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The Analysis of Trace Contaminants in High Purity Ethylene and Propylene Using GC/MS Agilent Technologies/Wasson ECE Monomer Analyzer Application

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The Analysis of Trace Contaminants in High Purity Ethylene and Propylene Using GC/MS Agilent Technologies/Wasson ECE Monomer Analyzer Application The Analysis of Trace Contaminants in High Purity Ethylene and Propylene Using GC/MS Agilent Technologies/Wasson ECE Monomer Analyzer Application (thermal conductivity detection), the Introduction Authors use of GC/MSD demonstrates com- Fred Feyerherm parable performance with respect to For the polymer industry, the 119 Forest Cove Dr. linearity and repeatability: for exam- purity of ethylene and propylene Kingwood, TX 77339 ple, for mercaptans and sulfides monomer feedstocks is a high (40–100 ppb) in the ethylene assay, priority. Trace contaminants at John Wasson correlation coefficients for calibra- the part-per-billion (ppb) con- Wasson-ECE Instrumentation tion curves range from 0.992 to 1.000 centration levels can affect 101 Rome Court and relative standard deviations yields dramatically by altering Fort Collins, Colorado 80524 range from 1.95% to 9.31% RSD. subsequent polymer properties Compared to GC/FID for the range of and characteristics. Additionally, contaminant analytes studied here, some trace impurities can irre- Abstract the sensitivity is increased 50-fold; versibly poison reactor catalysts. compared to GC/TCD, the sensitivity The competitive marketing A new product (Application 460B-00) is increased 5000-fold. While the strategies of monomer manufac- from Agilent Technologies/Wasson- sensitivity of MS detection is compa- turers include using new analyti- ECE uses a 5973N GC/MSD (gas rable to that of sulfur chemilumines- cal technologies to guarantee chromatograph/mass selective cence detection for sulfur-containing lower and lower trace impurity detector) for the determination of compounds, MS has the same sensi- levels. trace levels of impurities that are tivity for a broader range of com- moderate-to-low carbon-content pound types. Moreover, the use of Agilent Technologies/Wasson- such as oxygenates, mercaptans, MS detection provides specificity for ECE has focused on supplying sulfides, arsine, and phosphine in positive identification of analytes. In integrated application products ethylene and propylene. This work Application 460B-00 the multipart for the analysis of impurities in describes the performance of Appli- assays are automated via "composite polymer feedstocks. One of the cation 460B-00 with respect to lin- methods" [1]. The result is a tool that most recent products, Applica- earity, repeatability, and limits of provides higher productivity and tion 262-00, effectively combined detection (for most compounds, low more key information about feed- the separate analyses for ethyl- parts-per-billion). Compared to stock materials-both of which aid ene and propylene into a single determinations with GC/FID (flame the polymer industry. analytical system [2]. ionization detection) or GC/TCD Application 262-00 employs a MS detection is equivalently sen- For such a complex sample, no gas chromatograph (GC) with sitive for these compounds. How- single gas chromatographic two separate flame ionization ever, MS detection offers gains in column provides adequate sepa- detectors (FIDs), two capillary sensitivity for those compounds ration of the whole range of ana- columns, appropriate valving, with little or no FID response lytes and matrix components. and analytical methods to quan- factors, for example, oxygenates, Different selectivities of the cap- titate very low levels of carbon sulfur-containing compounds, illary column stationary phases monoxide and carbon dioxide by and compounds with no carbon- must be invoked to separate the a methanizer FID and paraffins hydrogen bonds (hydrogen sul- various groups of very similar and olefins up to n-pentane by fide, carbonyl sulfide, arsine, analytes. For this reason, direct FID. Recently Agilent phosphine). Moreover, the selec- Agilent Technologies/Wasson- Technologies/ Wasson-ECE has tivity afforded by MS detection is ECE employs a multivalve, expanded the capabilities of important because it provides multicolumn approach to the Application 262-00 by adding confirmation that an analyte in chromatograph configuration. mass spectrometric (MS) detec- question is indeed present by tion in another product, Applica- examining its mass spectrum Agilent Technologies/Wasson-ECE tion 460B-00. This note describes (scan mode) or monitoring of Application 460B-00 applying GC/MS instrumentation multiple, specific ions (selected and methods to analyze trace ion monitoring - SIM mode). A new application product was contaminants in polymer grade developed to merge the advan- ethylene and propylene The GC/MS methods described tages of MS detection with the feedstocks. here address a range of