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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Nebulizer

Classification: Manifold component -> Nebulizer

Citations 86

"Determination Of Mercury In Biological Samples Using Organic Compounds As Matrix Modifiers By Inductively Coupled Plasma Mass Spectrometry"
J. Anal. At. Spectrom. 1999 Volume 14, Issue 8 Pages 1183-1186
Cao Shuqin, Chen Hangting and Zeng Xianjin

Abstract: A method was developed for the determination of total mercury in biological samples. The effects of aqueous ammonia, ethylenediamine and triethanolamine on Hg signal intensity by inductively coupled plasma mass spectrometry has been evaluated and the possible mechanisms discussed. It has been proved that the signal intensity of Hg significantly increases with adding, in the presence of small amounts of aqueous ammonia, ethylenediamine or triethanolamine. The normalized intensity (the signal intensity ratio with amine and without amine) of Hg increases as the concentration of aqueous ammonia, ethylenediamine or triethanolamine increases, but the degree of enhancement of aqueous ammonia was smaller than that of ethylenediamine and triethanolamine. The normalized intensity of Hg with aqueous ammonia, ethylenediamine and triethanolamine decreases as the nebulizer flow rate increases, but decreasing degree of aqueous ammonia was smaller than that of ethylenediamine and triethanolamine. The higher the RF powers the higher the normalized intensity of Hg at the same nebulizer flow rate. The addition of aqueous ammonia, ethylenediamine and triethanolamine into analytical solutions significantly improved the transport efficiency of Hg. The detection limit of Hg is improved about ten times by the addition of ethylenediamine or triethanolamine under the optimum experimental parameters. The method has been used to determine mercury in biological standard reference materials (SRM). The analytical results are very close to the certified values and the determined values for similar samples.

"Development Of A New Liquid Chromatography Method For The Separation And Speciation Of Organic And Inorganic Selenium Compounds Via Particle Beam-hollow Cathode Glow Discharge-optical Emission Spectroscopy"
J. Anal. At. Spectrom. 2002 Volume 17, Issue 2 Pages 99-103
W. Clay Davis, Fuxia Jin, Melissa A. Dempster, Jennifer L. Robichaud and R. Kenneth Marcus

Abstract: A system for the separation and detection of inorganic and organic selenium compounds utilizing particle beam-hollow cathode glow discharge-optical emission spectroscopy (PB-HC-OES) as a selenium-specific detector has been investigated. The PB interface includes a thermoconcentric nebulizer to generate a finely dispersed aerosol, a heated metal spray chamber for desolvation, and a two-stage momentum separator, which removes solvent vapor. The resulting beam of dry analyte particles are introduced into a heated (similar to250°C) hollow cathode, where they are vaporized, atomized and excited within the plasma. Using LC-PB-HC-OES the following compounds were examined: selenocystine, selenomethionine, selenoethionine, sodium selenate, and sodium selenite. A reverse phase ion-pairing chromatography method was developed to separate these five compounds (both organic and inorganic), with UV absorbance monitored at 210 nm. The Se I 204.0 nm atomic emission intensity was then monitored by coupling the LC column with the PB-HC-OES system. Emission responses for the selenium of both the organic and inorganic compounds in flow injection mode using 200 µL injection volumes indicate detection limits of similar to200 ppb (100 ng) with less than 10% RSD variability for triplicate injections over a range of 200-1960 ng. The retention times of the five analyte peaks are similar to those detected by UV absorbance, demonstrating the ability of the PB interface to preserve the chromatographic integrity of the separation. Optical emission detection of liquid chromatographic separations of the selenium-containing compounds demonstrates the feasibility of the PB-HC-OES system as a simple selenium-specific detector for liquid chromatography.

"Determination Of Cadmium By Suction-flow Liquid - Liquid Extraction Combined With Inductively Coupled Plasma Atomic-emission Spectrometry"
Anal. Chim. Acta 1985 Volume 174, Issue 1 Pages 183-189
Takahiro Kumamaru, Yoko Nitta, Fumio Nakata and Hiroshi Matsuo, Masahiko Ikeda

Abstract: A flow-manifold system is proposed that permits specific online suction-flow liquid extraction of Cd as its diethyldithiocarbamate from a discrete aqueous sample into CCl4 (I). The organic extract is fed into the nebulizer of the ICP spectrometer by a peristaltic pump, to achieve a 250-fold increase in sensitivity compared with direct aspiration of the aqueous solution The sampling frequency is 20 h-1 and the consumption of I and of 5% (w/v) Na diethyldithiocarbamate solution is 0.6 mL min-1. The calibration graph is rectilinear up to 300 ppb of Cd, the detection limit is 0.4 ppb, the coefficient of variation (n = 10) at the 50-ppb level is 1.5%, and only Mn(II), Co(II) and Ni interfere significantly. Such interference can be decreased or eliminated by the addition of citrate to the buffer solution Interference by large amounts of alkali and alkaline-earth metals and most anions can be avoided by extraction. The proposed method was applied to the determination of Cd in NBS SRM 1571 orchard leaves, NIES (Japan) CRM No. 1 pepperbush and CRM No. 6 mussel to give results in good agreement with the certified values.
Cadmium NIST 1571 NIES 1 NIES 6 Plant Spectrophotometry Sample preparation

"Determination Of Boron In Water By Flow Injection Inductively Coupled Plasma Emission Spectrometry"
Anal. Chim. Acta 1989 Volume 218, Issue 1 Pages 69-76
Phillip L. Kempster and Henk R. Van Vliet, Jacobus F. Van Staden

Abstract: An 11 mL mini-cloud chamber, containing a tangentially attached aerosol exit tube that induced spiral motion in the aersol within the chamber, was incorporated into a flow injection ICP-AES system (illustrated) for the cited analysis. The carrier stream (H2O) was pumped through each 300 µL sample loop, or in turn to the ICP nebulizer, the opposite sample loop being filled via the sample via negative pressure. The carrier outlet port of the sampling valve was connected to the nebulizer by polyethylene tubing, and B was determined at 249.68 nm. The calibration graph was rectilinear from 0.5 to 25 mg L-1 of B, and the coefficient of variation for 2.5 to 25 mg L-1 were 5.4% (n = 10). 'Memory effects' were ~5-fold smaller with the mini-cloud chamber than with a 110 mL cloud chamber. Aluminum, Ca, Cr, Fe, Na and P did not interfere. Sample throughput was 320 h-1 at a carrier flow rate of 3.5 mL min-1. The method was also applied in the determination of Ca, Mg, Mn and Sr in water.
Boron Calcium Magnesium Manganese Strontium Environmental Spectrophotometry

"Signal Analysis And Data Processing For Inductively Coupled Plasma-atomic Emission Spectrometry With Microliter Sample Introduction. 1. Introduction, Signal And Noise Characteristics"
Anal. Chim. Acta 1989 Volume 226, Issue 1 Pages 53-72
P. J. H. Scheeren, P. J. H. Seeverens, F. J. M. J. Maessen and H. C. Smit

Abstract: The introduction of microlitre samples has found widespread applications when inductively coupled plasma-atomic emission spectrometry (ICP-AES) is used for detection in liquid chromatography or in flow-injection systems. This technique for introducing small samples is poorly characterized. The properties of the transient signals and the noise associated with 'plug' sample introduction are examined here to establish guidelines for improving the technique. The analytical performance is characterized by parameters deduced from the signal-to-noise power ratio. The influence of the operating conditions of ICP-AES on the technique is described for cross-flow, concentric and high-solids nebulizers. The performance of microlitre sample injection proved to be similar to that of continuous sample introduction for the cross-flow and concentric nebulizers.
Spectrophotometry

"Flow Injection For Continuous Sample Introduction In Solid-substrate Room Temperature Phosphorescence"
Anal. Chim. Acta 1990 Volume 231, Issue 2 Pages 289-293
A. D. Campiglia, A. Berthod and J. D. Winefordner

Abstract: A flow injection system is described and illustrated for continuous sample introduction in two-nebulizer phosphorescence analysis. Thallium acetate (0.1M) in aqueous 50% ethanol was used as heavy-atom enhancer, and sprayed continuously on to the moving filter paper at a flow rate adjusted to deliver ~10 µL cm-2 of substrate. The method was tested with use of phenanthrene (I), pyrene and 4-aminobenzoic acid (II) as model analytes. Detection limits were in the ng range and, for I and II, calibration graphs were rectilinear over 2 orders of magnitude. Precision was 10.6 to 12.8%.
Phenanthrene Pyrene 4-Aminobenzoic acid Phosphorescence

"Determination Of Gold In Ore By Flame Atomic Absorption Spectrometry With Flow Injection Online Sorbent Extraction Preconcentration"
Anal. Chim. Acta 1991 Volume 245, Issue 1 Pages 7-11
Shukun Xu, Lijing Sun and Zhaolun Fang

Abstract: A section of plastic Eppendorf pipette tip, measuring 0.6 and 5.0 mm i.d. at the lower and upper ends, respectively, was packed tightly (~2 cm) with Amberlite XAD-8 resin (25 to 50 mesh) (~220 µL). The column was fitted in the flow injection manifold such that adsorbed complexes were collected mainly at the narrower end and eluted from the broader to the narrower end. Samples (10 g) were heated (570°C, 30 min) in a muffle and then digested (50 min) in boiling 1:1 aqua regia (80 ml). After evaporation almost to dryness, concentrated HCl (10 ml) was added and brought to the boil. After cooling, the leachate and undissolved residue were made up to 250 mL with water. The complexes formed were adsorbed on the XAD-8 resin (7.6 mL min-1) and, after 40 s, adsorbed analyte was eluted with aqueous 95% ethanol (3.6 mL min-1) into the nebulizer and flame for determination by AAS (242.8 nm). The calibration graph was rectilinear up to 0.5 µg mL-1 and the detection limit was 2 ng mL-1 in the leachate, corresponding to 0.05 mg kg-1 in the ore. The coefficient of variation (n = 11) was 1.4% at 0.25 µg mL-1 for a single digest solution; the overall coefficient of variation was 3 to 5%. Recoveries of known amounts added to samples were 97 to 107%. The sampling rate was 60 h-1.
Gold Geological Sample preparation Spectrophotometry Sample preparation

"Frontiers In Elemental Analysis By Mass Spectrometry"
Anal. Chim. Acta 1991 Volume 250, Issue 1 Pages 61-70
R. S. Houk*, S. C. K. Shum and D. R. Wiederin

Abstract: New developments in inductively coupled plasma mass spectrometry (ICP-MS) and laser desorption-time-of-flight mass spectrometry (LD-TOF-MS) for inorganic analysis are described. These include fundamental studies of the ion extraction, process in ICP-MS, development of a highly efficient nebulizer, isotope tracer studies, measurement of elemental speciation by liquid chromatography with ICP-MS detection and characterization of the structures of solids by ion association. The possibilities of determining inorganic species in solutions by electrospray MS are also described.
LC Mass spectrometry

"Supercritical Carbon Dioxide As A Carrier For Sample Introduction In Atomic Absorption Spectrometry"
Anal. Chim. Acta 1992 Volume 258, Issue 1 Pages 55-60
S. R. Bysouth and J. F. Tyson*

