Flow-injection determination of 9,10-phenanthrenequinone with catalytic photometric detection

A catalytic photometric method with a flow-injection system is described for the determination of 9,10-phenanthrenequinone. It is based on the catalytic effect of 9,10-phenanthrenequinone on the redox reaction of 1,2-dinitrobenzene with formaldehyde under alkaline conditions. 9,10-Phenanthrenequinone at the 5.0 x 10(-8)-5.0 x 10(-6)M level can be determined at a rate of 20 samples/hr. The detection limit is 1.0 x 10(-8)M (40 pg in a 10-microl injection).     

Flow-injection photometric determination of trace copper in natural waters

A procedure for the flow-injection photometric determination of trace copper(II) in fresh natural waters is developed using a sorption preconcentration on the Diasorb-IDK-130 adsorbent with iminodiacetate groups. The procedure provides the determination of copper in the concentration range from 0.5 to 20 μg/L     

Flow injection determination of trace vanadium with catalytic photometric detection

A catalytic photometric detection system based on the chromotropic acid—bromate reaction is adapted to a flow injection system for the rapid, simple and sensitive determination of vanadium. Vanadium in the range 0.3–4.8 ng (10–160 ppb) can be determined at a rate of ca. 60 samples per hour.     

Flow-injection determination of trace amounts of dopamine by chemiluminescence detection

A flow-injection analysis (FIA) for the determination of dopamine has been developed. The method is based on the inhibition effect of dopamine on the iron(II)-induced chemiluminescence (CL) of 10,10'-dimethyl-9,9'-biacridinium dinitrate (lucigenin). The presence of a non-ionic surfactant, polyoxyethylene (23) lauryl ether (Brij 35), caused an increase in the inhibition effect. The present method allows the determination of dopamine over the range 1x10(-8)-2x10(-7) mol dm(-3). The relative standard deviation was 0.7% for eight determinations of 6x10(-8) mol dm(-3) dopamine. The detection limit (S/N=3) was 2x10(-9) mol dm(-3) with the sampling rate of 40 samples h(-1). The effect of other catecholamines and compounds of similar structure on the lucigenin CL reaction was studied: quinone, hydroquinone, norepinephrine, pyrocatechol and l-dopa suppressed the CL intensity.     

催化动力学光度法测定痕量锰

在H2SO4介质中,在表面活性剂壬基酚聚氧乙烯(7)醚的活化下,Mn(Ⅱ)催化溴酸钾氧化甲基紫褪色,建立了动力学光度法测定痕量Mn(Ⅱ)的新方法.考查了最佳试验条件并进行了动力学参数的测定;该方法检出限为2.3×10-7 g/L;线性范围0.0002～0.014 μg/mL;最大相对标准偏差为4.8%.用于水和面粉的测定,回收率在95.0%～104.7%之间;对面粉样用石墨炉原子吸收法进行了对比试验,方法相对误差低于±5.0%.     

Flow-injection catalytic kinetic determination of manganese using stopped-flow and gradient calibration

Based on the principle of Mn(II) catalysis of the Tiron-hydrogen peroxide reaction, a catalytic kinetic spectrophotometric determination of traces of manganese (ca. 10^?7 M) by flow injection was established. In combination with a microcomputer, by using gradient dilution and the stopped-flow method, onlya single standard solution was needed for calibration. The method has a high selectivity and a sampling rate of 40 h^?1. Traces of manganese in natural water were determined with a maximum relative standard deviation of 5.5% (n = 6).     

Study on catalytic fluorimetric determination of trace manganese

A new kinetic fluorimetric method has been proposed for the determination of trace manganese. The method is based on the catalytic oxidation of rhodamine 6G with potassium periodate in the presence of nitrilo triacetic acid as activator, in near neutral media. The detection limit for manganese is 0.018 ng/ml. The linear range of the determination is 0.04-1.00 ng/ml. The proposed method suffers from few interferences in the presence of more than 30 foreign ions. The method has been used to determine trace manganese in hair, urine, fish and water samples. The results are satisfactory.     

Flow-injection catalytic determination of molybdenum with blamperometric detection in a microprocessor-controlled system

The flow-injection determination of molybdenum(VI) is based on its catalytic effect on the oxidation of iodide by hydrogen peroxide. The triiodide ion formed in this reaction is detected amperometrically in a flow-through cell containing two platinum wire electrodes polarized at 100 mV. After optimization of the measuring conditions, the detection limit is 1.2 μg l^?1 Mo(VI) and the linear range extends to 1 mg l^?1. Interference of various metal ions and their removal is described. The procedure was tested on the determination of molybdenum(VI) in soil extracts.     

