Merging zones in flow injection analysis : Part 4. Simultaneous spectrophotometric determination of total nitrogen and phosphorus in plant material

The merging zones approach is used in a single flow injection system for the simultaneous Spectrophotometric determination of nitrogen and phosphorus in plant material based on the Berthelot and molybdophosphate reactions. A multiple proportional injector is designed to introduce samples and reagents into water carrier streams in such a way that only one analytical path with one detection unit is required. For both processes, catalysis is employed; a detailed study of the reagent composition is reported for the Berthelot reaction. The proposed system is characterized by a high degree of sample and reagent dispersion; 60 samples per hour can be analyzed with a consumption of reagents in the range of microliters per determination. Total recoveries of 98.3% N and 99.1% P were estimated from 20 runs of a typical plant sample containing around 3% N and 0.3% P in dry matter. The results of the present method agree with those obtained by Technicon AutoAnalyzer procedure.     

Determination of total chromium by flow injection analysis

The determination of total chromium by flow injection analysis is described. Cerium(IV) and nitric acid are used to convert chromium(III) to chromium(VI); the oxidation rate is enhanced by placing the reaction coil in an 80°C oil bath. 1,5-Diphenylcarbazide is used to form a colored complex with chromium(VI) that is measured at 540 nm. For both chromium(III) and chromium(VI), relative standard deviation of less than 1% is achieved with a sampling rate of 40 per hour. Linear response is obtained for 0.5–10 mg l^?1 chromium.     

Determination of phosphate species in nutrient solutions and phosphorus in plant material as phosphovanadomolybdic acid by flow injection analysis

A flow-injection spectrophotometric method for the determination of orthophosphate is described. The signal from the yellow phosphovanadomolybdic acid complex is recorded at 400 nm. The detection limit is 0.1 mg P 1^?1 (as orthophosphate), the calibration graph is linear up to 30 mg P 1^?1 and up to 240 samples can be analysed per hour. The method is used in the determination of phosphorus in digested plant material, and is also applicable for separating free orthophosphate from acid-labile aluminium phosphate colloids in nutrient solutions.     

Determination of total nitrogen in food by flow injection analysis (FIA) with a potentiometric differential detection system

A flow injection set-up based on potentiometric detection and gas diffusion device for the determination of total nitrogen in food is described. The detection system consisted of two ammonium-sensitive electrodes placed sequentially and each alternately operating as reference electrode. Tubular electrodes without an inner reference solution were prepared with a PVC membrane composed of nonactin in Tris (2-ethylhexyl) phosphate and potassium tetrakis (4-chlorophenyl) borate to reduce the membrane resistance. The food sample digests were inserted into the system, and the ammonium present was converted into ammonia gas. The gas diffused through a gas-permeable membrane to a buffer acceptor stream with a pH that ensured transformation to the ammonium cation, which was potentiometrically detected. Good agreement between FIA results and those provided by the reference procedure was obtained, with relative deviation errors below 5%. Using the proposed system, low reagent consumption is possible, a sampling rate of about 30 samples/h was achieved, as well as a good reproducibility for consecutive injections of the same sample (variation coefficient < 2%).     

Determination of total nitrogen in food by flow injection analysis (FIA) with a potentiometric differential detection system

A flow injection set-up based on potentiometric detection and gas diffusion device for the determination of total nitrogen in food is described. The detection system consisted of two ammonium-sensitive electrodes placed sequentially and each alternately operating as reference electrode. Tubular electrodes without an inner reference solution were prepared with a PVC membrane composed of nonactin in Tris (2-ethylhexyl) phosphate and potassium tetrakis (4-chlorophenyl) borate to reduce the membrane resistance. The food sample digests were inserted into the system, and the ammonium present was converted into ammonia gas. The gas diffused through a gas-permeable membrane to a buffer acceptor stream with a pH that ensured transformation to the ammonium cation, which was potentiometrically detected. Good agreement between FIA results and those provided by the reference procedure was obtained, with relative deviation errors below 5%. Using the proposed system, low reagent consumption is possible, a sampling rate of about 30 samples/h was achieved, as well as a good reproducibility for consecutive injections of the same sample (variation coefficient < 2%). Received: 8 October 1998 / Revised: 7 January 1999 / Accepted: 12 January 1999     

Determination of total sulphur in soil and plant material

A rapid and accurate method for the determination of the total sulphur content of soil or plant material is described. The sample is heated with sodium bicarbonate and silver oxide at 550° for ₃h, and the sulphur content of the whole residue is reduced to hydrogen sulphide and determined as methylene blue. The results compare favourably with those of other methods.In routine use, at least 30 analyses may be completed in a day.     