Abstract: A manifold was constructed to interface a flow injection supercritical CO2 system with the spray chamber of an AAS system or the quartz tube of a graphite furnace. The manifold consisted of 0.38 mm stainless steel tubing connected at one end to a reciprocating pump via a pressure transducer; the pump was cooled with ethylene - water mixture which was chilled in dry ice. The other end of the manifold was heated by means of a heating block to 260°C and connected to the spray chamber or quartz tube. The performance of the system was investigated by injecting portions of a copper complex in MIBK into the supercritical CO2 carrier stream; highest sensitivity was obtained when the working pressure was 1000 psi. The use of a supercritical carbon dioxide carrier to transport organic solutions of metal complexes to a heated restrictor is demonstrated as a means of aerosol or vapor generation for sample introduction in flame atomic absorption spectrometry. Calibrations obtained using conventional pneumatic nebulization of continuously aspirated solutions or using flow injection into a water carrier are compared with those obtained using the carbon dioxide carrier. Injection of solutions of copper pyrrolidinedithiocarbamate in MIBK into a carbon dioxide carrier at 1000 psi was shown to be 1.2 times more sensitive than injection of the same solutions into a water carrier with conventional nebulization. The sensitivity of continuous nebulization of the solutions, however, was not achieved. Dissolution of solid copper acetylacetonate in supercritical carbon dioxide is demonstrated and subsequent vaporization followed by atomization in a heated quartz furnace is shown to occur.
Copper Spectrophotometry Spectrophotometry

"Ultratrace Determination In High-purity Molybdenum And Tungsten With Ion Chromatographic Trace-matrix Separation. 3. Ultratrace Analysis Using Atomic Spectrometry"
Anal. Chim. Acta 1992 Volume 258, Issue 1 Pages 109-122
A. Seubert

Abstract: Ultratrace anal. of Mo and W using direct coupling of ion chromatography (IC) trace-matrix-sepns. (SMT) and inductively coupled plasma atomic emission spectrometry (ICP-AES) as an atomic spectrometric detection technique is described. The right choice of the nebulizer unit of the ICP system and appropriate chromatography eluents and flow-rates result in a stable, highly sensitive detection system IC-SMT-ICP. The characteristics of ICP-AES as a chromatography detection method and the application of internal standaridization during the measurement of a transient signal are discussed. The importance of the integration time for the registration of transient signals is pointed out. Every elution peak should be covered by 8-16 data points. The final comparison with known batch procedures for trace-matrix-sepns. demonstrates the clear advantage of the combined method IC-SMT-ICP with direct coupling of ion chromatography and atomic spectrometry.
Metals, trace High purity High purity HPIC Spectrophotometry

"Coupled Flow Injection Analysis - Flame-atomic Absorption Spectrometry For The Quantitative Determination Of Aluminum In Beverages And Waters Incorporating Online Cation-exchange"
Anal. Chim. Acta 1992 Volume 269, Issue 1 Pages 1-7
Henryk J. Salacinski, Philip G. Riby, Stephen J. Haswell*

Abstract: Tea leaf samples (0.5 g) were digested at 85°C for 45 min in a mixture of HNO3 (4 ml) and HClO4 (1 ml) and diluted to 10 mL with 5% HNO3. Samples of tea and coffee infusions and water were acidified with 5% HNO3. These samples (250 µL) were injected via a loop into a SCX preparative column (500 mg) with water as the carrier, followed by elution with 4 M HCl (250 µL) directly into the nebulizer of a flame AAS for the determination of Al. The AAS and nebulizer were optimized for max. absorbance prior to the determination and the peristaltic pump of the flow system set to give an equivalent delivery. Rectilinear calibrations were obtained from 0.07 to 6.45 µg mL-1 of Al from various timed depositions with a coefficient of variation of 1.1% and a detection limit of 75 ng mL-1. A method for determining the aluminum levels in local water, tea leaf digest, tea and coffee infusions by means of online cation exchange flow injection - flame atomic absorption spectrometry (FIA-FAAS) is described. Quant. results can be carried out down to 75 ng mL-1 of Al using sample volumes in the range 6.0-24.0 mL. The method using a conventional FAAS system was found to be rapid, simple and relatively inexpensive offering good selectivity and typical relative standard deviation of 1-2% (n=10) with a relative error of about 2%.
Aluminum Environmental Leaves Tea Coffee Ion exchange Sample preparation Sample preparation Spectrophotometry

"Rapid Determination Of Zinc And Iron In Foods By Flow Injection Analysis With Flame Atomic Absorption Spectrophotometry And Slurry Nebulization"
Talanta 1990 Volume 37, Issue 7 Pages 711-718
João Carlos de Andrade*, Frederick C. Strong, III and Nadir J. Martin

Abstract: A rapid method of determining zinc and iron in food by flame atomic absorption spectrophotometry with slurry nebulization into an air-acetylene flame has been developed. A V-groove, clog-free Babington-type nebulizer, coupled to a single-line flow injection analysis (FIA) system, was employed to introduce the slurry into the spray chamber. Under the FIA conditions described, an injection frequency of 120/hr is possible, with negligible carry-over and memory effects. The calibration graphs were obtained by using various concentrations (up to 0.1 g/ml) of white bean homogenate as standards, rather than solutions. The method has been applied to various kinds of foods, including grains, vegetables, fruits and sausage. Homogenization of semi-prepared samples to form slurries took only 4 min. Relative deviations between results by the slurry and solution methods for both elements averaged 2-3%. Detection limits by the slurry method were 0.3 µg/ml Zn and 0.6 µg/ml Fe. A V-groove, Babington-type nebulizer, coupled to a single-line flow injection analysis system, was used to introduce sample slurry into the spray chamber for AAS determination. An injection frequency of 120 h-1 was possible, with negligible carry-over and memory effects. Calibration graphs were obtained by using 0.1 g mL-1 of white bean homogenate as standards. Homogenization of semi-prepared samples to form slurries took 4 min. Of air - acetylene and air - propane flames for the AAS, the former was preferred due to its rectilinear calibration graph. Relative deviations of results by slurry and solution methods for both Zn and Fe were 2 to 3%. Detection limits for the slurry method were 0.3 and 0.6 µg mL-1 of Zn and Fe, respectively. The method was applied to various foods, including grains, vegetables, fruits and sausage.
Iron Zinc Food Vegetable Grain Spectrophotometry

"Validation Of The Determination Of Copper And Zinc In Blood Plasma And Urine By ICP-MS With Cross-flow And Direct Injection Nebulization"
Talanta 1997 Volume 44, Issue 8 Pages 1389-1396
J. Szpunar*, J. Bettmer, M. Robert, H. Chassaigne, K. Cammann, R. Lobinski and O. F. X. Donard

Abstract: Use of a Perkin-Elmer cross-flow nebulizer and a direct-injection nebulizer (Microneb 200, CETAC, Omaha, Ne, USA) were compared for the ICP-MS determination of Cu and Zn using an Elan 600 instrument (Perkin Elmer SCIEX). Plasma and urine were diluted 20- and 10-fold, respectively, in 0.05% HNO3 and 10 µg/l 89Y was added as internal standard. Isobaric interferences were eliminated for 65Cu and most of the Zn nuclides. Flow injection direct-injection nebulization was optimized for the analysis of 1-2 µL samples (parameters tabulated). Standard additions was used to eliminate matrix effects. Results using the flow injection method on reference materials agreed with the certified values.
Copper Zinc Blood Plasma Urine Mass spectrometry

"Investigation Of Performance Enhancement Of Flame Photometric Signal Using A Cylindrical Impactor In The Spray Chamber"
Talanta 1997 Volume 44, Issue 10 Pages 1919-1922
Ladislau Kékedy-Nagy

Abstract: The effect of a cylindrical impactor in the spray chamber of a flame photometer on the characteristics of the aerosol formed, on the transport-efficiency of the nebulizer-spray chamber system, as well as on the analytical signal has been investigated. The variables were: the diameter Φ of the cylindrical impactor and its position, i.e., the distance d in front of the tip of pneumatic nebulizer capillary where the impactor was fixed. The performance characteristics of an 1 mm Φ impactor was fixed at d=5 mm was superior to that of a conventional 8 mm Φ spherical bead.
Spectrophotometry

"Determination Of Lead In Blood Using Flow Injection And A Nebulizer Interface For Flame Atomic Absorption Spectrometry"
Analyst 1988 Volume 113, Issue 4 Pages 591-594
Olle Nygren, Carl-Axel Nilsson and Anders Gustavsson

Abstract: Blood samples (4.0 g), deproteinized by shaking with HNO3 - trichloroacetic acid followed by centrifugation, were injected into the flow system and were carried by water (2 mL min-1) via shrinkable tubing to the nebulizer interface, which consisted of a concentric glass nebulizer mounted in an aerosol chamber heated by two tapes (operated at 220 V a.c.) and connected to the flame AAS burner head. The nebulizer gas was air (1.5 l min-1), and an air - acetylene flame was used. Evaluation of the absorbance signal was improved with use of a personal computer system. The calibration graph, obtained by the standard-additions method, was rectilinear from 0.3 to 4.5 µM; the detection limit was 0.06 µM-Pb, which was a 12-fold improvement compared with that obtained with unmodified instrumentation, and the coefficient of variation was 5% at 0.5 µM-Pb in blood (n = 3). The method was used to determine Pb in blood samples from exposed workers. Results correlated well with those of an electrothermal atomization - AAS method.
Lead Blood Spectrophotometry

"Models For Dispersion In Flow Injection. 2. Two Tanks In Parallel Model"
Analyst 1989 Volume 114, Issue 11 Pages 1453-1458
David C. Stone and Julian F. Tyson

Abstract: The application is discussed of two models, based on the stirred mixing tanks, the well stirred tank and the two tanks in parallel models; results are presented for flow manifolds with both flame AAS and solution spectrophotometric detectors. Either model can be applied to describe the dispersion generated by the nebulizer spray chamber of a flame AAS. They can also be applied to manifolds under conditions giving rise to peaks having exponential-type rise and fall curves.
Spectrophotometry Spectrophotometry

"Determination Of Cobalt In Two Glasses By Atomic Absorption Spectrometry After Flow Injection Ion-exchange Preconcentration"
Analyst 1991 Volume 116, Issue 11 Pages 1141-1144
M. C. Valdés-Hevia y Temprano, J. Pérez Parajón, M. E. Díaz García and A. Sanz-Medel

Abstract: Ground glass (0.5 g) was digested with concentrated HNO3 - concentrated HCl04 - HF (details given) and the digest was treated with HCl, boric acid, NaOH and sodium citrate. After dilution with 0.1 M ammonium acetate - HCl buffer solution of pH 2.7 (buffer A), a 1 mL portion of the solution was injected into a carrier stream (0.5 mL min-1) of buffer A and passed through a reaction coil (3 ml). The mixture was merged with a second carrier stream (2.5 mL min-1) of 1 M NH3 - NH4Cl buffer solution of pH 8.5 and passed sequentially through a reaction coil (5 m) and a minicolumn (10 cm x 3 mm) loaded with Chelex-100. After 5 to 6 min, 200 µL of 5 M HNO3 was injected into the system to elute the Co directly into the nebulizer of the spectrometer. A schematic diagram of the flow manifold is given; operating conditions are tabulated. The calibration graph was rectilinear for 1.2 µg mL-1 of Co; the detection limit was 20 ng mL-1. For 0.5 µg mL-1 of Co, the coefficient of variation (n = 10) was 1.5%. The detection limit was 4-fold better than that obtained by direct aspiration without pre-concentration.
Cobalt Commercial product Sample preparation Ion exchange Spectrophotometry

"Investigation Of Small Volume Cloud Chambers For Use In Inductively Coupled Plasma Nebulisation"
J. Anal. At. Spectrom. 1987 Volume 2, Issue 8 Pages 823-828
Phillip L. Kempster, Jacobus F. Van Staden and Henk R. Van Vliet

Abstract: The characteristics of three small volume cloud chambers, constructed with the aim of reducing sample wash-in and wash-out times in inductively coupled plasma atomic emission spectrometry were investigated, and compared with the characteristics of a commercially available 110 mL double-barrel type cloud chamber. Analytical performance was evaluated with respect to drainage, nebulisation efficiency, sensitivity, precision, detection limits, wash-in and wash-out times and the evaluation of volatilisation interferences from phosphate and aluminium on calcium, as well as the effect of sodium on calcium emission intensity.
Spectrophotometry

"Impulse Nebulization Atomic Absorption Spectrometry. 1. Model For The Response Of A Flame Atomizer"
J. Anal. At. Spectrom. 1988 Volume 3, Issue 1 Pages 217-225
László Bezúr

