.3 μmol l−1, respectively. The pH values for 82% of the collected samples are greater than 5.0. The spectrophotometeric method developed in this work that uses enzyme immobilized on the resin ion-exchange compared with the amperometric method did not present any significant difference in the results.  相似文献   

10.
Bismuth as BiCl4 and BH4 ware successively retained in a column (150 mm × 4 mm, length × i.d.) packed with Amberlite IRA-410 (strong anion-exchange resin). This was followed by passage of an injected slug of hydrochloric acid resulting in bismuthine generation (BiH3). BiH3 was stripped from the eluent solution by the addition of a nitrogen flow and the bulk phases were separated in a gas–liquid separator. Finally, bismutine was atomized in a quartz tube for the subsequent detection of bismuth by atomic absorption spectrometry. Different halide complexes of bismuth (namely, BiBr4, BiI4 and BiCl4) were tested for its pre-concentration, being the chloride complexes which produced the best results. Therefore, a concentration of 0.3 mol l−1 of HCl was added to the samples and calibration solutions. A linear response was obtained between the detection limit (3σ) of 0.225 and 80 μg l−1. The R.S.D.% (n = 10) for a solution containing 50 μg l−1 of Bi was 0.85%. The tolerance of the system to interferences was evaluated by investigating the effect of the following ions: Cu2+, Co2+, Ni2+, Fe3+, Cd2+, Pb2+, Hg2+, Zn2+, and Mg2+. The most severe depression was caused by Hg2+, which at 60 mg l−1 caused a 5% depression on the signal. For the other cations, concentrations between 1000 and 10,000 mg l−1 could be tolerated. The system was applied to the determination of Bi in urine of patients under therapy with bismuth subcitrate. The recovery of spikes of 5 and 50 μg l−1 of Bi added to the samples prior to digestion with HNO3 and H2O2 was in satisfactory ranges from 95.0 to 101.0%. The concentrations of bismuth found in six selected samples using this procedure were in good agreement with those obtained by an alternative technique (ETAAS). Finally, the concentration of Bi determined in urine before and after 3 days of treatment were 1.94 ± 1.26 and 9.02 ± 5.82 μg l−1, respectively.  相似文献   

11.
Wang J  Zhang C  Wang H  Yang F  Zhang X 《Talanta》2001,54(6):146-1193
A simple, fast chemiluminescence (CL) flow-injection method based on the reaction of luminol with H2O2 in the presence of a cationic surfactant (cyltrimethylammonium bromide, CTMAB) has been described for the direct determination of dichlorvos pesticide (DDVP). Under the optimal conditions, the CL intensity was linear to the DDVP concentration in the range of 0.02–3.1 μg ml−1 (r=0.9998, n=10). The relative standard deviation was 3.4% at 0.35 μg ml−1 (n=10), with a detection limit (3σ) of 0.008 μg ml−1 DDVP. The possible reaction mechanism was also discussed. This method has been successfully applied to the determination of trace DDVP residue in vegetable sample and results have been compared with that of the UV method.  相似文献   

12.
A new rapid flow injection procedure for the simultaneous determination of nitrate, nitrite and ammonium in single flow injection analysis system is proposed. The procedure combines on-line reduction of nitrate to nitrite and oxidation of ammonium to nitrite with spectrophotometric detection of nitrite by using the Griess-llosvay reaction. The formed azo dye was measured at 543 nm. The influence of reagent concentration and manifold parameters were studied. Nitrite, nitrate and ammonium can be determined within the range of 0.02–1.60 μg mL−1, 0.02–1.60 μg mL−1 and 0.05–1.40 μg mL−1, respectively. R.S.D. values (n = 10) were 2.66; 1.41 and 3.58 for nitrate, nitrite and ammonium, respectively. This procedure allows the determination and speciation of inorganic nitrogen species in soils with a single injection in a simple way, and high sampling rate (18 h−1). Detection limits of 0.013, 0.046 and 0.047 μg mL−1were achieved for nitrate, nitrite and ammonium, respectively. In comparison with others methods, the proposed one is more simple, it uses as single chromogenic reagent less injection volume (250 mL in stead of 350 mL) and it has a higher sampling rate.  相似文献   