Flow injection analysis : Part II. Ultrafast determination of phosphorus in plant material by continuous flow spectrophotometry

The effect of sample volume, tube length, tube diameter, peak height and sampling rate on the determination of phosphorus in acidic plant digests was investigated, and optimal conditions for the flow injection method are described. Sampling rates of 420 samples per hour were achieved without incurring problems from carryover of samples, and evidence was obtained that rates as high as 700 samples per hour are possible. The flow injection method was proved to be suitable for routine analyses and has obvious advantages over other automated or manual methods in sampling rate, simplicity of design and cost.     

Flow injection analysis : Part III. Comparison of continuous flow spectrophotometry and potentiometry for the rapid determination of the total nitrogen content in plant digests

The Berthelot reaction for the determination of ammonia by formation of indophenol blue, has been adapted to continuous flow spectrophotometry and the effects of acidity, temperature, ethanol content and sampling rate have been investigated; optimal conditions are described for the determination of nitrogen in Kjeldahl digests. Comparison of results obtained by this method, the air-gap electrode and classical distillation show no statistical difference at the 1% level, but the flow injection technique can be run at a much higher sampling rate (110–180 samples per h) than any other method and uses as little as 0.3 ml of digest per analysis.     

流动注射在线分析法测定海水中的亚硝酸盐氮

建立流动注射在线分析法测定海水中亚硝酸盐氮的含量.样品中的亚硝酸盐与N-(1-萘基)-乙二胺盐酸盐及磺胺发生重氮反应,生成可溶于水的紫红色化合物,在波长520 nm处检测.海水中的亚硝酸盐氮质量浓度在0.00～5.00 mg/L范围与吸光度线性相关,海水中亚硝酸盐氮的检出限为0.005 mg/L.样品加标回收率为90....     

Determination of total primary amines in seawater and plant nectar with flow injection sample processing and fluorescence detection

Flow injection sample processing is used with fluorescence detection for the determination of total primary amines in seawater and nectar. The effects of carrifer stream flow rate and dispersion tube length on sensitivity and sampling rates were studied. Relative responses of several amino acids and other primary amines were determined using two dispersion tube lengths. Linear calibration curves were obtained over the ranges 0–10^-6 M and O–1O^-5 M glycine. Precisions of better than 2% at 10^-6 M and a detection limit of 1 × lO^-8 M glycine were obtained. Applications to the analysis of seawater from the vicinity of a baited lobster trap and diluted nectar samples from Erythrina sp. are described.     

Determination of phenol in water by flow injection analysis

Summary The adaptation of the manual standard method for the determination of phenols is described, e.g., condensation with 4-amino-antipyrine with subsequent oxidation and spectrophotometric detection. A FIA manifold for the automation of the phenol determination in the ranges 0.05–1.0 ppm and 1–15 ppm is presented. At a maximum injection frequency of 105/h the repeatability of consecutive injections is generally better than 1.5% r.s.d. resp. 1.0% r.s.d. By application of a new extraction module also the chloroform extraction step of the formed dye is automized. Compared to the direct FIA manifold a maximum sensitivity enhancement of 3.5 is obtained. The detection limit is 0.005 ppm phenol. In addition to the FIA methods a forced steam distillation procedure is described, which allows the distillation of phenols within 2–5 min.

