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Analyzing a Specific Component using Group Analysis of msFineAnalysis Ver. 2 - MSTips 303

In 2018, we announced the msFineAnalysis software which was designed to automatically integrate two types of data acquired by EI and soft ionization. Recently, we developed msFineAnalysis Version 2, an enhanced version with additional features. msFineAnalysis Version 2 incorporates two new features: Chromatographic Deconvolution and Group Analysis. In this work, we use the group analysis capabilities of the software to evaluate the pyrolysis GC-MS results for a vinyl acetate resin.

Non-targeted analysis of electronics waste by comprehensive two-dimensional gas chromatography combined with high-resolution mass spectrometry: Using accurate mass information and mass defect analysis to explore the data

Comprehensive two-dimensional gas chromatography (GC×GC) and high-resolution mass spectrometry (HRMS) offer the best possible separation of their respective techniques. Recent commercialization of combined GC×GC–HRMS systems offers new possibilities for the analysis of complex mixtures. However, such experiments yield enormous data sets that require new informatics tools to facilitate the interpretation of the rich information content. This study reports on the analysis of dust obtained from an electronics recycling facility by using GC×GC in combination with a new high-resolution time-of-flight (TOF) mass spectrometer. New software tools for (non-traditional) Kendrick mass defect analysis were developed in this research and greatly aided in the identification of compounds containing chlorine and bromine, elements that feature in most persistent organic pollutants (POPs). In essence, the mass defect plot serves as a visual aid from which halogenated compounds are recognizable on the basis of their mass defect and isotope patterns. Mass chromatograms were generated based on specific ions identified in the plots as well as region of the plot predominantly occupied by halogenated contaminants. Tentative identification was aided by database searches, complementary electron-capture negative ionization experiments and elemental composition determinations from the exact mass data. These included known and emerging flame retardants, such as polybrominated diphenyl ethers (PBDEs), hexabromobenzene, tetrabromo bisphenol A and tris (1-chloro-2-propyl) phosphate (TCPP), as well as other legacy contaminants such as polychlorinated biphenyls (PCBs) and polychlorinated terphenyls (PCTs).

Molecular Characterization of Volatiles and Petrochemical Base Oils by Photo-Ionization GC×GC-TOF-MS

The characterization of organic mixtures by comprehensive two-dimensional gas chromatography (GC×GC) coupled to electron impact (EI) ionization time-of-flight mass spectrometry (TOF-MS) allows the detection of thousands of compounds. However, owing to the exhaustive fragmentation following EI ionization, despite the use of mass spectral libraries, a majority of the compounds remains unidentified because of the lack of parent ion preservation. Thus, soft-ionization energies leading to organic compounds being ionized with limited or no fragmentation, retaining the molecular ion, has been of interest for many years. In this study, photoionization (PI) was evaluated as the ion source for GC×GC-TOF-MS measurements. First, capabilities and limitations of PI were tested using an authentic mixture of compounds of several chemical classes. Ionization energy exhibited by PI, equivalent to 10.8 eV, resulted in significant retention of molecular ion information; [M]+• for alkanes, ketones, FAMEs, aromatics, [M–H]+• for chloroalkanes, and [M–H2O]+• for alcohols. Second, considering the potential of PI for hydrocarbons, base oils, complex mixtures of saturated and unsaturated hydrocarbons blended for finished lubricant formulations, were extensively evaluated. Several chemical classes of hydrocarbons were positively identified including a large number of isomeric compounds, both aliphatics and cyclics. Interestingly, branched-alkanes were ionized with lower excess internal energy, not only retaining the molecular ions but also exhibiting unique fragmentation patterns. The results presented herein offer a unique perspective into the detailed molecular characterization of base oils. Such unprecedented identification power of PI coupled with GC×GC-TOF-MS is the first report covering volatiles to low-volatile organic mixtures.

Compositional elucidation of heavy petroleum base oil by GC × GC‐EI/PI/CI/FI‐TOFMS

Comprehensive two‐dimensional gas chromatography (GC × GC) coupled to time‐of‐flight mass spectrometry is a powerful separation tool for complex petroleum product analysis. However, the most commonly used electron ionization (EI) technique often makes the identification of the majority of hydrocarbons impossible due to the exhaustive fragmentation and lack of molecular ion preservation, prompting the need of soft‐ionization energies. In this study, three different soft‐ionization techniques including photo ionization (PI), chemical ionization (CI), and field ionization (FI) were compared against EI to elucidate their relative capabilities to reveal different base oil hydrocarbon classes. Compared with EI (70 eV), PI (10.8 eV) retained significant molecular ion (M+·) information for a large number of isomeric species including branched‐alkanes and saturated monocyclic hydrocarbons along with unique fragmentation patterns. However, for bicyclic/polycyclic naphthenic and aromatic compounds, EI played upper hand by retaining molecular as well as fragment ions to identify the species, whereas PI exhibited mainly molecular ion signals. On the other hand, CI revealed selectivity towards different base oil groups, particularly for steranes, sulfur‐containing thiophenes, and esters, yielding protonated molecular ions (M + H)+ for unsaturated and hydride abstracted ions (M‐H+) for saturated hydrocarbons. FI, as expected, generated intact molecular ions (M+·) irrespective to the base oil chemical classes. It allowed elemental composition by TOFMS with a mass resolving power up to 8000 (FWHM) and a mass accuracy of 1 mDa, leading to the calculation of heteroatomic content, double bond equivalency, and carbon number of the compounds. The qualitative and quantitative results presented herein offer a unique perspective into the detailed comparison of different ionization techniques corresponding to several hydrocarbon classes.