Continuous flow system for the determination of trace vanadium in natural waters utilizing in-line preconcentration/separation coupled with catalytic photometric detection

A sensitive and rapid method is presented for the determination of vanadium at ng to sub-ng ml(-1) levels in natural waters, in which in-line preconcentration/separation is directly coupled with catalytic detection of vanadium in a flow-injection system. Vanadium was adsorbed on a small column packed with Sephadex G-25 gel and desorbed with a small volume of 0.010 M HCl. The catalytic action of vanadium on the oxidation of chromotropic acid (1,8-dihydroxy-3,6-naphthalenedisulphonic acid) by bromate in pH 3.8 buffered media was used in the sensitive determination of vanadium. Effective preconcentration/separation of trace vanadium can be achieved from Fe(III), Cu(II) and a large excess of sodium chloride in seawater sample. A linear calibration using a 5 m sample loop was obtained for vanadium in the range 0-2.5 ng ml(-1). The limit of detection was 0.02 ng ml(-1) and the relative standard deviation was 1.2% for 1.0 ng ml(-1) vanadium (n=5). The present FIA system is rapid and sensitive and can be readily applied to river water and coastal seawater samples.     

Flow-injection photometric determination of mercaptans in light oil products with chromatomembrane extraction

A procedure was developed for the flow-injection photometric determination of mercaptans in light oil products. The use of sodium nitroferricyanide as the photometric reagent at 540 nm provides a detection limit of mercaptan sulfur of 0.3 mg/L at a volume of the sample of 3 mL; the analytical range is from 1 to 50 mg/L.     

催化动力学光度法测定锰

研究了在活化剂氮三乙酸(NTA)存在下,Mn2 催化KIO4氧化刚果红(Gongo Red)褪色反应的条件。建立了催化动力学光度法测定痕量锰的新方法。在测定波长496 nm时,锰测定的线性范围为0~2.8×10-9g/mL,检出限为2.76×10-11g/mL,探讨了有关的反应机理,考察了20余种共存离子对测定的影响,用于大米、绿豆、小米和水样中痕量锰的测定。     

催化光度法测定水中痕量亚硝酸根

利用在硫酸介质中亚硝酸根催化溴酸钾氧化吖啶橙的褪色反应 ,建立了测定痕量亚硝酸根的新方法。方法检出限为 7.6× 1 0 -8mol/ L,线性范围 0～1 .1 2× 1 0 -6mol/ L。本法可用于测定雨水和自来水中的痕量亚硝酸根     

流动注射在线萃取色谱分离原子吸收光谱法测定痕量铂

研究了流动注射在线分离富集原子吸收光谱法测定痕量铂的方法。以自制的GDX501-TBP萃取树脂为微型分离柱，在优化后的分离富集条件下，进样时间为60s，洗脱时间为45s。在线分离测定时间为3min，方法检出限为0．25μg/L，线性范围10—600μg/L，加标回收率为97．8％-103．6％，相对标准偏差3．49％-4．25％。方法已用于矿物管理样中铂的测定。     

Flow-injection determination of lead by hydride generation and conductometric detection

Plumbane produced from the lead analyte in a flow-injection manifold by reaction with sodium borohydride is passed through a porous poly(tetrafluoroethylene) membrane in a gas-diffusion cell. The hydride reacts with bromine in the acceptor stream resulting in ionization which is detected by conductivity measurement. Direct mixing of the carrier with a reagent stream yields a limit of detection of approximately 1 mg/L. An improved detection limit of about 200 g/L can be achieved by the incorporation of an auxiliary stream containing persulphate as oxidizing agent. The application of the method to the determination of lead in road dust and soil samples is demonstrated.     

Flow-injection determination of lead by hydride generation and conductometric detection

Plumbane produced from the lead analyte in a flow-injection manifold by reaction with sodium borohydride is passed through a porous poly(tetrafluoroethylene) membrane in a gas-diffusion cell. The hydride reacts with bromine in the acceptor stream resulting in ionization which is detected by conductivity measurement. Direct mixing of the carrier with a reagent stream yields a limit of detection of approximately 1 mg/L. An improved detection limit of about 200 microg/L can be achieved by the incorporation of an auxiliary stream containing persulphate as oxidizing agent. The application of the method to the determination of lead in road dust and soil samples is demonstrated.     