Abstract: A model for predicting the instrumental response with impulse-nebulization or flow injection sample introduction is developed, based on the mass balance of the atomizer, axial dispersion and the time constant of the spectrometer, and involving all the important parameters, e.g., sample concentration, volume and flow rate, nebulization efficiency and gas flow rate. It gives good agreement with experiment for impulse nebulization, and shows that the dispersion increases from the front to the rear of a flow injection AAS peak.
Manganese Spectrophotometry

"Characteristics Of Flow Injection Inductively Coupled Plasma Mass Spectrometry For Trace Metal Determination"
J. Anal. At. Spectrom. 1988 Volume 3, Issue 2 Pages 349-354
John R. Dean, Les Ebdon, Helen M. Crews and Robert C. Massey

Abstract: Flow injection sample introduction in ICP-MS alleviates problems arising from high salt content, viscosity and high acid concentration. A commercial ICP-MS instrument (Plasmaquad) was used, sample aerosol generation was achieved with either a fixed cross-flow nebulizer or a high-solids nebulizer, and a manually operated flow injection valve was used. All operating conditions are tabulated. Biological reference materials were analyzed, following digestion by various methods, by ICP-MS with external calibration or isotope dilution. Results agreed well with certified values for both methods. The technique was applied to determine Pb in powdered mixed diet samples and Zn isotope ratios in blood plasma. The main advantage of flow injection over continuous nebulization was the small amount of sample required.
Lead Metals, trace Zinc Blood Plasma Powder Mass spectrometry Mass spectrometry Sample preparation

"Analysis Of Samples With High Dissolved Solids Content Using Flow Injection Flame Atomic Absorption Spectrometry"
J. Anal. At. Spectrom. 1989 Volume 4, Issue 1 Pages 91-95
Zhaolun Fang, Berhard Welz and Gerhard Schlemmer

Abstract: The flow injection sample introduction system (see earlier in Section J) was applied to flame AAS analysis of solution with high solids content. Carrier flow rate, nebulizer uptake rate, sample volume and sampling frequency were optimized with use of 1 mg L-1 of Cu in aqueous 30% NaCl as model sample; values of 6 mL min-1, 10.5 mL min-1, 330 µL and 125 h-1, respectively, were chosen. For the above solution, 1 mg L-1 of Cu in saturated aqueous lithium borate and 5 mg L-1 of Cu in a concentrated K2HPO4 solution, the coefficient of variation for Cu were 2.0, 1.5 and 2.0%, respectively. After 167 injections of the NaCl solution, peak size had decreased by 10%, but the precision was maintained.
Copper Spectrophotometry

"Optimization Of Experimental Parameters For Flow Injection Flame Atomic Absorption Spectrometry"
J. Anal. At. Spectrom. 1989 Volume 4, Issue 1 Pages 83-89
Zhaolun Fang and Bernhard Welz

Abstract: The optimization of liquid transfer from a flow injection system to flame AAS was studied in respect of, e.g., nebulizer uptake rate (10 mL min-1), carrier stream flow rate (0.2 to 6 mL min-1), air and water compensation at low carrier flow rates, and the use of a flow spoiler. Lead and Ca were used as test analytes. Flow compensation was not generally necessary if the carrier flow rate was much lower than the nebulizer uptake rate. Insertion of the flow spoiler gave improved precision, which was also obtained by addition of air compensation if the carrier flow was 0.4 mL min-1.
Lead Calcium Spectrophotometry

"Study Of The Possible Benefits Of Flow Injection Sample Introduction For Flame Atomic Absorption Spectrometry"
J. Anal. At. Spectrom. 1989 Volume 4, Issue 2 Pages 191-194
Julian F. Tyson, Christina E. Adeeyinwo and Stephen R. Bysouth

Abstract: A brief review is presented, with 30 references, of flow injection techniques used in conjunction with atomic spectrometry. The possible benefits of flow injection sample introduction at reduced flow rates to reduce interference and improve detection limits were studied. Conclusions are that such sample introduction does not result in any fundamental differences in signals compared with conventional nebulization, in that different operating parameters are still required for different figures of merit. The best approach for optimum detection limits in flow injection sample introduction is to maximize the peak height and minimize noise. By generation of a volatile metal chelate in a flow injection manifold for subsequent determination and with appropriate solvent extraction and heated tubing, it is possible to increase considerably the atomization efficiency over conventional nebulization. A brief review is presented, with 30 references, of flow injection techniques used in conjunction with atomic spectrometry. The possible benefits of flow injection sample introduction at reduced flow rates to reduce interference and improve detection limits were studied. Conclusions are that such sample introduction does not result in any fundamental differences in signals compared with conventional nebulization, in that different operating parameters are still required for different figures of merit. The best approach for optimum detection limits in flow injection sample introduction is to maximize the peak height and minimize noise. By generation of a volatile metal chelate in a flow injection manifold for subsequent determination and with appropriate solvent extraction and heated tubing, it is possible to increase considerably the atomization efficiency over conventional nebulization.
Spectrophotometry

"Direct Atomic-spectrometric Analysis By Slurry Atomization. 8. Flow Injection Inductively Coupled Plasma Atomic-emission Spectrometry"
J. Anal. At. Spectrom. 1989 Volume 4, Issue 2 Pages 219-222
Andrea J. Ambrose, Les Ebdon, Michael E. Foulkes and Philip Jones

Abstract: The analysis of slurries by flow injection ICP-AES was studied, with particular reference to the controlling parameters, viz, spray chamber design, sample injection volume, carrier stream flow rate and effect of torch injector size. A novel low-volume spray chamber was developed. Sample injection volume of 500 µL gave equivalent sensitivity to that of continuous nebulization; the optimum torch injector tube i.d. was 3 mm. By using this technique, excellent agreement with certified values and precision of 2% were obtained in determination of Ca, Fe, Mg, Mn, Cu and V in reference soils. (For Part VII see Anal. Abstr., 1989, 51, 1B192).
Calcium Copper Iron Magnesium Manganese Valine Environmental Spectrophotometry

"Evaluation Of Three Low-volume Interfaces For Organic Solvent Introduction To The Inductively Coupled Plasma - Applications To Flow Injection"
J. Anal. At. Spectrom. 1989 Volume 4, Issue 4 Pages 341-345
Timothy J. Brotherton, Peter E. Pfannerstill, John T. Creed, Douglas T. Heitkemper, Joseph A. Caruso and Sotiris E. Pratsinis

Abstract: Three low-volume sample delivery systems (described and illustrated) were evaluated for continuous solution nebulization and for flow injection introduction into the ICP: (i) a cooled mini-spray chamber, (ii) a desolvation interface, and (iii) a partial-suction injector. Each system was operated under the same conditions (tabulated). The max. solution delivery rates for each interface were >2 mL min-1 for both methanol and acetonitrile. Calibration graphs were rectilinear over three to four orders of magnitude in each instance. Detection limits under continuous solution nebulization conditions were in the mid- to sub ng mL-1 range. Flow injection peak widths were narrower for (i), (ii) and (iii) than for systems involving spray chambers with larger volume.
Spectrophotometry

"High-efficiency Low-sample-consumption Online Ion-exchange Preconcentration System For Flow Injection Flame Atomic Absorption Spectrometry"
J. Anal. At. Spectrom. 1989 Volume 4, Issue 6 Pages 543-546
Zhaolun Fang and Bernhard Welz

Abstract: The cited system was used for determination of heavy metals. Only 1.6 mL of sample solution was required for analysis, 120 samples h-1 could be analyzed, and enrichment factors of 25 to 31 were achieved for Cu, Cd and Pb. The coefficient of variation were 1.2 to 2.8%; e.g., for 100 µg L-1 of Cu the coefficient of variation was 1.5% (n = 81). The CPG/8-Q ion exchanger was used, and conical columns, short, small-bore conduits and three-dimensional disoriented reactors were used to limit the dispersion of the eluted sample zone. Low elution flow rates and high nebulizer uptake rates were used to improve nebulization efficiency. Application of the method in analysis of seawater is discussed.
Copper Cadmium Lead Metals, heavy Sea Spectrophotometry

"Minimization Of Non-spectroscopic Matrix Interferences For The Determination Of Trace Elements In Fusion Samples By Flow Injection Inductively Coupled Plasma Mass Spectrometry"
J. Anal. At. Spectrom. 1991 Volume 6, Issue 8 Pages 605-608
Jiansheng Wang, E. Hywel Evans and Joseph A. Caruso

Abstract: The efficiency of various ion lens tuning strategies, flow injection and the use of an internal standard were investigated for the determination of trace elements in real samples. Spiked recoveries showed that the use of an internal standard was preferable, if a 100% recovery was to be obtained. Good recoveries were also obtained by tuning the ion lenses for a max. 115In+ signal in a matrix blank solution containing 100 ng g-1 of In, while using continuous nebulization sample introduction. Tuning the ion lenses in the presence of the matrix yielded improved recoveries compared with tuning the lenses for a standard solution This work supplements Ibid., 1990, 5, 445.
Trace elements Mass spectrometry Sample preparation

"Transport Effects With Dribble And Jet Ultrasonic Nebulizers"
J. Anal. At. Spectrom. 1992 Volume 7, Issue 6 Pages 813-817
Matthew A. Tarr, Guangxuan Zhu and Richard F. Browner

Abstract: Ultrasonic nebulizers improve analyte transport compared with pneumatic types, but require partial or total solvent removal. Aerosol desolvation using a heated chamber and condenser reduced the solvent loading in plasma and increases analyte transport relative to transport without desolvation. The influence on emission signals of the interaction of each component in the introduction system is reported. The dribble and jet type sample injectors are compared; the jet type shows greater repeatability and improved peak shape for flow injection measurements.
Spectrophotometry

"Performance Of A Modular Thermospray Interface For Signal Enhancement In Flame Atomic Absorption Spectrometry Coupled Online To Flow Injection [analysis] Or Liquid Chromatography"
J. Anal. At. Spectrom. 1993 Volume 8, Issue 4 Pages 659-664
Erik H. Larsen and Jean-Simon Blais

Abstract: A simple and inexpensive thermospray interface is described that was connected to a flame AAS system without modification of the nebulizer and burner assembly. Details are provided of its construction and performance characteristics. The interface provided improved signal-noise and signal enhancement in a flow injection - AAS system with rectilinear calibration and detection limits of 1.9 ng of Cd, 8.5 ng of Cu and 27 ng of Pb. The use of the interface to couple HPLC to AAS was demonstrated for the determination of metallothioneins in biological samples.
Cadmium Copper Lead Biological Spectrophotometry

"Online Thermospray Continuous Volatilization Of Cobalt, Aluminum And Chromium Volatile Chelates And Determination By Heated-quartz-tube Atomic Absorption Spectrometry"
J. Anal. At. Spectrom. 1993 Volume 8, Issue 4 Pages 665-669
Maria S. Jiménez, José M. Mir and Juan R. Castillo

Abstract: A system for the introduction of gas-phase metal samples into an AAS is described. Analyte solutions at an appropriate pH for complex formation were pumped through one channel of a flow injection system and 0.5 mL portions were injected into the chelating reagent stream. The reactor has a sample loop (50 µL) and the complex was injected into an air-flow, transported into the thermospray (24 cm x 0.5 mm) and the vapor introduced into a quartz tube in the spectrometer heated in an air - acetylene flame. Optimum operating parameters and interference effects are examined and analytical parameters compared with analyzes using a nebulizer for sample introduction.
Cobalt Aluminum Chromium Spectrophotometry

"Detection Limits Versus Matrix Effects: Analysis Of Solutions With High Amounts Of Dissolved Solids By Flow Injection Inductively Coupled Plasma Mass Spectrometry"
J. Anal. At. Spectrom. 1993 Volume 8, Issue 6 Pages 927-931
Peter Richner

