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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NIST 1633

Citations 9

"Determination Of Arsenic And Vanadium In Airborne Related Reference Materials By Inductively Coupled Plasma-mass Spectrometry"
Anal. Chim. Acta 1999 Volume 392, Issue 2-3 Pages 299-306
Chu-Fang Wang, C. Y. Chang, C. J. Chin and L. C. Men

Abstract: This study investigated sample digestion techniques and instrumental interference in determining As and V in airborne related reference materials using inductively coupled plasma mass spectrometry (ICP-MS). Four reference materials, NIST SRM 1648 urban particulate matter, BCR Reference Material No. 176 city waste incineration ash, NIST SRM 2709 San Joaquin soil, and NIST SRM 1633b coal fly ash were dissolved by acid mixture high-pressure bomb digestion. A HNO3+H2O2+HF mixed acid digestion with a low temperature evaporation procedure is proposed as an effective sample pretreatment method for the determination of As in all samples. The addition of HF is required especially for dissolving geologically originated samples such as soil or dust. It was found that, with the proposed digestion procedure, the determinations of V are still unacceptable for highly chlorinated samples when using quadrupole ICP-MS. It was also proved that sector-field ICP-MS is sufficiently sensitive for the determination of V, and can be utilized as a valid tool to investigate the amount and direction of biased results obtained from ICP-MS.
Arsenic Vanadium Mass spectrometry Optimization Interferences Reference material

"A Flow Injection/hydride Generation System For The Determination Of Arsenic By Inductively-coupled Plasma Atomic Emission Spectrometry"
Anal. Chim. Acta 1984 Volume 161, Issue 1 Pages 275-283
R. R. Liversage and J. C. Van Loon, J. C. De Andrade

Abstract: After optimizing the concentration. of HCl and NaI in the test solution, the concentration. of NaBH4, sample and reductant volume and flow rate, Ar carrier-gas flow rate and r.f. power, As (10 to 1000 ppb) was determined in NBS orchard leaves, coal fly ash and river sediment and NRCC MESS-1 and BCSS-1 standard reference materials with good accuracy and precision by using an ARL 34000 Quantometer. The coefficient of variation (n = 10) at the 100-ppb level of As was 7.2%, and the detection limit was 1.4 ng for a 0.17 mL sample volume The calibration graph was rectilinear for 0.01 to 1 ppm of As. Cobalt, Ni, Ag, Au, Bi, Te and Sn interfered. About 200 injections h-1 were possible.
Arsenic Spectrophotometry Interferences Reference material

"Determination Of Hexavalent Chromium In Industrial Hygiene Samples Using Ultrasonic Extraction And Flow Injection Analysis"
Analyst 1997 Volume 122, Issue 11 Pages 1307-1312
Jin Wang, Kevin Ashley, Eugene R. Kennedy and Charles Neumeister

Abstract: A simple, fast, and sensitive method was developed for the determination of hexavalent chromium (Cr(VI)) in workplace samples. Ultrasonic extraction in alkaline solutions with 0.05 M (NH4)2SO4-0.05 M NH3 provided good extraction efficiency of Cr(VI) from the sample and allowed the retention of Cr(VI) on an ion-exchange resin (95%). The Cr(VI) in the sample solution was then separated as an anion from trivalent chromium [Cr(III)] and other cations by elution from the anion-exchange resin with 0.5 M (NH4)2SO4 in 0.1 M NH3 (pH 8) buffer solution. The eluate was then acidified with hydrochloric acid and complexed with 1,5-diphenylcarbazide reagent prior to flow injection analysis. By analyzing samples with and without oxidation of Cr(III) to Cr(VI) using Ce(IV), the method can measure Cr(VI) and total Cr. For optimizing the separation and determination procedure, preliminary trials conducted with two certified reference materials (CRMs 013-050 and NIST 1633a) and three spiked samples (ammonia buffer solution, cellulose ester filters and acid washed sand) indicated that the recovery of Cr(VI) was quantitative (> 90%) with this method. The limit of detection for FIA-UV/VIS determination of the Cr-diphenylcarbazone complex was in the sub-nanogram range (0.11 ng). The technique was also applied successfully to a workplace coal fly ash sample that was collected from a power plant and paint chips that were collected from a heating gas pipe and a university building. The principal advantages of this method are its simplicity, sensitivity, speed and potential portability for field analysis.
Chromium(VI) Chromium(III) Sample preparation Spectrophotometry Reference material Speciation

"Hydride-generation Atomic Absorption Spectrometry Coupled With Flow Injection Analysis"
Anal. Chem. 1985 Volume 57, Issue 7 Pages 1382-1385
Manabu Yamamoto, Makoto Yasuda, and Yuroku Yamamoto

