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Application News No. G292A Gas Chromatograph Analysis of Lower Aliphatic Aldehydes using Nexis GC-2030 LAAN-A-GC-E057A Lower aliphatic aldehydes are known to be associated with sick building syndrome. Thus various regulations require strict control of their concentrations. A common method of analyzing lower aliphatic aldehydes is to utilize 2,4-dinitrophenylhydrazine (DNPH) derivatization. Trace level analysis of these compounds is then enabled by using a flame thermionic detector (FTD/NPD). In this applications news, methods for collecting aldehydes in atmospheric air, extraction and elution using commercially available cartridges and the analysis of lower aliphatic aldehydes using GC-2030 with FTD-2030 are described. K. Gregory, K. Kawamoto Fig. 1 Nexis GC-2030 Sample Collection Method In this set-up, two commercially available cartridges saturated with 2,4-dinitrohydrazine are connected in series. The pump flow rate is set to about 0.1 L / min, and air sample is collected for 24 hours continuously. The amount of air extraction can be measured by using an integrating flow meter. In order to prevent decomposition of aldehyde-DNPHs by atmospheric ozone, install an ozone scrubber cartridge in front of the collection cartridge (Fig. 2). Fig. 2 Schematic Diagram of Collection Method Cartridge Elution Method The aldehydes react in the cartridge to form aldehyde- DNPHs and is eluted with acetonitrile. During elution, unreacted DNPH which may interfere with the analysis may also be eluted. This can be remove by using a cation exchange resin. Since acetonitrile can also be detected by FTD, the eluate should further be extracted with ethyl acetate (Fig. 3). Fig. 3 Schematic Diagram of Elution Method Collection Method Note Trace amounts of aldehydes may also be present in containers, cartridges and in some reagents. Therefore, it is important to always analyze a blank before the actual sample. Depending on the cleanliness of the environment where extraction is performed, it is also possible that unwanted contaminants can make their way to the sample extract. Ozone scrubber Cartridges Pump Integrating flow meter Cartridge with collected Aldehydes Acetonitrile Cation exchange resin Eluate
Application News No. G292A www.shimadzu.com/an/ Shimadzu Corporation For Research Use Only. Not for use in diagnostic procedures. This publication may contain references to products that are not available in your country. Please contact us to check the availability of these products in your country. The content of this publication shall not be reproduced, altered or sold for any commercial purpose without the written approval of Shimadzu. See http://www.shimadzu.com/about/trademarks/index.html for details. Third party trademarks and trade names may be used in this publication to refer to either the entities or their products/services, whether or not they are used with trademark symbol “TM” or “”. Shimadzu disclaims any proprietary interest in trademarks and trade names other than its own. The information contained herein is provided to you "as is" without warranty of any kind including without limitation warranties as to its accuracy or completeness. Shimadzu does not assume any responsibility or liability for any damage, whether direct or indirect, relating to the use of this publication. This publication is based upon the information available to Shimadzu on or before the date of publication, and subject to change without notice. © Shimadzu Corporation, 2017 First Edition: Jun. 2017 Revision A: Mar. 2023 01-00000-EN Analysis Results Fig. 4 Chromatogram for DNPH-Derivatized Lower Aliphatic Aldehydes (1 μg/mL Ethyl Acetate Solution) * Stereoisomers exist for C2 and subsequent aldehydes-DNPH Instruments Used and Analytical Conditions Gas Chromatograph Nexis GC-2030 Flame Thermionic Detector FTD-2030 Autosampler AOC-20i Software LabSolutions LC/GC Injection Unit Temp. 200 °C Carrier Gas He (99.999 %) Carrier Gas Control Constant linear velocity (41.7 cm/sec, purge flowrate: 3 mL/min) Injection Mode Splitless (Sampling time: 1 min; then split (1:30)) Sample Injection Volume 1µL Column SH-5 (0.25 mm I.D. × 30 m, d.f. 0.25 µm) *1 Column Temp. 80 °C (1 min) - 20 °C/min - 200 °C (10 min) – 5 °C/min – 250 °C (0 min) Total 27 min Detector Temp. 280 °C Current 1.00 pA Detector Gas Flowrate H2: 1.5 mL/min, Air: 145 mL/min Makeup Gas Flowrate 27.5 mL/min (He) *1 P/N: 221-75701-30 1 : acetaldehyde-DNPH1 2 : acetaldehyde-DNPH2 3 : propionaldehyde-DNPH1 4 : i-butylaldehyde-DNPH1 5 : propionaldehyde-DNPH2 6 : i-butylaldehyde-DNPH2 7 : n-butylaldehyde-DNPH1 8 : n-butylaldehyde-DNPH2 9 : i-valeraldehyde-DNPH1 10 : i-valeraldehyde-DNPH2 11 : n-valeraldehyde-DNPH1 12 : n-valeraldehyde-DNPH2
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