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Bestimmung von Phenol im Wasser mit Hilfe der Fließ-Injektionsanalyse

     

Determination of total and dissolved amount of iron in water samples using catalytic spectrophotometric flow injection analysis

A flow injection spectrophotometric method has been developed for the determination of dissolved and total amounts of iron in tap and natural water samples. The method for the determination of iron employs a sample acidification step in order to decompose iron hydroxide and iron-complexes into free iron, Fe(III) and Fe(II). The amounts of free iron were detected using a catalytic action of Fe(III) and Fe(II) on the oxidation of N,N-dimethyl-p-phenylenediamine in the presence of hydrogen peroxide. Increase in absorbance of oxidized product was detected spectrophotometrically at 514 nm. The proposed method allows 0.02 and 0.06 μg l⁻¹ of LOD and LOQ, respectively, with relative standard deviation (RSD) below 2%. The accuracy and the precision of the method were evaluated by the analysis of the standard reference material, river water. The developed method was successfully applied to real water samples.     

Sequential injection system for on-line analysis of total nitrogen with UV-mineralization

An automatic method for the determination of total nitrogen in wastewater by sequential injection analysis and mineralization with UV radiation has been developed. The method is based on the mineralization of the samples with sodium persulphate in basic medium under UV radiation. Small volumes of sample and reagents are firstly aspirated into a single channel and then propelled by flow reversal to the UV reactor and then to the detector. The organic and inorganic nitrogen compounds are oxidized to nitrate that is then measured at 226 nm. The sequential injection procedure has been optimized and the factors affecting the efficiency of the oxidation have been studied with a number of test substances with different chemical structures and properties. Solutions in the concentration range 1-56 g l⁻¹ of nitrogen can be analyzed with the described procedure. The sample rate is of 30-40 samples h⁻¹. The LOD is 0.6 mg l⁻¹ N and the reproducibility is 1.8% (28 mg l⁻¹ N). Organic carbon in the form of glucose was added to a number of test solutions to study the potential interference of organic matter.The method was compared with the Kjeldahl digestion method by analyzing 15 wastewater samples with both methods. The nitrate and nitrite content of the non-oxidized samples were subtracted from the corresponding nitrogen content determined after photo-oxidation and the value compared with the Kjeldahl nitrogen content.     

Rapid determination of protein in plant material by flow injection spectrophotometry with trinitrobenzenesulfonic acid

The rapid determination of protein in plant material based on spectrophotometric determination of amino acids in protein hydrolysates with trinitrobenzenesulfonic acid has been adapted to flow injection analysis. With the manifold described, a routine sampling rate of 120 samples/h is possible, though this, as well as sensitivity, can easily be varied. The method was calibrated against the Kjeldahl method and a good correlation was obtained between the two methods over a wide range of protein values for beans.     

智能一体化蒸馏仪蒸馏-全自动流动注射分析仪测定底泥中挥发酚

采用碱液浸提底泥中挥发酚后,由于溶液浑浊,且存在干扰,若直接采用流动注射分析仪进行测定,极易堵塞仪器的管路,进而影响后续测定,故将提取液在酸性条件下加入硫酸铜于全自动智能一体化蒸馏器蒸馏,消除硫化物等的干扰,用全自动流动注射分析仪测定底泥中挥发酚。实验对磷酸、硫酸铜加入量、震荡时间、蒸馏功率和蒸馏体积进行了优化,并确定磷酸过量5mL,加入5g硫酸铜,震荡10min,蒸馏功率为50W,蒸馏重量设置为225g。标准曲线的线性关系良好,相关系数为0.999 9以上,样品和空白加标回收率在89.3%～103%,检出限为0.03mg/kg。实验方法测定底泥中挥发酚样品与传统分光光度法结果一致,不仅实现自动化,而且对环境和人均友好。     

Flow injection analysis : Part V. Simultaneous determination of nitrogen and phosphorus in acid digests of plant material with a single spectrophotometer

The rapid simultaneous determination of nitrogen and phosphorus in a single acid digest of plant material based on the Berthelot and phosphomolybdate colorimetric methods, respectively, has been adapted to Flow Injection Analysis with a dual-channel manifold. A routine sampling rate of 200 determinations per hour can be achieved with a single spectrophotometer; evidence is presented that 400 determinations per hour are possible with two spectrophotometers. The effect of sample volume on absorbance, and the methods of obtaining different proportions of sample split are discussed.