13.
Mao L  Shi G  Tian Y  Liu H  Jin L  Yamamoto K  Tao S  Jin J 《Talanta》1998,46(6):1547-1556
A novel thin-layer amperometric detector (TLAD) based on chemically modified ring-disc electrode and its application for simultaneous measurements of nitric oxide (NO) and nitrite (NO2) in rat brain were demonstrated in this work. The ring-disc electrode was simultaneously sensitive to nitric oxide (NO) and nitrite (NO2) by modifying its inner disc with electropolymerized film of cobalt(II) tetraaminophthalocyanine (polyCoTAPc)/Nafion and its outer ring with poly(vinylpyridine) (PVP), respectively. The ring-disc electrode was used to constitute a novel TLAD in radial flow cell for simultaneous measurements of NO and NO2 in rat brain combined with techniques of high performance liquid chromatography (HPLC) and in vivo microdialysis. It was found that the basal concentration of NO in the caudate nucleus of rat brain is lower than 1.0×10−7 mol l−1, NO2 concentration is 5.0×10−7 mol l−1 and NO exists in brain maybe mainly in the form of its decomposed product.  相似文献   

14.
Flow injection determination of nitrite by fluorescence quenching   总被引:2,自引:0,他引:2  
A simple, sensitive and selective fluorimetric method for the determination of nitrite ion in waters using a merging zones flow injection system is described. The fluorimetric determination is based on the measurement of the quenching effect produced by nitrite on proflavine (3,6-diaminoacridine) fluorescence (λexem=290/519 nm).

The optimum experimental conditions were investigated by merging 0.5 ml of the sample and 0.5 ml of a solution of 5 mg l−1 of proflavine (in 0.1 M HCl) in a flow injection system, on-line connected to a flow-cell placed in the conventional sample compartment of a spectrofluorimeter. The selected carrier solution and final flow rate were 0.1 M HCl and 0.5 ml min−1, respectively. A reaction coil of 2 ml was used. As a result of the simplicity of this system, a sample throughput of about 50 samples h−1 can be achieved with the proposed methodology.

The detection limit was 1.1 ng ml−1 (3σ criterion) of nitrite. The repeatability for five sample injections containing 100 ng ml−1 of nitrite was ±0.3% and the observed linear range extended up to 400 ng ml−1. Also, the effect of interferences from various metals and anions commonly present in waters was also studied.

The method was successfully applied to the determination of low levels of nitrite in different water samples (river, fountain, tap and commercial drinking waters).  相似文献   


15.
Vanadium(V) is determined by a simple bead injection spectroscopy–flow-injection analysis (BIS–FIA) system with spectrofluorimetric detection using a commercially available flow cell (Hellma 176-QS). The 500 μl of a homogeneous bead suspension of an anionic resin (Sephadex QAE A-25) previously loaded with the fluorogenic reagent 1,2-dihydroxyanthraquinone-3-sulfonic acid (Alizarin Red S) was injected to fill the flow cell. Next, V(V) is injected into the carrier and reacts with the immobilized reagent on the active solid support placed in the flow cell to form a fluorescent chelate in the absence of surfactant agents. The complex is so strongly retained on the beads that the regeneration of the solid support becomes extraordinarily difficult, so needing the renovation of the sensing surface which is achieved by means of bead injection. At the end of the analysis, beads are automatically discarded from the flow cell and transported out of the system by reversing the flow.

The measurement of fluorescence is continuously performed at an excitation wavelength of 521 nm and an emission wavelength of 617 nm. Using a low sample volume of 800 μl, the analytical signal showed a very good linearity in the range 2–60 ng ml−1, with a detection limit of 0.45 ng ml−1 and a R.S.D. (%) of 4.22 for 50 ng ml−1 of V(V) concentration (n = 10). The sensor showed both a good selectivity, which could also be increased by the addition of EDTA and F as masking agents, and applicability to the determination of V(V) in waters, physiological samples (serum and urine) and mussel tissues.  相似文献   


16.
Nakano S  Tanaka K  Oki R  Kawashima T 《Talanta》1999,49(5):85-1082
A sensitive flow-injection spectrophotometric procedure is proposed for the determination of manganese(II), based on its catalytic effect on the oxidation of 2,2′-azinobis(3-ethylbenzothiazoline-6-sulfonic acid) (ABTS) with periodate. By monitoring the change in absorbance of the oxidation product of ABTS at 415 nm, manganese(II) in the range 0.05–1.0 ng ml−1 can be determined with a sampling frequency of 30 h−1. A relative standard deviation (R.S.D.) (n=10) is 1.6% at the 0.5 ng ml−1 level. The proposed method suffers from few interferences and has been successfully applied to the determination of manganese in river, lake and seashore water samples.  相似文献   

