Technical Help Desk

Technical Tip

GC Liner Labyrinth - How to choose the right Injector insert

J. Kuipers, N. Reuter*, E. de Witte, Technical Helpdesk Europe, Middelburg, The Netherlands

Injections and vaporization in gas chromatography are influenced by a number of variables. The liner always
plays a significant role. The most important ones are liner design and volume, sample composition, injector
heat capacity, heat transfer and adsorption effects. These factors together with the type of injection deter-
mine for a large extent the choice of liner.

Liner Types
Three major types of injection based on flash vaporization of the sample can be distinguished:

1. Direct injection
After flash vaporization the entire sample is transferred to the column. The sample transfer speed in
the injector is determined by column flow and volume of the injector liner. This injection type is most
commonly applied for 0.53 mm ID columns or packed columns. Injection volumes usually do not ex-
ceed 1 µl. This maximum in injection volume is related to the internal volume of the liner.

2. Split injection
After flash vaporization the sample is divided into two streams. One directed towards the column, the
other to the split vent. Here, the sample transfer speed in the injector is mainly determined by the flow
of the split vent and the liner volume. The column flow plays an insignificant role. A high transfer speed
of the sample is critical for the quick introduction of the compounds into the capillary column maintain-
ing the columns separation efficiency Split injections are used for all capillary columns with ID‘s rang-
ing from 100 µm to 530 µm. The maximum injection volume for split injections is about 1 µl.

3. Split/Splitless
During the initial splitless period the vaporized sample is transferred to the column. The capillary col-
umn flow and the liner volume determine the speed and efficiency of this process. Larger injection vol-
umes are possible for splitless type injections; volumes up to 5 µl are not uncommon. These large in-
jection volumes can never be injected at once because of possible liner overload but must be careful
introduced at a rate of about 1 µl/sec.

Liner volume
The sample gas volume, which at one time resides in the injector, should in all cases be smaller than the
internal volume of the liner. If not, the liner is overloaded and back flash of the sample into various (metal)
parts of the injector may occur. This phenomenon will cause poor injection profiles, bad peak shapes, ad-
sorption and possible sample carry over. Many liners used for direct and split injection have dimensions of
about 80 mm x 4 mm resulting in an internal volume of ca. 1ml. The effective volume available for the sample

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is however significantly lower as part of the liner volume will always be filled with carrier gas. The list below
indicates the solvent expansion volume per µl at 250 °C and 50 kPa

Methanol 0.65 ml
n-hexane 0.2 ml
Isopropanol 0.34 ml
Water 1.46 ml
Dichloromethane 0.41 ml

It is clear from the above that water and methanol in particular quickly can cause liner overload and some
care must taken if these solvents are used. For these solvents smaller injection volumes than 1 µl are to be
recommended.

Injector heat capacity

The efficient and quick evaporation of the sample is influenced by the following factors:

• sample volume
• type of solvent and sample components
• injector temperature
• injector and liner geometry and design
• presence of quartz wool or other liner fillings

The last three determine the heat capacity of the injector and its ability for heat transfer to the sample. The
below list compares the amount of energy needed for evaporation of methanol and water relative to cyclo-
hexane.

Water 5.22
Methanol 3.29
Cyclohexane 1.00

Solvents like methanol and water require much more energy than other common solvents for their evapora-
tion therefore they need a larger heat capacity and better heat transfer system for a quick evaporation.

This can be accomplished by using higher injector temperatures (>275 °C) and larger liner surface areas.
Glass or quartz wool is often used to increase the injectors heat transfer capacity. The evaporation of higher
boiling compounds also requires more energy and also in those cases quartz wool is often used. Besides
benefits glass or quartz wool also has a few disadvantages. The wool can become adsorptive especially if
some fibers are broken or when it has become dirty. It should be exchanged at a regular basis to prevent
chromatographic problems

Discrimination effects
The main aim and challenge of injections is to maintain sample integrity and sample composition during its
transition from the liquid to the gaseous state and also during the sample transfer from injector to the column.
The evaporation process of low boiling compounds is always quicker than that of high molecular weight
ones. This difference accounts for the often-mentioned discrimination effects caused by injections. In gen-
eral, the quicker and more complete the evaporation of the sample, the less discrimination effects will be ob-
served. Higher injector temperatures, special liner design and quartz wool will help to minimize these effects.
Inconsistent discrimination profiles will result in poorer repeatability.

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Liners for splitless injections
Straight liner

These are low cost liners for samples with a narrow boiling point range and little risk of ther-
mal decomposition. Can be packed with quartz wool to aid evaporation, limit discrimination
and trap non-volatile materials. Do not use for high boiling samples. Comes usually in 2 or 4
mm ID. Use the 4 mm version for sample volumes > 2 µl to prevent liner overload.

Gooseneck

Minimizes breakdown of active compounds and improves the splitless efficiency. The
gooseneck prevents the sample from reaching metal injector parts, which could cause de-
composition of sensitive compounds. The gooseneck is positioned at the top of the injector.
It is generally regarded as the best splitless liner.

Gooseneck with wool

The single gooseneck can be easily packed with quartz or glass wool to minimize
discrimination. Wool is also a risk as it can become active and adsorptive due to the trapping
of non-volatile residues. Replace it at regular intervals.

Double Gooseneck

The two goosenecks isolate the sample vaporization cloud from any metal injector parts.
The risk of catalytic breakdown is reduced. This type of liner can not packed with glass wool.

Recessed Gooseneck

This model has the same advantages as the other goosenecks but in addition it can be
packed with glass wool at the top. It can also be used for dual column analysis

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Liners for split injections
Frit Splitter

The ceramic frit will prevent dirt and non-volatiles from reaching the column. The frit can be-
come active. The gooseneck prevents back flash.

Inverted -or Laminar Cup Splitter

The cup will promote evaporation and mixing of the sample with the carrier gas. It is the best
splitter for higher molecular weight compounds. Slightly larger injection volumes are possible
because the cup will hold the sample liquid until it vaporizes. It is difficult to clean and is rela-
tively expensive.

Baffle Splitter

The baffle creates a turbulent flow, which results in more reproducible injections. Not well
suited for higher boiling compounds because of incomplete vaporization and thus subject to
discrimination.

Liners for direct injections

Straight tube

This type of liner is more suited for packed columns than it is for 0.53 mm ID columns. The
wide-bore column should be positioned at the bottom of the liner just piercing through the
ferrule. This will minimize the effects of possible dead volume during injections although in-
jector parts, which are swept poorly with carrier gas will result in poor injection profiles.

Gooseneck

This is a different type of gooseneck liner where the gooseneck holds the wide-bore column
in position. This design effectively eliminates any dead volume in the injector and provides
the best possible injection profile for wide-bore columns. In reversed position it can also be
used for on-column injections on 0.53 mm columns.

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