Flow-injection determination of meptazinol with electrochemical detection

A flow-injection analysis system incorporating a glassy carbon voltammetric detector cell is described. Meptazinol (0.01–10 μg ml^-1) can be determined by electro-chemical oxidation in a carrier stream of 0.05 M sodium acetate—0.1 M acetic acid in 98% ethanol at sampling rates up to 80 samples per hour.     

Rapid method for the photometric determination of manganese in ores and alloys

Summary A procedure for the rapid photometric determination of manganese in the range of 4–24 mg/50 ml, is based on the oxidation of manganese(II) to manganese(III) by excess potassium dichromate in a medium of 8.0 to 9.0 M phosphoric acid at room temperature. Interferences are few when compared to the methods currently available. The method can be successfully employed for the estimation of manganese in ores and alloys and the results obtained compare favourably with standard methods. The method is therefore recommended for adaption for rapid routine analysis.

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Schnelle Methode zur photometrischen Bestimmung von Mangan in Erzen und Legierungen

Zusammenfassung Ein Verfahren zur raschen Bestimmung von Mangan im Bereich von 4–24 mg/50 ml wird beschrieben. Es beruht auf der quantitativen Oxydation von Mn(II) zu Mn(III) mit Dichromat in 8,0–9,0 M phosphorsaurer Lösung bei Raumtemperatur. Die Störmöglichkeiten sind geringer als bei sonst üblichen Methoden. Das Verfahren wurde mit Erfolg zur Manganbestimmung in Erzen und Legierungen angewendet und gute Übereinstimmung mit Standardmethoden erzielt. Es wird für die schnelle Routineanalyse empfohlen.

     

催化光度法测定粮食中的痕量锰

研究了测定痕量锰的新催化光度法,方法基于氨三乙酸为活化剂,锰（Ⅱ）催化高碘酸钾氧化溴酚蓝的反应。测定锰的线性范围为0．4－10ng/mL,检出限为0．082ng/mL,对于4.0ng/mL Mn(Ⅱ）的测定,相对标准偏差为3．4％（n=9),其方法已用于粮食中锰的测定。     

催化动力学光度法测定铬的研究

在稀HCl介质中,微量铬(Ⅲ)对K2S2O8氧化酸性大红GR的褪色反应有明显的催化作用。据此建立了催化动力学光度法测定微量铬(Ⅲ)的新方法。确定了反应的最佳条件,并讨论了动力学参数。方法线性范围为0.008~0.4mg/L,检出限为2.96×10-6g/L。方法已用于自来水、钢厂废水、污水中微量铬(Ⅲ)的测定。     

Flow-injection methods for the determination of uracil derivatives with voltammetric detection

Flow-injection methods are described for the determination of 18 uracil derivatives and related compounds, by means of differential-pulse amperometry (d.p.a.) or differential-pulse cathodic stripping voltammetry (d.p.c.s.v.). The carrier stream is a borax/KNO₃/HNO₃ (of NaOH) solution containing 0.001% (v/v) Triton X-100. This surfactant displaces the oxygen reduction peak to such negative potentials that deaeration is unnecessary for detection of compounds having peak potentials in the range 180–70 mV (vs. Ag/AgCI) at pH 7.6. At the hanging mercury drop electrode, the uracil derivative is deposited from the flowing sample at a fixed potential more positive than the relevant peak potential and stripped under stopped-flow or slow-flow conditions. In the amperometric mode, a constant potential also more positive than the relevant peak potential is applied to the dropping mercury electrode and the resulting peak is measured under flow conditions. Linear calibration graphs were found for most of the compounds at 10^?6–10^?7 M by d.p.a, and about one order of magnitude lower by d.p.c.s.v.. The limit of determination for 5-iodouracil was 5×10^?9 M (ca. 1.2 ng ml^?1). Separation is needed for applications to blood or urine. Simple deproteination followed by high-performance liquid chromatography with a reversed-phase column proved satisfactory. Separations of various uracil derivatives, and of 5-fluorouracil, uric acid and 5-fluorodeoxyuridine, are described; spectrophotometric and amperometric detectors were used sequentially to check performance.