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Analytical Instrumentation


High-Sensitivity Gas Chromatograph Incorporates Novel Plasma Technology to Enable Trace Analysis


Shimadzu Corporation (Germany) recently introduced the Tracera, a high-sensitivity gas chromatograph. Tracera is equipped with the newly developed barrier discharge ionisation detector (BID), which is capable of detecting all types of trace organic and inorganic compounds, with the exception of helium (He) and neon (Ne), at the 0.1 ppm level (i.e. sub-ppm, where ppm refers to parts per million). Tracera GC is applicable for many types of high-sensitivity analyses typically performed with GC systems incorporating different detectors.


Gas chromatographs are used for research & development and quality control in a number of fields, involving petrochemistry, fine chemicals, the environment, pharmaceuticals, foods, electronics/semiconductors, and fragrances. In recent years, demands for higher sensitivity and trace quantity analyses have increased. Examples include impurity analysis on the order of a few ppm for materials used in fine chemical products, and gas purity analysis for semiconductor manufacture.


Thermal conductivity detectors (TCD) and flame ionisation detectors (FID) are general-purpose detectors used in conventional gas chromatographs. A TCD detects a variety of inorganic and organic compounds, excluding the carrier gas component, but the sensitivity is insufficient. An FID is capable of detecting trace components at the ppm level, but can only detect organic compounds (excluding formaldehyde and formic acid). Analysis has thus required complex systems incorporating a variety of detectors to suit the target component.


With this issue in mind, Shimadzu has investigated the basics of plasma detection technology as a means for increasing sensitivity stability and the detectable concentration range. This has resulted in the barrier discharge ionisation detector (BID), a new detector capable of the high-sensitivity detection of both organic and inorganic compounds, while providing excellent durability.


“The Tracera is a ground breaking new system that combines this new type of detector, offering features not provided by conventional detectors, with the Shimadzu GC-2010 Plus high-performance capillary gas chromatograph,” Said Masahito Ueda, General Manager of GC & TA Business Unit, Analytical & Measuring Instruments Division. “It is expected to improve the efficiency of high-sensitivity, trace-quantity analyses, and to reduce equipment and analysis costs.”


The built-in barrier discharge ionisation detector (BID) generates helium plasma. The extremely high photon energy of this plasma ionises the sample components, enabling high-sensitivity detection. This system achieves at least 100 times the sensitivity of a conventional TCD, and at least twice the sensitivity of FID, enabling the detection of all types of trace components at the 0.1 ppm level.


The new BID helium plasma has an extremely high energy. It can detect all organic and inorganic compounds, with the exception of He and Ne, with no difference in sensitivity. It improves analysis sensitivity even with aldehydes, alcohols, and halides, for which sensitivity decreases with FID. A single Tracera system can perform analyses that conventionally required complicated systems equipped with multiple detectors and units. Examples include the analysis of hydrogen and organic compounds such as formic acid, generated as part of the reaction process during artificial photosynthesis, and the analysis of low concentration hydrocarbons and permanent gases generated in lithium ion rechargeable batteries.


Specialists in Titration & Electrochemistry Technology


Aquamax KF Coulometric Karl Fischer titrator for low level water content determination down to 1ppm.Volumetric Karl Fischer titrator for measuring water contents in the milligram through to high percentage ranges.


Titra-Max Total Acid Number, Total Base Number and Mercaptan Sulphur determinations all on one easy to use system. Micro TAN titrator specifically designed for Total Acid Number determinations of transformer insulating oils.


E-Chem


The E500 series of high precision benchtop pH and conductivity meters.


Worldwide distributor network – contact us for details


G.R. Scientific Ltd P.O. Box 242, Ampthill, Bedfordshire, MK45 5AQ,


Tel. +44 1525 404747 • Fax. +44 1525 404848 Email info@grscientific.com • Web www.grscientific.com


Reader Reply Card No 81


With the new BID, the plasma is generated inside a quartz tube, so it makes no contact with the discharge electrode used for plasma generation. As a result, the detector electrode is not degraded, achieving long-term analytical stability.


Reader Reply Card No 80


Intelligent Sample Preparation System Maximising Safety and Minimising Use of Hazardous Materials in the Analytical Lab


The use of aggressive and dangerous acids is a common and potentially hazardous activity in almost all analytical laboratories and therefore the need to have sufficient health, safety and environmental precautions in place are essential. Lab Automation and Robotic sample handling can offer a perfect solution here.


Nucomat (Belgium) is proud to present the ‘HOTCELL Compact’; an embedded robotic sample preparation system into a completely closed fume extraction cabinet (necessary to minimise the amount of contact between dangerous materials and laboratory personnel).


With 25 years of experience in system integration, and strong roots in the nuclear sector, the functionality of this system offers a lot of benefits on very demanding working environments. Every sample is identified and monitored by the event driven ROBIN software. By a menu-driven interface, you can select and predefine all parameters for the sample preparation; sample identification and weighing, acid dispensing with 4 different acids, hotplate leaching and digestion, final dilution, make to volume, etc…


To ensure the precision and traceability, gravimetric control can be adapted in every preparation step. Analysers, spectrometers and/or electrodes can be integrated into the system, and will also be supervised by the ROBIN software as a real time task organiser (SCADA). The air/fume extraction will be monitored by laminar air flow sensors, and the acid container refills are controlled also. Any leakage or breakdown in the sequence will be announced by ROBIN, and the platform goes into a safety mode.


Reader Reply Card No 82


Reliable Sample Preparation of Volatile Samples


radiello™ SO2 /NO2


radiello is the ideal passive air sampling device for low levels of Hydrogen Sulfide (H2


/HF, and other compounds in petrochemical


environments. Experience radiello’s fast sampling rates, low detection limits and high capacity.


Where Other Devices Fail S), Aldehydes, BTEX/VOCs,


Succeeds


Exeter Analytical Inc. (UK) has developed a reliable sample preparation technique that enables accurate determination of the percentage Carbon (C), Hydrogen (H) and Nitrogen (N) in difficult to analyse volatile samples. The same sample preparation technique has been found to also generate excellent results from air sensitive and hygroscopic samples.


Knowledge of the CHN content of volatile petroleum products and lubricants can be useful in determining their performance characteristics. However, the CHN microanalysis of such volatile samples, especially those with high hydrogen content, requires careful sample handling, wide detector linearity and easy sample residue removal.


©2013 Sigma-Aldrich Co. LLC. All rights reserved. SIGMA-ALDRICH and SUPELCO are trademarks of Sigma-Aldrich Co. LLC, registered in the US and other countries. Solutions within is a trademark of Sigma-Aldrich Co. LLC. Radiello is a trademark of Fondazione Salvatore Maugeri IRCCS. Supelco brand products are sold through Sigma-Aldrich, Inc.


To order a starter kit, visit sigma-aldrich.com/radiello


11782


The sample preparation technique, described in technical report 233, involves hermetically sealing samples into heavy walled tin capsules under an inert atmosphere inside a glove box. The tin capsule is cold welded shut using an Exeter Analytical capsule sealer. This careful sample preparation technique together with controlled introduction of the sealed capsules into an Exeter Analytical Model 440 CHN analyser is demonstrated to eliminate the problems associated with analysing air sensitive, hygroscopic and volatile samples.


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APRIL / MAY 2013 • WWW.PETRO-ONLINE.COM


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