University of North Florida
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Stuart Chalk, Ph.D.
Department of Chemistry
University of North Florida
Phone: 1-904-620-1938
Fax: 1-904-620-3535
Email: schalk@unf.edu
Website: @unf

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Phosphorus

  • IUPAC Name: phosphane
  • Molecular Formula: P4
  • CAS Registry Number: 12185-10-3
  • InChI: InChI=1S/H2P/h1H2
  • InChI Key: XYFCBTPGUUZFHI-UHFFFAOYSA-N

@ ChemSpider@ NIST@ PubChem

Citations 113

"A Sequential Injection System For The In-line Digestion And Colorimetric Determination Of Phosphorus In Milk"
J. Food Sci. 2002 Volume 67, Issue 9 Pages 3280-3283
M.J. Reis Lima, S.M.V. Fernandes, A.O.S.S. Rangel

Abstract: A sequential injection analysis (SIA) system involving in-line digestion for the determination of total phosphorus in milk is presented. The developed manifold consists mainly of 2 phases: conversion of all forms of phosphorus into orthophosphates by hydrolysis and oxidation catalyzed by UV radiation (necessary for the efficient oxidation of organic phosphates) and spectrophotometric determination of the phosphomolybdenum blue formed. The proposed method was applied to several cow milk samples and the results were in good agreement with those provided by the reference method, with a maximum relative deviation of 5.2%. The detection limit of the method was around 2 mg P/L with a sampling rate of approximately 17 h-1.
Cow Spectrophotometry Sequential injection UV reactor Online digestion Method comparison

"Method Development For Measurement Of Elements In Hungarian Red Wines By Inductively Coupled Plasma Optical Emission Spectrometry (ICP-OES)"
Acta Aliment. 2000 Volume 29, Issue 2 Pages 105-122
Csiktusnádi-Kiss, G. A., Keszler, Á., Candeaias, M., Bronze, M. R., Boas, L. V., Spaugner, I.

Abstract: ICP-OES (inductively coupled plasma optical emission spectrometry) was used to determine the element content of red wines. Development of the method involves various procedures of sample handling as well as repeatability and reproducibility measurements. Measurements were made for the following 16 elements: Al, B, Ba, Ca, Cd, Co, Cr, Cu, Fe, K, Mg, Mn, Na, P, Sr and Zn. The relative standard deviation of repeatability ranged from 0.41% (potassium) to 27% (cadmium) and that of reproducibility varied between 0.73% (boron) to 52% (cobalt). Recovery of the elements was determined by standard addition with results ranging from 90.6% (phosphorus) to 116.2% (boron). After that, 15 red wine samples were measured. Significant differences were found in the Al, B, Ca, Co, Cr, Cu, Fe, K, Mg, Mn, Na, P, Sr and Zn (P<0.001) concentration of wine samples. Correlation studies revealed parallel changes in phosphorus-potassium, phosphorus-magnesium and zinc-manganese concentrations (r=0.857, 0.875, 0.838). According to principal component analysis, measurements of zinc-, sodium-, boron-, copper- and strontium content gave almost the same results as obtained with 16 different elements. According to a two dimensional non-linear map of absolute values of principal component analysis, wines from Szekszard and Eger could be differentiated, whereas the analysis of wines from Villany, the Matra Mountains and Lake Balaton showed overlapping results.
Wine Red Spectrophotometry Volatile generation Standard method

"Flow Injection Analysis. 2. Ultra Fast Determination Of Phosphorus In Plant Material By Continuous-flow Spectrophotometry"
Anal. Chim. Acta 1975 Volume 79, Issue 1 Pages 79-91
J. Rika and J. W. B. Stewart

Abstract: The effect of sample volume, tube length, tube diameter, peak height and sampling rate on the determination of P in acidic plant digests was investigated, and optimal conditions for the flow injection method were described. Sampling rates of 420 samples/hr were achieved without incurring problems from carryover of samples, and evidence was obtained that rates ≤700 samples/hr were possible. The flow injection method was proved to be suitable for routine analyzes.
Plant Kidney Sample preparation Spectrophotometry Optimization

"Merging Zones In Flow Injection Analysis. 4. Simultaneous Spectrophotometric Determination Of Total Nitrogen And Phosphorus In Plant Material"
Anal. Chim. Acta 1980 Volume 119, Issue 2 Pages 305-311
B. F. Reis, E. A. G. Zagatto, A. O. Javcintho, F. J. Krug and H. Bergamin F

Abstract: 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.
Plant Spectrophotometry Merging zones Proportional injector Simultaneous analysis

"Determination Of Some Phosphorus-containing Compounds By Flow Injection With A Molecular Emission Cavity Detector"
Anal. Chim. Acta 1985 Volume 170, Issue 2 Pages 331-336
J. L. Burguera, M. Burguera and Daniel Flores

Abstract: Optimum conditions (e.g., flow rate, sample volume, dimensions of the tubing and flame composition) have been established for the determination of P-containing inorganic and organic compounds by the cited technique. The ranges of rectilinear response, detection limits and coefficient of variation (typical values being 10 to 200 ng, 2.5 and 3%, respectively) are tabulated for H3PO4, H3PO3, H3PO2, trimethyl phosphite, triethyl phosphite and tributylphosphine; sensitivity improved with decreasing O content of the compounds. The sample throughput was 20 h-1. As peaks were well separated, components of ternary mixtures could be determined.
Spectrophotometry Spectrophotometry Optimization

"Determination Of Phosphorus In Biological Tissues By Aluminum Block Digestion And Flow Injection Spectrophotometry"
Anal. Chim. Acta 1988 Volume 209, Issue 1 Pages 299-302
W. Maher, D. Lambert, J. Furlonger and P. Cullen

Abstract: The sample (0.1 g dry wt.) was digested with concentrated HNO3 (5 ml) at room temperature for 12 h and then with HClO4 (0.5 ml) with heating just until fuming, and the solution was diluted to 25 mL with water. The P was determined at 413 nm as the molybdovanadophosphate complex by using the flow injection system described by Royset (Ibid., 1985, 178, 217). The response was rectilinear up to 5 µg mL-1 (200 µL injection) and the limit of detection was 0.3 µg mL-1. Recoveries were 96% and the coefficient of variation (n = 10) for 1 and 25 µg mL-1 of P in standards taken through the entire procedure were 0.7 and 0.4%, respectively. Matrix interference was negligible. The results for seven standard reference materials were in agreement with certified values.
Biological tissue Clinical analysis Spectrophotometry Interferences Online digestion Reference material Tecator

"Spectrometric Determination Of Phosphorus In River Water Based On The Reaction Of Vanado-molydophosphate With Malachite Green"
Anal. Chim. Acta 1988 Volume 211, Issue 1 Pages 119-127
Shoji Motomizu, Mitsuko Oshima and Atsushi Hirashima

Abstract: The formation of an ion-associate between vanadomolybdophosphate and malachite green in aqueous acidic solution (0.5 M sulfuric acid) enables trace amounts (0-1 x 10^-5M) of phosphate to be determined. The molar absorptivity is 1.05 x 10^5 l mol-1 cm-1 at 620 nm. The complex was stabilized in solution by adding poly (vinyl alcohol). Other ions generally found in river waters did not interfere. Interference by silicate is less than that found in the corresponding malachite green molybdophosphate procedure; interference of arsenate is avoided by reduction with thiosulfate. The method is applied to the determination of µg L-1 amounts of phosphorus in river water; the results obtained were in good agreement with those obtained by an extraction-spectrophotometric method with malachite green.
River Spectrophotometry

"Rapid Spectrophotometric Determination Of Total Phosphorus In Industrial Wastewaters By Flow Injection Analysis Including A Capillary Digestor"
Anal. Chim. Acta 1988 Volume 214, Issue 1-2 Pages 229-237
M. Aoyagi, Y. Yasumasa and A. Nishida

Abstract: Sample solution in water (as carrier) merged with oxidizing agent (K2S2O8 in H2O) before passing to a digestion unit consisting of 10 m of PTFE tubing holding 10 m of platinum wire (0.2 mm diameter) wound round an aluminum bobbin and heated to 160°C. The solution then mixed sequentially with reducing agent (aqueous 5% Na2S2O3) and color-forming reagent [aqueous malachite green (C. I. Basic Green 4) and (NH4)6Mo7O24.4H2O in ~15% H2SO4] and the absorbance was measured at 650 nm. Calibration graphs were rectilinear for up to 500 ng mL-1 of P and the determination limit was 2 ng mL-1. The coefficient of variation (n = 5) at 200 and 2 ng mL-1 were 0.3 and 6.0%, respectively. Recoveries were quantitative. The method was applied to determine P in industrial waste water and seawater; results agreed with those from the standard procedure.
Sea Waste Water Spectrophotometry Sample preparation Calibration Catalysis Online digestion Heated reaction Standard method

"Flow Injection Technique For The Determination Of Low-levels Of Phosphorus In Natural Waters"
Anal. Chim. Acta 1990 Volume 234, Issue 2 Pages 409-416
Paul R. Freeman, Ian D. McKelvie and Barry T. Hart, Terence J. Cardwell

Abstract: A flow injection instrument for determining low concentration. of P in waters is described and illustrated. The main feature is the use of an inexpensive detector consisting of a flow cell and a photometer that incorporates a super-bright red-light emitting diode as the source and a photodiode as the detector. The procedure is a modification of the tin(II) chloride - molybdate method (cf. Tecator Application Note ASN 60-01183, Tecator AB, 1983) optimized by a modified simplex optimization method. Silicate interference (5 mg mL-1) was removed by addition of aqueous 0.1% tartaric acid. The calibration graph was rectilinear up to 100 µg L-1 of P and the detection limit was 0.6 µg l-1. The coefficient of variation were 2.9% and 0.5% for 2.0 and 50 µgl-1 of P, respectively. An inline pre-concentration anion-exchange column was used to obtain a lower detection limit of 0.1 µg l-1.
Environmental Spectrophotometry Detector Flowcell Calibration Detection limit Preconcentration Column Light emitting diode Simplex Interferences Photodiode Optimization

"Intelligent Flow Injection Inductively Coupled Plasma System For Matrix Matching"
Anal. Chim. Acta 1990 Volume 234, Issue 1 Pages 207-212
M. F. Gin&eacute;, H. Bergamin, B. F. Reis and R. L. Tuon

Abstract: Estuarine waters of varying salinity were analyzed by a flow injection analysis system, with ICP-AES detection of Ca, Mg, Al, Fe, P and Si. The sampling zone approach was used to balance the salt content of samples and standards in order to compensate for matrix effects. This matching was achieved automatically by processing the sample Na signal with a microcomputer and adding Na+ as necessary. The matrix-matching procedure and the decision process are discussed. Interference by Na+ was thus minimized, allowing analysis of samples containing 2.5% of NaCl. The sampling rate was 60 h-1. Recoveries were >96%.
Estuarine Spectrophotometry Interferences

"Determination Of Total Phosphorus In Waters With Amperometric Detection By Coupling Of Flow Injection Analysis With Continuous Microwave Oven Digestion"
Anal. Chim. Acta 1990 Volume 236, Issue 2 Pages 345-350
S. Hinkamp and G. Schwedt

Abstract: In the manifold (illustrated) of a FIAstar 5020 flow injection analyzer., the sample is injected into a carrier stream of 5 mM H2SO4 (pH 2), which is mixed with 0.06 M HClO4 as decomposing solution before passing through a coil within a microwave oven operated at 650 W. The stream is passed through a gas diffusion unit to remove bubbles before merging with acidic molybdate solution [10 g L-1 of (NH4)6Mo7O24.4H2O and 35 mL L-1 of concentrated H2SO4] and reaction in a coil. The product was reduced to molybdenum blue in an amperometric detector incorporating a vitreous-carbon electrode in wall-jet configuration maintained at +0.26 V vs. Ag - AgCl (3 M KCl). Response based on peak height was rectilinear up to 30 mg L-1 of P, and the detection limit was 0.1 mg L-1 in standard solution The coefficient of variation (n = 5) was 3% at 5 mg L-1 of P. The method gave recoveries ranging from ~63% for pyrophosphate to 91 to 98% for various organic P compounds added to domestic waste water.
Waste Amperometry Electrode Sample preparation Gas diffusion Tecator Microwave Online digestion

"Monitoring And Control Of Biological Removal Of Phosphorus And Nitrogen By Flow Injection Analyzers In A Municipal Pilot-scale Waste-water Treatment Plant"
Anal. Chim. Acta 1990 Volume 238, Issue 1 Pages 191-199
K. M. Pedersen, M. K&uuml;mmel and H. S&oslash;eberg

Abstract: The flow injection system monitors the concentration. of NH4+, NO3- and PO43- in four places: in the inlet, in the outlet of the anaerobic pretreatment tank, in one of the aeration tanks and in the outlet of the plant. Sampling is carried out via a cross-flow filter system, based on an ultra-filtration membrane. The analyzer.s employ highly pulsating, single-piston LC pumps. Synchronization of injection time and pump pulses eliminates the need for pulse-damping devices and ensures high reproducibility. The chemical methods are based on classical colorimetric methods. Design emphasis is on long-term stability, low reagent consumption and minimum maintenance.
Waste LC Spectrophotometry Filter Membrane Pulse dampener Reagent consumption

"Dual Flow Injection Analysis System For Determining Bromide And Reactive Phosphorus In Natural Waters"
Anal. Chim. Acta 1993 Volume 282, Issue 2 Pages 379-388
Paul R. Freeman, Barry T. Hart and Ian D. McKelvie

Abstract: A computer-controlled injection system (description given) and a manifold constructed from PTFE tubing were used in the simultaneous determination of P and bromide by methods based on previously published methods (cf. Ibid., 1990, 234, 409; and Anagnostopoulou and Koupparis, Anal. Chem., 1986, 58, 322). The bromide was determined first by injecting a sample (60 µL) into a stream of water (0.75 ml/min) which was mixed (0.31 ml/min) with 2.4 mM HCl in a 30 cm coil before removal of dissolved organic matter in a PVC column (2 cm x 2.8 mm i.d.) containing Sep-Pak C18. Streams (0.31 ml/min) of 0.01 or 0.02 g/l of phenol red, e.g., in 50 mM acetate buffer, and chloramine T, were mixed in a 60 cm coil before mixing with the column eluate in a 43 cm coil and detection at 583 nm. To determine P, a sample (600 µL) was injected into a stream of water (1.2 ml/min) and mixed with acid molybdate and SnCl2 streams (0.54 ml/min) in 30 and 120 cm coils, respectively, before detection at 650 nm. Calibration graphs were linear up to 2 mg/l of bromide and 50 µg/l of P and the detection limits were 4 and 0.6 µg/l, respectively. The corresponding RSD ranged from 0.3-5.3 (n = 10) and 0.5-2.9% (n = 3).
Environmental Spectrophotometry Computer Buffer

"Determination Of Total Phosphorus In Waters And Waste Waters By Online Microwave-induced Digestion And Flow Injection Analysis"
Anal. Chim. Acta 1994 Volume 291, Issue 3 Pages 233-242
Richard L. Benson*, Ian D. McKelvie and Barry T. Hart, Ian C. Hamilton

