11 Analytical Instrumentation
the syringe, providing a cost-effective solution as the syringe has no direct contact with the sample, resulting in an annual replacement of the syringe. This integration results in a compact analyzer setup.
The new Vectra, which succeeds the Archie autosampler, operates on the direct syringe injection principle. With a substantial capacity of up to 150 sample positions for standard 2 mL vials, the Vectra has additional options for high-throughput laboratories.
Offering high-performance conditioned tray modules, with 50 sample positions each, the Vectra introduces both cooling and heating capabilities. Such thermal control options were previously unavailable on the Xplorer-V when used with its internal autosampler.
Combining the Vectra autosampler with the Xplorer-V analyzer results in a powerful synergy, leveraging the strength of both systems. To validate the performance of this combination, an extensive matrix evaluation study was conducted on a wide range of sample matrices, affirming the power of the setup. This paper presents an extract of the results from this research.
Calibration:
For calibration of the Xplorer-V with the Vectra autosampler, the following calibration samples were introduced into the analyzer combination (N = 5 per calibration level). This resulted in a calibration line with a coefficient (R2 of 0.999941 for Total Sulfur.
) Matrix evaluation:
A wide variety of different sample matrices was collected from a renowned contract laboratory and injected into the Xplorer-V equipped with a Vectra autosampler over a period of five days. Each sample matrix was subjected to five repetitions daily, with the average concentration and Relative Standard Deviation (RSD) calculated and validated. The variation in Initial Boiling Points (IBP) and Final Boiling Points (FBP) effectively show a good representation of the variation in sample matrices. The average results for Total Sulfur are reported in mg/kg.
System performance:
For verification of the repeatability and system performance, 3 matrices were selected to inject over an extended period of time: - Gasoline - Diesel - B100/ FAME
The three sample matrices were injected in triplicate into the Xplorer-V and Vectra combination. Especially the B100/ FAME samples are notoriously heavy on cleanliness and have a high impact on system performance. This matrix may contain higher salts and Glycerin concentrations, which take a high toll on the needle of the syringe and the quartz combustion tube of the analyzer.
The collected data shows consistent long-term performance with 534 injections for B100/FAME samples over more than 100 days, achieved without re-calibrating the system.
Commercial Gasoline and Diesel are subject to maximum Sulfur levels as stipulated by US EPA Tier III and EU Euro 5 regulations. These kinds of matrices are typically analyzed in large quantities by various laboratories.
The following graph (see graph 1) illustrates the performance over approximately 350 injections for commercially available Gasoline and Diesel samples. The results, expressed in mg/kg, were obtained without re-calibrating the system.
Used system setup:
For the validation study, the combination of Xplorer-V with the Vectra autosampler was utilized. TE Instruments developed a special adapter bracket to seamlessly integrate the Vectra autosampler with the Xplorer-V. Maintaining the Xplorer-V as the smallest and most compact analyzer for combined analyses of Total Sulfur and Total Nitrogen on the market.
The system holds three sample trays, each with 50 sample positions for 2 ml vials. Additionally, two optional sample trays with temperature conditioning (heating/ cooling) can be included to enhance the configuration.
A notable feature of the Vectra is its capability for automatic syringe switching. The system can mount three syringe holders,
Graph 1: Long run on Commercial Gasoline and Diesel samples
allowing for automatic syringe switching. This option improves system robustness and workflow as follows:
- Automatic switching to different syringe volumes without operator intervention
- Automatic switching to a new syringe acting as a redundant option
Typically, injection volumes of 50 μL gave the best repeatability, results, and peak forms for all the tested matrices. All matrices were injected with a single uniform system method offering a robust solution for analysts operating the analyzer.
Table 2: System settings Parameter
Oxygen Flow Argon Flow
Inlet cleaning time
Furnace Temperature I Furnace Temperature II
Internal System Temperature Injection Speed Injection Volume
Setting
400 mL/min 50 mL/min 10 seconds 800 °C
1050 °C 31 °C 1 µL/s 50 µL
Table 1: Overview of sample matrices results and day to day average/RSD.
Author Contact Details Sebastian Sanchez • TE Instruments
• Address: Voltaweg 22, 2627 BC Delft, The Netherlands
• Tel: +31 (0) 15 879 55 59 • Email:
sales@teinstruments.com • Web:
www.teinstruments.com
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