Abstract: The ICP-MS determination of trace impurities in high-purity nickel with use of flow injection or conventional solution nebulization was compared. The ability to analyze solution with high dissolved-solid content in flow injection mode in a carrier solution of 1% sample injections (0.2 ml) allowed 3 to 40-fold improvements in detection limits to achieve ppb levels; detection limits for 16 elements were tabulated and limits were defined mainly by blank values in the reagents and containers used.
Metal Mass spectrometry Spectrophotometry

"Evaluation Of A Microconcentric Nebulizer-cyclonic Spray Chamber For Flow Injection Simultaneous Multielement Inductively Coupled Plasma Optical Emission Spectrometry"
J. Anal. At. Spectrom. 1998 Volume 13, Issue 5 Pages 483-488
Terrance D. Hettipathirana and David E. Davey

Abstract: Merits of a µconcentric nebulizer and a cyclonic spray chamber for sample introduction to simultaneous multielement inductively coupled plasma optical emission spectrometry (ICP-OES) were evaluated. Sample delivery was both continuous and by flow injection (FI). All signal profiles were acquired and processed in the time-resolved mode. At solvent flow rates of 0.1 and 1.0 mL min-1, solvent transport efficiency to the ICP is ~90 and 50%, respectively. As a consequence, improvements in detection limits were observed compared with those using a conventional concentric nebulizer. Application of Sc as an internal standard to improve precision with FI sample delivery was also studied.
Metals Spectrophotometry

"Determination Of Technetium In Seawater Using Ion Exchange And Inductively Coupled Plasma Mass Spectrometry With Ultrasonic Nebulization"
J. Anal. At. Spectrom. 1998 Volume 13, Issue 9 Pages 875-878
Ahmet E. Eroglu, Cameron W. Mcleod, Kinson S. Leonard and David Mccubbin

Abstract: An enrichment-separation scheme employing a strong-base type anion-exchange resin was developed for the determination of99Tc in sea-water by inductively coupled plasma mass spectrometry utilising ultrasonic nebulisation with membrane desolvation. Samples were processed through an anion-exchange column to enrich Tc and to eliminate sea-water matrix ions. The limit of detection for 99Tc in sea-water based on processing a 14 mL sample was 0.03 ng l-1. Accuracy was verified with spike recovery experiments. The potential for rapid on-line sample processing via a microcolumn-flow injection system was demonstrated.
Technetium Sea Ion exchange Mass spectrometry

"Sensitivity Enhancements For Flow Injection Analysis-inductively Coupled Plasma Atomic Emission Spectrometry Using An Online Preconcentrating Ion-exchange Column"
Anal. Chem. 1985 Volume 57, Issue 1 Pages 21-25
Steven D. Hartenstein, Jaromir Ruzicka, and Gary D. Christian

Abstract: The construction of 0.1 mL-capacity Chelex 100 ion-exchange columns for the pre-concentration of analyte elements is described. Separate, buffered (pH 9) samples are pumped through two parallel columns (to double the sampling frequency), and sequentially eluted directly into the nebulizer of the ICP by using a flow injection system. This method gives detection limits for simultaneous multi-element analysis that are a 20-fold improvement over those with conventional continuously aspirated systems for Ba, Be, Cd, Co, Cu, Mn, Ni and Pb. The sampling rate is 30 h-1.
Barium Beryllium Cadmium Cobalt Copper Lead Manganese Nickel Ion exchange Spectrophotometry

"Two-valve Injector To Minimize Nebulizer Memory For Flow Injection Atomic Absorption Spectrometry"
Anal. Chem. 1985 Volume 57, Issue 9 Pages 2015-2016
James M. Harnly and Gary R. Beecher

Abstract: A single-line flow injection system for flame AAS with use of a pneumatic nebulizer has been modified to include three pumps and a second six-port rotary value (to reduce memory effects). The system was applied to the determination of K, Mg, Na and Zn in urine at a flow rate of 1.6 mL min-1. The blank signal returned to its starting value after two atomizations, and a 10-fold reduction of the nebulizer memory over the previous system was achieved.
Potassium Magnesium Sodium Zinc Urine Spectrophotometry

"Thermospray Interfacing For Flow Injection Analysis With Inductively Coupled Plasma Atomic Emission Spectrometry"
Anal. Chem. 1986 Volume 58, Issue 12 Pages 2558-2561
J. A. Koropchak and D. H. Winn

Abstract: Details and a diagram are given of a thermospray device for interfacing between the flow injection system and the ICP torch. Operating conditions (specified) were selected for optimizing signal-to-noise ratios for the continuous introduction of standards with the cross-flow nebulizer. The system gives improved detection limits compared with a concentric nebulizer, and affords adequate detection for low levels in small sample volume The effects of increasing the liquid sample flow rate are discussed.
Spectrophotometry

"Separation Of Trace Metal Complexes For Analysis Of Samples Of High Salt Content By Inductively Coupled Plasma Mass Spectrometry"
Anal. Chem. 1989 Volume 61, Issue 2 Pages 149-153
Michael R. Plantz, James S. Fritz, Fred G. Smith, and R. S. Houk

Abstract: Solutions of trace metals (Au, Bi, Co, Cr, Cu, Fe, Hg, Mo, Nb, Ni, Pt, Tl, U and V) in aqueous media of high salt content were treated with bis(carboxymethyl)dithiocarbamate reagent (prep. described) and injected into the loading solvent (0.05 M formate buffer of pH 3.25) for application to a column of Amberlite XAD-4 resin. The adsorbed complexes were eluted with aqueous 0.1 M NH3 (pH 11) and the eluate was analyzed by ICP-MS on a Sciex Elan model 250 instrument fitted with a continuous-flow ultrasonic nebulizer. Detection limits in salt-rich aqueous solution ranged from 6 ng L-1 for Bi to 80 ng L-1 for Pt. The method has been used to determine Cr, Ni and Pt in urine, and trace metals in seawater.
Chromium Nickel Platinum Sea Urine Mass spectrometry

"Determination Of Aqueous Fluoride With A Helium Microwave-induced Plasma And Flow Injection Analysis"
Anal. Chem. 1989 Volume 61, Issue 7 Pages 674-677
J. M. Gehlhausen and John W. Carnahan

Abstract: The sample solution is introduced directly or in 0.5 mL increments into a CETAC (Ames, IA) ultrasonic nebulizer, which supplies the He microwave-induced plasma (modified TM010 cavity; demountable silica torch; 500-W microwave generator at 2.45 GHz). The F emission is measured at the 685.6-nm (I) line. Although detection limits are 36 and 4 ppm for flow injection and direct nebulization, respectively, of test solution containing 1% of HNO3, flow injection is preferred because extended direct nebulization of aqueous F- causes memory effects. The calibration graph is curvilinear. The highest signals are obtained at pH~0.7. The F- signal is enhanced in the presence of Cu, Zn, K, Li and Na, and suppressed by Al; reasons for the effects are suggested. The determination of aqueous fluoride by flow injection analysis (FIA) with a helium microwave-induced plasma (He-MIP) is described. This system operates at 500 W and utilizes a modified TM010 resonator cavity with a demountable plasma torch. Both direct nebulization and FIA in conjunction with ultrasonic nebulization (USN) were investigated. FIA was found to be the most reliable method because extended nebulization of aqueous fluoride was found to cause memory effects. Detection limits for aqueous fluoride of 35 and 4 ppm were observed for FIA and direct USN, respectively. The interference effects of pH and selected elements were also studied.
Fluoride Spectrophotometry

"Flow Injection Donnan Dialysis Preconcentration Of Cations For Flame Atomic Absorption Spectrophotometry"
Anal. Chem. 1989 Volume 61, Issue 13 Pages 1410-1414
John A. Koropchak and Lori Allen

Abstract: The sample loop of a conventional HPLC injector was replaced by a coil of cation-exchange tubing, allowing Donnan dialysis to pre-concentrate cations before flame AAS determination. Nafion 811 (0.64 mm i.d.) was used, typically containing 0.5 M Sr(NO3)2 - 1.2 mM Al(NO3)3 - 0.1 M HNO3; the coil was lowered into the stirred sample solution for various times before introducing the receiver solution to the flame AAS instrument at optimum nebulizer flow rates. Enrichment factors of 100-fold were achieved. The method was applied in the determination of Pb in drinking water.
Cations Lead Water Spectrophotometry

"Direct-injection Nebulization For Inductively Coupled Plasma Mass Spectrometry"
Anal. Chem. 1991 Volume 63, Issue 3 Pages 219-225
Daniel R. Wiederin, Fred G. Smith, and R. S. Houk

Abstract: An improved direct-injection nebulizer is described and illustrated for use in the continuous-flow mode in ICP-MS. It is easier to build and more robust than a previous design, and the sample and solvent do not make contact with any metal surfaces, thus preventing contamination. Precision is typically 0.5% (for signals not limited by counting statistics), an improvement by a factor of 4 over that obtained with conventional nebulizers. A rinse time of 15 s is sufficient to reduce the analyte signal to 0.1% of its steady-state value, even for elements such as Hg and iodine. Relative detection limits are similar to those obtained with conventional nebulizers, but the absolute detection limits are up to an order of magnitude better, as the flow rate is only 120 µL min-1. Matrix effects of Na are similar to those observed with other nebulizers.
Mass spectrometry

"Online Standard Additions With Direct Injection Nebulization For Inductively Coupled Plasma Mass Spectrometry"
Anal. Chem. 1991 Volume 63, Issue 15 Pages 1626-1631
Daniel R. Wiederin, Ronald E. Smyczek, and R. S. Houk

Abstract: A flow injection system is described (with diagram) for online standard additions in trace element determination by the cited technique. Carrier solution is passed through Tefzel tubing (0.5 mm i.d.) to a PEEK tee (0.25 mm i.d.) connected to two high-pressure metal-free flow injection valves via Tefzel tubing. Sample solution are injected via one valve and standard solution are sequentially injected via the second valve. The valves are connected to a second PEEK tee via fused-silica transfer lines (50 µm i.d.). Solutions are passed from the second PEEK tee to the nebulizer through a fused-silica tube. To minimize salt deposition, the direct injection nebulizer tube diameter was reduced to 1 mm, and the tip was modified to accommodate the reduction and the make-up gas flow rate was increased to 0.4 l min-1. The system was applied in the determination of 9 elements in NIST SRM 2670 Toxic Metals in Freeze-Dried Urine. Correction for instrumental drift, viscosity and background effects are discussed.
Trace elements NIST 2670 Urine Mass spectrometry

"Investigation Of An ICP-injection Technique For The Analysis Of Small-volume Samples"
Fresenius J. Anal. Chem. 1980 Volume 301, Issue 2 Pages 105-106
J. A. C. Broekaert, F. Leis and K. Laqua

Abstract: UFL
Iron Blood Serum Spectrophotometry Spectrophotometry

"Acid Effects In ICP-AES"
Fresenius J. Anal. Chem. 1989 Volume 335, Issue 1 Pages 25-33
E. G. Chudinov, I. I. Ostroukhova and G. V. Varvanina

Abstract: Interference by acid matrices (viz. HCl, HNO3, HClO4, H2SO4 and H3PO4) in ICP-AES was studied for 16 elements and 9 spectrometers. The effects of type and concentration. of acid, type and tuning of ICP generator and flow injection or two nebulizer sample introduction were examined. The main effects of acid are depression of analyte signals, irregular signal changes for different elements and a decrease in plasma temp.
Spectrophotometry

"Flow Injection Determination Of Boron, Copper, Molybdenum, Tungsten, And Zinc In Organic Matrices With Direct-current Plasma Optical-emission Spectrometry"
Fresenius J. Anal. Chem. 1989 Volume 335, Issue 8 Pages 893-899
M. C. Brennan and G. Svehla