Abstract: Digestion was performed using a flow-through reactor in a modified domestic microwave oven and the orthophosphate formed was detected as phosphomolybdenum blue after online filtration. Different digestion mixtures were evaluated and a 10 g/l acidified solution of potassium peroxydisulfate was selected. Phosphorus standards or unfiltered effluent samples were continuously mixed online with the digestion reagent and the solution was passed through the microwave reactor. A 30 µL portion of the solution was injected into a water carrier stream via a PTFE rotary valve, and sequentially merged with a further water carrier stream, the colorimetric reagent and the reducing reagent. The transmittance was monitored by a solid-state photometer incorporating red a light-emitting diodes (635 nm). The technique was rapid (7 samples/h, 4 replicates). The calibration graph was linear upto 18 mg/l of P with a detection limit of 0.09 mg/l.
Environmental Waste Sample preparation Microwave Online digestion Filter Light emitting diode

"Determination Of Phosphorus In Aqueous Solution Via Formation Of The Phosphoantimonylmolybdenum Blue Complex Re-examination Of Optimum Conditions For The Analysis Of Phosphate"
Anal. Chim. Acta 1995 Volume 302, Issue 1 Pages 69-74
L. Drummond and W. Maher*

Abstract: This paper describes an investigation of the conditions affecting the determination of phosphate using the reduced phosphoan-timonylmolybdic acid method. The aim was to develop a determination method with faster kinetics than the original procedure of Murphy and Riley, for automation using flow-injection analysis. Optimum color formation was found to occur at [H+]/[MoO2-4] ratios between 50-80 at all pH values tested (0.36-1.06). The maximum rate of formation occurs at a [[H+]/[MoO42-]] ratio of 70 within a pH range of 0.57-0.88 when an antimony concentration greater than 0.06 mM and ascorbic acid concentration greater than 0.009 M in the final solution are used. Full color development occurs within 0.8-1 min. The ascorbic acid reagent was found to be stable for 30 days. The results of the study indicated that by suitable selection of reagent conditions, rapid chromophore development can be achieved.
Spectrophotometry Kinetic Optimization Complexation

"Determination Of Phosphorus In Turbid Waters Using Alkaline Potassium Peroxodisulphate Digestion"
Anal. Chim. Acta 1995 Volume 315, Issue 1-2 Pages 123-135
L. Woo and W. Maher*

Abstract: The evaluation of the use of alkaline peroxodisulphate digestion with autoclaving or microwave heating for the determination of total phosphorus in turbid lake and river water is described. Procedures were evaluated by the analysis of suspensions (20, 50 and 100 g P/l) of two standard reference materials, National Institute of Environmental Science, Japan No. 3 Chlorella and No. 2 Pond Sediment. Suspensions were prepared by adding these materials to distilled deionized water (pH 6) and homogenisation using shaking, sonification and stirring. Best recoveries of phosphorus were found when the final solution was 0.045 M in potassium peroxodisulphate and 0.04 M in sodium hydroxide and solutions digested in an autoclave at 120°C for 60 min. or heated in a microwave oven at 450 W for 10 min. Complete recoveries of phosphorus (99-103%) from 20, 50 and 100 g P/l Chlorella suspensions were obtained using both autoclave and microwave heating. For the Pond Sediment complete recoveries of phosphorus (99-107%) from the 20 and 50 g P/l suspensions were obtained using both heating methods. Higher recoveries from the 100 g P/l Pond Sediment suspensions were obtained using microwave heating (96 ± 1%) than autoclaving (88 ± 5%). Recoveries of phosphorus compounds (phosphates, and phosphonates) added to distilled deionized water and turbid lake water were near quantitative (91-117%) for both digestion procedures. Further analysis of Pond Sediment suspensions showed that complete recovery of phosphorus (98 ± 1%) from 60 g/l suspensions was achieved with incomplete recoveries (92.3 ± 0.7%, 91 ± 2% and 91 ± 1%) from 70 g P/l, 80 g P/l and 90 g P/l suspensions respectively. Comparison with the APHA-AWWA WPCF, nitric-sulphuric acid digestion method showed no difference in phosphorus measurements for the microwave procedure but that the autoclave procedure gave significantly lower recoveries of phosphorus (p < 0.01), however, differences were only 2-8%.
NIES 2 NIES 3 Pond Lake River Sample preparation Sample preparation Reference material Method comparison

"Use Of Immobilized 3-phytase And Flow Injection For The Determination Of Phosphorus Species In Natural Waters"
Anal. Chim. Acta 1995 Volume 316, Issue 3 Pages 277-289
I. D. McKelvie*, B. T. Hart, T. J. Cardwell and R. W. Cattrall

Abstract: A proportion of dissolved organic phosphorus (DOP) compounds found in natural waters may be utilized by algae and bacteria through hydrolysis by extracellular phosphomonoesterases such as alkaline phosphatase. The fraction of DOP remaining unhydrolyzed may consist of organic phosphorus species such as myo-inositol hexakisphosphate (phytic acid), and comprise part of the pool of biologically unavailable or even refractory DOP. Of this bio-unavailable DOP fraction, a major portion is amenable to hydrolysis by 3-phytase, a phosphohydrolytic enzyme which is not found widely in aquatic systems. This paper describes the development and application of a flow injection system which utilises immobilized 3-phytase for the determination of phytase hydrolyzable phosphorus (PHP) present in natural waters. The product of enzymatic hydrolysis is orthophosphate, and a conventional phosphomolybdenum blue detection method was used. The use of a suitable flow injection manifold and a multiple linear regression calibration procedure for quasi-simultaneous determination of phytase-hydrolysable and dissolved reactive phosphorus (DRP) coexisting in natural waters is outlined. The proposed technique is rapid (ca. 40 injections h-1), sensitive and reproducible, and the immobilized phytase exhibited good operational and storage stability over a period of several months.
Environmental Immobilized enzyme

"Sequential Analyte Removal In Flow-analysis Determination Of Nitrogen, Phosphorus And Potassium In Fertilizers"
Anal. Chim. Acta 1995 Volume 317, Issue 1-3 Pages 239-245
Patricia Benedini Martellia, Jos&eacute;Anchieta Gomes Netoa, Elias Ayres G. Zagattoa,*, Sandra M. Boscolo Brienzab, M. Concei&ccedil;&atilde;o B. S. M. Montenegrob and Jos&eacute;Luis F. Costa Limab

Abstract: A new approach for multiparametric determinations in now analysis based on successive sequestering of analytes is proposed and exemplified in the determination of water soluble nitrogen, phosphorus and potassium in fertilizers. The analytes are partially and reproducibly removed from the sample zone in the main stream towards specific analytical channels without significant alterations in the flowing sample plug. By using gas diffusion, dialysis and asymmetric stream splitting, ammonium, potassium and orthophosphate ions are stripped out and determined by flow potentiometry, flame photometry and spectrophotometry, respectively. The system permits up to 75 samples to be examined per hour, requires 90 mg tris(hydroxymethyl)aminomethane plus 75 mg ammonium heptamolybdate tetrahydrate plus 75 mg ascorbic acid per sample, and yields reproducible results (RSD usually < 3%) in agreement with usual manual procedures. The feasibility of an analogous modular system with a random selection of procedures is discussed. (17 References)
Commercial product Spectrophotometry Spectrophotometry Potentiometry Gas diffusion Sample splitting Dialysis

"Model Compounds For The Determination Of Organic And Total Phosphorus Dissolved In Natural Waters"
Anal. Chim. Acta 1996 Volume 318, Issue 3 Pages 385-390
Roger K&eacute;rouel and Alain Aminot*

Abstract: Methods for the determination of organic and total P in natural waters based on the hydrolysis and oxidation of all complexed forms of P to phosphate by acidic and alkaline persulfate oxidation, continuous-flow UV irradiation and high temperature combustion (HTC) were studied. Ten compounds were used to test the efficiency of these hydrolysis/oxidation reactions. The results indicated that in such methods, recoveries should be tested using model compounds with HTC as the reference method. One labile compound (phosphoenolpyruvate, glycerophosphate or riboflavin-5-phosphate) and one refractory compound (aminoethylphosphonic acid, phytic acid or phosphorylcholine) should be used to determine an upper and lower recovery, respectively. The recoveries depended on the matrix; quantitative recoveries were obtained with fresh water but not with seawater. For the determination of P in seawater the alkaline persulfate oxidation method is recommended.
Sea Environmental Environmental

"Determination Of Total Phosphorus In Waters And Waste Waters By Online UV/thermal Induced Digestion And Flow Injection Analysis"
Anal. Chim. Acta 1996 Volume 326, Issue 1-3 Pages 29-39
Richard L. Benson*, Ian D. McKelvie, Barry T. Hart, Yen B. Truong and Ian C. Hamilton

Abstract: The online FIA method utilized a two-stage UV photo-oxidation/thermal digestion procedure and oxidizing/hydrolyzing reactions to convert phosphorus compounds to orthophosphate for detection by the phosphomolybdenum blue reaction. A sample stream (0.69 ml/min) was merged with 6 g/l ammonium peroxydisulfate in 2.1 M perchloric acid (0.69 ml/min) and passed through a UV digestor (8 W) and a thermal digestor at 90°C. A 60 µL portion of the digestate was injected into a water carrier stream (1.24 ml/min) and sequentially merged with a water diluent (0.58 ml/min), 10 g/l ammonium molybdate in 35 ml/l H2SO4 (0.86 ml/min) and 0.2 g/l tin(II) chloride/2 g/l hydrazinium sulfate in 28 ml/l H2SO4 (0.58 ml/min). The transmittance of the mixture was monitored with a solid-state photometer equipped with a red light-emitting diode (635 nm) and an optical path of 0.8 mm. The method was validated with a series of organic and condensed phosphorus species at concentrations of 10 mg/l; recoveries of >85% were obtained. The calibration graph was linear for 0.5-18 mg P/l and the detection limit was 0.15 mg/l. The sample throughput was 8 samples/h. The method was applied to waste water and the results were confirmed by a conventional batch digestion method.
Environmental Waste Spectrophotometry Sample preparation Light emitting diode UV reactor Photochemistry

"Elimination Of The Schlieren Effect In The Determination Of Reactive Phosphorus In Estuarine Waters By Flow Injection Analysis"
Anal. Chim. Acta 1997 Volume 351, Issue 1-3 Pages 265-271
Ian D. McKelvie*, Darren M. W. Peat, G. Peter Matthews and Paul J. Worsfold

Abstract: Conventional flow injection manifolds with sample injection for the determination of reactive phosphorus in estuarine waters are limited by the Schlieren or refractive index (RI) effect which can cause major errors in quantification. A simple flow injection (FI) manifold which obviates this RI error in reactive phosphorus measurement is reported. It involves the injection of acidic molybdophosphate reagent into a carrier stream of sodium chloride solution of similar refractive index, which is then sequentially merged with a sample (the salinity of which may vary widely from sample to sample) and a reductant. Despite the occurrence of sizeable blank signals, reactive phosphorus has been successfully measured in samples with salinities ranging from 0 to 34 parts per thousand using calibration standards prepared in deionised water, with a detection limit of 6 µg L-1 P. 21 References
Estuarine Refractive index Portable Optimization

"Affinity Enzymometric Assay For Detection Of Organophosphorus Compounds"
Anal. Chim. Acta 1997 Volume 357, Issue 1-2 Pages 13-20
Alexander Makower, Anatoli Barmin, Tatjana Morzunova, Arkadi Eremenko, Ilya Kurochkin, Frank Bier and Frieder Scheller*

Abstract: A new method for the detection of organophosphorus compounds has been developed. Organophosphorus compounds are recognized by binding of an excess of bienzyme conjugate (BEC) built up by butyrylcholinesterase as a receptor and horseradish peroxidase as the signal generating and amplifier element. The separation of the analyte-free bienzyme conjugate from the analyte-loaded bienzyme conjugate is performed on an affinity support formed by a Langmuir film containing an amphiphilic paraoxon derivative (B1). The analyte-free bienzyme conjugate binds irreversibly to the affinity support. Bienzyme conjugate with bound analyte is prevented from binding to the B1 film modified support and can thus be detected in the eluate solution by the horseradish peroxidase activity. This activity is directly proportional to the concentration of organophosphorous compounds. The assay procedure was developed for both the steady-state and the flow-injection mode. In both cases the lower limit of detection was about 1 pM for diisopropylflurophosphate.
Enzyme

"A Polyvalent Flow Injection System For Multielemental Spectrophotometric Analysis Of Plant Materials"
Anal. Chim. Acta 1998 Volume 370, Issue 1 Pages 39-46
F. V. Silva, A. R. A. Nogueiraa,*, G. B. Souzaa and E. A. G. Zagattob

Abstract: A polyvalent flow injection system consisting of a single manifold suitable to perform different determinations after only minor adaptations was conceived. Its use is particularly attractive for labs. processing a large number of samples including several analytes. The system was applied to spectrophotometric determination of iron, copper, manganese and zinc (micronutrients) as well as calcium, magnesium and phosphorus (macronutrients) in plants. With the proposed system, slight variations in the coefficients of the calibration equations (usually <3%) were found after 4 h working periods. Results were precise (0.8% Plant Spectrophotometry Reference material Optimization

"Sample Preparation In Sequential Injection Analysis. Spectrophotometric Determination Of Total Phosphorus In Food Samples"
Anal. Chim. Acta 1998 Volume 371, Issue 1 Pages 57-62
Cl&aacute;udio Celestino Oliveiraa, Elias Ayres Guidetti Zagattoa,*, Alberto N. Ara&uacute;djob and Jos&eacute; Luis F. Costa Limab

Abstract: A sequential injection (SI) procedure involving inline sample preparation is proposed. A natural suspension or a slurry is transported together with nitric acid towards a home-made digestion bomb placed inside a microwave oven for subsequent digestion. The sample zone is stopped inside the oven and, after digestion, directed in reverse flow towards a holding coil and then towards detection. This is a good strategy because the SI system is versatile; the formed air bubbles are efficiently disposed of, thus avoiding the need for a debubbler unit, and the digestion bomb acts also as a mixing device promoting easy homogenization regardless of the number of required reagents. As application, the spectrophotometric determination of total phosphorus in foodstuffs based on the molybdenum blue method was selected. The proposed system is very robust and yields reproducible measurements, (RSD usually <3%) for 20.0-400.0 mg L-1 P-PO4. Results are in agreement with a conventional spectrophotometric procedure involving manual sample digestion.
Food Spectrophotometry Sample preparation Microwave Online digestion Method comparison Sequential injection

"Procedures For The Storage And Digestion Of Natural Waters For The Determination Of Filterable Reactive Phosphorus, Total Filterable Phosphorus And Total Phosphorus"
Anal. Chim. Acta 1998 Volume 375, Issue 1-2 Pages 5-47
W. Maher* and L. Woo

