Tandem Mass Spectrometry (MS/MS) for Analysis of Additives in a Rubber Vulcanizate

1988 ◽  
Vol 61 (4) ◽  
pp. 658-668 ◽  
Author(s):  
Robert P. Lattimer

Abstract MS/MS appears to have considerable potential as a means for improved direct mass spectral characterization of organic additives in rubber compounds. In this report, we have shown how daughter-ion, parent-ion, and neutral-loss scans can improve the specificity for identification of organic additive components in rubber vulcanizates. The use of MS/MS to reduce the “chemical noise” in the direct analysis of complex mixtures is demonstrated. MS/MS should not be viewed as a technique that will replace other mass spectral methods in rubber applications. For example, desorption ionization methods, GC/MS, LC/MS and high-resolution mass measurements will still have important roles. MS/MS can serve as a supplemental tool for direct mixture analysis that is both rapid and powerful.

1988 ◽  
Vol 61 (4) ◽  
pp. 639-657 ◽  
Author(s):  
R. P. Lattimer ◽  
R. E. Harris ◽  
C. K. Rhee ◽  
H-R. Schulten

Abstract Three carbon-black-filled rubber compounds of known composition were analyzed by mass spectrometry. Direct thermal desorption was used with three different methods of ionization (EI, CI, FI). In addition, the three rubbers were examined by FAB-MS (without liquid matrix) as a means for surface desorption/ionization. Extracts of the rubbers were also examined using two different solvents (acetone and acetonitrile). Each extract was examined directly by five methods of ionization (EI, CI, FI, FD, FAB). Of the various vaporization/ionization methods, it appears that FI/FD is the most efficient for identifying typical organic additives in rubber stocks. The analysis can be carried out using either the untreated rubber (FI mode) or else a solvent extract (FD mode). Molecular ions are dominant, which facilitates the characterization of the complex organic additive mixtures that are present in typical compounded rubbers. For samples in which the identity of FD/FI molecular ions is unclear, further analysis using other methods (EI, CI, FAB, MS/MS, GC/MS, LC/MS, high resolution) can be carried out to gain additional information. We conclude that FD and FI yield the most useful information in the shortest period of time. The main difference between the results of this study and those of the volcanizate study is with respect to the curatives. Intact accelerator molecules could readily be observed in the spectra from the uncured stocks, while only accelerator fragments could be observed from the vulcanizates.


1984 ◽  
Vol 57 (5) ◽  
pp. 1013-1022 ◽  
Author(s):  
Robert P. Lattimer ◽  
Robert E. Harris ◽  
Doyle B. Ross ◽  
Hugh E. Diem

Abstract From the results presented here, it is clear that FD-MS and FAB-MS are very effective analytical methods for the identification of organic additives in extracts from rubber compounds. In the examples above, the molecular weight information provided by FD and FAB provided a nice complement to the IR data. In cases where IR could give only a general answer (i.e., a compound class), the mass spectral data provided a very specific compound identification. It is encouraging that all the samples examined gave useful spectra by both FD and FAB analysis. In most cases, the same information was obtained by both techniques. Certain compounds, however, were observed by FD but not by FAB (wax, oil, isocyanurate antioxidant). While FD provided only molecular weight information, FAB also provided fragmentation to aid in the confirmation of component assignments. Both the FD and FAB mass spectra were fairly complex for most of the extracts, but for different reasons. In FD, oil and wax oligomers gave many molecular ions over a wide mass range. FAB spectra, on the other hand, were somewhat cluttered due to the normal background ions produced by the sputtering process. With both techniques, however, the various components in some fairly complex mixtures were readily identified.


