Ingenious sample handling ITEX Dynamic Headspace Powerful Sample Enrichment for GC

ITEX (In-tube extraction) Dynamic Headspace Tool Purge & Trap (P&T) sensitivity without the pitfalls of P&T Systems – Rapid and efficient enrichment of volatile and semi-volatile compounds from solid, liquid and gaseous samples – In-tube extraction and thermal desorption using industry standard adsorbents – Syringe-only concept: no sample loops, transfer lines, or switching valves that could be contaminated – Active cooling allows for rapid sample preparation and short cycle times – No modifications of the GC injector needed – PAL Robotic Tool Change enables head space, SPME and ITEX-sampling...

ITEX Dynamic Headspace Extraction Procedure The sample is heated and / or agitated in a sealed vial. Sample conditioning The ITEX needle pierces the sealed vial and the heated syringe pumps the the headspace gas through the cold trap. An additional step to remove water from the trap can be added. The loaded ITEX trap is flash heated up to 350°C and analytes are desorbed into the hot GC injector. After thermal desorption the hot ITEX trap is cleaned with inert flush gas. Active cooling allows for short cycle times. Trap cleaning Active cooling

Powerful options for ITEX Dynamic Headspace The PAL RTC (Robotic Tool Change) takes productivity to new levels

Robotic Tool Change and ITEX Dynamic Headspace, ingeniously productive. – Headspace, SPME and ITEX sampling within the same sequence – Automatic selection of the syringe with optimal accuracy, e.g. for adding standards or preparing serial dilutions – Automated optimization of methods e.g. by selecting the most suitable ITEX trap and conditions – Derivatization reactions performed without manual intervention for productivity, process safety and protection against hazardous chemicals – Possibility to permanently configure several workflows on one system for a walk-up prep station, e.g. Liquid/...

Environmental application VOCs, BTEX in water at ppt levels, EPA 502.2 VOCs, full scan mode, 2 µg/L Retention time Sample preparation: Chromatography (Shimadzu GC-2010 Plus): Full scan data: 2 µg/L MegaMix® Standard, 524.2 73 components), Restek PN 30601 Temperature program: Restek catalog # 23321.1, 3.5 mm Splitless Single Tpr Gsnk SIM scan data: 10 ng/L MegaMix® Standard, 502.2 (54 components), Restek PN 30432 10mL water + standard, filled into 20 mL headspace vial, + 3g NaCl ITEX Dynamic Headspace conditions Incubation temp. Incubation time Syringe temp. Extraction strokes Extraction speed...

Food application Comparison of flavors/softeners ITEX Dynamic Headspace vs. Poropak Filter 3 gr sample, 30 minutes equilibration time, 40°C 70 60 Porapak Filter Technique 5 gr sample, 20 hours equilibration time, 25°C Name Limonene Eucalyptol Methylhexylketone cis-3-Hexenylacetate Rose oxide Cyclal C Tetrahydrolinalool Tetrahydromyrcenol Linalool Verdox Vertenex Citronellylacetate Pelargol Undecavertol Gardenol Benzylacetate DMBC acetate Allylcyclohexylpropionate Phenylethylacetate alpha-Methylionone Verdylacetate n-Methyl-alpha-Ionone Verdylpropionate Diphenyloxide Lilial Iso E super alpha-Hexylcinnamic...

Environmental application Purgable organic compounds (VOCs) in water by GC/MS, Full Scan Chromatogram (m/z 49-180) at 1 \x%l I. Target compounds: 3) methyl tert-butyl ether, 4) ethyl tert-butyl ether, 7) tert-amyl methyl ether, ITEX ppt sensitivity for volatile or semi-volatile compounds Instrumentation Conditions GC Thermo Trace GC Ultra 40°C for 1 min., 4°C/ min. to 130°C, 10°C/ min. to 200°C for 10 min. MS Thermo DSQII El 70ev, Scan mode m/z 49-180 Injector AtasGL Optic 3 with cryfocusing unit 280°C Cryotrap - 165°C for 30 sec, 30°C/ sec. to 250°C GC Column Restek VMS 60 m x ,0.32 mm i.d.,...

Sensitivity comparison between ITEX Dynamic Headspace and Purge & Trap Sensitivity Comparison of ITEX with Purge & Trap ITEX Dynamic Headspace Purge & Trap MDL: Method detection limit Ref: Laaks J, Jochmann MA, Schilling B, Schmidt TC ; Anal. Chem. 2010, 82, 7641-7648 Further application examples Environmental In-Tube Extraction of Volatile Organic Compounds from Aqueous Samples: An Economical Alternative to Purge and Trap Enrichment Jens Laaks,† Maik A. Jochmann,*,† Beat Schilling, and Torsten C. Schmidt† Anal. Chem. 2010, 82, 7641–7648 Clinical Headspace In-Tube Extraction Gas Chromatography–Mass...

PAL System Tools and Modules complementing ITEX Dynamic Headspace

ITEX Dynamic Headspace Specifications Trap temperature range Syringe temperature range Extraction flow rates Extraction stroke cycles (strokes/sample) Extraction volume Incubation time Standard adsorption material Tenax TA 80/100 mesh, other materials upon request Water removal step with adjustable trap temperatures Ventilated trap for quick sample processing Fast cooling of trap < 2 minutes PAL System Modules and Tools Agitator Module – – – – Incubation and agitation of 6 samples Incubation temperatures 40-200°C Agitation speed 250-750 rpm For 2 mL, 10 mL, 20 mL vials Vortex Mixer Module – Efficient...

PAL is a registered trademark of CTC Analytics AG, Switzerland Part No. PAL Broch-ITEX - 2015 | Rev 1– February 2015 For more information on the new generation PAL Systems visit: