Thermal energy analysis

N-Nitroso contamination in pesticide products was first reported by D. Fine and co-workers (] ) who had developed a novel and specific analytical method for N-nitroso compounds, called thermal energy analysis. 

Thermal Energy Analysis and Nitrogen-Selective Detectors 381... 

Gas chromatography is one of the most powerful analytical techniques available for chemical analysis. Commercially available chemiluminescence detectors for GC include the FPD, the SCD, the thermal energy analysis (TEA) detector, and nitrogen-selective detectors. Highly sensitive detectors based on chemiluminescent reactions with F2 and active nitrogen also have been developed. 

J.M.P. Douse, Trace analysis of explosives at the low nanogram level in handswab extracts using columns of Amberlite XAD-7 porous polymer beads and sdica capillary column gas chromatography with thermal energy analysis and electron capture detection , J. Chromatogr., 328 (1985) 155-165. 

D. H. Fine and D. P. Rounbehler, Trace analysis of volatile N-nitroso compounds by combined gas chromatography and thermal energy analysis. Journal of Chromatography, 1975,109(2), 271-279. 

The prototype of the tobacco specific nitrosamines, NNN, has been detected in both tobacco smoke and unburned tobacco. Various analytical methods have been used including gas chromatography (GLC) (13,14,15,16) combined GLC-mass spectrometry (17), thin layer chromatography (18) high pressure liquid chromatography (HPLC) (19,20), and combined HPLC-thermal energy analysis (21). 

For the analyses discussed here, we have used Gas Chromatography-Thermal Energy Analysis (GC-TEA ) and/or High Pressure Liquid Chromatography-Thermal Energy Analysis (HPLC-TEA). The TEA has been used as the detector... 

J. M. F. Douse, Dynamic Headspace Method for the Improved Clean-up of Gunshot Residues prior to the Detection of Nitroglycerine by Capillary Column Gas Chromatography with Thermal Energy Analysis Detection, Journal of Chromatography 464 (1989) 178. 

Volatile and gaseous products of propellant combustion remain inside the gun barrel and cartridge case for some time and their detection and quantitative determination by means of gas and liquid chromatographic methods (thermal desorption GC-MS, GC-thermal energy analysis, LC-MS/MS) can help in establishing, whether the gun was fired up to 3 days, 2-3 weeks or more than 3 weeks before examination [19, 20]. 

Gray, J.I. Stachiw, M.A. Gas chromatographic-thermal energy analysis method for determination of volatile N-nitrosamines in baby bottle rubber nipples collaborative study. J. AOAC 1987, 70 (1), 64-68. 

Billedeau SM, Thonpson HC Jr, Miller BJ, et al. 1986. Volatile N-nitrosamines in infant pacifiers sold in the United States as determined by gas chromatography/thermal energy analysis. J Assoc Off Anal Chem 69 31-... 

Fine DH, Rounbehler DP, Sawicki E, et al. 1977a. Determination of dimethylnitrosamine in air and water by thermal energy analysis validation of analytical procedures. Environ Sci Technol 11 577-580. 

Thompson HC Jr, Billedeau SM, Miller BJ. 1986. Gas chromatographic thermal energy analysis method for N-nitrosodibutylamine in latex infant pacifiers collaborative study. J Assoc Off Anal Chem 69 504-507. 

Maddock, J. Lewis, P.A. Woodward, A. Massey, P.R. Kennedy, S. Determination of isosorbide dinitrate and its mononitrate metabolites in human plasma by high-performance liquid chromatography-thermal energy analysis. J.Chromatogr., 1983, 272, 129-136... 

Mola, M., G. Lionetti, and A. Nunziata Determination of tobacco specific nitrosamines in mainstream smoke by gas chromatography-thermal energy analysis 57th Tobacco Science Research Conference, Program Booklet and Abstracts, Vol. 57, Paper No. 10, 2003, p. 23. 

Fine, D.H., D.P Rounbehler, E. Sawicki, and K. Krost Determination of dimethylnitrosamine in air and water by thermal energy analysis Validation of analytical procedures Environ. Sci. Technol. 11 (1977) 577-580. Fine, D.H., D.P. Rounbehler, A. Rounbehler, A. Silvergleid, E. Sawicki, K. Krost, and G.A. de Marais Determination of dimethylnitrosamine in air, water and soil by thermal energy analysis Environ. Sci. Technol. 11 (1977)581-584. 

Theiler, R., K. Sato, T. Aspelund, and A. Miller Inhibition of A-nitrosamine formation in a cured ground pork belly model system J. Food Sci. 49 (1984) 341-344. Thompson, H.C. Jr, S.M. BUledeau, B.J. Miller, E.B. Hansen Jr, J.P. Freeman, and M.L. Wind Determination of A-nitrosamines and A-nitrosamine precursors in rubber nipples from baby pacifiers by gas chromatography thermal energy analysis J. Toxicol. Env. Hlth. 13 (1984) 615-632. 

Although GC/MS techniques remain the basic hallmark of analysis for pesticides and their derivatives, it is important to stress the need and the specific role of additional methodologies such as thermal energy analysis and electrochemical detectors. The former technique was discussed with particular emphasis on its utility of the determination of trace levels of nitrosamines and nitrosated pesticides in agricultural products and residues. 

The use of GC for the analysis of GSR is limited due to the incompatibility of many of the analytes, such as the nitrate esters, and the lack of volatility of nitrocellulose, the major component of smokeless propellant. Despite this, GSR has been successfully analyzed using GC employing a variety of detectors including flame ionization, electron capture, and thermal energy analysis. Thermal energy analysis has been found to be particularly useful as it is selective for the nitro-containing compounds present in GSR. Recent attempts have been made to individualize GSR to a particular class of firearm and/or ammunition using chemometric techniques. 

Potentiometric titration Potentiometric titration TLC Gas chromatography after reduction Thermal energy analysis Water total nitrogen color... 

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