Rapid determination of dissolved organic phosphorus in soil leachates and runoff waters by flow injection analysis with on-line photo-oxidation

A rapid method suitable for the determination of dissolved organic phosphorus (DOP) in soil leachates and runoff waters is presented. The flow injection (FI) manifold contains an in-line PTFE reaction coil wrapped around a low power UV lamp and is based on the spectrophotometric determination of dissolved reactive phosphorus (DRP) and mineralised DOP at 690 nm after reduction of phosphomolybdate to molybdenum blue with tin(II) chloride. The linear range was 0-1.5 mg 1(-1) PO(4)-P, with a detection limit (3 s) of 7 mug 1(-1) and a sample throughput of 40 h(-1). Tolerance to potential matrix interferences in soil pore waters, particularly Al(III), Si(IV), Fe(II) and Fe(III), was achieved using a combination of on-line sample pre-treatment by a strong acid ion exchange column, low photoreactor pH and acid induced control of the kinetics of the molybdenum blue reaction. The results obtained with this manifold were in good agreement with those obtained by a batch spectrophotometric reference method.     

Determination of phosphorus in organic compounds: A new micro procedure

Summary A new micro procedure for the determination of phosphorus in organic compounds has been developed. It is based on the yellow complex produced by mixing ammonium vanadate, molybdate, and phosphate. The procedure is rapid, simple, and suited for series determinations; the reagents and the colored compounds are stable. A precision of ± 0.2% phosphorus is obtained with samples of 3 to 10 mg weight.

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Zusammenfassung Das beschriebene Mikroverfahren für die Phosphorbestimmung in organischen Substanzen beruht auf der photometrischen Auswertung des gelben Komplexes mit Vanadat und Molybdat. Es ist einfach, schnell, und für Serienbestimmungen geeignet. Die dafür nötigen Reagenzien sind gut haltbar, die gefärbte Verbindung ist beständig. Eine Genauigkeit von ± 0.2% Phosphor wird mit Probemengen von 3 bis 10 mg erhalten.

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Résumé On présente un micro-procédé de dosage du phosphore dans des composés organiques. Il repose sur le complexe jaune produit en mélangeant des vanadate, molybdate et phosphate d'ammonium. Le procédé est rapide, simple et convenable pour les dosages en série. Les réactifs et les composés colorés sont stables. Une précision de ± 0,2% sur le phosphore est obtenue avec des échantillons allant de 3 à 10 mg.

     

Determination of phosphorus in organic compounds by NMR

Summary A method is described for the microdetermination of phosphorus by FTNMR in organic compounds containing transition metals. Approximately 10 mg of compound is digested for the determination and 2 mg Cr added as relaxation agent.

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Zusammenfassung Eine Mikromethode zur Bestimmung des Phosphors in organischen, Übergangsmetalle enthaltenden Verbindungen mit Hilfe der Fourier-Transform P³¹ kernmagnetischen Resonanz wurde beschrieben. Ungefähr 10 mg Substanz werden mit Schwefelsäure-Perchlorsäure aufgeschlossen und 2 mg Cr^III werden als Relaxans zugegeben.

     

Extraction of soil organic phosphorus

Organic phosphorus is an important component of soil biogeochemical cycles, but must be extracted from soil prior to analysis. Here we critically review the extraction of soil organic phosphorus, including procedures for quantification, speciation, and assessment of biological availability. Quantitative extraction conventionally requires strong acids and bases, which inevitably alter chemical structure. However, a single-step procedure involving sodium hydroxide and EDTA (ethylenediaminetetraacetate) is suitable for most soils and facilitates subsequent speciation by nuclear magnetic resonance spectroscopy. Analysis of extracts by molybdate colorimetry is a potential source of error in all procedures, because organic phosphorus is overestimated in the presence of inorganic polyphosphates or complexes between inorganic phosphate and humic substances. Sequential extraction schemes fractionate organic phosphorus based on chemical solubility, but the link to potential bioavailability is misleading. Research should be directed urgently towards establishing extractable pools of soil organic phosphorus with ecological relevance.     

The photo-oxidation of solutions of arsenicals to arsenate: A convenient analytical procedure

The separation of arylarsonic acids by HPLC on a reverse-phase C₁₈ column is described. Solutions containing these arsenicals and others such as arsenobetaine are photo-oxidized to arsenate by ultraviolet (UV) radiation (1200 W, 1 h exposure). This allows the analysis of the solution for arsenic by hydride generation techniques. The method, UV HGAA, is developed and applied to the determination of arsenic in the methanol extracts of the Manila clam (Verupis japonica) and the Horse clam (Schizothoerus nutalli).     

