Eliminate Column Breakage in High Temperature Biodiesel Analysis

Beat high temperature column breakage with Restek MXT-Biodiesel TG columns. More stable than fused silica, for accurate, reliable performance and longer column lifetime. Available with either factory-coupled or fully-integrated retention gaps.

Restek has raised the bar with a new high-temperature MXT-Biodiesel TG column line to complement our fused silica column line for biodiesel analysis. These new MXT-Biodiesel TG columns are stable to 430 °C and offer unique retention gap options that minimize dead volume and leaks. Choose either a 0.32 mm column factory-coupled to a 0.53 mm retention gap, or select a single unit 0.53 mm column featuring Integra-Gap, a built-in retention gap that eliminates the need for a connector. Both designs are extremely stable at high temperatures and produce fast elution times and sharp peaks for high molecular weight glycerides.

Unsurpassed Stability

The high temperature programs required for analysis of biodiesel oils (B100) by either ASTM D-6584 or EN-14105 methodology present a significant challenge to the analytical column. High-temperature fused silica tubing breaks down under these extreme conditions, but the metal MXT tubing does not degrade, even at temperatures up to 430 °C (Figure 1). This allows analysts to bake out any residue eluting after the triglycerides, preventing carryover without damaging the column.

So how well do the MXT-Biodiesel TG columns perform? We conducted a benchmarking experiment comparing an MXT-Biodiesel TG column with an Integra-Gap retention gap to a high-temperature fused silica column which was coupled to a conventional 0.53 mm retention gap. Methodology followed ASTM method D-6584, except the final temperature was modified to 430 °C. Both columns were subjected to 100 temperature cycles up to 430 °C and then derivatized B100 was injected to check column performance.

This evaluation was performed using a Shimadzu 2010 gas chromatograph equipped with a flame ionization detector, a model AOC 20i + S autosampler with a 10 µL SGE syringe and 42mm 26-gauge needle, and a cold on-column programmable injector with a stainless steel injector insert. A Parker hydrogen generator supplied the carrier gas. Peak symmetry and retention time were evaluated as indicators of thermal stability.

Peak symmetry of butanetriol on a commercial high-temperature fused silica column deteriorates after just 20 injections, compared to the excellent symmetry that is maintained on the MXT-Biodiesel TG column (Figure 2). In addition to peak shape, retention time stability was used to evaluate column performance. The decrease in retention time seen on the high-temperature fused silica column indicates the liquid phase is being lost (Figure 3). In contrast, the consistent retention times obtained on the MXT-Biodiesel TG column demonstrate its stability. Practically, this translates into reliable performance and longer column lifetimes.

Analytical Alternatives

Factory connected 0.32 mm MXT-Biodiesel TG columns & 0.53 mm retention gaps

For accurate analysis of heavy triglycerides, on-column injection is required. ASTM D-6584 describes the use of a 0.32 mm analytical column coupled with a 0.53 mm retention gap. The 0.53 mm ID retention gap allows the cool on-column technique to be used, but care must be taken to minimize dead volume and to establish a leak-tight connection. Restek’s 0.32 mm MXT-Biodiesel TG columns are factory-coupled to a 0.53 mm MXT retention gap with an MXT low-dead-volume connector, ensuring a leak-tight connection. Target analytes resolve well and the solvent and triglyceride peaks show excellent symmetry (Figure 4).

0.53 mm MXT-Biodiesel TG columns

The 0.53 mm MXT-Biodiesel TG columns are a simpler alternative to using a 0.32 mm column coupled to a 0.53 mm retention gap. Restek applied Integra-Gap technology to the 0.53 mm MXT-Biodiesel TG columns, eliminating the column coupling. These single unit leak-proof columns feature a built-in retention gap, reducing the risk of peak broadening and tailing. Chromatography from the 0.53 mm MXT-Biodiesel TG with Integra-Gap technology (Figure 5) is excellent and comparable to that obtained on the 0.32 mm ID column in Figure 4.

Conclusion

As demonstrated, for high temperature GC analysis, the metal MXT-Biodiesel TG column is a rugged column that withstands the harsh temperatures required for total residual glycerin analysis. The column has the resolution needed for accurate, reliable results and is more stable at high temperatures than competitive fused silica columns, leading to longer column lifetimes. To improve the reliability and robustness of your biodiesel analyses, try a Restek MXT-Biodiesel TG column.

Column	MXT-Biodiesel TG, 15 m, 0.32 mm ID, 0.10 μm (cat.# 70291) with a 2 m x 0.53 mm MXT retention gap connected with an MXT low-dead-volume connector (17 m total length)
Standard/Sample	Biodiesel (B100), derivatized
Diluent:	Heptane
Injection
Inj. Vol.:	1 µL cold on-column
Temp. Program:	Oven track
Oven
Oven Temp.:	50 °C (hold 1 min) to 180 °C at 15 °C/min to 230 °C at 7 °C/min to 380 °C at 30 °C/min (hold 5 min)
Carrier Gas	H2, constant flow
Flow Rate:	3 mL/min

Detector	FID @ 380 °C

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Column	MXT-Biodiesel TG, 14 m w/2 m Integra-Gap (16 m total length), 0.53 mm ID, 0.16 µm (cat.# 70289)
Standard/Sample	Biodiesel (B100), derivatized
Diluent:	Heptane
Injection
Inj. Vol.:	1 µL cold on-column
Temp. Program:	Oven track
Oven
Oven Temp.:	50 °C (hold 1 min) to 180 °C at 15 °C/min to 230 °C at 7 °C/min to 380 °C at 30 °C/min (hold 5 min)
Carrier Gas	H2, constant flow
Flow Rate:	4 mL/min

Detector	FID @ 380 °C

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