Abstract: A review, with 150 references, is given. An overview of the forms of P species likely to be encountered in natural waters and the implications for the measurement of filterable and total P is given. Procedures reported in the literature for the storage and digestion of water samples for filterable reactive P (FRP), total filterable P (TFP) and total P (TP) measurements are summarized and the advantages and limitations of methods discussed. Water samples for FRP and TFP measurements need to be filtered immediately on collection as exchange on and off particles may occur in the sample container. Slow freezing of filtered or turbid water samples in acid washed low density polyethylene bottles appears to be satisfactory for the long term storage (years) of a variety of water sample types. Storage of water samples at room temperature or refrigeration (1-5°C) with a preservative is suitable only for short term storage (days-months). If water samples contain <20 µg P/L, adsorption to containers may be significant. Batch digestion of samples with alkaline or acid peroxodisulfate using autoclave or microwave heating offers the advantages of ease, simplicity and precision. Good recoveries of P from a range of P compounds containing P-O-P, C-O-P and C-P bonds expected in natural waters have been reported. If turbid samples are to be analyzed, caution must be exercised to ensure that the C or suspended solids concentration. does not exceed the capacity of the digestion procedure to oxidize the C present and release occluded P from particulate materials. Better recoveries of P from turbid water samples are achieved using microwave heating with closed vessels, probably because of the higher temps. and pressures generated. The use of online heating (microwave, thermal induced) coupled with flow injection analysis and using peroxodisulfate or an oxidizing acid mixture should also allow the automation of TFP and TP measurements. Reliable procedures for the removal of unwanted particulate material prior to or after the digestion step need to be developed.
Water Environmental Waste Sample preparation Review

"Speciation Of Dissolved Phosphorus In Environmental Samples By Gel Filtration And Flow Injection Analysis"
Talanta 1993 Volume 40, Issue 12 Pages 1981-1993
I. D. McKelvie* and B. T. HartT. J. Cardwell and R. W. Cattrall,

Abstract: Water (0.6 ml) was chromatographed on columns (10 cm x 1 cm i.d.) of Fast Desalting Sephadex G25, with a mobile phase (1.2 ml/min) of Tris hydrochloride of pH 4.65 (I = 0.005M). Sediments were extracted with 25 mM borate buffer of pH 9.2, the extracts were filtered and diluted (1:9). Portions (0.35 ml) of these solution were chromatographed on columns (4.2 cm x 1 cm i.d.) of Sephadex G25 Superfine, with the same mobile phase (0.65 ml/min). These columns partially separated high-mol.-wt. P compounds (exemplified by phytic acid, I) from low-mol.-wt. P compounds (exemplified by phosphate, II). The column effluent was mixed with 148 mM potassium persulfate solution in 25 mM borax (1.2 ml/min) and P compounds were oxidized by exposure to UV radiation. Subsequent reagents, 8.1 mM ammonium molybdate in 0.63 M H2SO4 (1 ml/min) and 0.89 mM SnCl2 and 15 mM hydrazine sulfate in 0.5 M H2SO4 (0.7 ml/min) were mixed in separately and absorbances were measured at 690 nm. Calibration graphs were linear for 100-1000 and 10^-100 µg/l of P with detection limits for I and II for the lower range were 27 and 1.1 µg/l as P.
Environmental Water Spectrophotometry Sample preparation Speciation Filtration Extraction

"High-sensitivity Flow-based Analysis System Using A Semiconductor Laser And Thin Long Flow-through Cell For The Determination Of Total Phosphorus In Water"
Talanta 1996 Volume 43, Issue 9 Pages 1471-1479
Takashi Korenagaa,* and Fusheng Suna

Abstract: A flow-through cell with an optical pathlength of 10 cm machined from a 2.5 cm diameter PTFE rod (details given) was used in conjunction with a GaAlAs semiconductor laser source (emission wavelength 793 nm) and a Hamamatsu model S1087-01 photodiode detector. A light-emitting diode (Toshiba model TLS143) and a second photodiode were used to generate a reference signal. In the flow injection determination of P in water, a 300 µL portion of sample was injected into a stream of 0.3% K2S2O8 solution (600 µL/min) and the resulting mixture was passed through a reaction coil (10 m x 1 mm i.d.) at 140°C and then mixed with color reagent prepared by mixing 7.2% ascorbic acid solution with with 0.048% antimony potassium tartrate hemihydrate/1.2% ammonium molybdate tetrahydrate solution in 8% H2SO4 in the ratio 1:5. The mixture was passed through a second reaction coil (10 m x 1 mm i.d.) at 140°C and then into the detector cell. The calibration graph was linear for 1-50 µg/l of P, and for 20 µg/l of P the RSD was 1% (n = 10). The limit of detection was 0.6 µg/l and recoveries of various P compounds were 94-107%. The method was applied to eight samples of waste water, 18 samples of treated water and five samples of natural water; the results agreed with those obtained by an official method.
Environmental Waste Environmental Spectrophotometry Light emitting diode Photodiode

"Rapid Determination Of Dissolved Organic Phosphorus In Soil Leachates And Runoff Waters By Flow Injection Analysis With Online Photooxidation"
Talanta 1997 Volume 45, Issue 1 Pages 47-55
D. M. W. Peata, I. D. McKelvieb, G. P. Matthewsa, P. M. Haygarthc and P. J. Worsfolda,*

Abstract: 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 inline 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 L-1 PO4-P, with a detection limit (3s) of 7 µg L-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 online sample pretreatment 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.
Leachates Environmental Ion exchange Spectrophotometry Photochemistry Interferences Kinetic Method comparison UV reactor

"Rapid Determination Of Nitrogen, Phosphorus And Potassium In Fertilizers By Flow Injection Analysis"
Analyst 1977 Volume 102, Issue 1219 Pages 714-722
E. H. Hansen, F. J. Krug, Animesh K. Ghose and J. Ruzicka

Abstract: Nitrate, K, phosphate, and NH3 were determined in fertilizers by flow injection analysis of samples of 30 µL (and as low as 5 µL) using potentiometric and spectrophotometric detection; 85-120 samples per h were analyzed with high reproducibility and low reagent consumption. The results agreed well with those obtained by the fertilizer manufacturers by conventional techniques. Based on the flow injection technique and routinely using sample injections of 30 µL, and as low as 5 µL, reliable and sensitive methods for the determination of nitrate, potassium, phosphate and ammonia in fertilisers are described in which potentiometric and spectrophotometric detection is used. At sampling rates of 85-120 samples per hour high reproducibility of measurement and low reagent consumptions were achieved. The good agreement between the results obtained with the flow injection methods and those attained by the manufacturer of the fertilisers with conventional techniques shows that flow injection analysis is potentially suitable for the routine analysis of these and similar substrates.
Commercial product Electrode Electrode Potentiometry Spectrophotometry Method comparison

"Spectrophotometric Determination Of Dissolved Organic Phosphorus In Natural Waters Using Inline Photo-oxidation And Flow Injection"
Analyst 1989 Volume 114, Issue 11 Pages 1459-1463
Ian D. McKelvie, Barry T. Hart, Terence J. Cardwell and Robert W. Cattrall

Abstract: The method involves mixing of the sample (100 or 600 µL) in a water carrier stream (1.3 mL min-1) with a solution (1.3 mL min-1) of K2S2O8 (4%) and NaBH4 (3.4%) and irradiation in a UV source. The mixture is debubbled and mixed with a solution (0.5 mL min-1) of 8.1 mM ammonium molybdate in 0.63 M H2SO4, and passed through a coil (30 cm x 0.5 mm), and this mixture is then mixed with a solution (0.36 mL min-1) of 0.89 mM SnCl2 and 15 mM hydrazine sulfate in 0.5 M H2SO4 and passed through a coil (60 cm x 0.5 mm), and a debubbler. Finally, detection is at 690 nm. The calibration graph is rectilinear for 6 mg L-1 of such P, and the detection limit is 10 µg l-1. Recoveries were 97.6 to 100.2%. About 50 and 72 samples h-1 could be analyzed for 0.1 and 0.1 to 4 mg l-1, respectively.
Environmental Spectrophotometry Debubbler Photochemistry UV reactor

"Rapid Differential Flow Injection Of Phosphorus Compounds In Wastewater By Sequential Spectrophotometry And Inductively Coupled Plasma Atomic Emission Spectrometry Using A Vacuum Ultraviolet Emission Line"
Analyst 1990 Volume 115, Issue 8 Pages 1055-1058
Jamshid L. Manzoori, Akira Miyazaki and Hiroaki Tao

Abstract: Sample was injected into 0.5 M HNO3 as carrier stream, which was mixed with a reagent stream comprising (NH4)6Mo7O24 and NH4VO3 in HNO3. Phosphate was determined as molybdovanadophosphate by spectrophotometry at 470 nm, and the eluate was fed to an ICP-AES system for determination of total P at 177.499 nm. The calibration graphs were rectilinear for 200 µg mL-1 of P for both detection methods, and the limits of detection were 0.8 and 0.5 µg mL-1, respectively. Of several common ions examined, only Cr interfered in the spectrophotometric method. The coefficient of variation was 2.0% for 10 µg mL-1 of P (n = 11). Eighty samples per hour could be analyzed. The method was applied to treated sewage and metal-plating waste water.
Waste Spectrophotometry Calibration Detection limit Interferences

"Determination Of Micro-amounts Of Phosphorus With Malachite Green Using A Filtration-dissolution Preconcentration Method And Flow Injection Spectrophotometric Detection"
Analyst 1995 Volume 120, Issue 1 Pages 187-191
Joko P. Susanto, Mitsuko Oshima, Shoji Motomizu, Hiroshi Mikasa and Yoshikazu Hori

Abstract: Sample solution (10 ml) was mixed with 1 mL 6.5 M HCl and 1 mL reagent solution (prepared by dissolving 7.1 g ammonium heptamolybdate in 30 mL water and adding 48 mL concentrated HCl and 10 mL malachite green solution containing 0.023 g malachite green oxalate; the solution was diluted to 100 mL with water, mixed for 12 h and filtered). The mixture was allowed to stand for 5 min and was then filtered through a cellulose nitrate membrane filter under suction. The solid was washed with 10 mL water. The solid and the membrane filter were dissolved in 1 mL methyl cellosolve. A portion (100 µL) of the resulting solution was injected into a carrier stream (0.5 ml/min) of methyl cellosolve and the absorbance was measured at 627 nm (ε = 210 000). The calibration graph was linear up to 19 ppb of P; the detection limit was 0.06 ppb. The RSD (n = 6) was 0.57%. The method was used to determine P (as phosphate) in seawater.
Sea Spectrophotometry Preconcentration

"Determination Of Dissolved Reactive Phosphorus In Estuarine Waters Using A Reversed Flow Injection Manifold"
Analyst 1997 Volume 122, Issue 12 Pages 1477-1480
Stefan Auflitsch, Darren M. W. Peat, Ian D. McKelvie and Paul J. Worsfold

Abstract: The Schlieren or refractive index (RI) effect is a major problem in the determination of dissolved reactive phosphorus in estuarine waters using conventional flow injection (FI) manifolds with sample injection, This is because differences in RI between the injected sample zone and the carrier stream give rise to a lensing effect which is superimposed on the blank response and causes significant error in quantitation, A simple reversed flow injection (rFI) manifold using spectrophotometric detection which removes these quantitation errors is reported. Acidic molybdate is injected into a sulfuric acid carrier stream of the same refractive index and sequentially merged with sample and reductant (ascorbic acid), Reduction of phosphomolybdate to phosphomolybdenum blue is carried out in a coil thermostated at 60°C. Dissolved reactive phosphorus has been successfully determined in estuarine waters with salinities ranging from 0 to 30 parts per thousand using calibration standards prepared in deionized water, with a detection limit of 2 µg L-1 PO4-P and a linear range of 2-100 µg L-1 PO4-P (r2 = 0.9998).
Estuarine Spectrophotometry Reverse Refractive index Heated reaction

"New Approach To Sequential Injection Analysis: Using The Sample As Carrier"
Analyst 1998 Volume 123, Issue 7 Pages 1541-1546
Francisca Mas, Andreu Cladera, Jos&eacute; Manuel Estela and V&iacute;ctor Cerd&agrave;

Abstract: A new way of implementing sequential injection analysis involving the use of the sample as a carrier is proposed. These systems are especially suitable for constructing continuous monitoring set-ups with no restrictions regarding the amount of sample which can be processed. A new standard addition methodology was used to calibrate the proposed system. The methodology was applied to the determination of Fe(II) with o-phenanthroline (a reaction which involves a single reagent) and that of P by formation of a blue heteropoly acid (a reaction involving two reagents). The anal. rate is 8 min per sample (3 standard additions). The manifold design together with an adequate program of aspiration-impulsion movements avoids the memory effects between samples. Determination of Fe(II) is linear between 0.25 and 6 mg L-1 Fe(II). In the analysis of a sample containing 2.3 mg L-1 Fe(II) (n = 10) a relative standard deviation of 1.7% was obtained. The detection limit (3s) is 0.06 mg L-1 Fe(II) and the determination limit (10s) 0.2 mg L-1 Fe(II). Determination of P is linear between 0.1 and 1 mg L-1 P and in the analysis of a sample containing 0.75 mg L-1 P (n = 10) a relative standard deviation of 4.1% was obtained. The detection limit is 0.02 mg L-1 P and the determination limit 0.1 mg L-1. Both methods were applied to the determination of Fe and P in spiked waters. The use of the methodology based on the standard addition was evaluated in the case of P determination to eliminate interferences of the multiplicative type.
Water Spectrophotometry Sequential injection Standard additions calibration Interferences Reverse

"Monosegmented System For Continuous-flow Analysis. Spectrophotometric Determination Of Chromium(VI), Ammonia And Phosphorus"
Anal. Chem. 1985 Volume 57, Issue 13 Pages 2575-2579
Celio Pasquini and Walace A. De Oliveira

Abstract: The system described is based on established flow injection analysis apparatus, into which the sample is introduced into the flow manifold between two air bubbles. The bubbles are removed with a permeation membrane before the stream reaches the detector. The characteristics of the system, evaluated in the absence of reactions, showed that the approach can be used for analytical methods requiring long residence times. In the spectrophotometric determination of NH3, P and Cr(VI) the detection limits were 5, 20 and 3 ng mL-1, respectively, at the 99.7% confidence level. The precision was better than 1%, and samples could be introduced at 120 h-1. The system can replace the classical segmented continuous-flow analysis or flow injection analysis methods, with improved sampling rate, sensitivity, and reagent and sample consumption.
Spectrophotometry Membrane

"Determination Of Phosphorus As Molybdovanadophosphoric Acid In Phosphate Rock With A Flow Injection Procedure"
Fresenius J. Anal. Chem. 1981 Volume 307, Issue 5 Pages 373-377
Willem D. Basson, Jacobus F. van Staden and Peter M. Cattin

Abstract: Based on the flow injection principle and by using small sample volumes and splitting of the colorimeter output, a good reliable and reproducible method for the determination of P2O5 in phosphate rock covering the range of 0-40% on a routine basis was achieved. The system described is suitable for the routine analysis of P2O5 in the prepared phosphate rock samples at a rate of approximately 90 samples per hour with a coefficient of variation of better than 1%.
Phosphate Commercial product Spectrophotometry Signal splitting

"Consecutive Determination Of Nitrogen, Phosphorus And Calcium In Animal Feeds On A Single Channel Flow Injection Analyzer With A Common Analytical Manifold"
Fresenius J. Anal. Chem. 1982 Volume 311, Issue 1 Pages 23-26
W. D. Basson

Abstract: A procedure is described for the consecutive determination of N, P and Ca in animal feeds by means of a single-channel flow injection analyzer with common manifold. The sample is decomposed with K2SO4, HgO and H2SO4 and is directly injected into the system after dilution. The following reagents are employed: phenol/hypochlorite for N (protein), molybdate/ascorbic acid for P and cresolphthalein complexone/aminomethylpropanol for Ca. Comparison with the results of the Kjeldahl, vanadate and AAS methods, respectively, revealed good agreement.
Feed Spectrophotometry