BMC Chemistry ◽  
2021 ◽  
Vol 15 (1) ◽  
Author(s):  
Masresha Mamo ◽  
Henok Kassa ◽  
Lalit Ingale ◽  
Stefaan Dondeyne

Abstract Background The present study evaluated the compost quality from municipal solid waste (MSW) and organic additives of coffee by-products and leaf of Millettia ferruginea. Compost sample (n = 30) was taken from fresh compost materials and MSW and different organic additive treatments (T1, T2, T3, T4, and T5). Compost treatments phytotoxicity test was conducted using lettuce seed (Lactuca Sativa L. var. crispa). Analysis of variance (ANOVA) was performed using SPSS (version 22) on major compost quality characteristics. Results The compost Physico-chemical characteristics like temperature (26.4 °C), moisture content (45.5%), electrical conductivity (4.6 mS/cm), pH (7.9), total nitrogen (1.2%) and phosphorous content (2918 ppm) in T4 and T5 were analogous but both are significantly different from T3, T2 and T1 compost treatments. Phytotoxicity test using 100% compost treatment media showed that T4 (101%) and T5 (102%) are phytonutrient for lettuce plant. While, T3 and T2; and T1 compost treatments are non-phytotoxic and moderately phytotoxic respectively to lettuce plant. Conclusion Therefore, compost from MSW + M. ferruginea (T4) and MSW + coffee pulp + M. ferruginea (T5) are important for improving the physico-chemical characteristics of compost and are phytonutrient for lettuce plant. Thus, for effectively management of the 75% of organic fraction of waste generated from households in the study area, recycling methods like composting with organic additives must be used at large.


2003 ◽  
Vol 800 ◽  
Author(s):  
Brady J. Clapsaddle ◽  
Lihua Zhao ◽  
Alex E. Gash ◽  
Joe H. Satcher ◽  
Kenneth J. Shea ◽  
...  

ABSTRACTIn the field of composite energetic materials, properties such as ingredient distribution, particle size, and morphology, affect both sensitivity and performance. Since the reaction kinetics of composite energetic materials are typically controlled by the mass transport rates between reactants, one would anticipate new and potentially exceptional performance from energetic nanocomposites. We have developed a new method of making nanostructured energetic materials, specifically explosives, propellants, and pyrotechnics, using sol-gel chemistry. A novel sol-gel approach has proven successful in preparing metal oxide/silicon oxide nanocomposites in which the metal oxide is the major component. Two of the metal oxides are tungsten trioxide and iron(III) oxide, both of which are of interest in the field of energetic materials. Furthermore, due to the large availability of organically functionalized silanes, the silicon oxide phase can be used as a unique way of introducing organic additives into the bulk metal oxide materials. As a result, the desired organic functionality is well dispersed throughout the composite material on the nanoscale. By introducing a fuel metal into the metal oxide/silicon oxide matrix, energetic materials based on thermite reactions can be fabricated. The resulting nanoscale distribution of all the ingredients displays energetic properties not seen in its microscale counterparts due to the expected increase of mass transport rates between the reactants. The synthesis and characterization of these metal oxide/silicon oxide nanocomposites and their performance as energetic materials will be discussed.


2000 ◽  
Vol 51 (2) ◽  
pp. 183 ◽  
Author(s):  
Maria Byrne ◽  
Peter A. Vesk

The Australian freshwater mussel Hyridella depressa sequesters elements in calcium phosphate (CaP) granules that form extensive aggregations in its tissues. Elements contained in these granules were determined by X-ray microanalysis of river and lake mussels from the Hawkesbury–Nepean River system, New South Wales. Granules in freeze-substituted mantle tissue were analysed to determine the variation in element profiles in granules among mussels and among sites. For the common elements Ca, P, Fe, Mg and Mn, granule composition reflected catchment lithology and site trophic status and indicated exogenous input. These were most important for differentiation among lake sites and also indicated differences between lake and river mussels. Site differences seen with some common elements in granules from lake mussels correlated with differences in water chemistry. Trace elements, particularly Al, Cu, Zn and Pb, were also important in lake and river site differentiation. The granules play a major role in element dynamics in freshwater mussel tissues and provide a focal structure for direct analysis of element accumulation by these bivalves. The results indicate that characterization of element content of granules in mussel populations would provide valuable insights into animal–element interactions in freshwater systems for ecological and ecotoxicological investigations.


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