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10

By Scott Grossman

• For some manufacturers, only a portion of the GC inlet is actually at the temperature setpoint;

a significant thermal gradient exists both above and below this zone.

• The thermal profile of one GC inlet can vary from other similar inlets—and vary dramatically

between different styles.

• Removal or damage to GC insulation can have a large effect on the inlet’s thermal profile.

Injecting a liquid sample into a hot GC inlet is a dynamic and com-

plex event. Of the many parameters that affect the success of an

injection, inlet temperature is one of the most significant. Raising or

lowering the inlet temperature setpoint can have a profound effect

on how much sample is transferred onto the column depending on

sample volatility and thermal sensitivity. But, once the inlet tempera-

ture is set, how much of the inlet is actually kept at that setpoint?

Moreover, how might thermal profiles change between inlets?

Temperature Varies Within and Between Similar Inlets

The motivation for this work came from a question about the actual

temperature of an O-ring installed in an Agilent split/splitless inlet at a

given inlet temperature setpoint. (See Figure 1 to identify the compo-

nents of a GC inlet.) Instead of just measuring the temperature inside

a liner near the O-ring’s location, we used a thermocouple to measure

temperature along the entire length of the liner at a constant inlet tem-

perature setpoint of 250 °C. The resulting thermal profile confirmed that

a temperature gradient exists within the inlet.*

In previous work

(www.restek.com/hotseptum)

, we also discussed this

gradient within GC inlets and noted that inlet thermal profiles can vary

greatly between manufacturers, but would they vary between similar

inlets from the same manufacturer?We checked another similar inlet to

compare the thermal profiles and found that the second inlet exhibited

a different thermal profile from the first. After measuring several more

Agilent GC inlet temperature profiles, we found inlet-to-inlet variation in

all cases, even in ostensibly identical inlets (Figure 2).

Insulation is Crucial to Minimizing

Temperature Variation

We did observe one split/splitless inlet with significantly lower tempera-

tures at the top and bottom. After investigating, we discovered that

the top ring of insulation, which sits just below the perforated disk of

the Agilent 6890 split/splitless inlet weldment, was missing. Some of

the insulation at the bottom of the inlet, along with the thermal nut,

was also not installed. Simply placing insulation in the top cavity and

installing the thermal nut caused the temperature of the inlet liner to

more closely match the other inlets (Figure 2). This test was a valuable

reminder of the need to carefully reconstruct the inlet whenever the

insulation is disturbed.

It’s AMatter of Degrees, but Do Degrees Really Matter?

An Observation of GC Inlet Temperature Profile and Inlet-to-Inlet Temperature Variability

Figure 1:

Considering how little of the GC inlet is actively heated

by the heating element, it’s no surprise a temperature gradient

exists—especially if insulation is missing from the top or bottom.

Oven

Wall

Open Air

Oven

Column

Reducing Nut

Nut Warmer Cup

Inlet Seal

Thermal Nut

Aluminum

Heater Block

Heating Element

Heater Sensor

Liner

Point of

Injection

O-Ring

Inlet Body

Perforated Disk

Insulation

1.2

cm

* For these experiments, we only measured the thermal profile of the

liner inside the inlet, not the entire inlet.