Abstract: The sample was dissolved in a suitable solvent, and the solution was diluted with isobutyl methyl ketone and introduced via a 600 µL loop into a stream of anhydrous acetic acid (4.5 mL min-1) and then to the nebulizer of the spectrometer via a 25-cm silicon rubber tube (0.8 mm i.d.). The line intensities were measured at 249.773, 324.754, 379.825, 400.875 and 202.548 nm for B, Cu, Mo, W and Zn, respectively. Calibration graphs were rectilinear up to 500 ng mL-1 of B, Cu, Mo and Zn and up to 1000 ng mL-1 of W with detection limits of 21, 14, 28, 120 and 20 ng mL-1 for B, Cu, Mo, W and Zn, respectively. The throughput was 100 samples h-1. The continuous introduction of the carrier liquid into the plasma cleaned out the nebulizer and reduced memory effects.
Boron Copper Molybdenum Tungsten Zinc Spectrophotometry

"Miniature Hydride-generator System For Inductively Coupled Plasma Atomic-emission Spectrometry"
Fresenius J. Anal. Chem. 1990 Volume 336, Issue 5 Pages 423-424
Katsuhiko Yokoi, Mieko Kimura and Yoshinori Itokawa

Abstract: In the cited continuous-flow hydride-generator system (described and illustrated), sample solution is mixed with trichloroacetic acid solution and NaBH4 solution in NaOH and passed through a gas - liquid separator (diagram given). The generated hydrides were passed into the ICP by Ar carrier gas (1 l min-1). A Shimadzu ICPS-1000 II sequential plasma spectrometer was used to determine Sn and Ge at 189.989 and 209.423 nm, respectively. The detection limits were 30 and 150 pg mL-1 for Sn and Ge, respectively; ~100-fold better than those of conventional pneumatic nebulizer ICP-AES.
Tin Germanium Spectrophotometry

"Online Preconcentration Of Silver On Activated Alumina And Determination In Borehole Water By Flow Injection Atomic Absorption Spectrophotometry"
Fresenius J. Anal. Chem. 1990 Volume 336, Issue 3 Pages 201-204
P. P. Coetzee, I. Taljaard and H. de Beer

Abstract: Silver in borehole water is pre-concentrated on a polyethylene micro-column (3 cm x 1 mm) of activated alumina (basic form) connected to a flame AAS instrument (schematic diagram given). Sample (pH 4.0) is passed through the column for 3 to 6 min at 5 mL min-1 with water as carrier stream, elution is with 0.5 mL of 2 M HNO3 and regeneration is with 0.15 M NH4OH (2 min at 5 mL min-1). The effluent is directed to a nebulizer and analyzed by AAS at 328.1 nm. The calibration graph is rectilinear for up to 100 µg mL-1 of Ag, with coefficient of variation (n = 10) of ±5 and 18% for >10 and 5 µg l-1, respectively. The detection limit is 4 µg l-1. Sodium, Mg and Ca salts at 0.1 M to 0.5 M decrease the Ag signal by 10%.
Silver Borehole Spectrophotometry Sample preparation

"Determination Of Arsenic, Antimony, Bismuth, Selenium And Tin In Biological And Environmental Samples By Continuous-flow Hydride-generation ICP-AES Without Gas-liquid Separator"
Fresenius J. Anal. Chem. 1991 Volume 340, Issue 1 Pages 41-47
P. Schramel and Li-Qiang Xu

Abstract: Arsenic, Sb, Bi, Se and Sn were simultaneously determined in samples by ICP-AES with use of the cited hydride-generation system (diagram given) at 1.5 kW. Samples were digested (i) under pressure with 70% HNO3 in a closed vessel at 170°C for 10 h and (ii) with HNO3 - ClHO4 - H2SO4 (details given). Sample solution in 30% HCl - 20% HNO3 were mixed with a reductant solution consisting of 3% NaBH4 and 2% KI prior to nebulization in the ICP spectrometer and determination by AES. Interferences caused by Cu and Ni ions were eliminated with use of the reductant. In general results were in good agreement with certified values; detection limits were at the ng level.
Antimony Arsenic Bismuth Selenium Tin Biological Environmental Sample preparation Spectrophotometry

"High Performance Flow Atomic Spectrometry: New Nebulization Techniques, Online Speciation And Online Sample Pretreatment"
Fresenius J. Anal. Chem. 1996 Volume 355, Issue 5-6 Pages 555-558
H. Berndt and J. Yáñez

Abstract: An interface-free combination of HPLC separation techniques and methods for element determination by atomic spectrometry can be achieved by hydraulic high-pressure nebulization (HHPN). With high-temperature HHPN (300°C) super heated liquids can be nebulized providing aerosol yields of up to 90% in flame AAS. This new nebulization method combines the advantages of HHPN and thermospray techniques (very small aerosol droplets, high aerosol yield, nebulization of saturated salt solutions).
Sample preparation Spectrophotometry

"Evaluation Of The Analytical Performance Of Flow Injection - Flame Atomic Absorption Spectrometry"
Microchim. Acta 1995 Volume 119, Issue 1-2 Pages 95-102
Renli Ma, Willy Van Mol and Freddy Adams

Abstract: The influence of various parameters including sample flow rate, nebulizer uptake rate and coupling tube length on the performance of flow injection flame AAS was investigated using Cu as a model analyte. Both direct introduction of aqueous solutions into the flow manifold (Perkin-Elmer FIAS-200 Flow Injection Analysis System, 1990) or introduction of an alcoholic eluate after online extraction on a C18 column (Portala and Guo, Perkin Elmer Report Nr 4.8 E, 1991) were used. The carrier was 0.2% HNO3, methanol and ethanol were used for sorbent extraction, 0.1% ammonium diethyldithiophosphate in 0.1 M citric acid of pH 2 or 0.1% diethylammonium diethyldithiocarbamate in 0.1 M acetic acid/0.2 M NH3 of pH 9 were used as chelating agent for sorbent extraction; detection was at 324.8 nm. A 28 cm nebulizer capillary tube and a 5 cm PTFE tube were optimal for coupling. A low nebulizer uptake rate with a high sample flow rate produced high sensitivity with RSD of 2%. Optimal rates (details given) were dependent on the nebulization characteristics of the solvent used.
Copper Spectrophotometry

"Some Observations On The Sensitivity Of Flow Injection Techniques For Atomic Absorption Spectrophotometry"
Microchem. J. 1989 Volume 40, Issue 2 Pages 233-241
Carbonell, V.;De La Guardia, M.;Salvador, A.;Burguera, J.L.;Burguera, M.

Abstract: Means of improving sensitivity of flow injection AAS systems are discussed, including use of T-connector interfaces, different carriers and flow compensation solvents. The optimized system was applied in the determination of Mn and Cu in sewage sludge.
Copper Manganese Sludge Spectrophotometry

"Determination Of Selected Noble Metals By MPT-AES Using A Pneumatic Nebulizer"
Microchem. J. 1995 Volume 52, Issue 2 Pages 181-187
Liang F., Zhang D. I., Lei Y. H., Zhang H. Q. and Jin Q. H.

Abstract: The system used was similar to that described by Ye et al. (Anal. Chim. Acta., 1993, 9, 12). For continuous analysis, sample was pumped into a pneumatic nebulizer and carried in Ar via a heating condensation desolvation system and a concentrated H2SO4 desiccator to the microwave plasma torch. For FIA, sample was injected into a stream of water and carried to the nebulizer. The effect of various operating parameters and interfering ions on the AES emission intensity for Au, Ag, Pd, Pt and Rh (wavelengths used tabulated) were examined. A microwave forward power of 60 W and an observation height of 6-8 mm were optimal. Fe decreased the interference from Al. The calibration graphs for Au, Ag, Pd, Pt and Rh were linear over 4-5 orders of magnitude, the detection limits were 0.74, 5.1, 2.9, 8.9 and 7.6 ng/ml, respectively, for continuous-flow analysis and 3.7, 26, 12, 30 and 30 ng/ml, respectively, for FIA. The RSD were 0.81-4.7% for continuous-flow analysis and 1.8-3.8% for FIA (n = 11).
Metals, noble Gold Silver Palladium Platinum Rhodium Spectrophotometry

"Flow Injection Sample Introduction Into Microwave Plasma"
Microchem. J. 1996 Volume 53, Issue 1 Pages 69-78
Hanqi Zhanga, Dongmei Yea, Jinghong Zhaoa, Jinglei Yua, Ruizhi Mena, Qinhan Jin a, and Defan Dongb

Abstract: The optimization of experimental parameters viz. microwave power, support and carrier gas flow rate, HCl concentration in the sample solution and sample-loop volume was investigated for the detection of fifteen elements (listed) by microwave plasma torch AES (MPT-AES) using a flow injection/pneumatic nebulization (PN) sample introduction system (schematic shown). Under optimized conditions, viz. 60 W microwave power, 650 ml/min carrier gas flow rate, a sample-loop volume of 300 µL and a concentration of 0.05 M HCl in the sample solution the detection limits (DL; 36) obtained for the elements were in the range 5-103 ng/ml. The Dl were almost the same as those obtained with a moderate powered He MPT-AES with an ultrasonic nebulization desolvation system (DS) and are much lower than those obtained by low-powered MPT-AES with PN but without DS as well as moderate-powered Ar CMP with PN-DS. For 0.5-5 µg/nl of added elements RSD were 1.3-5%. Spectral interferences from easily ionizable elements in the matrix were investigated. The method was applied to the analysis of three elements viz. Cu, Ni and Mo in two standard steel samples. Results were in good agreement with certified values.
Copper Nickel Molybdenum Alloy Spectrophotometry

"Flame Atomic Absorption Spectrometric Determination Of Total Chromium And Chromium(VI) In Cigarette Ash And Smoke Using Flow Injection/hydraulic High-pressure Sample Introduction"
Microchem. J. 1998 Volume 58, Issue 3 Pages 251-255
Csilla Sógor, Attila Gáspár and József Posta

Abstract: Total chromium and Cr(VI) contents of cigarets, ash, and smoke formed while burning cigarets were determined The determinations of chromium species were carried out according to procedures developed earlier. Cr(VI) was determined in a combined system, which involves a flow injection (FI) sorption pre-concentration system, hydraulic high-pressure nebulization (HHPN) sample introduction technique, and flame atomic absorption spectrometric (FAAS) detection. The total chromium of samples in Cr(VI) form was determined in this same combined system after ashing cigarets at 800°C [after total conversion of Cr(III) of the sample to Cr(VI)]. It was found that while burning cigarets 0.8-1.2% of the original chromium content of the cigarets comes to smoke in the toxic Cr(VI) form.
Chromium(VI) Chromium, total Smoke Ash Spectrophotometry

"Dispersion Of Discrete Sample Signals Within Aerosol Spray Chambers: Preliminary Investigations"
Spectrochim. Acta B 1996 Volume 51, Issue 14 Pages 1733-1745
John A. Koropchak*, Salma Sadain and Bogdan Szostek

Abstract: A cylindrical glass spray chamber (14.8 cm x 3.1 cm i.d.) ed a three-plate (separation 1.2 cm) polypropylene baffle gave aerosol particle sizes that were generally too large for diffusion to influence band broadening to an extent that would be significant in mass-senve systems, e.g., flow injection ICP-AES, but such diffusion as did occur would probably be important in particle-number-sensitive detectors. A barrel-type spray chamber with a baffle system and various other structures were used for characterization of band-broadening phenomena occurring within aerosol spray chambers, with an ICP-AES detector used in this case. Absolute values of aerosol particle size distributions from nebulizer/spray chamber systems were measured and found to be affected by the relative positions of impact surfaces with respect to the nebulizer. Smaller particles, but less total mass was observed as the baffle was moved closer to the nebulizer tip. However, based on measurements herein, it does not appear that particle sizes in any case will be small enough within the spray chamber for diffusion to influence band broadening for the bulk of the aerosol mass, as particularly important for mass sensitive detectors such as ICP-AES, although diffusion is likely to be important to particle number sensitive detectors. 26 References
Spectrophotometry

"Flow Injection Analysis With Inductively Coupled Plasma-atomic Emission Spectroscopy. Critical Comparison Of Conventional Pneumatic, Ultrasonic And Direct Injection Nebulization"
Spectrochim. Acta B 1985 Volume 40, Issue 10-12 Pages 1495-1504
Kimberly E. LaFreniere, Gary W. Rice* and Velmer A. Fassel

Abstract: The performance has been evaluated of a total-injection micro-concentric nebulizer (cf. Anal. Abstr., 1984, 46, 10J96) intended to overcome the constraints placed on detection limits in flow injection ICP-AES by the poor nebulization and transport efficiency of conventional pneumatic and ultrasonic nebulizers. The optimum sample volume and carrier-stream flow rates for the total-injection nebulizer, a pneumatic nebulizer, and an ultrasonic nebulizer with or without aerosol desolvation were 30, 200 and 500 µL and 0.12, 2.5 and 2.5 mL min-1, respectively. Under these conditions there was little difference between corresponding detection limits obtained by flow injection and direct aspiration for each of the nebulization methods, and the detection limits obtained with the total-injection nebulizer were similar to those obtained with the pneumatic nebulizer and the ultrasonic nebulizer without desolvation, those obtained with the ultrasonic nebulizer with desolvation being generally superior. The results are also reported of a comparison of the detection limits obtained by use of the total-injection nebulizer under flow injection conditions with those obtained by electrothermal-vaporization, graphite-cup direct-insertion and graphite-rod insertion ICP-AES with small sample volume and of studies of the reproducibility obtained with the total-injection nebulizer and of inter-element effects observed with it.
Spectrophotometry

"Characterization Of A Nebulizer Interface For Flame Atomic Absorption Spectroscopy"
Spectrochim. Acta B 1987 Volume 42, Issue 7 Pages 883-888
Anders Gustavsson, Olle Nygren

Abstract: A nebulizer interface is described (with diagram) for the coupling of low-flow-rate techniques (e.g., flow injection analysis and HPLC) with flame AAS. It consists of a concentric nebulizer, a heated aerosol chamber, a PTFE adapter and an SP9 burner head. The interface was connected to Varian model 1475 and Pye Unicam SP1900 flame AAS instruments with water, CHCl3 and aqueous methanol as test solution and simulated normal flow injection analysis and HPLC conditions.
Spectrophotometry

"Characterization Of An Interface For Sample Introduction Into An Inductively Coupled Plasma"
Spectrochim. Acta B 1987 Volume 42, Issue 1-2 Pages 111-118
Anders Gustavsson

Abstract: The interface, which is suitable for connecting an ICP as a concentration.-sensitive detector in HPLC or flow injection analysis, consists of a glass Meinhard concentric nebulizer, a heated aerosol-desolvation chamber, and a jet separator to remove most of the solvent vapor and nebulization gas. Analyte transport efficiencies of ~35% can be attained, with much enhanced aerosol analyte concentration. at acceptable plasma solvent loads by comparison with conventional nebulization systems.
Spectrophotometry

"Coupling Of HPLC And ICP-AES For Speciation"
Spectrochim. Acta B 1991 Volume 46, Issue 6-7 Pages 1089-1098
F. Laborda and M. T. C. De Loos-Vollebregt, L. De Galan

Abstract: The cross-flow nebulizer and the thermospray vaporizer can both be used as an interface for coupling high performance liquid chromatography with inductively coupled plasma-atomic emission spectrometry. The dispersion and the peak asymmetry are acceptable for both. With the thermospray system the sensitivity is threefold higher and the fraction of methanol in methanol/water mixtures introduced into the plasma can be as high as 75%, compared with 25% for the cross-flow nebulizer. Initial results obtained for the speciation of selenium in (CH3)3Se+, SeO32- and SeO42- are promising.
HPLC Spectrophotometry

"Characterization Of A New Single-bore High-pressure Pneumatic Nebulizer For Atomic Spectrometry .2. Discrete Sample Introduction In Flame Atomic Absorption Spectrometry"
Spectrochim. Acta B 1993 Volume 48, Issue 12 Pages 1461-1470
José Luis Todolí, Antonio Canals and Vicente Hernandis

Abstract: A study has been made of the analytical behaviour, with discrete sample introduction, of a new high-pressure pneumatic nebulizer as part of sample introduction systems in flame atomic absorption spectrometry. The nebulizer possesses a single bore for the gas and liquid flows. In comparison to the standard Meinhard nebulizer and under identical conditions, the new nebulizer exhibits a greater relative sensitivity (up to 4.5 times) that increases the lesser the gas flow and the greater the liquid flow. Precision is similar with both nebulizers, the detection limits being lower for the pressure nebulizer. The memory effect is likewise of the same order of magnitude for both nebulizers. The pressure nebulizer has also proven satisfactory when working with high salt content or organic solutions. [References: 24]
Spectrophotometry LC

"Characterization Of Aerosols Produced By Pneumatic Nebulizers For Inductively Coupled Plasma Sample Introduction: Effect Of Liquid And Gas Flow Rates On Volume-based Drop-size Distributions"
Spectrochim. Acta B 1995 Volume 50, Issue 4-7 Pages 285-303
John W. Olesik* and Lisa C. Bates

Abstract: The effect of liquid sample uptake rate and nebulizer gas flow rate on analyte transport rates and volume based primary and tertiary drop size distributions were studied for two pneumatic, concentric nebulizers with a Scott type spray chamber. Experimentally measured Sauter mean diameters and spans were compared to those predicted by an empirical model. One of the two nebulizers produced analyte transport rates that were a factor of two or more higher than the other nebulizer under all uptake rate and gas flow rates studied, despite that the nebulizers were of the same model. When the sample uptake rate is increased 400% (from 0.4 to 2.0 ml/min) the aerosol transport rate increased by only 60 to 68%. Losses of aerosol of all drop sizes due to secondary and tertiary processes result in a decrease in the sample transport efficiency as the uptake rate is increased. When the nebulizer gas flow rate was increased from 0.4 to 1.0 l/min the analyte transport rate increased more than a factor of five. The increase in analyte transport rate (and efficiency) as the gas flow rate was increased from 0.4 to 0.6 or 0.7 l/min was due to both a larger volume of small primary aerosol drops produced and less severe losses of drops due to secondary and tertiary processes. The relative increase in volume of small primary aerosol drops produced when the nebulizer gas was increased from 0.6 or 0.7 to 1.0 l/min was similar to the relative increase in analyte transport rate. The higher transport rates produced by one of the two nebulizers was due to a higher production/loss ratio due to secondary and tertiary processes for drops of all sizes less than 20 µm in diameter rather than differences in the volume of primary aerosol contained in small drops.
Mass spectrometry Spectrophotometry

"Characteristics Of Nebulizers For Microwave-induced Plasma Atomic Emission Spectrometry"
Spectrochim. Acta B 1997 Volume 52, Issue 12 Pages 1801-1812
Krzysztof Jankowski, Dorota Karmasz, Leszek Starski, Andrzej Ramsza and Andrzej Waszkiewicz

Abstract: Frit and microcapillary array nebulizers were designed and evaluated as low-flow introduction devices of liquid samples to the low-power microwave-induced plasma. Zirconia ceramics were examined as a new frit material. A critical evaluation has been carried out of the nebulization stages, such as the formation of the primary aerosol, separation of large droplets in the spray chamber and aerosol transport to the plasma torch; changes in the design of the nebulizers studied were introduced on this basis. The characteristics of nebulizers were supplemented by spectroscopic measurements of the measured signal stability, detection limits for selected elements and wash-out times.
Spectrophotometry

"Determination Of Plutonium In Seawater Using Co-precipitation And Inductively Coupled Plasma Mass Spectrometry With Ultrasonic Nebulization"
Spectrochim. Acta B 1998 Volume 53, Issue 6-8 Pages 1221-1233
Ahmet E. Eroglua, Cameron W. McLeoda,*, Kinson S. Leonardb and David McCubbinb

Abstract: A flow injection-inductively coupled plasma-mass spectrometric (FI-ICP-MS) procedure, utilizing ultrasonic nebulization with membrane desolvation (USN/MD), was developed for the determination of Pu in seawater at fg/L concentration. levels. Seawater samples (11), after filtration, were subjected to co-precipitation with NdF3, followed by ion exchange to enrich Pu and to reject seawater matrix ions and co-existing U. The seawater concentration (1.0 mL) was then analyzed by FI-ICP-MS. The limit of detection for 239Pu in seawater based on an enrichment factor of 1000 was 5 fg/L, and precision at the 0.80 pg/L level was 12% RSD. Accuracy was verified via recovery experiments, and by comparing survey data for the Irish Sea with that derived by standard methodology based on co-precipitation and α-spectrometry. Concentrations for dissolved 239Pu and 240Pu in the Irish Sea were 0.267-0.941 pg/L (0.614-2.164 mBq/L) and 0.051-0.196 pg/L (0.428-1.646 mBq/L), respectively.
Plutonium-239 Plutonium-240 Sea Ion exchange Mass spectrometry

"Determination Of Germanium, Palladium And Platinum In Highly Concentrated Solutions Of Phosphoric Acid And Ammonium Nitrate By Flow Injection Inductively Coupled Plasma Mass Spectrometry (FI ICP-MS)"
Spectrochim. Acta B 1991 Volume 46, Issue 6-7 Pages 1051-1061
Zicheng Peng, H. Klinkenberg, T. Beeren and W. Van Borm

Abstract: The elements in a solution containing 2.5 M H3PO4 and 1.5 M NH4NO3 were mixed with a standard addition solution of the elements and an internal standard of 103Rh. The mixture was merged with a carrier stream of 1% HNO3 and passed into the nebulizer. Two standard samples containing 10 and 20 ng mL-1 of the elements gave an average coefficient of variation (n = 5) of ~7%. The limits of detection were between 0.2 and 1.0 ng mL-1.
Germanium Palladium Platinum Inorganic compound Inorganic compound Mass spectrometry

"The Performance Of A Low Consumption Thermospray Nebulizer For Specific Use In Micro-HPLC And General Use In FI With ICP-AES Detection"
Spectrochim. Acta B 1991 Volume 46, Issue 6-7 Pages 1073-1088
J. W. Elgersma, J. Balke and F. J. M. J. Maessen

Abstract: The thermospray interface comprised a nebulizer with a fused silica vaporizer tube and a desolvation system containing a heated spray tube and condenser. The carrier stream was methanol - water (4:1) at 120 µL min-1 for HPLC and between 100 and 500 µL min-1 for the FI with an optimum at 400 µL min-1 and a sample of 80 µL. The limits of detection for eleven elements were 0.1 to 23 ng mL-1 in the FI mode.
Spectrophotometry HPLC

"Analysis Of Trimethylgallium Etherate By Flow Injection Inductively Coupled Plasma Mass Spectrometry"
Anal. Proc. 1992 Volume 29, Issue 3 Pages 94-96
James H. D. Hartley, Les Ebdon

Abstract: Trimethylgallium etherate (I) was stabilized in ethyl ether and introduced into a flow injection system via a carrier stream of 2% HNO3. Sample solution was desolvated with use of a membrane which separates the nebulizer gas from a counter flow of dry Ar. The Ar acts to purge the water and solvent through the membrane resulting in a drying effect on the nebulizer gas before entering the plasma for ICP-MS detection. Optimum conditions were obtained by the variable stepwise Simplex procedure for the determination of In in ethyl ether and applied to the cited determination. The detection limit was in the ng mL-1 range and decreased with an increase in sample size. Trace metal impurities in trimethylgallium (TMG) were determined by stabilizing TMG in diethyl ether to form an etherate. The diethyl ether solution was analyzed by inductively coupled plasma-mass spectrometry (ICP-MS) by injecting small volumes (25 µL) of the ether into a carrier stream of dilute nitric acid (2%(v/v)). A membrane separator was used to desolvate the sample. Trace Al, Cu, In, and Zn were determined in TMG.
Aluminum Copper Indium Zinc Inorganic compound Mass spectrometry

