Automated pyrolysis

Step 5. Automated pyrolysis MS using a novel, highly reproducible ionization mode and a TOF mass analyzer. 

Automated pyrolysis MS analysis of lysed vegetative cells in a disinfecting suspension. 

Meuzelaar, H. L. Kistemaker, R G. Eshuis, W. Boerboom, H. A. Automated pyrolysis-mass spectrometry application to the differentiation of microorganisms. Adv. Mass Spectrom. 1976, 7B, 1452-1456. 

Aries, R. E. Gutteridge, C. S. Ottley, T. W. Evaluation of a low-cost, automated pyrolysis-mass spectrometer. J. Anal. Appl. Pyrolysis 1986, 9, 81-98. 

J.P. Dworzanski, W.H. McClennen, P.A. Cole, S.N. Thornton, H.L.C. Meuzelaar, N.S. Arnold and A.P. Snyder, Field-portable, automated pyrolysis-GC/IMS system for rapid biomarker detection in aerosols A feasibility study, Field Anal. Chem. Technol., 1 (1998) 295-305. 

The method has been described extensively in previous papers (ref. 358,359). The extract (1 mg) was suspended in methanol (1 ml) by mild ultrasonic treatment. From this suspension, 5-pl samples were applied to ferromagnetic coated wires and the solvent was evaporated under rotation. The coated wires were mounted in glass reaction tubes. The automated pyrolysis mass spectrometry... 

Screening of estuarine and marine sediment samples by automated pyrolysis mass spectrometry combined with factor-discriminant analysis leads to a useful classification related to the geographical position and the sources of the organic matter. The mass spectral data give preliminary information about the organic matter composition. Analysis of the characteristic mass peaks m/z=86 and 100 by PMSMS and PGCMS points to bacterial poly-alkanoates in the mud fraction of the river sediments. 

The pyrolysis methods applied in this study are used as a tool for a general characterization of the organic matter from the sediments. We describe here the results from screening of estuarine and open sea sediment samples by automated pyrolysis low voltage mass spectrometry combined with factor-discriminant analysis. Characteristic mass peaks resulting from this procedure were investigated in more detail by pyrolysis-tandem mass spectrometry and pyrolysis-photoionization GCMS. 

Pyrolysis Mass Spectrometry and Multivariant Data Analysis. The automated pyrolysis mass spectrometer and the multivariant data analysis by factor-discriminant analysis (f.d.a.) procedure used have been... 

Figure 1. Advantages and trade-offs of new analytical techniques for stable isotope analysis (see Table 1). At present, the best accuracy and precision is achieved for 5 0 by IR-laser fluorination of chips or powdered samples the fastest and least expensive analyses are made by automated pyrolysis systems with continuous flow mass-spectrometers (CFMS) and the smallest samples and best in situ spatial resolution is attained by ion microprobe. The capabilities of in situ UV-laser fluorination are intermediate.

Snelling, R.D., King, D.B. and Worden, R. (1994) An automated pyrolysis system for the analysis of polymers. Poster, lOP, Proceeding of the Pittsburgh Conference, Chicago, IL, 1994. 

Step 4. Automated sampling and application of cell suspension to a pyrolysis probe tip. 

C) Rock-Eval Pyrolysis - was performed on the samples using the equipment and techniques outlined in (11). The technique employs automated equipment providing controlled heating (25°C/min) of the sample under N2 from ambient to 550°C with subsequent detection and quantitation of evolved hydrocarbons and CO2. 

Analytical pyrolysis has a number of characteristics that can make it a very powerful tool in the study of polymers and composite materials. The technique usually requires little sample and can be set with very low limits of detection for a number of analytes. For Py-GC/MS the identification capability of volatile pyrolysate components is exceptionally good. A range of information can be obtained using this technique, including results for polymer identification, polymer structure, thermal properties of polymers, identification of polymer additives, and for the generation of potentially harmful small molecules from polymer decomposition. In most cases of analysis of a polymer or composite material, the technique does not require any sample preparation, not even solubilization of the sample, which may be a difficult task for the type of materials analyzed. The analysis can be easily automated and does not require expensive instrumentation (beyond the cost of the instrument used for pyrolysate analysis). 

When the major alkaloid in tobacco samples is nor-nicotine, the commonly used steam-distillation method and automated procedures result in poor estimates of nicotine and nornicotine. Rosa18 therefore developed a pyrolysis-gas chromatographic method, whereby pyrolysis was carried out with a Victoreen pyrolyzer fitted to the gas chromatograph. Nicotine is relatively volatile and readily released by pyrolysis, even at 100°C. Nornicotine, being less volatile, showed maximum release by pyrolysis at 300°C. The pyrolysis-gas chromatography was carried out with ca. 1 mg of tobacco. The results obtained with the method are presented in Figure 5.3. 

The evolution of hydrocarbon products from shale as the pyrolysis temperature increased was monitored with a flame ionization detector and a yield versus temperature profile produced. Initially, pyrolysis was done with the CDS pyroprobe, but major limitations were observed, mainly with ensuring prompt removal of products. Subsequently, an automated concentrator and high-temperature pyrolysis furnace produced by Envirochem, Inc. was employed. This system permitted use of larger (50-100 mg) samples and the helium sweep gas effectively removed pyrolysis products (pyrolysates). However, the pyroprobe system is still used to measure YP as it provides a rapid, consistent determination. 

HMF, and a 50-minute incubation with 12.5 mmol/liter (final concentration) thiobarbituric acid for color development. Acid pyrolysis could be reduced to 2 hours by using a pressure cooker or autoclave. Some 50 specimens can be processed (albumin purification, autoclave pyrolysis, and automated color development and recording) every 2 days. Glycosylated serum albumin values should be monitored every 3 weeks. 

In this paper, we have presented test results of two methods of adhesion improvement on a specific aluminum alloy and a stainless steel. The methods are based on flame pyrolysis of silane precursors and a laser pretreatment in connection with a primer. While the first method seems to be most favorable for steel surfaces, the latter gives good results on both aluminum and steel. Both methods are well suited for application in the railroad industry since they are effective under atmospheric conditions and are therefore promising for integration in an automated production line. 

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