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: Oil -> lubricating

Citations 6

"Determination Of Potassium In Gasoline And Lubricating Oils By A Flow Injection Technique With Flame Atomic Emission Spectrometric Detection"
Anal. Chim. Acta 1990 Volume 234, Issue 2 Pages 439-444
Gavin E. Roscoe and Richard Miles, Colin G. Taylor

Abstract: Petroleum spirit (b.p. 100°C to 120°C or 120°C to 160°C) is used as carrier stream for gasoline or lubricating oil (the latter diluted 100-fold). The stream is transferred via PTFE tubing and aspirated into the photometer. For gasoline, the carrier also acts as the fuel supply to the flame. The calibration graph (peak area) is rectilinear up to 20 µg kg-1 of K. Gasoline volatility affects response so sample and standard should be matched. Precision at 10 mg kg-1 is 3%. Oxygenates and halogenated hydrocarbons do not interfere, and recoveries are ~100%. Sample throughputs are 40 and 100 h-1 for gasoline and oil, respectively. The method may be applied in the determination of other alkali and alkaline-earth metals in lubricating oils and fuels.
Potassium Metals, alkali Metals, alkaline earth Spectrophotometry Interferences

"Analysis Of Oil With Inductively Coupled Plasma: Total Process Automation"
Spectrochim. Acta B 1985 Volume 40, Issue 1-2 Pages 49-55
Susan J. Evans and Robert J. Klueppel

Abstract: An automated injection and dilution system (details given) based on the flow injection principle provided the delivery of a uniform and highly reproducible dilute sample to the plasma. Through-put rates of 80 samples h-1 were routinely achieved, and errors due to variations in viscosity were negligible. The method was applied to the determination of 21 elements in lubricating oils, with use of organometallic standards for calibration. The short-term coefficient of variation was 1 to 2%, and multi-operator long-term coefficient of variation averaged 3.1%; drift during the long-term test was negligible. Recoveries averaged 102%.
Metals, wear Spectrophotometry Automation Viscosity

"Use Of A Robot And Flow Injection For Automated Sample Preparation And Analysis Of Used Oils By ICP Emission Spectrometry"
Spectrochim. Acta B 1987 Volume 42, Issue 1-2 Pages 169-180
M. P. Granchi, J. A. Biggerstaff, L. J. Milliard and P. Grey

Abstract: The system comprises, inter alia, a Zymark laboratory robot, a balance, a hotplate, an SC-110 automatic sample changer, a FIAtron model SHS-300 microprocessor-controlled flow injection solution-handling system (FIAtron Systems, Oconomowoc, WI), an ICP emission spectrometer controlled by a PDP-11/34 minicomputer, and an IBM/XT personal computer. The personal computer co-ordinates the activities of the microprocessor and the PDP-11/34 (used for data acquisition, background correction and calculation of results) corrects for spectral interference, displays the results on a printer and stores them on floppy disc, and, with the approval of the operator, transmits them to a laboratory information-management computer. The robot is programmed to perform the various sample-preparation steps (heating at ~70°C for 35 min, dilution with xylene, and weighing). The precision of the transient signal integration was at least an order of magnitude better than for conventional steady-state integration, and results by the two types of measurement were equivalent.
Metals, wear Sample preparation Spectrophotometry Automation Computer Heated reaction LIMS Interferences Method comparison Robot

"Potentiometric FIA Of Acids And Bases In Nonaqueous Solvents And Its Application To Lubricating Oils"
Bunseki Kagaku 1990 Volume 39, Issue 2 Pages 109-114
Katafuchi, A.;Imato, T.;Yagi, J.;Takahara, K.;Ishibashi, N.

Abstract: Sample (200 µL) was injected into an ethanol stream and merged with 5 mM tetrabutylammonium butyrate - 5 mM butyric acid buffer solution containing 0.1 M LiCl. The change in pH was measured with use of a glass electrode. The method was applied in the determination of organic acids and aliphatic and aromatic amines. Calibration graphs covered the range 0 to 5 mM. The coefficient of variation was 0.5% and the analysis time was 40 samples h-1. The method was also applied in the determination of the alkalinity of lubricating oils.
Acids, organic Amines, aliphatic Amines, aromatic Alkalinity Potentiometry Electrode Buffer Calibration

"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 Spectrophotometry Emulsion Injector Nebulizer Precision Sensitivity Injection technique Surfactant

"Application Of A Fractionary Factorial Design To The Determination Of Tin In Lubricating Oils By Continuous Flow Hydride Generation-atomic Absorption Spectrometry"
Fresenius J. Anal. Chem. 1999 Volume 364, Issue 6 Pages 527-532
M. Begoña Martín-García, Dolores Bellido-Milla, Andrés Jimenez-Jimenez, María Purificación Hernández-Artiga

Abstract: The determination of wear metals and metalloids in used lubricating oils allows the prediction of equipment failure. A number of procedures to determine wear metals in lubricating oils by atomic spectrometry has been published. Industry has lately shown a special interest in the determination of tin, since its appearance at certain levels in used oils indicates severe engine wear. Therefore, a method for the determination of the total tin content in used lubricating oils by hydride generation-atomic absorption spectrometry (HG-AAS) is described. Unused marine lubricating oils spiked with the analyte were digested in closed vessels in a microwave oven and the diluted product was used for continuous stannane generation. There are many factors that influence effective SnH4 generation; therefore, fractionary factorial design was used to obtain an adequate sensitivity and also to stabilize the signal. Six variables were taken into account and a 26-2IV design was used with spiked samples containing 30 ng g-1 Sn. The reproducibility, stability, calibration curve and limit of detection were established. The method was applied to different kinds of used lubricating oils. In all cases, the results were higher than those obtained in the industry by simple dilution.
Tin Spectrophotometry Volatile generation Optimization Factorial design