"Flow Injection Analysis In Soil Research And Plant Analysis"
Fresenius J. Anal. Chem. 1988 Volume 329, Issue 6 Pages 701-706
K. Schaller, R. Lenhardt, V. Weber und C. Euler

Abstract: Flow diagrams and experimental conditions are given for the determination of N in soils, of NH3 in grape musts and juices, of P in soil extracts, of NO3- in plant extracts and of total amino-acid content, proline and arginine in plants. Each analysis is discussed and compared with other methods.
Environmental Plant Juice Musts Sample preparation Method comparison Review Tecator

"Simultaneous Determination Of Silicon And Phosphorus In Biological Standard Materials With Online-column Flow Injection Spectrophotometry"
Fresenius J. Anal. Chem. 1988 Volume 332, Issue 2 Pages 162-166
Yoshio Narusawa, Tsutomu Katsura and Fuki Kato

Abstract: Biological standard material (1 g), viz, NIES chlorella or pepperbush or NBS bovine liver, was ashed, the ash was fused with Li2CO3 - H3BO3 for 15 min at ~1000°C, and the cooled melt was dissolved in and diluted to 100 mL with 1 M HCl. A 2.5 mL portion of extract was diluted with water (2.5 ml) and the mixture was cleaned up by cation exchange on a column (3 cm x 8 mm) of Dowex 50W-X8 (100 to 200 mesh) pre-conditioned with 2 M HCl (10 ml) and water (2 x 10 ml). Elution was effected with 0.5 M HCl (5 x 2 ml), the combined eluates were evaporated to dryness, 0.5 mL of 0.25 M Na2CO3 was added and, after evaporation to dryness, the residue was fused at ~1000°C for 15 min. The melt was dissolved in water containing 0.01 M EDTA (1 ml) and the solution was diluted to 25 mL with water. Phosphorus and Si were then determined by flow injection analysis as previously described (Anal. Abstr., 1988, 50, 8B123) with online anion-exchange separation on a column (15 cm x 4.6 mm) of TSK-gel SAX (5 µm). Most commonly occuring ions, e.g., Ca and Mg, were removed on the cation-exchange column; however, arsenate and germanate were not. Results agreed with those by ICP-AES.
Biological material NIES 1 NIES 3 NIST 1577 Ion exchange Spectrophotometry Merging zones Method comparison Simultaneous analysis Reference material

"Spectrophotometric Determination Of Phosphorus As Phosphate In Organic Compounds And Materials Of Biological Origin Using A Flow Injection Manifold With A Mixing Chamber"
Fresenius J. Anal. Chem. 1992 Volume 342, Issue 9 Pages 734-736
D. Thorburn Burns, N. Chimpalee and M. Harriott

Abstract: Serum was treated with 10% trichloroacetic acid and the mixture was centrifuged. A portion of the supernatant solution was diluted with water and injected into a carrier stream (2.6 mL min-1) of aqueous 1% PVC which merged sequentially with streams (all at 1.3 mL min-1) of 20% HNO3, 0.5 mM Crystal violet (C. I. Basic Violet 3) and 0.1 M sodium molybdate. After passing through a reaction coil, the absorbance of the mixture was measured at 560 nm. The calibration graph was rectilinear up to 1.25 µg mL-1 of phosphate; the detection limit was 0.01 µg mL-1. The coefficient of variation (n = 10) was 0.6% for 0.5 µg mL-1. Sample throughput was 100 h-1. The method was also applied to the determination of P in organic compounds and plants. A flow injection manifold with mixing chamber has been developed for the determination of phosphate by reaction with molybdate and Crystal Violet. The insoluble blue dye salt is kept in colloidal solution with poly(vinyl alcohol) and the absorbance is measured at 560 nm. The injection rate is 100 h-1. The detection limit is 0.01 µg of PO43-/mL based on 250 µL injection volumes The system has been applied to the determination of phosphate in serum samples and after appropriate mineralization to organic compounds and to plant materials.
Blood Serum Plant Sample preparation Spectrophotometry Mixing chamber

"Flow Injection System With Gas Diffusion For The Sequential Determination Of Total Nitrogen And Phosphorus In Vegetables"
Fresenius J. Anal. Chem. 1997 Volume 358, Issue 5 Pages 657-662
Jos&eacute; L. F. C. Lima, Antonio O. S. S. Rangel, M. Renata S. Souto

Abstract: Dried, ground vegetables were digested with Se and H2SO4/salicylic acid/H2O2 and then diluted in 0.8 M H2SO4. A portion (180 µL) of the solution was injected into a stream of 0.8 M H2SO4, which merged with a stream of 2.5 M NaOH and passed through a gas diffusion unit. The NH3 diffused into a secondary stream of 0.01 M Tris hydrochloride of pH 7.5 which converted it to ammonium prior to detection with an ISE. The primary stream, now purged of NH3, passed through a stream splitter to reduce the total flow and then merged with a stream containing ammonium molybdate, stannous chloride and hydrazine sulfate in H2SO4. The primary stream then passed through a flow cell for determination of phosphate at 710 nm. The calibration graphs were linear from 0.34-2.4 mM phosphate and up to 0.11 M ammonium, the detection limits were 43 µM phosphate and 1.4 mM ammonium, and the RSD (n = 10) were <3.5%. The sampling rate was 40-60/h. The ammonium and phosphate levels were indicative of the total N and P contents of the vegetables analyzed.
Vegetable Electrode Sample preparation Spectrophotometry Dual detection Gas diffusion

"A New Concept For The Quasi Non-destructive Microsampling Of Historical Glasses"
Fresenius J. Anal. Chem. 1997 Volume 358, Issue 6 Pages 694-698
G. Schulze, I. Horn, H. Bronk

Abstract: A glass object was sampled by filing with a diamond-coated Cr file. For the determination of Si, the file was sonicated for 20 min in 5 mL 6% Na2CO3/K2CO3 (1:1) to remove the sample material, and was also washed with water. The slurry and washings were combined and evaporated to dryness, and then fused at 1000°C for 20 min. For other determinations, the file was immersed in 0.4 mL HF or HF/HClO4 (3:1), then rinsed with water. The combined solution and washings were evaporated to dryness and the residue was reconstituted prior to analysis. Digestion of the residue with Cl/H2O was used prior to the determination of Au. Si and P were determined by FIA with photometric detection (based on the molybdenum blue reaction). Other elements were determined by ion chromatography or GFAAS (details given).
Commercial product Spectrophotometry Sample preparation Sample preparation

"Determination Of Phosphorus In Silicate Rocks By Flow Injection Method Of Analysis"
Microchim. Acta 1984 Volume 82, Issue 5-6 Pages 377-383
Rokuro Kuroda, Iwao Ida and Koichi Oguma

Abstract: A 0.1-g sample of powdered rock is fused for 15 min at 1000°C with 0.3 g each of Li2CO3 and H3BO3, the melt is dissolved to 100 mL in 1 M HCl, and a 3 mL portion is diluted to 10 mL with water. A six-way loop valve is used to inject 318 µL of this solution into a carrier stream of 0.3 M HCl (1.5 mL min-1), which meets a stream of 0.13% (NH4)6Mo7O24.4H2O - 0.024% Sb K tartrate solution [containing also tartaric acid and poly(vinyl alcohol)] and one of 0.096% ascorbic acid solution (each 0.75 mL min-1). The mixture is passed through a mixing coil immersed in a water bath at 90°C and then through a water-cooled coil, after which the absorbance is measured at 710 nm vs. air. Two levels of P2O5 (0.123 and 0.247%) have been determined successfully in the presence of 28.5 to 85.6% of SiO2. The method has been applied to eight US and Japanese standard rocks, with generally good agreement with recommended or reported values. Twenty samples can be analyzed in the flow system per hour.
Silicate Spectrophotometry Heated reaction Reference material

"Analyte Enrichment And Matrix Removal In Flow Injection Analysis-inductively Coupled Plasma-atomic Emission Spectrometry. Determination Of Phosphorus In Steels"
Spectrochim. Acta B 1985 Volume 40, Issue 1-2 Pages 57-62
C. W. McLeod and I. G. Cook, P. J. Worsfold, J. E. Davies and J. Queay

Abstract: Acidified solution of digested steel were injected on to a PTFE column of activated alumina (75 to 120 µm); PO43- was retained on the column, and matrix cations were carried to the nebulizer. The PO43- was then eluted by the injection of 200 µL of 0.5 M KOH, and passed to the ICP plasma for emission measurement at the P I 213.62-nm line. A constant analytical response over an extended period, with PO43- recovery of ~90%, was achieved. The calibration graph was rectilinear for 0 to 50 µg mL-1 of P, and the coefficient of variation was 1.6% at the 20 µg mL-1 level; the limit of detection was 0.6 µg mL-1. Analysis of a standard reference steel gave a value of 0.041% of P compared with the certified value of 0.043%.
Alloy Sample preparation Spectrophotometry Activated alumina Reference material

"Simultaneous Determination Of Total Phosphorus And Total Nitrogen By Flow Injection System"
Anal. Sci. 1989 Volume 5, Issue 2 Pages 235-236
M. AOYAGI, Y. YASUMASA and A. NISHIDA

Abstract: A flow injection system, the Sumigraph NP-2500, is described (diagram given) and conditions are tabulated for determination of total P and total N in a single sample. The method is based on digestion of the sample in dual capillary digestors with S2O82- for P and S2O82- - NaOH for N, and subsequent detection of PO43- and NO3- independently of one another in an acidified solution of ammonium molybdate containing malachite green (C. I. Basic Green) at 650 nm. In general, results agreed with those obtained by an official method. The method was applied in the determination of total P and total N in industrial waste water; analysis took 5 min. The coefficient of variation (n = 10) for 10 ng mL-1 of N was 0.9%.
Waste Sample preparation Spectrophotometry Method comparison Standard method

"Inline Pre-treatment Method For Flow Injection Analysis Of Total Phosphorus And Nitrogen Impurities In Hydrogen Peroxide Solution"
Anal. Sci. 1991 Volume 7, Issue 2 Pages 347-348
M. AOYAGI, Y. YASUMASA and A. NISHIDA

Abstract: Hydrogen peroxide is catalytically decomposed by use of Pt wire at 100°C, prior to analysis for total N and total P by the flow injection procedures described previously (cf. ibid., 1989, 5, 235, and Anal. Chim. Acta., 1988, 214, 229). For 50 to 150 mg mL-1 of P and N recoveries were 100.1 to 112% and 99.2 to 103.8%, respectively, and coefficient of variation were 0.7% (n = 3). The method is considerably quicker than an offline pre-treatment method used previously (cf. Bunseki Kagaku, 1990, 39, 131).
Inorganic compound Electrode Catalysis Heated reaction

"Determination Of Trace Amounts Of Phosphorus In Copper After Preconcentration By Carrier Precipitation And Flotation"
Anal. Sci. 1994 Volume 10, Issue 4 Pages 669-670
T. TANAKA, S. KAYUKAWA and A. MIZUIKE

Abstract: Cu wire was etched with acetic acid ultrasonically for 5 min, rinsed with water, dipped in acetone and dried in a vacuum desiccator. HCl and 31% H2O2 were added, the solution was boiled to remove excess peroxide, diluted with water and 5 mg/ml Al solution and aqueous 15 M ammonia were added to form flocculent hydrated aluminum oxide carrier precipitates and the ammine complex of Cu(II) at pH 8.5. Sodium oleate and sodium dodecylbenzenesulfonate in 70% ethanol were added and the solution was filtered. The foam was destroyed with 99.5% ethanol and the precipitate was washed with 6% ammonium chloride of pH 8.5 and dissolved in 1 M HCl. HBr (48%) was added to the filtrate and evaporated to dryness. The residue was dissolved in 1 M HNO3 and mixed with 1 M HNO3 containing 5% ascorbic acid or 5% ascorbic acid and Al. The solution was diluted with HNO3 and injected into the FIA system previously described (Ibid., 1994, 10, 389) to determine the phosphate content spectrophotometrically. A large excess of ascorbic acid was required to eliminate interference from Cu. The calibration graph was linear up to 20 µg of phosphate with a detection limit of 0.16 µg/g of P and recovery of >95%.
Metal Spectrophotometry Sample preparation Interferences Preconcentration Precipitation

"Online Pretreatment With Cobalt(III) Ions For A Flow Injection Spectrophotometric Determination Of Organic Phosphorus"
Anal. Sci. 1995 Volume 11, Issue 5 Pages 787-792
H. TANAKA, T. FUKUOKA and K. OKAMOTO

Abstract: Portions (500 µL) of solutions of standard organophosphorus compounds (1 mg/l as P; tabulated) were injected into a carrier stream of water and mixed with a stream of water containing 32 mM Co(III) in a coil (5 m x 1 mm i.d.) containing a Pt wire (3 m x 0.2 mm i.d.). The mixed solution was treated with ammonium molybdate/ascorbic acid reagent injected into the flow system and mixed in a coil (1 m x 1 mm i.d.) at 75°C and the absorbance of the colored product formed was measured at 880 nm. The calibration graph was linear up to 1.5 mg/l of P and the detection limit was 0.005 mg/l. RSD (n = 10) was 3% for 1 mg/l (as P) disodium phenyl phosphate. Average recoveries were ~100% for all the model compounds studied. The method was applied to the determination of P in water samples. Results were in good agreement with those obtained by Official methods except for water samples with high-chloride content (i.e. seawater). Sample throughput of 10^-12/h was achieved by this method.
Sea Spectrophotometry Heated reaction Standard method Method comparison

"Determination Of The Inorganic Phosphorus Content In Serum By The Use Of Immobilized Enzyme Reactions In An FIA System"
Anal. Sci. 1996 Volume 12, Issue 1 Pages 137-139
H. MORI, M. KOGURE, H. TAKEI and H. YAMAMOTO

Abstract: Serum was diluted 1:100 with carrier solution (see below) and a 50 µL portion was injected into a carrier stream of 100 mM PIPES buffer of pH 7.5 containing 100 mM sucrose, 3 mM MgCl2, 1 mM NADP+ and 50 µM-glucose diphosphate (0.4 ml/min) of a flow injection system (schematic shown). The mixture was transferred via an ODS column (4 cm) to an enzyme reactor column (8 cm x 2 mm i.d.) operated at 30°C and packed with 40 iu each of sucrose phosphorylase, phosphoglucomutase and glucose-6-phosphate dehydrogenase immobilized on aminopropyl-bonded glass beads by the method of Mori et al. (Anal. Lett., 1994, 24, 309). The NAPDH formed by the enzyme reactions was fluorimetrically detected at 460 nm (excitation at 340 nm) on a Hitachi F-1000 spectrofluorimeter with a 12 µL flow cell. The calibration graph was linear from 1-100 µM-phosphate (2-6 mg P/100 ml). The RSD (n = 10) was 2.8% for 12.6 µM-phosphate. Results agreed well with those obtained by the method of Berti et al. (J. Clin. Chem. Clin. Biochem., 1988, 26, 399) using an immobilized purine nucleoside phosphorylase-xanthine oxidase-peroxidase enzyme mixture and the Molybdenum Blue method.
Blood Serum Fluorescence Glass beads Immobilized enzyme