17.
A novel method for the spectrophotometric determination of nitrite in water   总被引:4,自引:0,他引:4  
Aydın A  Ercan O  Taşcıoğlu S 《Talanta》2005,66(5):1181-1186
A rapid, simple, selective and sensitive method for the spectrophotometric determination of nitrite in water has been developed and optimum reaction conditions along with other analytical parameters have been evaluated. Nitrite reacts with barbituric acid in acidic solution to give the nitroso derivative, violuric acid. At analytical wavelength of 310 nm, Beer's law is obeyed over the concentration range 0.00–3.22 ppm of nitrite. The molar absorptivity is 15330 ± 259.7 (95%) with pooled standard deviation of 355.57 and R.S.D. of 2.32%. As well as the method is sensitive (2.99 × 10−3 μg NO2 cm−2) and selective, it tolerates most of the potential interferents. It has been successfully applied to nitrite determination in natural waters by use of a calibration graph with determination limit of 1.66 μg NO2 in 100 mL working solution corresponding to minimum 9.5 ppb NO2–N in water samples. Lower concentrations of nitrite (3.0 μg NO2/L sample) is precisely analyzed by using the method of dilution with sample, with R.S.D. of lower than 0.5%. The results were compared with standard N-(1-naphtyl)ethylenediamine dihydrochloride method and very good agreement between the data was observed. The method can easily be applied in the field.  相似文献   

18.
Ahmed MJ  Banoo S 《Talanta》1999,48(5):711-1094
The very sensitive, fairly selective direct spectrophotometric method for the determination of trace amount of vanadium (V) with 1,5-diphenylcarbohydrazide (1,5-diphenylcarbazide) has been developed. 1,5-diphenylcarbohydrazide (DPCH) reacts in slightly acidic (0.0001–0.001 M H2SO4 or pH 4.0–5.5) 50% acetonic media with vanadium (V) to give a red–violet chelate which has an absorption maximum at 531 nm. The average molar absorption coefficient and Sandell’s sensitivity were found to be 4.23×104 l mol−1 cm−1 and 10 ng cm−2 of Vv, respectively. Linear calibration graph were obtained for 0.1–30 μg ml−1 of Vv: the stoichiometric composition of the chelate is 1:3 (V: DPCH). The reaction is instantaneous and absorbance remain stable for 48 h. The interference from over 50 cations, anions and complexing agents has been studied at 1 μg ml−1 of Vv. The method was successfully used in the determination of vanadium in several standard reference materials (alloys and steels), environmental waters (potable and polluted), biological samples (human blood and urine), soil samples, solution containing both vanadium (V) and vanadium (IV) and complex synthetic mixtures. The method has high precision and accuracy (s=±0.01 for 0.5 μg ml−1).  相似文献   

19.
Radiation induced decomposition of halogenated organic compounds in water   总被引:2,自引:0,他引:2  
Decomposition by ionizing radiations of p-chlorophenol and tetrachloroethylene in synthetic water samples at about 2 mg Cl L−1, has been studied on laboratory-scale experiments. Bicarbonate/carbonate and nitrate ions, at two concentration levels (20 and 200 mg HCO3−1 and 1 and 50 mg NO3L) were added to synthetic samples in order to evaluate their influence on decomposition yield. At 5 kGy γ dose level, a quantitative degradation of p-chlorophenol is obtained whereas only qualitative consideration can be drawn on tetracholoroethylene. Comparative study with respect to degradation of p-cholophenol solutions (about 2 mg Cl L−1) by γ-rays and electron beam irradiation treatment at 0.5 kGy dose level, are in progress; preliminary results indicate that irradiation with γ-rays seems to be more efficient in terms of removal efficiency respect to electron beams source.  相似文献   

20.
Organic-rich natural waters from peat bogs in continental (Switzerland) and maritime (Shetland Islands, Scotland) areas were analysed for Cl, NO2, Br, NO3, HPO42−, SO42− and oxalate using ion chromatography. These anions can be determined simultaneously in the surface and pore water samples from the continental bogs using a 250-μl injection loop. Using this loop, the detection limits were ca. 5 ng/g for the monovalent anions and SO42− and 10 ng/g for HPO42− and oxalate. An organics-removal cartridge (Dionex OnGuard P) was used to remove humic materials. These cartridges did not significantly affect the measured concentrations of anions in blind standards. Analyses of deionized water treated with these cartridges are not significantly different from those for untreated deionized water. For the maritime bogs, the relatively high concentrations of Cl (more than 100μ/g in many samples) and SO42− (up to 50 μg/g) require two separate determinations for complete analyses. A 10-μl injection loop was used to determine Cl, Br and SO42−. A 250-μl injection loop was used to measure NO2, NO3, HPO 42− and oxalate. In each instance a Dionex OnGuard P cartridge was used to remove humic materials. In addition, a chloride-removal cartridge (Dionex OnGuard AG) was used to remove Cl when the larger injection loop was used. This cartridge has no significant effect on the measurement of HPO4-2− at concentrations of 20 ng/g. In each of the bog water chromatograms there were usually a number of unknown peaks. These are probably due mainly to organic anions.  相似文献   

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