Abstract: Flow injection analysis was combined with the gas-segmentation method described by Skeggs (Am. J. Clin. Pathol., 1957, 28, 311) for the determination of As, Sb, Bi, Se and Te. On synthetic samples the coefficient of variation were between 0.5 and 0.8% (n = 10) with detection limits between 0.04 and 0.3 ng. The results on NBS steel, wheat and rice flour, orchard leaves and coal fly ash were close to certified values and the differential determination of As and Sb in thermal water was possible. Tolerance limits for diverse ions are listed.
Arsenic Antimony Bismuth Selenium Tellurium Spectrophotometry Reference material Segmented flow

"Certification Of A New NIST Fly Ash Standard Reference Material"
Fresenius J. Anal. Chem. 1995 Volume 352, Issue 1-2 Pages 193-196
Robert R. Greenberg, Jean S. Kane and Thomas E. Gills

Abstract: A new fly ash standard reference material was prepared from the burning of mixed Appalachian range coals in a single coal-fired power plant. The material was certified by a number of different analytical methods including isotope-dilution MS, NAA, XRF, ICP-AES, ETAAS, cold vapor AAS, flow injection AAS and flame emission spectrometry. The homogeneity of the sample was determined by NAA and XRF. Results are discussed.
Mercury Spectrophotometry Spectrophotometry Reference material

"Determination Of Trace Elements In Power Plant Emissions By Inductively Coupled Plasma Mass Spectrometry: Comparison With Other Spectrometric Techniques"
Microchem. J. 1998 Volume 59, Issue 2 Pages 203-218
M. Bettinelli, S. Spezia, U. Baroni and G. Bizzarri

Abstract: Particulate matter in stack effluents of coal-fired plants was collected with an isokinetic probe nozzle suitable for (a) total particulate samplings on membrane filters and (b) sampling with a low volume 10-stage single orifice cascade impactor plus a backup filter. A microwave digestion method using an acid mixture of HNO3-HCl-HF in a closed vessel was developed for the determination of major, minor, and trace elements in very small amounts of sample. Analyses were carried out by inductively coupled plasma mass spectrometry (ICP-MS). A recovery study was conducted using multielemental standard solutions, NIST1633a Trace Elements in Coal Fly Ash and NIST 1648 Urban Particulate Matter, to examine the capabilities of the method. The results for real samples dissolved by this procedure were compared with results obtained by instrumental neutron activation anal., graphite furnace atomic absorption spectrometry, and flow injection hydride generation atomic absorption spectrometry. The anal. capabilities of ICP-MS make it one of the techniques of choice for the determination of trace elements in emission particulate matter collected in different granulometric particle sizes.
Aluminum Arsenic Barium Cadmium Chromium Iron Manganese Nickel Lead Antimony Vanadium Zinc Mass spectrometry Sample preparation Method comparison Reference material

"Flow Injection Method For The Separation Of Thallium And Gold On A Sephadex Column And Their Extraction-photometric Determination With Rhodamine B"
Anal. Sci. 1990 Volume 6, Issue 3 Pages 421-424
H. KOSHIMA and H. ONISHI

Abstract: The method involves injection of a sample into 0.5 M HCl - 1 M LiCl as carrier solution (0.6 mL min-1), and passsage through a column (15 cm x 3 mm) of Sephadex G-25. The eluate is added to 0.04% rhodamine B (0.18 mL min-1), and the mixture is then mixed with benzene (0.2 mL min-1). After passage through a 2-m extraction coil and a phase separator, the absorbance of the organic phase is measured at 565 nm. The retention times for Tl and Au on the column are 5.5 and 11 min, respectively. From 0 to 5 mg L-1 of each metal can be determined. The method was applied to coal fly ash and ores. Recoveries were 97 to 98% for Tl and Au in the respective samples.
Thallium Gold Spectrophotometry Sample preparation Column Phase separator Organic phase detection Sephadex Solvent extraction Reference material

"Online Preconcentration Of Rare-earth Element By FIA-ICP-AES"
Anal. Sci. 1997 Volume 13, Issue suppl Pages 27-30
GAE HO LEE, SOON A. PARK, KYUSEOK SONG, HYUNGKI CHA, JONGMIN LEE, and SANG CHUN LEE

Abstract: A mini-column filled with Dowex 50x8 resin is developed and investigated for the analysis of trace level of rare earth element by ICP-AES. The column is installed between peristaltic pump and ICP-AES, and ng/ml level of rare earth element is analyzed directly by online FTA-ICP-AES. 6N hydrochloric acid is found to be an optimum concentration for stripping, and the optimum flow rates for loading and stripping are measured at 0.8 and 1.1 ml./min, respectively. Easily ionized elements from flux such as Na and K would be eliminated easily by 2N hydrochloric acid before stripping the rare earth element deposited on the resin. For an analysis of Sm, the absolute detection limit and linearity are found to be than 4% of reproducibility is observed for the analysis of Sm and Nd. The analytical result with NIST SRM 1633B is also found to be 20.3 ng/ml, which agrees well with tile certified value. 9 References
Metals, rare earth Samarium Neodymium Spectrophotometry Reference material Resin Optimization Column Preconcentration

"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 Spectrophotometry Spectrophotometry Reference material FIAS-200 Nebulizer Volatile generation Volatile generation