"Determination Of Trace Amounts Of Phosphorus In Steel After Preconcentration By Carrier Precipitation And Flotation"
Anal. Sci. 1996 Volume 12, Issue 1 Pages 149-150
T. TANAKA, K. SAKAI and A. MIZUIKE

Abstract: Steel chippings (50-500 mg) were digested with 15 mL HNO3 (1 + 1) and 2 mL HCl, 10 mL 70% HClO4 was added and the solution was heated until fumes of HClO4 commenced. On cooling, the salts were dissolved in 30 mL water and suitable portions of 12.5% aqueous EDTA solutions were added (details given). The pH was adjusted to 8.5 with 3 M aqueous NH3 and the precipitates formed were stirred for 10 min. The solution was diluted to 200 mL with water, 1 mL sodium oleate (6 mg/ml) was added and the mixture was transferred to a flotation cell. Nitrogen gas was passed through the mixture at 9 ml/min for 90 s and the mother liquor was removed by suction. A 5 mL portion of 99.5% ethanol was added and the precipitates were dissolved with 3 x 5 mL 1 M HNO3 and the resulting solution was filtered. The filtrate was mixed with 2 mL 10% ascorbic acid and 400 µL 5 mM Na2S2O3 and diluted to 20 mL with 1 M HNO3. Portions (200 µL) were injected into a flow injection system and detected spectrophotometrically by the method of Tanaka et al. (Ibid., 1994, 10, 669). The calibration graph was linear up to 20 µg phosphate (I). The method was applied to the analysis of I in three standard steel reference samples. Results agreed well with certified values with RSD of 14%.
Alloy Spectrophotometry Preconcentration Reference material Precipitation

"Online Photo-oxidative Decomposition Of Phosphorus Compounds To Orthophosphate And Its Application To Flow Injection Spectrophotometric Determinations Of Total Phosphorus In River And Waste Waters"
Anal. Sci. 1998 Volume 14, Issue 5 Pages 941-946
Keiro HIGUCHI), Hiromitsu TAMANOUCHI) and Shoji MOTOMIZU

Abstract: A simple and mild online photo-oxidative decomposition method for the highly sensitive flow injection spectrophotometric determination of total P in river water and wastewater was developed using low pressure mercury lamps. Organic and inorganic P compounds in sample solutions were injected into a carrier solution, which merged with the decomposition solution containing sulfuric acid and K peroxodisulfate. The solution components were decomposed oxidatively to orthophosphate while flowing in a photo-reactor. After the decomposition, orthophosphate was determined spectrophotometrically based on the formation of Molybdenum Blue. The photo-reactor consisted of two low pressure mercury lamps, a poly(terafluoroethylene) (PTFE) tubing and a reflection mirror. The PTFE tubing was wound directly around the Hg lamps, which were covered with reflection mirror. The detection limit for P was ~0.001 mg/L, and the sample throughput was ~20 samples/h for total P determination Using the photo-reactor, most of the P compounds were decomposed completely, whereas some condensed phosphates were less susceptible to photo-oxidation. The analytical results for practical samples obtained by the proposed method showed a good correlation with those obtained by using a heat-oxidation method, which indicates that the content of the condensed phosphates difficult to be decomposed was very scarce in the practical samples.
River Waste Spectrophotometry Photochemistry UV reactor Method comparison

"Automated Determination Of Nanogram Amounts Of Phosphorus By Molecular Emission Cavity Analysis"
Anal. Proc. 1982 Volume 19, Issue 6 Pages 320-321
I. H. El-Hag

Abstract: Molecular emission cavity analysis (MECA)1 is a flame photometric technique that relies on a cool flame source to generate band emissions, such as those from S,, BO, and HPO. The conventional manual method involves depositing the microlitre-volume sample into a cavity cut into the end of a rod, which is introduced manually to the flame, so that the emission generated within the cavity is viewed by the detector. The reproducibility of this method is unsatisfactory for fast emitting species because variables such as the exact time of injection, cavity residence time in the flame and cooling time after analysis need precise control.
Spectrophotometry Spectrophotometry

"Determination Of Phosphorus (blue Method) In Undiluted Soil Extracts By Flow Injection Analysis"
Landwirtsch. Forsch. 1990 Volume 43, Issue 2 Pages 128-130
Ketschau, U.; Schmid, R

Abstract: An automated method for the determination of phosphorus in soil by flow injection analysis is described. Although the method uses the molybdophosphoric blue reagent, concentration of up to 75 ppm P2O5 can be measured, and it is not necessary to dilute the soil extract.
Environmental Sample preparation Spectrophotometry Tecator

"Determination Of Total Phosphorus In Biological Samples By Flow Injection Analysis With Spectrophotometric Detection"
Bull. Chem. Soc. Jpn. 1993 Volume 66, Issue 3 Pages 966-968
Edison Munaf, Wenzhi Hu and Hiroki Haraguchi

Abstract: Sample (8 to 40 g) was digested using 40 mL of 1 M HClO4, shaken vigorously and centrifuged at 3000 rpm for 5 min. A 20 mL portion of the supernatant solution was adjusted to pH 6.5 with 1.5 M potassium hydrogen carbonate and a 20 µL portion of this solution was injected into a carrier stream which merged with a stream (100 µL min-1) of 4% potassium peroxodisulfate solution and passed through a PTFE reaction coil (8 m x 0.5 mm) at 140°C. The mixture then merged with a stream (100 µL min-1) of 2% ammonium molybdate solution containing 0.36% ascorbic acid and 1.5 M H2SO4 and passed through a second PTFE coil (5 m x 0.5 mm) before the absorbance was measured at 880 nm. The calibration graph was rectilinear for 0.5 to 20 µg mL-1 of P; the detection limit was 16 ng mL-1. The method was used to determine P in chicken heart, eggs of salmon and yellowtail fish and in livers of cow, pig, chicken and fish.
Heart Salmon Egg Yellowtail Egg Liver Liver Liver Liver Sample preparation Spectrophotometry PPB Heated reaction

"Factors Influencing The Flow Injection Analysis"
Bull. Inst. Chem. 1987 Volume 34, Issue 1 Pages 1-7
Hung, T.C.;Chuang, A.;Meng, P.J.

Abstract: The results for determinations of Cl-, NH4+, NO2-, NO3-, total N and total P in water are presented. The effects of flow rate, coil length, sample volume and temperature on accuracy were studied.
Environmental Optimization Review

"Determination Of Major Nutrients In Fertilizers"
Bunseki 1978 Volume 1978, Issue 11 Pages 803-809
Koshino, M.

Abstract: A review, with 42 refs., discussing official fertilizer anal. methods and determinations of N, P, K, B, Ca, and Mg in fertilizers. (SFS)
Commercial product Spectrophotometry

"Continuous-flow Method For The Determination Of Phosphorus Using The Fluorescence Quenching Of Rhodamine 6G With Molybdophosphate"
Bunseki Kagaku 1984 Volume 33, Issue 2 Pages 116-119
Motomizu, S.;Mikasa, H.;Oshima, M.;Toei, K.

Abstract: The method was based on the reaction in acid medium between PO43- and molybdate to form molybdophosphate, which in turn reduces the fluorescence of Rhodamine 6G (C. I. Basic Red 1; I). The carrier solution (distilled water) and reagent solution (0.035 M Mo(VI) and 10 µM-I in 0.8 M HCl) were propelled (at 0.98 mL min-1) by a double-plunger pump, and sample solution (160 µL) was injected into the carrier solution The two streams were mixed in a PTFE tube (20 cm long), and the mixture was passed through an 18 µL flow-cell, where the fluorescence of I was measured at 580 nm (excitation at 350 nm). The calibration graph was rectilinear for 0 to 45 ppb of P. In the analysis of two seawater samples by this method, results of 24.4 and 36.5 ppb of P were obtained, as compared with 23.8 and 35.2 ppb, respectively, by the malachite green method (cf. Anal. Abstr., 1983, 45, 3H60). Co-existing foreign species did not interfere. A schematic diagram of the flow system, which could deal with 20 samples per hour, is presented.
Sea Fluorescence Interferences Method comparison Quenching

"Automated System For Total Phosphorus In Wastewaters By Flow Injection Analysis"
Bunseki Kagaku 1984 Volume 33, Issue 12 Pages 683-686
Korenaga, T.;Okada, K.

Abstract: A 0.31 mL sample is injected into a stream (1.2 mL min-1) of S2O82- solution, which then passes through a heating coil at 120°C before merging with a stream (0.2 mL min-1) of acidic molybdate solution The stream passes through a further heating coil at 75°C, and its absorbance is monitored at 880 nm. The response is rectilinear for up to 10 mg L-1 of P, the limit of detection is 0.01 mg l-1, and the sampling rate is 10 h-1. The coefficient of variation (n = 10) ranged from 0.3 to 1%. Results for various effluents agreed with those by the conventional manual method.
Water Waste Spectrophotometry Heated reaction

"Continuous Monitoring Method Of Total Phosphorus In Wastewater Using Continuous Micro Flow Analysis"
Bunseki Kagaku 1988 Volume 37, Issue 1 Pages 52-55
Goto, M.;Nishimura, M.;Tominaga, T.;Ishii, D.

Abstract: The sample stream is mixed with a solution containing peroxydisulfate in dilute H2SO4; both solution are pumped at ~60 µL min-1 into a mixing joint, and then into a PTFE reaction tube (4 m x 0.64 mm) in an aluminum block bath at 120°C. A Pt wire (0.2 mm diameter) is inserted in the tube as catalyst for the oxidation reaction. All condensed phosphate and organic P compounds are converted into PO43- in the reaction. The stream carrying PO43- is mixed with a stream of molybdate and malachite green (C. I. Basic Green 4) to form a colored ion associate, the absorbance of which is measured at 600 nm in a flow cell.
Waste Spectrophotometry Catalysis Heated reaction

"Digestion Method For FIA Of Phosphorus And Nitrogen In Hydrogen Peroxide Solution"
Bunseki Kagaku 1990 Volume 39, Issue 2 Pages 131-133
Aoyagi, M.;Yasumasa, Y.;Nishida, A.

Abstract: A sample pre-treatment procedure for the determination of N and P in 30% H2O2 solution by flow injection analysis is described. Sample solution (10 ml) was heated at 100°C for ~90 min with 0.2 g of Pt gauze as catalyst. The method is suitable for solution containing 40 ng mL-1 of N and 100 ng mL-1 of P.
Inorganic compound Sample preparation

"Flow Injection Analysis: Adaptation To A Small Laboratory"
Can. J. Plant Sci. 1980 Volume 60, Issue 2 Pages 767-769
N. W. HOLT

Abstract: A flow injection system was used to analyze plant material for total nitrogen and phosphorus. A new, inexpensive sample injector was built which enabled the system to be completely automated.
Plant Apparatus Method comparison Injector

"Low Results For Inorganic Phosphorus With The SMAC Continuous-flow Analyser"
Clin. Chem. 1981 Volume 27, Issue 3 Pages 490-492
EA Robertson, RJ Elin and E Johnson

Abstract: Serum inorganic phosphorus concentrations as measured with the SMAC are lower than those found with other methods. To resolve this problem we analyzed patients' specimens and performed analytical recovery studies with four different systems (SMAC, AutoAnalyzer II, aca, and the Fiske-- SubbaRow method). With the SMAC, results for patients' specimens are significantly lower (p less than 0.0001) than with any of the other three methods. The SMAC recovered only about 87% of the added inorganic phosphorus. The value assigned to SMAC Reference I for inorganic phosphorus was 0.876 of the value obtained when the material was analyzed by the reference method. Thus there is a significant systematic error in the SMAC method for inorganic phosphorus determination, attributable to an erroneous inorganic phosphorus concentration assigned the SMAC calibration material by the supplier (Technicon).
Biological fluid Clinical analysis

"Acid-persulfate Digestion Procedure For Determination Of Phosphorus In Sediments"
Commun. Soil Sci. Plant Anal. 1987 Volume 18, Issue 4 Pages 359-369
Nelson, N.S.

Abstract: To sediment samples in culture tubes were added water and 5.5 M H2SO4 followed by solid K2S2O8 and the mixture was heated in an autoclave for 1 h at 130°C. The tubes were then set aside overnight, after which the supernatant solution were diluted with aqueous K2SO4 - H2SO4 for determination of PO43--P by a continuous-flow adaptation of the method of Murphy and Riley (Anal. Abstr., 1963, 10, 1219). This safe method released a large fraction of the P released by the hazardous HClO4 digestion method. Total P in stormflow sediments determined by HClO4 digestion can be predicted with acceptable accuracy from P determined by acid persulfate digestion provided that homogeneous replicate sub-samples are analyzed.
Environmental Sample preparation

"Simplified Method For The Extraction And Analysis Of Available Nitrogen, Phosphorus, And Potassium In Soils"
Commun. Soil Sci. Plant Anal. 1994 Volume 25, Issue 13-14 Pages 2543-2560
Puchades, R.;Llopis, A.;Raigon, M.D.;Peris Tortajada, M.;Maquieira, A.

Abstract: Soil was dried and homogenized and nitrate, P and K extracted by two methods. For extraction with CaCl2 10 g of soil was shaken for 2 h with 100 mL of 10 mM CaCl2, the mixture was filtered and the filtrate collected for analysis. Extraction with 0.5 M NaHCO3 was by the Spanish Ministry of Agriculture, Fisheries and Food official method (1986) without using charcoal as a decolorizing agent. Nitrate in the extracts was determined by the FIA method of Raigon et al. (Analysis, 1992, 20, 483), P was determined by the reversed FIA system of Perez-Garcia et al., (Soil Sci., 1991, 151, 349) and K was determined by AES. Results obtained were compared with those achieved by the official methods. NaHCO3 was only suitable for the simultaneous extraction of nitrite P and K in alkaline soil and CaCl2 was only suitable for nitrate extraction.
Environmental Sample preparation Spectrophotometry Reverse

"The Molybdate/ascorbic Acid Blue Method For The Phosphorus Determination In Very Dilute And Colored Extracts By Segmented-flow Analysis"
Commun. Soil Sci. Plant Anal. 1996 Volume 27, Issue 5-8 Pages 1363-1375
Coutinho, J.

Abstract: Soil was extracted by the method of Houba et al. (Ibid., 1990, 21, 2281) and the extract was injected into an FIA system for 100 s with air segmentation. The sample stream (1.6 ml/min) merged with a stream of 12 M HCl plus FFD6 wetting agent (0.1 ml/min), and the resulting stream passed through a five-turn mixing coil and then through a 20-turn mixing coil in a water bath at 50°C to a 70 cm dialyser for dialysis against an air-segmented stream of water containing 6 ml/l of FFD6 (0.8 ml/l). The dialysed stream then merged with streams of ammonium molybdate solution (0.1 ml/min) and ascorbic acid/antimony potassium tartrate solution (0.1 ml/min) and, after passage through a ten-turn mixing coil, the absorbance was measured at 880 nm. The calibration graph was linear for up to 400 µg/l of P with RSD (n = 10) of 0.6-5.6%. The detection limit was 2.8 µg/l of P. The method was also applied to waste water.
Environmental Waste Spectrophotometry Dialysis

"Statistical Evaluation Of Phosphorus Breakthrough Profiles Using A Segmented Exponential Model"
Commun. Soil Sci. Plant Anal. 1997 Volume 28, Issue 3-5 Pages 395-406
McGeehan, S.L.;Shafii, B.;Naylor, D.V.;Price, W.J.