GC-TOFMS Application: Natural Polymer Analysis by using Pyrolysis-GCxGC-MS - "Urushi" analysis with GCxGC/EI and GCxGC/PI

A Japanese lacquer film called "Urushi" is a natural polymer that has been used as a paint and adhesive for living-wares and craft-wares for approximately 8,000 years. "Urushi" has a complex structure that researchers are trying to understand using pyrolysis-gas chromatograph/mass spectrometer (Py/GC/MS) system. Recently, we developed a new gas chromatograph/high resolution time-of-flight mass spectrometer (GC/HR-TOFMS) system that can be used for comprehensive two-dimensional GC (GCxGC) measurements. Additionally, we have developed a unique combination electron ionization/photoionization (EI/PI) ion source that can be used with this GC/HR-TOFMS system. In this work, we measured "Urushi" samples using this unique Py/GCxGC/HR-TOFMS system in combination with our new combination EI/PI ion source.

Features and Applications of Newly-Developed GC-TOFMS “The AccuTOF GC”

A gas-chromatograph mass spectrometer (GC-MS) is a combined analyzer that has superior ability in analyzing organic compounds qualitatively and quantitatively. The first part, gas chromatograph, separates the compounds included in a sample (mixture), then the second part, mass spectrometer, obtains mass spectra of the compounds to carry out qualitative analysis. Quantitative analysis can be carried out as well from the peak area of the mass chromatogram of the compound. As a mass spectrometer of a GC-MS system, several types of mass spectrometers are on the market, such as magnetic field, quadrupole (QMS), ion trap (ITD), and time-of-flight (TOF). Each mass spectrometer has its own features and applications.

Using Volcano Plots to Compare Vinyl Acetate Resin Samples Measured by Pyrolysis GC-MS

Advances in mass spectrometry are enabling analysis of micro samples and unknown components that were not observable before. As the volume of information acquired from mass spectrometry increases, researchers are calling for simple techniques to analyze the numerous components observed, and as a result, there is a rise in demand for comprehensive analytical techniques including multiple classification analysis. In this work, we analyzed 2 samples in a high resolution GC-TOFMS, using EI, the most widely used ionization technique for GC-MS, and compared the data acquired by using a comprehensive analytical technique.

Type Analysis of Micro Crystalline Wax (Petroleum Wax) by Using Field Desorption (FD) Ionization

Petroleum waxes are a class of hydrocarbons that are solid at room temperature and are classified by the Japan Industrial Standards (JIS K2235) into 3 types: paraffin wax, micro crystalline wax, and petrolatum. A typical micro crystalline wax contains hydrocarbons having a carbon number of 30 to 60 and molecular weights between 500 and 800. In addition to paraffins, these waxes also include large quantities of isoparaffins and cycloparaffins. Field desorption (FD) is an ionization technique that utilizes the tunneling effect of electrons in the presence of a high electric field. The sample is applied directly onto an FD emitter filament, and then an electric current is applied to the filament to produce a high electric field across the emitter surface (including the whisker tips) to desorb and ionize the samples. As a soft ionization technique that minimizes fragmentation and produces molecular ions, FD has been previously used for analyzing refractory compounds and high molecular weight polymers. In this work we ionized a micro crystalline wax by using a JMS-T100GC AccuTOF-GC with FD ionization to do a sample type analysis that was based on the mass and intensity of the resulting ions.

The Qualitative Analysis of an Antioxidant Additive Using the Full Capabilities of the EI/FI/FD Combination Ion Source

JEOL has developed a unique EI/FI/FD combination ion source for the “AccuTOF GCv 4G”, a high- resolution GC-time-of-flight (TOF) MS system. This unique ion source provides the capabilities of GC/EI, GC/FI and FD measurements without having to break vacuum in order to switch between each ionization mode. Additionally, this combination is particularly powerful in that it provides library searchable fragmentation information by using EI and high mass accuracy molecular ion information by using FI and FD. In this work, we measured an antioxidant additive by using each ionization mode available on the AccuTOF GCv 4G combination ion source (EI/FI/FD).

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Corona - Glow Discharge (DART Ion Source)

February 22, 2020
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