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
Website: @unf

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Classification: Metal -> iron

Citations 5

"Combined Generator/separator. 2. Stibine Generation Combined With Flow Injection For The Determination Of Antimony In Metal Samples By Atomic Emission Spectrometry"
Analyst 1992 Volume 117, Issue 10 Pages 1603-1608
Hengwu Chen, Ian D. Brindle and Shaoguang Zheng

Abstract: A modified hydride generator/gas - liquid separator was designed for the determination of Sb in metals by flow injection DC-plasma AES (cf. Ibid., 1992, 117, 407). Reduction of Sb(V) to Sb(III) was effected offline with cysteine, the presence of which also accelerates the BH4- reaction and reduces interference from transition metals and other hydride-forming elements (except Se). The calibration graph was rectilinear from 50 to 250 ng mL-1, and the detection limit was 7.5 ng mL-1 for a 0.5 mL sample. The coefficient of variation (n = 12) at 200 ng mL-1 was 0.9%. The method was applied to iron and copper. Application of a new continuous hydride generator to the determination of antimony in metals by flow injection is described. A modified hydride generator/gas-liq. separator has been designed. The detection limit for antimony is 7.5 ng mL-1 for a 0.5 mL sample. For solutions containing 200 ng mL-1 of antimony, the relative standard deviation is 0.9%. Reduction of antimony(V) to antimony(III) is effected by off-line prereduction with L-cysteine. L-Cysteine also accelerates the tetrahydroborate(III) reaction and reduces interferences from transition elements and, with the exception of selenium, other hydride-forming elements. Results are reported for the determination of antimony in iron and copper samples.
Antimony Spectrophotometry Interferences Phase separator Volatile generation Volatile generation

"Isotope Dilution Analysis For Flow Injection ICP-MS Determination Of Microgram Per Gram Levels Of Boron In Iron And Steel After Matrix Removal"
Anal. Chem. 1996 Volume 68, Issue 6 Pages 991-996
Aurora G. Coedo, Teresa Dorado, Bernardo J. Fernandez, and Francisco J. Alguacil

Abstract: Steel or Fe (0.25 g) was mixed with HCl, HNO3, H2SO4 and water in a high-pressure digestion vessel and dissolved using a microwave oven. A 10B spike solution was added (250 ng B) and the solution was evaporated to form solid salts, which were redissolved in water. The solution was extracted with acetylacetone/CHCl3 (1:1) at pH 1.4, the organic phase was discarded, and the extraction procedure was repeated on the aqueous phase. The aqueous layer was mixed with 1 mL HNO3, the solution was evaporated to 2 mL and diluted to 5 mL with water. The resulting test solution corresponded to 50 mg/ml sample, with the total B and Fe contents 1 µg/ml. Flow injection sampling minimized problems arising from the total salt concentration. The ICP-MS detection limit was 0.02 µg/g and the RSD values for concentrations 10 times this limit were 1% (n = 4). Good accuracy was obtained for eight Fe reference materials with B contents 10 µg/g.
Boron Mass spectrometry Sample preparation Reference material Interferences Matrix removal

"The Determination Of Tin In Steel Samples By Flow Injection Hydride Generation Atomic Absorption Spectroscopy"
Spectrochim. Acta B 1992 Volume 47, Issue 7 Pages 897-906
Susan McIntosh, Zhang Li, Glen R. Carnrick and Walter Slavin*

Abstract: Copper, Ni and Co interfere in the cited determination. The interference occurs in the generation of hydride and not during the atomization of gaseous hydride. Tin was also determined in iron and river sediment samples. Hydride generation was in a saturated boric acid solution with a carrier solution of 2% HCl. Sample digestion in a pressure bomb was compared with that in aqua regia at 1 atmosphere. An Ar and O2 gas stream gas stream gave better sensitivity and peak symmetry than a pure Ar gas stream. The detection limit was 0.05 µg L-1 in a 500 µL sample with a coefficient of variation of 1 to 3% at higher concentration. of Sn. Conditions were studied for the determination of Sn in steel samples using flow injection, hydride generation, and atomic absorption spectroscopy. Interferences were found for the determination of Sn in steel samples and an investigation showed that the interferences occurred in the generation of the hydride, not in the atomization of the gaseous hydride. Conditions for the determination of Sn by flow injection hydride generation were improved by using integrated absorbance signals and by the addition of oxygen to the argon carrier gas stream. Typically, 500 µL of a 10 µg/L Sn standard provided an integrated absorbance signal greater than 0.5 A s. The method provided a detection limit of about 0.05 µg/L in a 500 µL sample. The precision ranged from 1 to 3% RSD at higher concentration levels of Sn. The method of additions yielded accurate results for several steel standard reference materials in those situations where the use of the standard calibration procedure was inadequate.
Tin Spectrophotometry Sample preparation Interferences Standard additions calibration Reference material Volatile generation Volatile generation

"Simple And Rapid Determination Of Trace Constituents In Iron And Steel By Flow Injection Analysis"
Curr. Adv. Mater. Processes 1997 Volume 10, Issue 3 Pages 676-679
YAMANE Takeshi

Abstract: NA

"Simple, Rapid, And Precise Determination Of Manganese In Iron And Steel By Flow Injection Analysis"
J. Iron Steel Inst. Jpn. 1993 Volume 79, Issue 4 Pages 492-496
Takeshi YAMANE, Masae SAITO

Abstract: In order to improve the simplicity, rapidity, accuracy and precision in the chemical analysis of iron and steel, a flow-injection analysis (FIA) has been studied for manganese determination with photometric detection. The FIA system consists of a direct on-line coupling of coloring reaction and absorbance measurement in a continuous now mode ; manganese is oxidized by ammonium peroxodisulfate to MnO4- and the absorbances of the resultant solution are measured before and after the addition of sodium nitrite. The FIA manifold and the optimum reaction conditions were established for allowing this simultaneous measurements of analytical and blank signals by single sample injection with single detector. The analytical results by the proposed method for four Japanese standards of steel (The Iron and Steel Institute of Japan) agreed well with the certified values for manganese and showed high precision of relative standard deviations of 0.25-0.50% which are much smaller than those usually observed in manually operated spectrophotometric methods. An injection rate of 12 sample solutions/h can be achieved. The most appealing feature of the proposed method is that the analysis is achieved in a continuous and nearly closed system without complicated manual operations, which can afford simpler and rapid as well I as accurate and precise determination of manganese.