Abstract: Few studies have utilized a statistical approach for the evaluation and comparison of breakthrough profiles obtained from soil column investigations. Our objective was to investigate the use of nonlinear estimation techniques to identify the phosphorus (P) breakthrough point and other parameters endemic to breakthrough data. Four soils exhibiting a range in physical and chemical properties were leached under saturated-flow conditions with a 10 mg P/Z solution for 34 days. Leachate P concentrations were analyzed by flow injection colorimetric analysis. A four-parameter segmented exponential model provided a good fit for the breakthrough data in each soil tested. In addition to identifying the breakthrough point, the model parameters provided estimates of other identifiable aspects of a breakthrough profile including background P concentration, equilibrium P concentration, and the rate of concentration change once breakthrough is attained. Estimation of these parameters also facilitated statistical comparison of breakthrough profiles from different soils. Single and joint hypothesis tests showed that significant differences existed among the breakthrough profiles, the breakthrough points, and the rates of concentration change. Additionally, simulation was used to examine the correlation structure between the estimated breakthrough point and 17 soil properties. The simulation showed that six soil properties-ammonium oxalate extractable aluminum (Al) and iron (Fe), citrate dithionite extractable Al, CaCl2, and acetate extractable P, and P sorption capacity-were strongly correlated with P breakthrough. 23 references.
Environmental Spectrophotometry Column Modeling Optimization

"Flow Injection Systems For Elemental Soil Analysis Determinations"
Commun. Soil Sci. Plant Anal. 1998 Volume 29, Issue 3-4 Pages 327-360
Ferreira, A.M.R.;Rangel, A.O.S.S.;Lima, J.L.F.C.

Abstract: A review with ~80 references. Flow injection analysis (FIA) is becoming an important automated procedure for the elemental anal. of agricultural and environmental samples. This paper reviews the application of the FIA technique for soil elemental anal. determinations, giving short descriptions of the required flow manifolds by highlighting some of their most important features. Flow injection analysis (FIA) is becoming an important automated procedure for the elemental analysis of agricultural and environmental samples. This paper reviews the application of the FIA technique for soil elemental analysis determinations, giving short descriptions of the required flow manifolds by highlighting some of their most important features.
Environmental Environmental Spectrophotometry Automation Review Merging zones

"Determination Of Total Phosphorus And Inorganic Phosphorus In Wines By Flow Injection Analysis"
Connaiss. Vigne Vin 1990 Volume 24, Issue 2 Pages 49-61
J.L.F.C. LIMA, A.O.S.S. RANGEL

Abstract: To determine inorganic P, wine was injected into a aqueous carrier stream which merged with a reagent stream of (NH4)2MoO4- SnCl2 (details given). After passing through a reaction coil, the absorbance of the mixture was measured at 710 nm. To determine total P, wine was evaporated to near-dryness on a water-bath and the residue was treated with concentrated HNO3 for 1 h, ignited at 650°C then dissolved in 3 M HCl. The resulting solution was then analyzed as above. The sample throughput for the determination of total P was 120 h-1 with a coefficient of variation of 2%. Inorganic P could be determined from 9 to 1000 mg mL-1 at a sample rate of 60 h-1 with a coefficient of variation of 2%.
Wine

"Direct Fluorometric And Flow Injection Fluorometric Methods For The Determination Of Trace Phosphorus"
Fenxi Ceshi Xuebao 1998 Volume 17, Issue 3 Pages 77-79
Song Gongwu, Feng Jian

Abstract: Direct fluorometric determination of trace P is based upon the quenching of the fluorescence of rhodamine 6G due to the formation of a nonfluorescent hetero-polynuclear acid of rhodamine-phosphoro-Mo ion-associates. The excitations wavelength is 350 nm, while the maximum emission wavelength is 555 nm. The flow injection fluorometric variant of this method has the advantages of high sensitivity, good selectivity and simplicity. It was satisfactorily employed for the determination of P in Cu alloys, steel, and Mn ores.
Alloy Alloy Manganese Fluorescence Quenching Indirect Ion pair formation

"Determination Of Soil Available Phosphorus By Flow Injection Analysis"
Fenxi Huaxue 1981 Volume 9, Issue 5 Pages 586-588
Sun, L.;Gao, Z.;Li, L.;Yu, X.;Fang, Z.L.

Abstract: Soil-available P was determined by the methods of J. Ruzicha et al. (1978) and of Zhaolun Fang (1981) (flow-injection anal.). A soil sample was extd. with 20 volumes of 0.5 M NaHCO3, and 10 mL of the ext. was treated with 2.5 mL of 2N H2SO4 and allowed to stand for 30 min. The ext. was analyzed by CLA-1600 type autoanalyzer (Carlo Erba Co.). An aliquot was injected into the analyzed at m.6 mL/min accompanied by injection of a solution containing NH4 molybdate, tartaric acid, concentrated H2SO4, and water at 6.7 mL/min, and a solution containing SnCl2, concentrated HCl, and water at 1.72 mL/min for color reactions. Results compared well with those determined by the conventional (manual) method. The relative standard deviation was 1.8% when 0.46 mg P2O5/100 g soil was analyzed but was 0.4% when a standard solution containing 0.8 ppm P2O5 was analyzed.
Environmental Spectrophotometry Method comparison

"Flow Injection Analysis Micellar-solubilization Spectrophotometry. 1. Determination Of Phosphorus At Microgram/liter Levels With The Ethyl Violet-heteropoly Acid-Triton X-100 System"
Fenxi Huaxue 1987 Volume 15, Issue 11 Pages 1022-1024
Yuan, Y.;Qu, K.

Abstract: The flow of the three reagent solution, viz, (A) 0.06 M in H2SO4 and 3 mM in MoO42-, (B) prepared by mixing 20 mL of 10% Na2S2O3 solution, 60 mL of 10% Na2SO3 solution (to eliminate interference of As(V)), 6 mL of 5% Triton X-100 solution and water to produce 200 ml, and (C) aqueous 0.12 mM ethyl violet (C. I. Basic Violet 4), is controlled by a peristaltic pump at 1.43 mL min-1, 0.67 mL min-1 and 1.41 mL min-1, respectively. solution A and B are mixed just before the injection of 1 mL of the sample or standard P solution (e.g., 42 µg l-1). solution C enters the system after passage of the sample solution through a coiled reaction tube (90 cm x 0.3 mm) and flow continues through another coiled reaction tube (300 cm x 0.8 mm) to an 8 µL detector cell for absorbance measurement at 553 nm. The calibration graph is rectilinear for up to 100 µg L-1 of P. The detection limit is 0.5 µg l-1. The method has been successfully applied to the determination of trace P in tap and well water.
Well Water Spectrophotometry Micelle Interferences Triton X Surfactant

"Application Of Flow Injection Analysis To Silicate Rocks With Series Detectors"
Fenxi Huaxue 1990 Volume 18, Issue 2 Pages 117-120
Lin, S.L.;Shuai, Q.

Abstract: Silicate rocks and National Standard reference rock samples (0.2 g) are digested with 5 mL of HF solution and 1 mL of 9 M H2SO4 by heating. The mixture is evaporated to fumeless and the residue is dissolved in 5 mL of 6 M HCl. The solution is evaporated to dryness and the residue is dissolved in dilute HCl and diluted to 100 mL (final concentration. of 2% in HCl.). Titanium and P are determined by photometry and Mg and Na are determined by AAS. The series detectors were situated with the spectrophotometer at the upstream and the AAS instrument at the downstream end. Results agreed well with certified values.
Silicate Sample preparation Spectrophotometry Spectrophotometry Reference material Dual detection

"Simultaneous Determination Of Phosphorus, Potassium And Sodium In Plants By Flow Injection Analysis"
Fenxi Huaxue 1992 Volume 20, Issue 2 Pages 196-198
Wu, J.;Cai, Y.;Rao, Z.

Abstract: Air-dried tobacco leaves (0.5 g) were washed and ashed at 500°C for 4 h and the ash was dissolved in and diluted with 1% HCl to 25 mL. A 40 µL portion of the solution was injected into a water carrier stream and merged with a stream of 0.02 M (NH4)6Mo6O24 containing 1 M HCl before mixing with a stream of 3 mM SnCl2 containing 1 M HCl (all streams were at 3.6 mL min-1). Phosphorus was detected spectrophotmetically at 620 nm and K and Na were detected upstream by flame photometry. Beer's law was obeyed for 1 to 4 µg mL-1 of P, 3 to 60 µg mL-1 of K and 6 to 40 µg mL-1 of Na; corresponding coefficient of variation were 1.4, 1 and 1.1%. Results were in good agreement with those by ICP-AES.
Leaves Spectrophotometry Spectrophotometry Dual detection Method comparison

"Flow Injection Analysis For The Determination Of Total Nitrogen And Total Phosphorus In Animal Wastewater"
Gesuido Kyokaishi 1988 Volume 25, Issue 286 Pages 74-80
Haga, Kiyonori; Osada, Takashi; Harada, Yasuo (SFS)

Abstract: PO43- and NO3- in animal rearing wastewater are determined by flow-injection anal. using molybdene blue spectrophotometry or UV spectrometry, after digestion of the wastes by the method of M. Hosomi (1983). The injection rate is 1/min. Correlation coefficients between this method and the conventional methods are 0.9976 and 0.9996 for N and P, respectively. (SFS)
Waste Spectrophotometry Sample preparation Merging zones Method comparison

"Flow Injection Analysis For Trace Phosphorus Determination With Fluorescence Quenching Of Rhodamine 6G With Phosphomolybdate"
Guangpuxue Yu Guangpu Fenxi 1991 Volume 11, Issue 3 Pages 59-61
Song, G.

Abstract: Copper alloys are heated to dissolution in 8 mL of HCl (1:8) and 2 mL of 30% H2O2, followed by gentle boiling for 4 min, concentration to ~4 ml, cooling and addition of 0.5 mL of 1.84 M H2SO4 and dilution with water to 50 mL. A 500 µL aliquot of the resulting solution is injected into a carrier stream of water (2.5 mL min-1) and flows to a reaction tube (50 cm x 0.8 mm i.d.) to mix with a stream (2.5 mL min-1) of reagent solution [containing 75 mM H2SO4, 0.81 mM (NH4)2MoO4, 13.4 µM-Rhodamine 6G and 0.1% poly(vinyl alcohol)] before detection at 555 nm (excitation at 350 nm). Linear relationship is observed for 0 to 80 ppb of P; detection limit is 0.343 ppb. When determining 80 ppb of P, interference from As(V) can be eliminated by addition of Na2SO3 - Na2S2O3. Results are satisfactory and compared with those obtained by fluorescence colorimetry. The method has also been applied to steels and Mn ores, with coefficient of variation of 0.7 to 1.4%.
Alloy Fluorescence Interferences PPB Quenching

"Determination Of Phosphorus And Calcium In Serum By Flow Injection With Spectrophotometric And Atomic Absorption Detectors In Series"
Guangpuxue Yu Guangpu Fenxi 1994 Volume 14, Issue 1 Pages 95-97
Zhang, H.X.;Ma, B.S.;Li, X.R.

Abstract: A 50 µL portion of diluted serum was injected into a stream of 1% ammonium molybdate, followed by mixing with a stream of 4% ascorbic acid in a FIA system (diagram given). Phosphorus was determined by spectrophotometry at 760 nm and Ca was determined by AAS. The AAS conditions were wavelength 422.7 nm, lamp current 2 mA, slit width 0.2 nm, air flow rate 6.5 l/min, acetylene flow rate 1.7 l/min and burner height 6 mm. Results showed RSD (n = 8) of 2.7 and 2.5% and recoveries of 99.7% and 102% for P and Ca, respectively.
Blood Serum Spectrophotometry Spectrophotometry

"Simultaneous Flow Injection Analysis Of Phosphorus And Potassium In Plant Samples With Detectors In Series"
Huaxue Tongbao 1991 Volume 54, Issue 11 Pages 41-42
Cai Yaqi, Wu Jinsui

Abstract: A 0.5-g sample was ashed at 500°C for 4 h and the residue was dissolved and diluted with 1% HCl. The solution was directly injected into a water carrier stream which merged with a reagent stream of 0.01 M NH4VO3 and 0.02 M (NH4)6Mo6O4 in 0.5 M HNO3 (both at 3.6 mL min-1). After reaction, P was determined spectrophotometrically at 420 nm and K was determined upstream by flame photometric detection. Calibration graphs were rectilinear for 5 to 60 and 15 to 240 µg mL-1 of P and K, respectively. Results agreed closely with those by ICP. Sampling rate was 120 runs h-1.
Plant Spectrophotometry Heated reaction

"Analysis Of Animal Feed In The UK Using FIAstar"
InFocus 1986 Volume 9, Issue 2 Pages 2-NA
Edmunds, B.K.;Shaw, A.

Abstract: NA
Feed Spectrophotometry Tecator

"Experience With Flow Injection Analysis In Limnological Research"
InFocus 1987 Volume 10, Issue 1 Pages 8-NA
Ripl, W.;Michel, J.

Abstract: NA
Sea Spectrophotometry Tecator

"Automated Stopped-flow / Unsegmented Solution-storage Analyzer"
Int. Lab. 1981 Volume 11, Issue 1 Pages 32-45
Malmstadt, H. V.; Walczak, K. M.; Koupparis, M. A. (SFS)

Abstract: An automated stopped-flow/unsegmented solution-storage analyzer provides rapid automatic aliquating, mixing, and sequential transfer of solutions to a storage coil. Various lengths of storage coil are used for specific analyzes in order to provide the desired delay times and sample conditioning cell. The analyzer can be used to advantage with analytical methods that require a 10^-30 s or longer delay time to reach equilibrium or for single-point reaction-rate methods. The analyzer was illustrated by equilibrium-method determination of Fe(III) and ascorbic acid and by determining P and protein N by single-point reaction-rate methods. (SFS)
Review Computer Stopped-flow

"Semiautomated Method For Simultaneous Determination Of Phosphorus, Calcium, And Crude Protein In Animal Feeds"
J. AOAC Int. 1977 Volume 60, Issue 4 Pages 845-852
Hambleton, Larry G.

Abstract: A semiautomated method was developed for the simultaneous delermination of phosphorus, calcium, and crude protein in animal feeds. Samples are digested with a block digcstor, diluted to volume, and analyzed at the rate of 40 samples/hr. Protein is determined by the official AOAC method, by measuring the absorbance of an ammonia-salicylate complex at 660 nm. Phosphorus and calcium arc determined by measuring the absorbances of the molybdovanadophosphate and calcium-cresolphthalein complexes at 420 and 570 nm. respectively. Samples are weighed according to the amount of protein they contain. Over 90% of the mixed animal feed samples analyzed for phosphorus and calcium fall within the range of the instrument; provisions are made for single determinations on those samples; that fall outside the specified ranges. Results correlate well for the semiautomatcd method and official AOAC methods on mixed feed check samples and NBS Standard Reference Orchard Leaves.
Feed Spectrophotometry Simultaneous analysis Technicon

"Simultaneous Determination Of Protein (nitrogen), Phosphorus, And Calcium In Animal Feeds By Multichannel Flow Injection Analysis"
J. AOAC Int. 1983 Volume 66, Issue 3 Pages 718-726
van Staden JF.