An assessment of analytical performance of dissolved organic nitrogen and dissolved organic phosphorus analyses in marine environments: a review

To better understand the cycling of marine dissolved organic matter, analytical methods are required allowing for data on dissolved organic nitrogen and phosphorus (DON and DOP) to be acquired with high analytical performance. The coverage of documented DON and DOP analytical performance is very limited; instead analytical data are mostly available for total dissolved N and P (TDN and TDP) analyses. This substitution overestimates analytical performance for DON and DOP measurements due to the cumulative effect of Standard Deviation applied for detection limit and precision evaluations. The little available data obtained by photolytic, chemical, a combination of both, and high temperature combustion methods indicate that current detection limit is 0.30 µM for DON and 0.010 µM for DOP. Precision for both analytes, in general, is ≤4.5%. The data on accuracy is scarce despite availability of Reference Materials for TDN and NO₃^? + NO₂^? analyses, and for the TDN measurement is <5%; even fewer data exist for TDP due to a lack of reference material for this analysis. The Beer–Lambert law is linear up to 200 µM for TDN and 5–6 µM for TDP. Current analytical abilities for DON/DOP measurements are not ready yet to set the level of dissolved organic carbon analysis. The advance in the analytical performance for DON and DOP measurements depends upon the possibility to improve the analytical performance for dissolved inorganic N and P measurements involved in DON and DOP estimations. For the DOP analysis, an international standard method becomes necessary to develop and evaluate collaboratively. The chemical oceanographers’ community should reconsider requirements needed for the coverage of analytical performance for DON and DOP measurements to make this data more shareable and transparent. The lack of these data protracts marine analysts from attaining further methods improvement and development.     

Multi-pumping flow system for the determination of dissolved orthophosphate and dissolved organic phosphorus in wastewater samples

A multi-pumping flow system (MPFS) for the spectrophotometric determination of dissolved orthophosphate and dissolved organic phosphorus in wastewater samples is proposed. The determination of orthophosphate is based on the vanadomolybdate method. In-line ultraviolet photo-oxidation is employed to mineralise organic phosphorus to orthophosphate prior to detection. A solenoid valve allows the deviation of the flow towards the UV-lamp to carry out the determination of organic phosphorus.Calibration was found to be linear up to 20 mg P L⁻¹, with a detection limit (3s_b/S) of 0.08 mg P L⁻¹, an injection throughput of 75 injections h⁻¹ and a repeatability (R.S.D.) of 0.6% for the direct determination of orthophosphate. On the other hand, calibration graphs were linear up to 40 mg P L⁻¹, with a detection limit (3s_b/S) of 0.5 mg P L⁻¹, an injection throughput of 11 injections h⁻¹ and a repeatability (R.S.D.) inferior to 2.3% for the procedures involving UV photo-oxidation.     

Determination of a strong organic ligand dissolved in seawater: Thorium-complexing capacity of oceanic dissolved organic matter

Studies have been made of loose water tritium (LWT) distribution and behavior in the soil samples taken from the region within a radius of 2 km to the HWRR stack of CIAE. The analytical results show that the LWT concentrations in most soil samples of the region are in the range from 24.8 Bq/l (3.6 Bq/kg) to 116 Bq/l (16.0 Bq/kg) with an average value of 58.1±24.8 Bq/l (10.3±4.5 Bq/kg). There are two areas with a higher LWT content; the first one (4.61 · 10⁴ m²) is located near HWRR with ahighest LWT concentration of 287 Bq/l (55.8 Bq/kg) and the second one (3.27 ·10⁵ m²) is located near Lab. A with a highest LWT concentration of 2.35 · 10⁴ Bq/l (2.56 · 10³ Bq/kg). It is estimated that the LWT inventories deposited in soil of the two areas are about 1.52 · 10⁹ Bq and 1.42 · 10¹⁰ Bq, respectively. The analytical results have been evaluated by comparing the possible tritium intake of the human body with the annual limit of intake recommended by ICRP, it can be concluded that the operations of all the nuclear facilities releasing tritium in CIAE are safe without causing any notable tritium contamination.     

Determination of hydrochloric acid in organic solutions by gas chromatography

Summary A method is described for the determination of small quantities of hydrochloric acid in two chlorinated organic solvents (CHCl₃ and CCl₄). An excess of gaseous ethylene oxide is added to a liquid sample; the 2-chloroethanol formed is then analyzed by gas chromatography. The procedure is simpler and more sensitive in comparison with other conventional methods. It can be modified for other organic solvents.D.G.R.C.S.T. grant.     

Determination of trace amounts of phosphorus in organic compounds by wickbold combustion

Summary Wickbold combustion in a standard quartz apparatus with a suction burner is suitable for phosphorus determination in acetonesoluble materials if the samples are burned together with an organic halide, e. g. carbon tetrachloride. Probably phosphorus halides are formed which pass through the hot parts of the apparatus fast enough not to react with the quartz walls. The recovery is 95–100% for amounts of phosphorus up to 3.5 mg per combustion.

