Application Notes: GC

This application details a fast, reliable and highly selective trace-level screening method for the quantification of polychlorinated biphenyls (PCBs) in environmental, food and biological samples, using gas chromatography and a triple stage quadrupole mass spectrometer. The analytical strategy is analogous to the well-established US Environmental Protection Agency (USEPA) Method 1668A.

QC test probes serve a vital function in ensuring the reproducibility of modern GC columns. These probes ensure that the columns have been properly deactivated, contain the correct amount of stationary phase, and have the same relative retention as the last column purchased. The choice of individual compounds in these test mixes varies widely and can have profound consequences on the performance of a column in the users' applications.

Synthetic fused silica capillary tubing is commonly used as the preferred substrate for chromatographic separation columns. In limited instances the absorption and diffusion of molecules into and through the fused silica deserves consideration.

Escalating costs and increasing demands for helium, coupled with diminishing helium supply, have given rise to the investigation and use of hydrogen as an alternate choice of carrier gas for use in gas chromatography (GC) applications. This application note illustrates that the use of hydrogen as a carrier gas as an alternative to helium in refinery gas applications is not only possible, but also results in improved performance and higher sample throughput.

Mycotoxins, toxic secondary metabolites of several fungal species, represent food safety issues of high concern. Deoxynivalenol, the most abundant trichothecene mycotoxin, can be found worldwide as a contaminant of wheat, barley, maize and other cereals (1,2). The transmission of deoxynivalenol from barley into beer has been reported in several studies (3,4). Therefore, its levels should be controlled.

Semivolatile analyses using methods similar to US EPA method 8270 (1) are important in environmental laboratories worldwide. A number of acidic compounds such as benzoic acid or 2,4-dinitrophenol and strong bases such as pyridine or benzidine are active species found in the semivolatile sample set. These highly polar species are particularly susceptible to adsorption into active surfaces in the sample flow path, including the column itself. System and column inertness are critical for effective analysis of these active chemical species.

Political priorities as well as economic interests have fueled a dramatic growth in the biofuel industry, due much in part to research funding and tax incentives. Currently the world's ethanol production is estimated to be over 16 billion gallons a year. This number is expected to increase in the next few years, reaching an estimated yearly production of 20 billion gallons by 2012. Today, many ethanol producers add fermentors to expand their production capacity. In order to continue using existing HPLC equipment for the increased monitoring, increased analytical throughput is needed.

Capillary flow technology (CFT) devices are microfluidic components that extend capillary GC capabilities through simple and robust connections between pressure/flow modules and columns. One of the most powerful and simple is the CFT Tee. This is especially useful in GC–MS analysis providing (1) rapid column and inlet maintenance without MSD venting and (2) the capability of rapidly removing late eluting interferences from the column by forcing their retreat into the injection port through "backflushing". Removing these interferences improves column and detector longevity and analytical integrity. Backflushing is very valuable for trace GC–MS analysis in samples from complex matrices like soil, foods or tissues. The CFT Tee uses pressure-pulsed injections and constant flow mode with minimal loss in the MS signal. This approach will be useful to all GC–MS users who want to improve their instrument uptime.

A new APCI/APLI source enables a high resolution TOF-MS to be coupled on LC and GC, thus increasing flexibility and performance of TOF-MS in combination with GC.

Synthetic fused silica capillary tubing has proven to be a vital component in many separation science techniques. Recently, it has expanded to serve an array of scientific markets. In most cases, an understanding of the internal surface chemistry is of fundamental importance.

There are many misconceptions about what it means to perform fast gas chromatography (GC) and what the term fast GC implies. Fast GC is often associated with the use of hydrogen as a carrier gas and, although this is certainly a good approach, it is not always necessary to shorten the analysis time. A second misconception is that changing column dimension results in time-consuming method development. Using high-efficiency GC columns can greatly reduce the analysis time and when coupled with the method translation software, the time spent on method development can be greatly minimized.

EPA Method 525.2 describes the procedure to determine low ppb levels of semi-volatile organic material in drinking water using solid phase extraction (SPE) or liquid-solid extraction (LSE) techniques. The City of Fort Worth, Water Department implemented an automated SPE process for the analysis of semi-volatiles by EPA Method 525.2, using the Atlantic "Certified for Automation" SPE Disk for EPA Method 525.2. Ethyl acetate, methanol, and water were used to condition the Atlantic disk prior to the extraction step. The extraction solvents used were a 1:1 mixture of methylene chloride and ethyle acetate. Extracts were then analyzed by GC–MS using a splitless injection technique.

The purge-and-trap (P&T) technique for analysis of volatile organic compounds (VOCs) was pioneered in the 1970s at the United States Environmental Protection Agency (USEPA) research laboratory in Cincinnati. Many of the operational parameters developed during this time period are still included in USEPA methods. While these parameters still produce good analytical results, they do not take advantage of advances in instrumentation that enable analysis of emerging contaminants such as fuel oxygenates, and increased sample throughput.

The Zebron ZB-Bioethanol GC column reduces fuel ethanol analysis time to less than 8 min, while providing complete resolution of methanol and ethanol from all denaturant components. This newly developed GC column is suitable for analysis following ASTM Method D 5501 and Europe prEN 15376.

A method for trace odor components, isopropyl-methoxypyrazine (IPMP), isobutyl-methoxypyrazine (IBMP), methylisoborneol (MIB), and geosmin in drinking water involving the use of solid phase microextraction (SPME) and the SLB-5ms capillary column using gas chromatography/mass spectrometry (GC–MS).

Gel permeation chromatography (GPC) has been used as an effective cleanup procedure for removing high molecular weight interfering molecules such as lipids, pigments, proteins, and polymers before GC or HPLC analysis. The GPC cleanup method has been extensively documented (1–3) and is also recommended in US EPA SW-846 Method 3640A. To demonstrate the efficacy of this method to extract polar and nonpolar substances by using the KNAUER Smartline GPC Cleanup Unit 6500, olive oil samples were investigated by spiking these with different types of organic pollutants, including PAHs, phthalates, phenols, and triazine.

Phthalates are added to plastics to increase flexibility. Recently, concerns have been raised over the effect of phthalate exposure from plastic materials on human health.

PLOT columns are often used in GC analyses when it is necessary or desirable to retain one class of solutes in favour of other solutes that have little or limited interactions with the surface of the stationary phase. With a PLOT column, chromatographers can even cause lower boiling point compounds to elute well after higher boiling point compounds, thus providing better qualitative and quantitative separations for the solutes of interest.

AC Analytical Controls developed a new chromatographic solution that complies with all ASTM & EN chromatographic test methods listed in biodiesel specifications: the AC all-in-one Biodiesel analyser. Analysis results demonstrate that the AC analyser complies with EN 14103, EN 14105, EN 14106, EN 14110 & ASTM D6584 methods.

The performance of lubricating oil is significantly degraded by the presence of fuel contaminants such as gasoline and diesel. Recycled oil is particularly susceptible to this form of contamination. Consequently, producers and distributors of lubricating oil must go to great lengths to ensure the levels of fuel contamination are kept to a safe limit (typically 4–5%) in these products.