Abstract: A 3-channel flow injection procedure was developed, which enables the simultaneous determination of protein, phosphorus, and calcium in a wide range of animal feeds from a single digestion. Samples are digested with a block digestor, diluted, and analyzed at a rate of 82 samples/h. Protein (nitrogen) as ammonia is determined colorimetrically by the indophenol method. Phosphorus and calcium are determined by measuring the absorbances of the molybdenum blue and calcium-cresolphthalein complexes at 660 and 580 nm, respectively. Protein is determined in the range from 0 to 75%, phosphorus in the range from 0 to 6%, and calcium in the range from 0 to 6%. The results obtained do not differ significantly from those obtained by proven manual methods, and considerable time, space, and reagents are saved.
Feed Sample preparation Spectrophotometry Complexation Multichannel Method comparison

"Determination Of The Phosphorus Content In The Wet Process For Phosphoric Acid Production By Flow Injection Analysis"
Huazhong Shifan Daxue Xuebao (Ziran Kexue Ban) 1988 Volume 22, Issue 2 Pages 182-186
Chen, Yeqing; Zhao, Tingren; Du, Yunqing (SFS)

Abstract: A method of FIA (Flow Injection Analysis) employed to measure the phosphorus content in the technological process of numid-phosphorue acid has been described in this paper. This mixture of ammonium molybdate and ammonium vanadate is served as a developer and a solution 0.48 mol L-1 hydrochloric acid as the carrier steam, in the method, which has been applied to the acid-solution and the extracted residual solution. The content of phosphorus ranging from 0 to 500rag/1 is able to be determined with satisfied results, which can be printed out directly by a computer. The datas obtained from the method are in agreement with those from the neutral titration.
Inorganic compound Industrial Spectrophotometry

"Fate Analysis Of Phosphorus Compounds In Environmental Waters By Flow Injection Analysis And High Performance Liquid Chromatography"
J. Flow Injection Anal. 1986 Volume 3, Issue 1 Pages 37-46
Norimasa YOZA,* Yasushi SAGARA, Hitomi MORIOKA, Takashi HANDA, Hisanobu HIRANO,Yoshinobu BABA and Shigeru OHASHI

Abstract: The concept of 'fate analysis' of phosphorus compounds in aquatic media was explained with several examples; a phosphorus compound is dissolved in a sample water to be examined and the conversion of its chemical form is monitored as a function of time to evaluate the quality - the chemical property and biological activity - of the water. The difference between the concepts of speciation and fate analysis was described. The interchangeable use of a high-pressure flow injection system as an HPLC detector was recommended to achieve such fate analysis of pyrophosphate and tripolyphosphate in deionized water and river water. The FIA system was improved with respect to the preparation method of a Mo(V)-Mo(V1) reagent and the use of a dry reactor with a heating aluminum block (140°C). Fate analysis in deionized water indicated the abnormally high catalytic activity of the deionized water for the hydrolysis of pyrophosphate and tripolyphosphate. The catalyst with pseudo-enzymatic function in the deionized water was deactivated by being autoclaved at 121°C . Pyrophosphate and tripolyphosphate in river water were hydrolyzed more rapidly than one could expect from kinetic data in chemical hydrolysis, but more slowly than in the deionized water.
Environmental Environmental HPLC Spectrophotometry

"Flow Injection Analysis For Phosphorus Compounds"
J. Flow Injection Anal. 1987 Volume 4, Issue 2 Pages 86-97
Norimasa YOZA,* Tokunori YOKOTA,* Annika SJODIN,** and Jurgen MOLLER**

Abstract: A review is presented, with 26 references, of flow injection and HPLC methods for the determination of inorganic and biochemical P. Various Mo reagents are investigated for the determinations and the design of a flow system that can be used convertibly for both flow injection analysis and HPLC is described.
Water Spectrophotometry Review Speciation

"Rapid Determination Of Total Nitrogen, Phosphorus, Magnesium, Potassium And Amylose In Milled Rice By Flow Injection Analysis"
J. Flow Injection Anal. 1991 Volume 8, Issue 2 Pages 127-135
Hideharu NAKAJ MA and *Ryoichi YANAGIHARA

Abstract: Sample (0.5 g) was digested with 3 mL of concentrated H2SO4 and 1 mL of HCl and then diluted with water. To determine N, 30 µL of the solution was injected into a stream of 6% H2SO4 (0.8 mL min-1) and mixed with 2.5 M NaOH of pH 10 (2 mL min-1), with warming at 30°C, and with an indicator stream (0.1 g of Tecator 5000-0295 mixed indicator, 0.4 g of NaH2PO4 and water to 1 l) (2.8 mL min-1) before detection at 590 nm. When determining P, 100 µL of the solution was injected into a stream of 6% H2SO4 (2 mL min-1), followed by dilution with water (2.8 mL min-1), reaction with a reagent stream [prepared with 4 g of NH4VO3, 270 mL of HNO3, 80 g of (NH4)6Mo7O24 and water to 1 l] (0.8 mL min-1) and detection at 420 nm. Magnesium and K were determined with use of the same apparatus equipped with an atomic absorption spectrophotometer by using 6% H2SO4 as carrier solution and 1% LaCl3 solution as reagent stream. For determination of amylose, 20 mg of the sample was heated at 90°C with 0.5 mL of ethanol and 2 mL of 1 M NaOH for 60 min, cooled, and diluted with H2O; 30 µL of the supernatant solution was injected into a stream of ethanol - 0.1 M NaOH (2 mL min-1) and mixed with 0.1 M NaOH (2.8 mL min-1), ~2% citric acid - Na acetate (2 mL min-1) and iodine solution (1.5 mL min-1) before detection at 620 nm. The coefficient of variation were 4%. Satisfactory results were obtained.
Rice Spectrophotometry Dilution Heated reaction

"Multi-channel Wastewater Monitoring System For Phosphorus Based On Flow Injection Analysis"
J. Flow Injection Anal. 1992 Volume 9, Issue 1 Pages 47-57
Masaya Aoyagi,Yoshiaki Yasumasa* and Tatsuo Himeo*

Abstract: Trace PO43--P was determined in wastewater by flow injection absorption spectrometry at 650 nm using 25% EtOH solution of 0.015 M (NH4)2MoO4 and 2.18 x 10^-4 M malachite green. The calibration graph was linear, and the determination limit was 5 ng/mL. The method was applied to multi-channel wastewater monitoring system for treatment of wastewater from agricultural organophosphorus chemical plant. The PO43--P concentrations in wastewater treated by the activated-sludge process and Ca(OH)2 precipitation process, and those in final effluent were 10^-30, 5-10, and 0.7-1.5 ppm, respectively, during 40 days operation. Trouble shooting and maintenance record during 8 yr operation are described.
Industrial Spectrophotometry Multichannel

"Reversed Flow Injection Analysis And Online Chemical Monitoring In Thermal Power Plants"
J. Flow Injection Anal. 1992 Volume 9, Issue 2 Pages 175-186
Li Yong-sheng and Yoshio Narusawa

Abstract: Online monitoring by reversed FIA is described for chemical monitoring in thermal power plants. Methods described include: the determination of phosphate and silicate in boiler water; the simultaneous determination of P and Si in steam water; the determination of Cu in steam water; the determination of SO42- in power plant water and natural water; and the spectrophotometric FIA determination of the exchange capacity of ion-exchange resins.
Water Environmental Spectrophotometry Reverse Process monitoring

"Rapid Determination Of HClO4-H2SO4 Degradation Nitrogen And Phosphorus In Farm Soils, Crops And Organic Manure Using Flow Injection Analysis"
J. Flow Injection Anal. 1993 Volume 10, Issue 2 Pages 224-235
Hideharu Nakajima *Ryoichi Yanagihara

Abstract: Sample (0.5 g) was decomposed with 25 mL of water, 3 mL of concentrated H2SO4 and 20.5 mL of HClO4 at 130°C for 10 min then heated to fuming at 200°C for 50 min. After cooling, water was added until the total weight was 50 g. To determine N, 30-200 µL of the supernatant was injected into the flow injection analyzer. and carried by a stream of 6% H2SO4 at 0.8 ml/min to mix with 2.5 M NaOH at 2 ml/min in a reaction tube at 30°C prior to reacting with a stream of Tecator NH3 indicator and detection at 590 nm. For P, 30-200 µL of the supernatant was carried by 6% H2SO4 at 2 ml/min to mix successively with 31 g/l of ammonium molybdate solution at 2.8 ml/min, water at 0.8 ml/min and 2% ascorbic acid at 0.8 ml/min with detection at 660 nm. For other samples vanadomolybdic acid was used instead of ammonium molybdate solution and ascorbic acid treatment, with detection at 420 nm. RSD for N and P were 2.1-5.4 and 1.8-8.6%, respectively. The results compared well with those obtained by other conventional methods.
Cow Faeces Crop Environmental Spectrophotometry Sample preparation Method comparison Tecator

"Determination Of Nitrogen, Phosphorus And Anionic Surfactant In Water By Flow Injection Analysis"
Kankyo Gijutsu 1986 Volume 15, Issue 7 Pages 525-530
Shoji MOTOMIZU

Abstract: The application and use of flow injection analysis in the determination of trace nitrogen, phosphorus, and anionic surfactants in water are discussed.
Water

"Rapid Differential Determination Of Phosphate And Total Phosphorus In Waste Water By Flow Injection Inductively Coupled Plasma Emission Spectrometry"
Kogai 1989 Volume 24, Issue 2 Pages 87-93
Miyazaki, A.;Bansho, K.

Abstract: The cited system was used for the determination of PO43- by the molybdovanadophosphoric acid method and total P by ICP-AES. For the latter a cyclone spray chamber performed best and measurement at 213.618 nm decreased interference from Mo and V. Detection limits were 5 and 0.6 ppm, respectively. Sampling rate was 40 per h.
Waste Spectrophotometry Nebulizer Interferences

"Monitoring Of Ntot And Ptot In The Outfall Of A Sewage Treatment Plant Using UV Disintegration And Flow Injection Analysis"
Korresp. Abwasser 1998 Volume 45, Issue 1 Pages 65-70
Brueckner, H.;Rennert, S.;Kroeber, H.;Riis, U.

Abstract: The aim of the investigations was the development and test of an equipment to measure total N and total P and subsequently in the outfall of a sewage treatment plant. A method was developed for disintegration of both total N and total P using UV radiation for subsequent flow injection determination as nitrate and orthophosphate in 1 step. In testing of the complex monitor in the outfall of a pilot sewage treatment plant over a period of 3 mo the results matched well with lab. experiments 76% Of all measured values from the monitor for total N deviated <20% from the lab. results in a range of 4.0-49.0 mg/L Ntot. With the determination of total P in the range 0.5-10.0 mg/L, 77% of all results had a deviation <20%.
Effluent UV reactor Process monitoring Method comparison

"High Speed Continuous-flow Analysis On A Conventional Continuous-flow Instrument"
Lab. Pract. 1977 Volume 26, Issue 7 Pages 541-545
Basson, W.D.

Abstract: A short review of factors influencing sampling rate is given and it is shown that if the magnitudes of the lag phase (L) and half-wash time (W1/2) are reduced, sampling rate could be increased considerably. By using an nonsequential stream and a high flowrate, this principle is applied to the anal. of solutions for NH4+ and P at a rate of ~200/h.
Spectrophotometry Theory Review

"Simultaneous Determination Of Total Calcium And Phosphorus In Milk Using Flow Injection Analysis"
Lab. Rob. Autom. 1998 Volume 10, Issue 4 Pages 235-238
Telis Dimitrakopoulos, John R. Farrell, Peter J. Iles

Abstract: The design, development, and testing of a flow injection analysis (FIA) manifold for the simultaneous determination of two species in milk samples is reported. Calcium is determined potentiometrically, and, following online sample treatment, spectrophotometric anal. of phosphorus is performed. Results obtained are consistent with manufacturers' estimates and, in the case of calcium, with atomic spectrophotometric measurements. The combination FIA system is a rapid, low-cost, highly reproducible method that uses small sample volumes and could be used to provide on-site near-real-time measurements.
Cow Spectrophotometry Remote instrument Low cost Simultaneous analysis

"Determination Of Alkaline Phosphatase-hydrolyzable Phosphorus In Natural Water Systems By Enzymatic Flow Injection"
Limnol. Oceanogr. 1994 Volume 39, Issue 8 Pages 1993-2000
SHAN, YING, IAN D. MCKELVIE, AND BARRY T. HART

Abstract: The method involves use of immobilized Escherichia coli alkaline phosphatase, which produces orthophosphate from phosphate monoesters, nucleoside polyphosphate, deoxynucleoside polyphosphate, inorganic pyro-phosphate, tripolyphosphate, and some S-phosphorothioate esters. The liberated orthophosphate is subsequently detected as phosphomolybdenum blue. Suppression of E. coli alkaline phosphatase activity is significantly reduced when the enzyme is immobilized and used in a packed-bed reactor. This method offers a means of characterizing organic P compounds in the dissolved nutrient pool and has been successfully applied to the study of freshwaters, wastewaters, and sediment extracts. Phosphatase-hydrolyzable P has potential use as an indicator of bioavailability of dissolved P other than orthophosphate in natural waters.
River Waste Spectrophotometry Enzyme

"The Rapid Diagnosis Of Nutritional States Of Crops. 1. The Rapid Procedure For The Analysis Of Inorganic Nutrients Of Plants By Combining H2SO4 - H2O2 Digestion With Flow Analysis And Atomic Absorption"
Miyagiken Nogyo Senta Kenkyu Hokoku 1987 Volume 55, Issue 1 Pages 1-12
Saito, K.;Hasegawa, E.;Sasaki, J.

Abstract: A rapid and labor-saving method was established for determining N, P, K, Ca, and Mg in crop plants by H2SO4-H2O2 digestion, flow anal., and atomic absorption. Si in rice was determined also. For determination of N and P, the digested samples were diluted with water and were subjected to flow anal. SiO2 ppt. in digests was dissolved in diluted aqueous HF and analyzed with a flow-analyzer. For Ca, Mg, and K determination, the digested samples were diluted with water containing 1500 ppm La and were subjected to atomic absorption spectrophotometry in an air-acetylene flame under atomic absorption and flame emission mode, respectively. Contents of these elements in rice, wheat, and soybean plants were determined by this and conventional methods, and the data agreed excellently. (SFS)
Rice Wheat Vegetable Sample preparation Spectrophotometry Method comparison

"New Analytical Methods For Phosphorus"
Mizu Shori Gijutsu 1982 Volume 23, Issue 12 Pages 1063-1067
Odashima, T.

Abstract: A review with 19 references of the new analytical methods for P such as flow injection analysis, thermal lens absorption analysis, and stripping voltammetry. (SFS)
Spectrometry Voltammetry Review

"Fundamentals And Applications Of Flow Injection Analysis. 2. Application Of The Method"
Jpn. J. Soil Sci. Plant Nutr. 1987 Volume 58, Issue 2 Pages 247-251
Koshino, Masayoshi

Abstract: A review on the application of flow injection analysis to soils and fertilizers. Determination of phosphorus, NH4+, NO2-, NO3-, SO42-, etc. with various detection systems such as spectrophotometry, electrochemical methods, atomic absorption spectrometry, and ICP-AES were explained. 29 references.
Environmental Commercial product Spectrophotometry Spectrophotometry Spectrophotometry Electrochemical analysis Review

"Determination Of Assimilable Phosphorus In Soils By Reversed-flow Injection Analysis"
Soil Sci. 1991 Volume 151, Issue 5 Pages 349-354
Perez Garcia, M.;Puchades, R.;Maquieira, A.

