====== Gas Chromatograph/Mass Spectrometer ====== * Manufacturer - Hewlett Packard * Model Number - HP 5890 II * Shown with Autosampler (on right) {{:atmos:535:projects:tekmar2.jpg|}} ======Theory====== * Six Basic Principles in Performing Gas Chromatography: * Flow Controller * Sample Introduction Device * Column * Oven * Detectors * Computer Interface (Data Management) ====Gas Chromatography==== * Process involves the physical separation of compounds in a mixture by injecting the mixture into a tube (column) that contains a silica based inert compound. The mixture is called the mobile phase and the silica compound is known as the stationary phase. A carrier gas is used to flush the mobile phase through the column. The stationary phase will pass some compounds and slow down others. * Compounds in mixture are identified by their retention times. * Retention time is the time it takes for the individual compound to pass through the entire column. ====Mass Spectrometry==== * Mass spectrometry deals with shattering compounds into component ions by passing sample through an ionization (high voltage) source. * The ions are separated by a large magnetic or electric field. The ions are then collected in "traps" and then analyzed. A charge to mass ratio is calculated and a mass spectra is generated. {{:atmos:535:projects:ms.png|}} ======Interface and Equipment====== {{:atmos:535:projects:gcsetup.png|}} ====GC Column==== * Capillary tube of length between 1 to 100 m and thickness range of 0.25 to 5 mm * Column is either packed with silicone based stationary phase or inside is coated with the material. {{:atmos:535:projects:column.png|}} ====Hardware==== * Nitrogen Gas Cylinder * Carrier gas for mobile phase, non-reactive and inert to sample being tested * Hydrogen Gas Cylinder * Used to combust sample at the end of the analysis * Plumb Lines * To connect cylinders to GC/MS * Vacuum Pump * Used for MS which operates under low pressure conditions ====Computer Interface==== * The GC/MS can either be run automatically or manually. * Both require use of computer program. * PC and software are Windows based. * Software contains program that controls oven temperature such that the oven starts at a low temperature and ramps up to a higher temperature at different heating rates. ======Calibration====== * Calibration standard is made of a pure compound (e.g. bromofluorobenzene) and is used for quality control of the GC/MS. * The compound has a specific retention time and a specific mass spectra. * Quality control is usually done at after a fixed number, usually 20, of samples have been analyzed. * Quality assurance is done whenever the instrument cannot be calibrated. * QA steps include: * Changing the check standard - an aged check standard can affect accuracy of instrument * Conditioning the column - bake the column to a temperature of 300oC to remove contaminants * Replacing the column - cracks and fissures * Checking the carrier gas flow rate - mobile phase may be going faster or slower than normal * Replacing the entire instrument - GC oven may be irreparable, internal plumbing damaged, etc ======Purpose and Performance====== * A combined GC/MS has the ability to detect minute quantities of a solute contained within a larger volume of solvent. For example, a properly calibrated GC/MS can quantify organic contaminants, such as volatile organic carbons (VOC) on the order of parts per billion present within large volumes of soil, water or air. * This is useful in environmental sampling especially when looking for compounds that adversely affect human health. * Liquid or air samples on the order of milliliters can be sampled. * If using the direct inject method, microliters of sample are usually used. * Sample Injection * Non-Direct Inject * Usually done with help of autosampler. * Nitrogen gas is bubbled into a tube containing sample to draw out the volatile parts of the mixture. * Semi or non-volatile compounds are not usually sampled by GC. * Mixture is held in a trap until GC signals the computer to start the oven program. * Mixture is injected into the inlet of both the GC and MS at the same time. Both instruments collect data at the same time. * As the compound is sent through and out of the column, the MS shatters each compound into ions as they are ejected and quantifies their mass spectra. * At the end of the column, there is a flame ionizing detector, FID, which combusts the sample with the aid of hydrogen gas. * The GC quantifies the amount of burn and the time of ionization to render a retention time and concentration. * Direct Inject * Analyst will start computer program and inject sample at same time rather than using autosampler. ======Data===== {{:atmos:535:projects:scan2.jpg|}} * Top picture shows the chromatogram. * Chromatogram shows peaks for each compound in the mixture according to retention time. It also shows concentrations of the compounds. * Integrated area of peak is the concentration. * Bottom picture shows the mass spectra. * Using the reference spectra library that comes with the GC/MS software, an analyst can identify each peak by clicking on the highest point of the peak. * At the end of the mass spectra is the molecular weight of the ion. * For example, chloroform is a chlorinated VOC with molecular weight of 119.5 g/mol. The ion molecular weight will be somewhere between 116 and 118 g/mol. The discrepancy is due to isotopes of carbon and chlorine. ======Usage and Deployment====== * Liquid samples are collected in bottles and air samples are collected in bags. * Air samples can be direct injected into GC/MS from the bag instead of by autosampler or syringe as with liquid samples. * Does not perform real time sampling. * In a production laboratory setting, a GC/MS can be dedicated to performing emergency sampling which requires a fast turn around. * Most samples that are being tested for VOCs have an average sampling time of 30 minutes from injection to the end of the analysis. * GC/MS is designed to be used in a stationary environment. * Complex setup of GC, MS, computer interface, carrier gas cylinders, and plumbing make it difficult to use in a mobile setting (e.g. aircraft). * Less sophisticated instruments can be used in mobile platforms. * Martian land rover has onboard GC/MS but uses much less sophisticated sampling techniques due to space constraints. * Fields Other Than Environmental and Space Science GC/MS Is Used for * Forensic Science * Toxicology * Drug Screening * Pesticides * Power Consumption * GC/MS can be used on standard 120 V (220 V if 50 Hz cycling alternating current) power line but requires high current for MS. * 800 W power consumption * Cost * $40,000 for GC/MS combination * $1000 for PC and software * $500 for gas cylinder - lasts approximately three weeks with 24 hour consumption ======Acknowledgments and References===== * GMI, Inc - [[http://www.gmi-inc.com/Products/HP%205890%20GC.htm]] * University of North Dakota, Chemistry Department, Abbott Hall GC/MS Lab * HP 5890 GC/Agilent 5973 MS User Manual * TestAmerica Labs, Inc (Formerly Severn Trent Labs), Edison, New Jersey