Programmed-temperature vaporization

Programmed-temperature vaporizers are flexible sample-introduction devices offering a variety of modes of operation such as spHt/sphtless, cool-sample introduction, and solvent elimination. Usually the sample is introduced onto a cool injection port liner so that no sample discrimination occurs as in hot injections. After injection, the temperature is increased to vaporize the sample. 

Together with the techniques described above, other techniques using hot injectors for the transfer of large-volumes in capillary gas chromatography have been developed. Transfer of large-volume solvents in a programmed temperature vaporizing... 

R J. Senorans, M. Heiraiz and J. Tabera, On-line reversed-phase liquid cliromatography using a programmed temperature vaporizer as interface , 7. High Resolut. Chromatogr. 18 433-437(1995). 

A programmed-temperature vaporizer (PTV) has also been used as an interface for introducing the LC fraction to the GC unit (84,96) and to desorb the analytes retained in the SPE sorbent contained in the PTV liner. Water samples can then be injected directly in to the PTV injector. 

Another interface for RPLC-GC is the programmed-temperature-vaporization (PTV) system, an interesting application of which is the determination of phthalates... 

Numerous types of GC injectors have been manufactured over the past four decades. The most commonly used injection techniques have been reviewed and described by Grob, who correctly states that analysts must fully understand the techniques before they can make the most appropriate choice for their particular application(s). For most GC capillary column applications, the split/splitless, programmed-temperature vaporization (PTV) and on-column injectors remain the most popular. However, over the last few years, technology has progressed rapidly to provide injectors that allow more of the sample extract on to the GC column without overloading it. 

If simple sample pretreatment procedures are insufficient to simplify the complex matrix often observed in process mixtures, multidimensional chromatography may be required. Manual fraction collection from one separation mode and re-injection into a second mode are impractical, so automatic collection and reinjection techniques are preferred. For example, a programmed temperature vaporizer has been used to transfer fractions of sterols such as cholesterol and stigmasterol from a reversed phase HPLC system to a gas chromatographic system.11 Interfacing gel permeation HPLC and supercritical fluid chromatography is useful for nonvolatile or thermally unstable analytes and was demonstrated to be extremely useful for separation of compounds such as pentaerythritol tetrastearate and a C36 hydrocarbon standard.12... 

Programmed temperature vaporization (PVT), gas chromatography, 4 612-613 6 421-422, 423 Programmer consoles, 20 669 Programming, of shape-memory polymer, 22 355-356... 

Programmed temperature vaporization (PTV) Most versatile inlet Allows large volume injection Little-no sample degradation Effective trace (to sub-ppb) analysis Expensive Requires optimization of many parameters Not well-known... 

For capillary GC, the split/splitless inlet is by far the most common and provides an excellent injection device for most routine applications. For specialized applications, there are several additional inlets available. These include programmed temperature vaporization (PTV) cool on-column and, for packed columns, direct injection. PTV is essentially a split/splitless inlet that has low thermal mass and a heater allowing rapid heating and cooling. Cool injection, which can be performed in both split and splitless mode with the PTV inlet, reduces the possibility of sample degradation in the inlet. Capabilities of the commonly available inlets are summarized in Table 14.3. 

Gas chromatograph systems are composed of an inlet, carrier gas, a column within an oven, and a detector (O Figure 1-1). The inlet should assure that a representative sample reproducibly, and frequently automatically, reaches the column. This chapter will cover injection techniques appropriate for capillary columns. These include direct, split/splitless, programmed temperature vaporization, and cool on-column injection (Dybowski and Kaiser, 2002). 

Introduction of the sample into a cool inlet characterizes programmed temperature vaporization. A temperature program is then utilized to vaporize the sample and introduce it into the column (Dybowski and Kaiser, 2002). 

Modern GC instruments represent high resolution systems that are fully automated from sample injection to final data reduction. Utilization of new injection devices has provided the means to enhance the performance level significantly. Studies have shown, for example, that injection of the tranquilizer propio-nylpromazine and its sulfoxide into a hot injection port gave much poorer results than on-column injection at low temperature (44). In the latter case, however, nonvolatile sample components could enter the column. This disadvantage of classic sample injection can be eliminated through use of a programmed temperature vaporization (PTV) injector. 

A programmed temperature-vaporization (PTV) injector (with a sorbent-packed liner) was used to preconcentrate and inject the sample. Thermal desorption was performed and the analytes were passed to a primary column (16 m X 0.32 mm i.d., film thickness 5 p.m, 100% methyl polysiloxane) and separated according to analyte vapour pressure. Selected heart-cuts were transferred to a second column (15 m X 0.53 mm i.d., Al203/Na2S04 layer, open tubular column with 10 (im stationary phase) where final separation was performed according to chemical functionality. 

Flores, G., M. Herraiz, G.P. Blanch, and M.L.R. del Castillo. 2007. Polydimethylsiloxane as a packing material in a programmed temperature vaporizer to introduce large-volume samples in capillary gas chromatography. J. Chromatogr. Sci. 45 33-37. 

Figure 4.13. Schematic diagrams of large-volume injection systems. Top on-column configuration with solvent vapor exit. (Drawing courtesy of Agilent Technologies.) Bottom programmed temperature vaporization configuration. (Drawing courtesy of ATAS, International.)...

Poy, F., Visani, S., and Tenosi, F. (1981). Automatic injection in high-resolution gas chromatography A programmed temperature vaporizer as a general purpose injection system. J. Chromatogr. 217, 81-90. 

PTV PU PVA PVAC PVAL PVC PVDC PVDF PVE PVF PXRD py Py PY Py-GC-MS pyr pyrr pz programmed-temperature vaporizer polyurethane poly (vinyl alcohol) poly(vinyl acetate) poly (vinyl alcohol) poly (vinyl chloride) poly(vinylidene dichloride) poly(vinylidene difluoride) poly (vinyl ether) poly(vinyl fluoride) powder X-ray diffraction pyridine (ligand) pyridine pyramidal (coordination compounds) pyrolysis-gas chromatography-mass spectrometry pyrazine (ligand) pyrrolidine (ligand) pyrazole (ligand)... 

Teske et al. [99] evaluated a programmed-temperature vaporizing injection for GC-MS determination of different drugs, among them cocaine, in biological fluids (blood, saliva, etc.). This method reduced the sample consumption (50p,L) and possessed good sensitivity. 

An interesting new development in injector design is the PTV (Programmed Temperature Vaporizer) [15, 16] which allows for solvent backflush in the injector. With this system, the sample can be injected at low temperature onto an adsori>ing cartridge and the non-adsorbed sample components are backflushed from the injector to vent. The temperature is then raised, vaporization of the analytes occurs and injection into the analytical column is performed. 

When the extracted analytes are to be retained directly on the chromatographic column or at the retention interface, their insertion can be accomplished in various ways, namely (a) by injection into the column, whether directly (SFC, GC) or with the aid of a cooling system (GC, HPLC) (b) by split-splitless injection (SFC, GC) (c) by using a programmed temperature vaporizer (GC) or (d) by injection into a cold trap and subsequent thermal desorption (GC) or elution (HPLC). 

An alternative for achieving a lower column load and enough analyte in the detector is to perform an additional separation before the analytes reach the analytical column. In this separation, part of the sample that is not of interest can be eliminated, and at the same time the important analytes can be kept. This preliminary separation can be done using bidimensional chromatography (see further), but simpler techniques are also reported, such as programmed temperature vaporization (PTV) injection, etc. 

---