analytes necessary resolution afforded by beyond the scope of Application appropriate chromatographic 262-00. columns and automatic control Using GC/MS for Trace of valved GC injections. The Contaminant Analyses Gas Chromatographic Separation application includes multiple special inert capillary columns Mass Spectrometric Detection Even with the inherent strengths that do not irreversibly bind the of a mass spectrometer, some analytes, addition of multiple Utilizing a mass spectrometer as chromatography must still be valves, passivation of all compo- the chromatographic detector employed. The detector's selec- nents along the sample path (for provides significant benefits: tivity is not absolute, especially example, valves, transfer lines), when simultaneously detecting • Increased sensitivity analytical methods for the components at vastly different GC/MS, and control software • Detection of analytes that do concentrations (ppb) versus bulk that coordinates the entire not produce a response with or percent levels). This means application. a FID that the ppb contaminants must be reasonably separated from In the multivalve, multicolumn • Selectivity their ethylene or propylene approach, the sample (a gas or • Positive identification matrix since coelution of a trace vaporized liquid) is purged through mass spectra contaminant with the major through the injection valve. In matrix component yields a false this manner, the injection valve As the impact of trace levels of positive with respect to the cont- contains an aliquot of original impurities becomes better aminant. Additionally, some of sample, sized appropriately for understood, the need for increas- the analytes may interfere with the column to be used. The flexi- ing sensitivity in an analytical each other by having the same bility of programming both valve technique becomes more impor- molecular weight and/or frag- operation and chromatographic tant. With flame ionization ment ions. Therefore, both chro- system pressures results in the detection in Application 262-00, matography and mass sequential injection of the detection levels for carbon spectrometry are needed to aliquot onto one of the multiple monoxide and carbon dioxide provide identification. columns, the appropriate one are on the order of 50 ppb while being selected with a portion of those for the paraffins and the total analysis in mind. Each olefins up to n-pentane are injection process defines a about 1 ppm (parts-per-million). 2 method, resulting in a total of Experimental characterized for the evaluation three sequential methods that of Application 460B-00. Note comprise a full “composite The instrumentation is outlined that the ethylene and propylene method” to perform the selected in Table 1. For the results pre- analyses each require three sep- assay. In executing a “composite sented here, an HP 5972 MSD arate GC/MS methods; these method,” Agilent Technologies/ was used. Table 2 outlines the methods are not the same. Wasson-ECE's Composite Analy- impurities that were sis Control Software (CACS) automatically sequences the sampling of the three separate Table 1. The Instrumentation and Control Software for the Ethylene and Propylene aliquots of a feedstock sample, Analyses in the Agilent Technologies/Wasson-ECE Product, Application 460B-00 applying the appropriate GC/MS methods to each, and produces a Mass spectrometer 5973 MSD and later models combined, final report. Gas chromatograph 6890 GC GC Valve configuration Provided by Agilent Technologies /Wasson-ECE. A Modular Approach to the Analysis Sample loops of 100 µL and 500 µL of Trace Contaminants: Building on Application 460B-00 Columns Provided by Agilent Technologies/Wasson-ECE: Wasson Part No. KZA and Wasson Part No. KZB Application 460B-00 is a build- Software G1701 DA ing block in a modular approach · to providing the degree of · Composite Analysis Control Software from automation appropriate to the Agilent Technologies/Wasson-ECE users' needs. As described just GC/MSD Methods Provided by Agilent Technologies/Wasson-ECE above, Application 460B-00 is suitable for use in the laboratory where an analyst connects one pressurized sample container at Table 2. Analytes Used to Characterize the Performance of Agilent Technologies/ a time to the system. However, a Wasson-ECE Application 460B-00 for Impurities found in Ethylene sampling system that automati- Component Quant ion Prepared analyte levels (ppb) cally and sequentially samples Methyl mercaptan 47 25, 35, 70, 115, 410 pressurized sample containers is available from Agilent Ethyl mercaptan 62 15, 25, 55, 105, 315 Technologies/ Wasson-ECE; once Methyl-t-Butyl ether 73 10, 20, 38, 75, 223 the samples are installed, no Methanol 31 28, 55, 110, 205, 625 user intervention is required. t-Butanol 59 12, 25, 45, 85, 265 Moreover, other products from Ethanol 31 18, 38, 75, 140, 433 Agilent Technologies/Wasson- ECE move Application 460B-00 isopropanol 45 15, 30,
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