"Simultaneous Determination Of Hydride And Non-hydride Forming Elements By Inductively Coupled Plasma Atomic-emission Spectrometry"
Anal. Proc. 1992 Volume 29, Issue 10 Pages 438-439
Zhang Li, Susan McIntosh and Walter Slavin

Abstract: Arsenic, Se, Sb, Bi, Cd, Cr, Cu, Fe, Mn, Ni and Pb were determined in the NIST environmental standard reference materials steel, coal fly ash, urban particulated and 1643b water by ICP-AES. A Perkin-Elmer FIAS-2000 flow injection system was used for hydride generation (experimental conditions tabulated). The sample solution was split into two streams, one being pumped directly to the nebulizer, the other mixed with HCl and NaBH4 solution in the mixing tubes of the chemifold. After separation, the hydride was swept into the spray chamber through a slightly modified cross-flow nebulizer cap. The hydride was then carried into the plasma together with sample aerosol. Recoveries of 20 µg L-1 of As, Sb and Se and 50 µg L-1 of non-hydride forming elements in river- and seawater standards were >80%.
Arsenic Selenium Antimony Bismuth Cadmium Chromium Copper Iron Manganese Nickel Lead NIST 1643 NIST 1633 NIST 1648 Particulates Alloy Environmental Coal Fly ash River Sea Spectrophotometry Spectrophotometry

"Determination Of Trace Amounts Of Arsenic By Flow Injection Analysis - Hydride Generation - Inductively Coupled Plasma Atomic-emission Spectroscopy"
Fenxi Ceshi Tongbao 1990 Volume 9, Issue 1 Pages 9-14
Chen Hao;Jiang Zucheng;Kong Linying;Zen Yun'e

Abstract: A double capillary nebulizer was used to generate the hydride of the analyte. Factors affecting line intensity in the flow injection system were investigated. The effects of several inorganic acids, their acidity and inter-element interference effects were examined. Under optimum conditions the detection limit of As was 5.2 mg mL-1; the coefficient of variation was 1.48% for 2 µg mL-1 (n = 10). Recoveries of Al from NaCl and AlCl3.xH2O were >95%.
Arsenic Spectrophotometry

"Application Of Flow Injection Standard Additions Method To ICP-AES For The Analysis Of Mixed Rare-earth Samples"
Fenxi Shiyanshi 1991 Volume 10, Issue 2 Pages 45-47
Shen Qing, Jiang Zucheng and Liao Zhenhuan

Abstract: Sample solution (in place of carrier solution) was pumped continuously to the nebulizer for analysis by ICP-AES and aqueous calibration solution were injected into the stream. Calibration graphs for determination of single rare-earth metals were rectilinear and the coefficient of variation (n = 11) was 4.2%. Recoveries of 3 ppm of Sm, 0.5 ppm of Lu, 1 ppm of Tb, 2 ppm of Pr and 0.8 ppm of Ho were 85 to 112%. The method can be applied in the analysis of mixed rare-earth metal samples.
Metals, rare earth Spectrophotometry

"Determination Of Copper In Water Samples By Flow Injection Solvent Extraction - Inductively Coupled Plasma Atomic-emission Spectrometry"
Fenxi Shiyanshi 1991 Volume 10, Issue 3 Pages 7-10
Wang Xiaoru and R. M. Barnes

Abstract: Sample is injected into the analyzer. (at 2.2 mL min-1) and is transferred to a 1.5-m extraction coil for extraction with 0.02% dithizone in CCl4 (at 0.03 mL min-1) for 80 s, before analysis of the organic extract by ICP-AES at 324.7 nm with use of an ultrasonic nebulizer. For 100 ng mL-1 of Cu, the coefficient of variation (n = 6) was 2.5% and the detection limit was 0.1 ng mL-1. A pre-concentration of ~100-fold can be achieved. Sampling rate was 25 h-1. The method was applied to NBS water standards and results compared well with certified values.
Copper Water Spectrophotometry Sample preparation

"Online Determination Of Trace Heavy Metals In Waters By ICP-AES Using A Recycling Nebulizing System With Flow Injection Solvent Extraction"
Fenxi Shiyanshi 1996 Volume 15, Issue 5 Pages 66-68
Cheng, X.H.;Zhou, J.M.;Liu, H.D.;Tang, Z.Y.;Shuai, Q.;Jin, Z.X.

Abstract: Sample (20 ml), was adjusted to pH 1 with HNO3 and heated for 10 min and cooled. The cooled solution was adjusted to pH 2.5 with ammonia water, 0.5 mL aqueous 2% ammonium 1-pyrrolidinecarbodithioate was added and the pH was re-adjusted to 2.5 with 5% HNO3. The mixture was diluted to 25 mL with water and a 240 µL portion of the diluted solution was injected into the flow injection liquid-liquid online extraction system of Shuai et al., (Dizhi Shiyanshi, 1996, in press), using an extraction coil (1.5 m x 0.8 mm i.d.) over 75 s, with IBMK for removal of metal impurities. The organic phase was transferred to the recycling nebulizing system for ICP-AES. Detection limits for Cd, Co, Cu, Fe, Mo, Ni and V were 0.1-2.2 µg/l, with RSD 3.2-7.6%. Recoveries were 93.5-104%. Sampling frequency was 20 runs per h.
Metals, heavy Cadmium Cobalt Copper Iron Nickel Vanadium Environmental Spectrophotometry Sample preparation

"Desolvation In ICP-AES System By Online Column Preconcentration And Flow Injection Analysis"
Guangpuxue Yu Guangpu Fenxi 1994 Volume 14, Issue 4 Pages 71-76
Peng, X.J.;Jiang, Z.C.;Zeng, Y.N.

Abstract: By incorporation of a self-designed heating and condensing device to the online column pre-concentration and FIA system for ICP AES, the effects of sample volume, desolvation temperature and carrier flow-rate on the signal intensity, detection limit and precision of the analysis were studied. When comparing with a non-desolvation system, at the desolvation temperature of 120°C, the desolvation efficiency of this system was 34.2% and that of the sampling was 72.5%; the signal intensity was improved sevenfold. The method was used to determine Cu, Mn, Fe, Cd and Al; detection limits were at ng/ml to sub ng/ml levels.
Trace elements Environmental Spectrophotometry

"Direct Analysis Of Carbon Isotope Variability In Albumins By Liquid Flow Injection Isotope Ratio Mass Spectrometry"
J. Am. Soc. Mass Spectrom. 1996 Volume 7, Issue 6 Pages 605-610
Richard J. Caimi and J. Thomas Brenna*

Abstract: Aqueous protein solutions (2O at a flow rate of 0.5 ml/min. The solution was passed through a pneumatic nebulizer and then sprayed on to a moving steel wire. The coated wire was passed through a 5 cm drying oven, where the solvent was evaporated at 190°C with 100 ml/min counterflowing He, then passed into a combustion furnace. The furnace (15 cm x 2 mm) was maintained at 900°C. The water of combustion was removed and the resulting CO2 gas was directed on to a silica column (5 m x 10 cm i.d.) then to the ion source inlet of a Finnigan-MAT 252 isotope ratio MS (IRMS) System. The IRMS was operated at 6 x 107 torr and an accelerating potential of 8 KV in continuous-flow mode. A summary of isotope ratio analyzes obtained by this method is tabulated; standard deviation was 0.45% (n = 20). The technique was rapid, precise and accurate; data was comparable with data obtained using standard preparation methods using combustion tubes and dual inlet analysis (results are presented and discussed).
Carbon-12 Carbon-13 Albumin LC Mass spectrometry

"Continuous-flow Vapor Generation For Inductively Coupled Argon Plasma Spectrometric Analysis. 1. Selenium"
J. AOAC Int. 1990 Volume 73, Issue 3 Pages 404-410
Tracy ML, Möller G.

Abstract: Sample (~1.5 g of solid or ~10 mL of liquid) is wet ashed with HNO3, H2SO4 and HClO4 at ~310°C; details are presented for treatment of different samples. The digest is cooled to room temp., 5 M HCl is added and the solution is diluted. In a simple continuous-flow manifold, sample solution is mixed with 12 M HCl and then 0.6% NaBH4 solution The H2Se produced is separated off by a standard pneumatic neublizer, and Se is determined by ICP-AES at 196.090 nm. The detection limit is 0.4 µg l-1, or 4 µg kg-1 for a nominal 1-g sample. The calibration graph is rectilinear for 4 mg kg-1. The method has been applied to biological tissues and fluids and to water. Results show good agreement with those by AAS and NAA.
Selenium Biological tissue Water Spectrophotometry

"Continuous-flow Vapor Generation For Inductively Coupled Argon Plasma Spectrometric Analysis. 2. Arsenic"
J. AOAC Int. 1991 Volume 74, Issue 3 Pages 516-521
Tracy ML, Littlefield ES, Moller G.

Abstract: Biological tissue, blood or water, is wet ashed in a 10 mL test tube on a programmed heating block with HNO3, H2SO4 and HClO4 at up to 310°C (details given). The cooled digest is treated with HCl and KI and the As present is reduced by NaBH4 to arsine in a simplified continuous-flow manifold. A standard pneumatic nebulizer effects the gas - liquid separation of AsH3 which is quantified by ICP-AES at 193.756 nm. The detection limit was 0.4 to 0.6 µg L-1 of As. Mean coefficient of variation were 1.2% for analysis of water samples (n = 27) and 2% for analysis of liver samples (n = 12). Recoveries ranged from 99 to 104% for tap water, bovine liver and rice flour.
Arsenic Water Liver Rice Flour Blood Spectrophotometry

"Micro-column High-pressure Liquid Chromatography With A Glass-frit Nebulizer Interface For Plasma Emission Detection"
J. Chromatogr. Sci. 1985 Volume 23, Issue 4 Pages 144-150
Mona Ibrahim, Wipawan Nisamaneepong and Joseph Caruso

Abstract: Microcolumn high pressure liquid chromatography (micro-HPLC) is rapidly gaining recognition as a practical separation tool for organometallic compounds. The use of the inductively coupled plasma (ICP) as a detector for micro-HPLC is studied. Several miniaturized glass-frit nebulizers are investigated as interfaces between the output of the microbore column and the ICP torch. Their performance with aqueous and methanolic solutions is evaluated by direct nebulization and flow injection analysis. The most efficient of these nebulizers is used in the micro-HPLC/ICP study of some Cd, Pb, and Zn organometallic compounds. Detection limits of 1.92 ng of Pb for tetramethyllead and 5.01 ng of Pb for tetraethyllead are obtained and compared with regular HPLC/ICP of these same compounds. Approximately equivalent detection limits were obtained when using a microwave induced plasma as an alternate plasma source. Several miniaturized glass-frit nebulizers were investigated as interfaces between the outlet of the micro-bore column and the ICP torch. Their performance was evaluated by using aqueous and methanolic solution of Cd with direct nebulization and flow injection analysis. The most suitable nebulizer was used in micro-HPLC of some organometallic Cd, Pb and Zn compounds, on a reversed-phase column of C2 material. Detection limits of 1.92 ng of Pb for tetramethyl-lead and 5.01 ng of Pb for tetraethyl-lead were obtained. These were compared with results of regular HPLC - ICP analysis; similar results were obtained with use of a microwave-induced plasma.
Cadmium Lead Zinc HPLC Spectrophotometry

"Sample Zone Cutting By Relocation Of A Coiled Reactor: An Alternative To Increase Manifold Versatility"
J. Flow Injection Anal. 1998 Volume 15, Issue 1 Pages 47-59
Rocha, F.R.P.;Nobrega, J.A.;Gouveia, S.T.