Abstract: Soil was extracted with 0.5 M NaHCO3 and the extract was diluted with water. The resulting solution was used as the carrier stream (3.3 mL min-1) in a reversed-flow injection analysis system, into which were injected 0.015% SnCl2 in 4 mM HCl (2.6 mL min-1) and 0.3% molybdate reagent (24 mM molybdic acid - 0.4N-HNO3 and 0.1% antimony - potassium tartrate; 3.3 mL min-1). The solution was passed through a reaction coil (75 cm x 0.8 mm) before the absorbance was measured at 660 nm. The calibration graph was rectilinear for 0.8 mg L-1 of P; the detection limit was 0.025 mg l-1. Sampling frequency was 70 h-1 and recoveries were quantitative.
Environmental Sample preparation Extraction Reverse

"Rapid Method Of Determination For Total Phosphorus In The Crops And Organic Manure By HClO4-H2SO4 Digestion Flow Injection Analysis"
Tohoku J. Agric. Res. 1989 Volume 42, Issue NA Pages 171-172
Nakajima, H.;Kawashima, H.

Abstract: NA
Crop Cow Faeces Sample preparation

"Rapid Determination Of Total Nitrogen And Phosphorus In Rice By HCIO4-H2SO4 Digestion-flow Injection Analysis"
Tohoku J. Agric. Res. 1990 Volume 43, Issue NA Pages 99-100
Nakajima, H.;Takahashi, K.

Abstract: NA
Rice Sample preparation

"Waste Water Quality Monitoring"
Trends Anal. Chem. 1997 Volume 16, Issue 7 Pages 419-424
Olivier Thomas*, Frederic Th&eacute;raulaz, Victor Cerd&agrave;, Daniel Constant, Philippe Quevauviller

Abstract: A sequential-injected analysis (SIA) system equipped with two spectrophotometric detectors is described for waste water quality monitoring. The system is portable and gives rapid results for global pollution parameters such as COD, dissolved organic C and total suspended solids and the determination of specific compounds such as nitrate and anionic surfactants using a direct UV method, SIA methods were devised for non-absorbent species such as NH3, organic nitrogen, orthophosphates and organic P.
Waste Spectrophotometry Portable Sequential injection

"Determination Of Total Phosphorus In Soil Digests By Flow Injection Analysis"
Turang Tongbao 1982 Volume 1982, Issue 4 Pages 40-42
Fang Zhaolun, Sun Lijing, Gao Zhan, Zhu Yan, Wang Xiuling, Li Lin

Abstract: In the early development of flow injection analysis, Ruzicka and other plants will soon successfully applied phosphorus molybdenum blue colorimetric assay, and in ensuring the accuracy of the analysis of 420 samples while achieving the highest / hour speed of analysis, but the Law reagent consumption is large. later after further improved significantly reduce reagent consumption. soil total phosphorus flow injection analysis has so far been reported. we build soil flow injection analysis of total phosphorus since 1977 work, repeatedly improved experimental device, choose the reagents and experimental conditions, the establishment of a method described in this article, after long trial, the effect is satisfactory. (Google translate)
Environmental Sample preparation Spectrophotometry

"Effect Of Soil Acidity On The Determination Of Available Phosphorus In Soil With Continuous-flow Analyser"
Turang 1987 Volume 19, Issue 6 Pages 324-327
Li, Aihua

Abstract: The acidity of soil samples affected the determination of phosphorus with a continuous-flow automated analyzer. It is recommended that the sample solution should contain 0.083N H2SO4.
Environmental

"Automated Analyzer ADM300 With Microcomputer-controlled Evaluator AE2-2"
Wasserwirtsch. Wassertech. 1985 Volume 35, Issue 5 Pages 98-99
Mueller, Albrecht; Eulenberg, Horst; Kopprasch, Wolfgang

Abstract: The ADM 300 analyzer for flow-injection anal. of water has a AE2-2 microcomputer-controlled evaluator and can process ~160 samples/day. The flow injection analysis app. can be used for determination of Fe, Mn, NH4+, NO2-, and NO3- in drinking water; P and N determinations in water monitoring; and Fe and P determination in optimization of the use of pptg. agents in wastewater treatment. (SFS)
Waste Water Computer Precipitation

"Aquatic Soluble Unreactive Phosphorus: HPLC Studies On Concentrated Water Samples"
Water Res. 1995 Volume 29, Issue 9 Pages 2138-2148
Mark A. Nanny*, Seungdo Kim and Roger A. Minear*

Abstract: Soluble unreactive phosphorus (SUP) in concentrated forest stream (Walker Branch, Tenn.) and lake water (Crystal Lake, Ill.) samples was analyzed with an anion-exchange high performance liquid chromatography (HPLC) system containing a phosphorus-specific detector. The detector, which utilized the ascorbic acid-molybdate reaction, consisted of a flow injection system, a post-column reactor, and a u.v.-vis detector. Before HPLC analysis, samples were concentrated and molecular size fractionated with a series of ultrafiltration and reverse osmosis membranes. The SUP composition was found to be a function of season in both Crystal Lake and Walker Branch, as well as a function of stream length for Walker Branch. Seasonal and spatial SUP variations could be explained using contemporary knowledge of nutrient cycling in streams and lakes. A signal, seen in many of the HPLC traces and which eluted with the solvent front, was characterized but not fully identified using several extraction and degradation methods, as a function of sample concentration.
Lake River HPLC Spectrophotometry Post-column derivatization

"Monitoring Of Dissolved Reactive Phosphorus In Waste Waters By Flow Injection Analysis. 1. Method Development And Validation"
Water Res. 1996 Volume 30, Issue 9 Pages 1959-1964
Richard L. Benson, Yen B. Truong, Ian D. McKelvie* and Barry T. Hart

Abstract: A laboratory-manufactured automated FIA system was used. Wastewater samples (40 µL) were injected into a water carrier stream (C1) and sequentially merged with a further carrier stream of 5.2 g/l KCl/7.1 m/l HCL (C2) then 10 g/l ammonium molybdate/35 ml/l H2SO4 (colorimetric reagent; R1) and 0.2 g/l tin (II) chloride/2 g/l hydrazinium sulfate/28 ml/l H2SO4 (reducing agent; R2). Flow rates were 1.2, 0.58, 0.86 and 0.58 ml/min for C1, C2, R1 and R2, respectively. Detection was at 635 nm. Calibration graphs were linear up to 25 mg/l P; detection limit was 0.05 mg/l. RSD were n=11). Results correlated well with those obtained using a standard batch method.
Waste Spectrophotometry Process monitoring Automation Method comparison

"Monitoring Of Dissolved Reactive Phosphorus In Waste Waters By Flow Injection Analysis. 2. Online Monitoring System"
Water Res. 1996 Volume 30, Issue 9 Pages 1965-1971
Richard L. Benson*, Yen B. Truong, Ian D. McKelvie*, Barry T. Hart, Glenn W. Bryant and William P. Hilkmann

Abstract: Modifications to a method described previously (Ibid, 1996, 30, 1959) are presented. The manifold is illustrated; the main differences are the removal of the carrier stream of KCl/HCl, an increase to an 80 µL injection loop and the use of two solenoid valves for injection. Waste water samples were filtered to 0.2 µm then injected into a water carrier stream. They were then sequentially merged with 10 g/l ammonium molybdate/35 ml/l H2SO4 (colorimetric reagent) and 0.2 g/l tin (II) chloride/2 g/l hydrazinium sulfate/28 ml/l H2SO4 (reducing agent). Detection was at 635 nm. Calibration graphs were linear up to 2 mg/l P; the detection limit was 0.05 mg/l. Details of construction, field testing and validation are presented. Results agreed with those obtained using a validated laboratory method.
Waste Spectrophotometry Standard method Process monitoring

"Determination Of Phosphorus And Silicon In Carbon Steel And Low-alloy Steel By Flow Injection Analysis"
Yejin Fenxi 1989 Volume 9, Issue 3 Pages 30-33
Shen, Jihua; Miao, Fengqin

Abstract: The determination is based on the molybdenum blue method. The sample solution is treated with NH4F to eliminate the interference of ferric molybdate. The sample solution is used as the carrier flow and mixed with ammonium molybdate solution to form the heteropolyacid. After a fixed amount of reducing agent is injected, molybdenum blue forms for determination of phosphorus and silicon. The method is simple and rapid in analysis of carbon and alloy steel.
Carbon Alloy Spectrophotometry Interferences

"Determination Of Phosphorus Content In Steels Using Flow Injection Into An Argon-water Carrier For Inductively Coupled Plasma-mass Spectrometry"
ISIJ Int. 1997 Volume 37, Issue 9 Pages 878-884
A. G. COEDO, T. DORADO, I. PADILLA and F. J. ALGUACIL

Abstract: This paper describes a methodology for the determination of phosphorus in steels using argon-water carrier, in flow injection with Inductively Coupled Plasma Mass Spectrometry. 31P is a monoisotopic element and its determination, at very low levels, is very difficult due to contamination problems and interference inherent in the plasma and solvents. These unduly raise the background being necessary a sample pretreatment step to achieve the required contents. To dissolve the samples in this study, a microwave digestion system was applied to minimize the sample preparation time, the quantities of reagents and the risk of contamination. A mercury cathode electrolysis was used for performing a rapid matrix removal/analyte enrichment. The use of an argon-water stream as carrier yielded an enhancement in sensitivity and the detection limit was improved by a factor of approximately 2.5 when compared with that experienced using flow injection into an all-water carrier. Optimization of the operating conditions for the argon-water flow injection and for Inductively Coupled Plasma Mass Spectrometer, were selected with respect to the peak height sensitivity and were found to be dependent on the nebulizer gas flow-rate, the radio frequency power, the sample injection volume and the carrier flow-rate. The detection limit based on a sample rate of 0.02 g ml-1 was 0.4 mg g-1 and the relative standard deviations at 100 and 10 mg g-1 P solution were 2.0 and 15 % respectively. Data are presented for three Standard Reference Materials: JSS 003-2, (from Japanese Iron and Steel Certified Reference Materials); and ECRMs 285-1 and 278-1 (from Bureau of Analysed Samples LTD).
Alloy Mass spectrometry Optimization Reference material Interferences

"Determination Of Phosphorus In Small Amounts Of Protein Samples By ICP-MS"
Anal. Bioanal. Chem. 2003 Volume 375, Issue 4 Pages 561-566
J. Sabine Becker, Sergei F. Boulyga, Carola Pickhardt, J. Becker, Stefan Buddrus, Michael Przybylski

Abstract: Inductively coupled plasma mass spectrometry (ICP-MS) is used for phosphorus determination in protein samples. A small amount of solid protein sample (down to 1 µg) or digest (1-10 µL) protein solution was denatured in nitric acid and hydrogen peroxide by closed-microvessel microwave digestion. Phosphorus determination was performed with an optimized analytical method using a double-focusing sector field inductively coupled plasma mass spectrometer (ICP-SFMS) and quadrupole-based ICP-MS (ICP-QMS). For quality control of phosphorus determination a certified reference material (CRM), single cell proteins (BCR 273) with a high phosphorus content of 26.8±0.4 mg g-1, was analyzed. For studies on phosphorus determination in proteins while reducing the sample amount as low as possible the homogeneity of CRM BCR 273 was investigated. Relative standard deviation and measurement accuracy in ICP-QMS was within 2%, 3.5%, 11% and 12% when using CRM BCR 273 sample weights of 40 mg, 5 mg, 1 mg and 0.3 mg, respectively. The lowest possible sample weight for an accurate phosphorus analysis in protein samples by ICP-MS is discussed. The analytical method developed was applied for the analysis of homogeneous protein samples in very low amounts [1-100 µg of solid protein sample, e.g. β-casein or down to 1 µL of protein or digest in solution (e.g., tau protein)]. A further reduction of the diluted protein solution volume was achieved by the application of flow injection in ICP-SFMS, which is discussed with reference to real protein digests after protein separation using 2D gel electrophoresis. The detection limits for phosphorus in biological samples were determined by ICP-SFMS down to the ng g-1 level. The present work discusses the figure of merit for the determination of phosphorus in a small amount of protein sample with ICP-SFMS in comparison to ICP-QMS.

"A Microplate Assay To Measure Soil Microbial Biomass Phosphorus"
Biol. Fert. Soils 2004 Volume 40, Issue 3 Pages 201-205
Richard Jeannotte, David W. Sommerville, Chantal Hamel, and Joann K. Whalen

Abstract: Quantification of phosphorus (P) concentrations in microbial biomass is required to better understand how P immobilization and turnover in soils are controlled by environmental and anthropogenic factors. Soil microbial biomass P (MBP) is generally extracted using the chloroform fumigation-direct extraction procedure and then analyzed for P using the ammonium molybdate-ascorbic acid method on a flow injection analysis (FIA) system. Our objective was to determine whether a microscale malachite green method on a microplate system would provide as accurate MBP analysis as the ascorbic acid method on an FIA system. Twelve soils were collected from agricultural fields in southwestern Quebec, fumigated with chloroform and extracted with 0.5 M NaHCO3 (pH 8.5). The dissolved inorganic phosphorus (DIP) concentration in fumigated soils was not affected by the method of analysis, and results from the two systems of analysis were significantly correlated (r =0.998, P <0.05). The MBP concentrations in these agricultural soils were between 0.36 and 60.05 µg P g-1, consistent with other published values. Our results indicate that MBP can be assessed equally well with the malachite green method using a microplate system as with the ascorbic acid method on an FIA system. The microplate system is rapid and requires smaller volumes of samples and reagents than the FIA system, thus reducing the quantity of waste produced. We conclude that the microscale malachite green method could be applied to measure the MBP concentration in a wide range of soils with good sensitivity, reproducibility and accuracy.
Environmental Spectrophotometry Method comparison

"Flow Analysis Techniques For Phosphorus: An Overview"
Talanta 2005 Volume 66, Issue 2 Pages 307-331
Jos&eacute; Manuel Estela and V&iacute;ctor Cerd&agrave;

Abstract: A bibliographical review on the implementation and the results obtained in the use of different flow analytical techniques for the determination of phosphorus is carried out. The sources, occurrence and importance of phosphorus together with several aspects regarding the analysis and terminology used in the determination of this element are briefly described. A classification as well as a brief description of the basis, advantages and disadvantages of the different existing flow techniques, namely; segmented flow analysis (SFA), flow injection analysis (FIA), sequential injection analysis (SIA), all injection analysis (AIA), batch injection analysis (BIA), multicommutated FIA (MCFIA), multisyringe FIA (MSFIA) and multipumped FIA (MPFIA) is also carried out. The most relevant manuscripts regarding the analysis of phosphorus by means of flow techniques are herein classified according to the detection instrumental technique used with the aim to facilitate their study and obtain an overall scope. Finally, the analytical characteristics of numerous flow-methods reported in the literature are provided in the form of a table and their applicability to samples with different matrixes, namely water samples (marine, river, estuarine, waste, industrial, drinking, etc.), soils leachates, plant leaves, toothpaste, detergents, foodstuffs (wine, orange juice, milk), biological samples, sugars, fertilizer, hydroponic solutions, soils extracts and cyanobacterial biofilms are tabulated.
Review