Identification of Organic Components in Uncured Rubber Compounds Using Mass Spectrometry

1988 ◽  
Vol 61 (4) ◽  
pp. 639-657 ◽  
Author(s):  
R. P. Lattimer ◽  
R. E. Harris ◽  
C. K. Rhee ◽  
H-R. Schulten
Keyword(s):  
Mass Spectrometry ◽  
Organic Additive ◽  
Molecular Ions ◽  
Organic Additives ◽  
Additional Information ◽  
Filled Rubber ◽  
Rubber Compounds ◽  
Surface Desorption ◽  
Direct Thermal Desorption ◽  
Ionization Methods

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.

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
Keyword(s):  
Neutral Loss ◽  
Direct Analysis ◽  
Organic Additive ◽  
Organic Additives ◽  
Mass Measurements ◽  
Chemical Noise ◽  
Mass Spectral ◽  
Rubber Compounds ◽  
Ionization Methods

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.

Identification of Rubber Additives by Field Desorption and Fast Atom Bombardment Mass Spectroscopy

1984 ◽  
Vol 57 (5) ◽  
pp. 1013-1022 ◽  
Author(s):  
Robert P. Lattimer ◽  
Robert E. Harris ◽  
Doyle B. Ross ◽  
Hugh E. Diem
Keyword(s):  
Molecular Weight ◽  
Mass Range ◽  
Molecular Ions ◽  
Organic Additives ◽  
Compound Identification ◽  
Mass Spectral ◽  
Rubber Compounds ◽  
General Answer ◽  
Background Ions ◽  
Normal Background

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.

Analysis of Components in Rubber Compounds Using Mass Spectrometry

1989 ◽  
Vol 62 (3) ◽  
pp. 548-567 ◽  
Author(s):  
Robert P. Lattimer ◽  
Robert E. Harris
Keyword(s):  
Mass Spectrometry ◽  
High Sensitivity ◽  
High Specificity ◽  
Mass Spectrometric ◽  
Rubber Compound ◽  
Organic Additives ◽  
Mixture Analysis ◽  
Rubber Compounds ◽  
Invaluable Tool ◽  
Modern Mass

Abstract A large number of very successful mass-spectrometric methods have been developed for rubber-compound analysis. The high sensitivity, high specificity, and superb mixture analysis capabilities of modern mass spectrometry make it an invaluable tool in the polymer industry, particularly for qualitative identification of organic additives. In many cases, mass spectrometry can provide unique information that is not available by use of any other technique.

A New Look at Direct Compound Analysis Using Pyrolysis Mass Spectrometry

1983 ◽  
Vol 56 (5) ◽  
pp. 1031-1044 ◽  
Author(s):  
Jerry B. Pausch ◽  
Robert P. Lattimer ◽  
Henk L. C. Meuzklaar
Keyword(s):  
Mass Spectrometry ◽  
Mass Range ◽  
Molecular Ions ◽  
Volatile Components ◽  
Pyrolysis Mass Spectrometry ◽  
Organic Additives ◽  
Single Experiment ◽  
Pattern Recognition Techniques ◽  
Temperature Programmed ◽  
Future Work

Abstract For direct compound analysis, pyrolysis mass spectrometry offers renewed hope that the time-consuming and costly separations currently required can be bypassed, at least in part. Polymer blends and copolymers are readily identified along with certain additives. The ability to achieve this information quickly from a single experiment is a valuable improvement. However, more work needs to be done to identify curatives, oils, and higher molecular weight rubber chemicals in compounds. For example, the mass range scanned needs to be expanded to detect higher molecular ions. Temperature-programmed Py-MS may prove useful in separating the more volatile components (nonpolymeric oils and organic additives) for easier detection. Future work will also assess the quantitative potential of the technique. The success with experiments on CPVC materials using pattern recognition techniques opens up a new dimension for compound analysis. Besides being able to determine composition, selected information about reaction mechanisms, morphology, physical properties, or other important parameters may now be possible.

Tandem Mass Spectrometry (MS/MS) for Analysis of Organic Additives in an Uncured Rubber Compound

1990 ◽  
Vol 63 (2) ◽  
pp. 298-307 ◽  
Author(s):  
R. P. Lattimer ◽  
H. Muenster ◽  
H. Budzikiewicz
Keyword(s):  
Mass Spectrometry ◽  
Direct Analysis ◽  
Molecular Ions ◽  
The Other ◽  
Ion Current ◽  
Diagnostic Tools ◽  
Ion Currents ◽  
Rubber Compound ◽  
Organic Additives ◽  
Other Hand

Abstract In this study, we examined the feasibility of obtaining MS/MS data for organic additives in an uncured rubber compound using several different ionization methods. EI-MS/MS worked well for those additives that gave intense molecular ions (M+·) via this mode of ionization. CI-MS/MS also worked quite well for most additives; the CI MH+ ion currents were generally quite intense and stable over a long period of time. Although fragmentation patterns for MH+ ions are different from those obtained from M+· ions, the fragments are still good diagnostic tools for identifying the original molecule. On the other hand, the FI- and FD-MS/MS analyses of these rubber samples were generally not very satisfactory. This was due to the fact that FI/FD ion currents were too weak and unstable to give daughter-ion spectra with good S/N. It may be concluded that the best way to detect and identify typical organic additives in a compounded rubber is to use a combination of EI- and CI-MS/MS. In this study, intact accelerators were successfully analyzed by MS/MS. The two accelerators in this particular rubber (OBTS and DPG) could be confirmed quite readily by daughter-ion analysis of their intense MH+ ions (CI-MS/MS). Daughter-ion analyses of M+· obtained by either EI, FI or FD modes were not very successful, however. In EI, the difficulty is that molecular ions are quite weak (or even absent) for typical rubber curatives. In FI and FD, on the other hand, a very large proportion of the ion current for accelerators resides in the molecular ion. The difficulty here is that the total ion current produced by FI or FD is rather low. The MS/MS approach has proven to be very useful for direct analysis of organic additives in rubber compounds. The principal advantage in using MS/MS is that more information is available from mixtures than can be obtained by direct analysis using conventional mass spectral methods. The MS/MS technique is also rapid experimentally compared to other techniques for mixture analysis such as GC/MS, LC/MS, or high resolution (AC-MS). Finally, since MS/MS involves two stages of mass analysis, it leads to a great reduction in the chemical noise associated with single-stage mass spectrometry. This leads to the facile confirmation of the presence (or absence) of specific components in a complex mixture.

scholarly journals Evaluation of compost quality from municipal solid waste integrated with organic additive in Mizan–Aman town, Southwest Ethiopia

BMC Chemistry ◽  
2021 ◽  
Vol 15 (1) ◽  
Author(s):  
Masresha Mamo ◽  
Henok Kassa ◽  
Lalit Ingale ◽  
Stefaan Dondeyne
Keyword(s):  
Municipal Solid Waste ◽  
Solid Waste ◽  
Organic Additive ◽  
Chemical Characteristics ◽  
Lettuce Seed ◽  
Organic Additives ◽  
Lettuce Plant ◽  
Compost Quality ◽  
Physico Chemical ◽  
Phytotoxicity Test

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.

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