Abstract: The versatility of flow systems can be extended by relocating manifold components, such as resin columns, flow cells, and coiled reactors. The feasibility of the relocation of a coiled reactor was investigated. This approach was applied to reduce the washing time, to adjust the sample concentration range, and to decrease the amount of sample introduced in the nebulization chamber of a flame atomic absorption spectrophotometer (FAAS). Relocation of the coiled reactor allowed cutting the rear of the sample zone and different strategies were implemented employing the same flow system. In nitrite determination using Griess's reaction, sampling rates were 212 h-1 and 327 h-1 without and with a 200 cm relocating reactor, respectively. The adjustment of the sample concentration to the linear response range of the detector was achieved by changing the delay time for relocating the coiled reactor. Relocation of the a coiled reactor also made feasible the direct determination of calcium in milk by FAAS decreasing by 62% the volume of the milk suspension introduced in the nebulization chamber, which is useful to avoid clogging. The accuracy of this procedure was checked using two kinds of whole milk powders standard reference materials (NIST 8435 and IAEA 153) and the results obtained agreed with the certified values at a 95% confidence level.
Nitrite Calcium Powder IAEA 153 NIST 8435 Spectrophotometry

"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.
Phosphorus Phosphate Waste Spectrophotometry

"Sorption Preconcentration And Flame Atomic Absorption Determination Of Chromium(VI) Using Hydraulic High-pressure Sample Introduction"
Magy. Kem. Foly. 1998 Volume 104, Issue 4 Pages 153-163
A. Gáspár, J. Posta and Cs. Sógor

Abstract: Sorption flow injection (FI) pre-concentration procedure was combined with hydraulic high-pressure nebulization sample introduction (HHPN) and flame atomic absorption spectrometric detection (FAAS). The online FI-HHPN/FAAS system was constructed and a method was developed for online sorption and determination of Cr(VI). A polyether-ether-ketone, PEEK loop pre-concentration unit was used for the sorption of Cr-pyrrolidinedithiocarbamate complexes. The detection limit (3s) of the pre-concentrated 5 mL sample solution containing Cr(VI) was 0.54 ng/mL. The precision was 2.8%RSD for 50 ng/mL Cr(VI) (N=6). The method was applied for the determined of Cr(IV) in some natural samples. It was proved that the total chromium content of the samples containing large amt. of organic materials can quant. be converted into Cr(VI) by ashing at 800°C in the presence of oxygen. Thus trace level total chromium contents of various samples were determined after ashing and sorption pre-concentration in form of Cr(VI).
Chromium(VI) Environmental Sample preparation Spectrophotometry

"Online Trace Metal Enrichment In Flow Injection Atomic Absorption Spectrometry"
Quim. Anal. 1989 Volume 8, Issue 2 Pages 159-170
Devi, S.;Habib, K.A.J.;Townshend, A.

Abstract: Aqueous samples containing Cu2+, Cd2+, Mg2+, Zn2+, Pb2+ and Hg2+ were pre-concentrated on a mini-column of 8-hydroxyquinoline-5-sulfonic acid immobilized on to controlled-pore glass and eluted with HNO3 or HCl (depending on the metal to be analyzed) directly into a nebulizer for AAS analysis. Calibration graphs were rectilinear from 0 to 100, 100 to 1000, 20 to 220, 10 to 100, 10 to 300 and 20 to 2000 ng mL-1 of Cd2+, Pb2+, Zn2+, Mg2+, Cu2+ and Hg2+, respectively; detection limits ranged from 0.5 ng mL-1 (for Cu) to 25 ng mL-1 (for Hg). . The coefficient of variation ranged from 1.1 to 2.9% (n = 4). Aqueous samples containing Cu2+, Cd2+, Mg2+, Zn2+, Pb2+ and Hg2+ were pre-concentrated on a mini-column of 8-hydroxyquinoline-5-sulfonic acid immobilized on to controlled-pore glass and eluted with HNO3 or HCl (depending on the metal to be analyzed) directly into a nebulizer for AAS analysis. Calibration graphs were rectilinear from 0 to 100, 100 to 1000, 20 to 220, 10 to 100, 10 to 300 and 20 to 2000 ng mL-1 of Cd2+, Pb2+, Zn2+, Mg2+, Cu2+ and Hg2+, respectively; detection limits ranged from 0.5 ng mL-1 (for Cu) to 25 ng mL-1 (for Hg). . The coefficient of variation ranged from 1.1 to 2.9% (n = 4).
Copper Cadmium Magnesium Zinc Lead Mercury Spectrophotometry

"Direct Determination Of Calcium In Lubricating Oils By Flow Injection Atomic Absorption Spectrometry Using Emulsions"
Quim. Anal. 1989 Volume 8, Issue 2 Pages 241-246
Borja, R.M.;Salvador, A.;De La Guardia, M.;Burguera, J.L.;Burguera, M.

Abstract: Oil samples were injected (100 µL; 0.5 to 5% in isobutyl methyl ketone) into a stream (0.2 mL min-1) of water and mixed with a stream (1.83 mL min-1) of a surfactant (aqueous 20% Nemol K39) ultrasonically in a 2-m reaction coil, and carried directly into the nebulizer of an AAS instrument. Results by flow injection analysis - AAS were more sensitive and precise than the batch method; coefficient of variation were 2.2 to 2.8%.
Calcium Oil Spectrophotometry

"Determination Of Hydride-forming Elements At Ultratrace Levels By Flow Injection Hydride-generation Atomic Absorption Spectrometry With Online Ion-exchange Column Preconcentration"
Quim. Anal. 1989 Volume 8, Issue 2 Pages 191-199
Zhang, S.;Xu, S.K.;Fang, Z.L.

Abstract: Soil samples, prepared by refluxing for 2 h, and acidified, filtered water samples were merged with ammonium acetate buffer solution (0.2 M at pH 5 or 1 M at pH 7 for Se or Bi, respectively) and pre-concentrated on dual ion-exchange columns of D-201 (60 to 100 mesh) for Se(IV) or CPG-8Q (60 to 100 mesh) for Bi(III), and eluted with 1 M HCl. The eluates were mixed with 0.5% NaBH4 solution in 0.1% NaOH as reductant and carried by Ar carrier gas into a heated silica atomizer for AAS analysis. The limits of detection were 0.002 and 0.001 µg L-1 for Se(IV) and Bi(III), respectively, and the corresponding coefficient of variation were 1.1 and 1.0% (n = 11). Effects of co-existing ions are tabulated; interference from Cu(II) was overcome by the addition of 0.5% thiourea to the HCl eluent. Overall recoveries from water and soil water extracts were 90 to 108%, except for Bi(III) in waste water (78 to 90%).
Selenium Bismuth Waste Environmental Environmental Ion exchange Sample preparation Spectrophotometry

"Pneumatic Nebulizer As A Dilution Chamber In A Flow Injection System For Multielement Analysis By ICP-MS"
Quim. Nova 1998 Volume 21, Issue 4 Pages 405-409
Gomes Neto, José Anchieta; Silva, José Bento B.; Rodrigues Neto, Renato; Curtius, Adilson José; Souza, Ivan G.

Abstract: An automatic dispenser based on a flow injection system used to introduce sample and anal. solution into an inductively coupled plasma mass spectrometer through a spray chamber is proposed. Anal. curves were constructed after the injection of 20 to 750 µL aliquots of a multielement standard solution (20.0 µg L-1 in Li, Be, Al, V, Cr, Mn, Ni, Co, Cu, Zn, As, Se, Sr, Ag, Cd, Ba, Tl, Pb) and the acquisition of the integrated transient signals. The linear concentration. range could be extended to ~five decades. The performance of the system was checked by analyzing a NiST 1643d reference material. Accuracy could be improved by the proper selection of the injected volume Besides good precision (relative standard deviation <2%), the results obtained with the proposed procedure were closer to the certified values of the reference material than those obtained by direct aspiration or by injecting 125 µL of several anal. solutions and samples.
Lithium Beryllium Aluminum Vanadium Chromium Manganese Nickel Cobalt Copper Zinc Arsenic Selenium Strontium Silver Cadmium Barium Thallium Lead NIST 1643 Mass spectrometry

"Isotopic And Ultratrace Analysis Of Uranium In Radioactive Waste Samples By Double-focusing Sector Field ICP-MS"
Schr. Forschungszent. Juelich, Reihe Energietech. 1998 Volume 2, Issue 1997 Pages 323-327
Kerl, W.;Becker, J.S.;Dietze, H.J.;Dannecker, W.

Abstract: To optimize the determination of U, ultrasonic nebulization for double-focused sector field ICP-MS was found to be the best nebulization method. With this method the detection limits for several actinide isotopes in highly pure water were determined A precision of <0.1% RDS was achieved for isotopic ratio determination in the ng/mL concentration. range, and the excellent agreement of isotopic ratios obtained by double-focusing sector field ICP-MS and α-spectrometry even for comparable small values of isotopic ratios down to 10^-6 demonstrated the capability of ICP-MS. To minimize the radioactive contamination in the instrument a microconcentric nebulizer in combination with an HPLC injection valve was suitable for flow injection analysis to reduce the sample volume to several µL.
Uranium Waste Waste Mass spectrometry

"Sensitive Quantitation Of Chromium-DNA Adducts By Inductively Coupled Plasma Mass Spectrometry With A Direct Injection High-efficiency Nebulizer"
Toxicol. Sci. 1998 Volume 46, Issue 2 Pages 260-265
Jatinder Singha, John A. McLean, Daryl E. Pritchard, Akbar Montaser, and Steven R. Patierno

Abstract: A novel method is described for the sensitive detection of Cr-DNA adducts. Cr-DNA adducts were determined in 1 µg DNA from normal human lung fibroblasts exposed to sodium chromate using microscale flow injection analysis with a direct injection high-efficiency nebulizer and inductively coupled plasma mass spectrometry detection. The frequency of Cr-DNA adducts increased in a dose-dependent sigmoidal manner, indicating satn. and toxicity. The low detection limits (on the order of parts per trillion) allows the detection of as few as 2 Cr adducts per 10,000 bases, which, coupled with the small DNA sample requirement, makes this technique suitable for measuring metal-DNA adducts as biomarkers of exposure to toxic and carcinogenic metals such as Cr, in cultured cells, animals, and humans. (c) 1998 Society of Toxicology.
Chromium, adducts, DNA Lung Mass spectrometry

"New Sample-introduction Devices For Analytical Atomic Spectrometry"
Trends Anal. Chem. 1989 Volume 8, Issue 9 Pages 336-338
Anders Gustavsson

Abstract: Recent devices for introduction of sample solution into AAS or AES instruments permit their coupling to flow systems, e.g., for HPLC or flow injection analysis. Three such devices are briefly described, viz, a nebulizer for flame AAS, and a jet separator and membrane separator for plasma AES.
Spectrophotometry Spectrophotometry

"Development Of An Ultrasonic Nebulizer Using A Domestic Humidifier"
Bull. Korean Chem. Soc. 1999 Volume 20, Issue 11 Pages 1277-1280
Pyung Heum Yeon, Young Min Cho, and Yong-Nam Pak*

Abstract: An inexpensive ultrasonic nebulizer (USN) was developed utilizing a home humidifier. The ultrasonic transducer was taken from a commercial USN and the power supply was from a humidifier. Sample was continuously fed into the nebulizer and the detection limit was improved 3-20 times over a pneumatic nebulizer. Undesirably, noise in signal was also increased several times. 0.5 ppm of Mn was used as an internal reference and the 'long-term' drift could be successfully corrected. Since the noise contained high and low frequency components, both could be effectively removed only by the real-time correction method such as the Myer-Tracy method, where the reference line was simultaneously monitored with the analytical lines. The performance of USN was tested with NIST SRMs and showed good agreement with the certified values.
Cadmium Beryllium Bismuth Nickel Lead Zinc Tin NIST 1566 NIST 1547 Mass spectrometry