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Bestimmung von Phosphorspuren in organischen Verbindungen durch Wickbold-Verbrennung

Zusammenfassung Die Wickbold-Verbrennung in einer normalen Quarz-Apparatur mit Saugbrenner ist zur Phosphor-Bestimmung in acetonlöslichen Substanzen geeignet, wenn gleichzeitig mit den Proben eine organische Halogen-Verbindung, z. B. Tetrachlorkohlenstoff, verbrannt wird. Vermutlich werden dabei Phosphorhalogenide gebildet, die die heißen Zonen der Apparatur so schnell passieren, daß keine Reaktion mit den Quarzwänden stattfindet. Die Wiederfindungsrate für Phosphormengen bis 3,5 mg pro Verbrennung beträgt 95–100%.

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Presented at the 8th International Microchemical Symposium, Graz, August 25–30, 1980.     

气相色谱法测烟草中拟除虫菊酯和有机磷类农残

建立了一种测定烟草中拟除虫菊酯类农药和有机磷类农药残留量的气相色谱法.用普通的聚苯乙烯凝胶柱代替昂贵的凝胶渗透色谱仪;层析柱填料用弗罗里硅土代替硅胶;用工作标准溶液过柱曲线作为标准曲线;有机磷类农药气相检测器用PFPD代替FPD.方法的检测量为0.01μg/g～0.04 μg/g,平均加标回收率为70.18%～95.86%,RSD为4.36﹪～9.96﹪,对样品进行了拟除虫菊酯类农药和有机磷类农药残留量的测定,结果满意.     

Determination of total dissolved phosphorus in water samples by axial inductively coupled plasma atomic emission spectrometry

A procedure was developed to determine total dissolved phosphorus in groundwater-like samples using axial ICP-AES. Severe and peculiar matrix effects (strongly positive at lower and leveling off at higher matrix concentrations) in the presence of Na and Ca were observed. To reduce these matrix effects, a double approach was utilized consisting of a so-called minimum matrix in combination with an internal standard (Ga in this case). The ‘minimum matrix’ (small amounts of K, Mg and Na) was only added to the standard solution(s) used for the calibration. The detection limit for the whole procedure was 12 μg/L using the P213 nm line. Residual matrix effects were less than 3% (P213 nm line). Received: 21 February 1997 / Revised: 5 June 1997 / Accepted: 6 June 1997     

Determination of total dissolved phosphorus in water samples by axial inductively coupled plasma atomic emission spectrometry

A procedure was developed to determine total dissolved phosphorus in groundwater-like samples using axial ICP-AES. Severe and peculiar matrix effects (strongly positive at lower and leveling off at higher matrix concentrations) in the presence of Na and Ca were observed. To reduce these matrix effects, a double approach was utilized consisting of a so-called minimum matrix in combination with an internal standard (Ga in this case). The ‘minimum matrix’ (small amounts of K, Mg and Na) was only added to the standard solution(s) used for the calibration. The detection limit for the whole procedure was 12 μg/L using the P213 nm line. Residual matrix effects were less than 3% (P213 nm line). Received: 21 February 1997 / Revised: 5 June 1997 / Accepted: 6 June 1997     

Determination of cobalt in zinc electrolyte by an automated flow-injection system

A flow-injection method has been developed for the spectrophotometric determination of cobalt in zinc electrolyte using 2-(5-bromo-2-pyridylazo)-5-(N-propyl-N-sulphopropylamino)aniline (5-Br-PSAA) as chromogenic reagent. A sample solution is injected into a carrier containing hydrochloric acid, diammonium hydrogenphosphate and hydrogen peroxide. The sample is then merged with the stream of ammonium acetate solution and PSAA solution is synclonously injected into the sample zone. After mixing with 2M sulphuric acid, the absorbance of cobalt-PSAA complex is measured at 617 nm. The flow injection system proposed is fully controlled with a personal computer. The flow-injection system permits throughput of 12 samples per hour. The relative standard deviation (n = 10) for 0.1 mug Co/ml solution is 5.0%.     

气相色谱-火焰光度法测定土壤中有机磷农药残留

建立了气相色谱-火焰光度(GC-FPD)分析土壤中敌敌畏、氧化乐果、二嗪农、乐果、甲基对硫磷、马拉硫磷、对硫磷、水胺硫磷、喹硫磷等9种有机磷农药残留量的方法。样品用丙酮-二氯甲烷(1:3)提取,浓缩、定容后用Hp-5MS(30m×0.25 mm×0.25μm)毛细管柱分离,FPD检测器检测。方法回收率在68.71%～110.39%之间;RSD在5.5%～11%之间;检出限在0.397～1.60μg/mL之间,方法可用于环境土壤样品中有机磷农药残留的测定。