Inlets

In This Section, You Will Learn:

Identifying the Types of Inlets Identifying the Components in the Packed and Split Inlets Understanding the Flow Dynamics of the Split Inlet Calculating Split Ratio Identifying preventative Maintenance and Troubleshooting

Inlet Systems

Purpose: To allow the insertion of a sample into the gas chromatograph in a repeatable, reproducible manner. The sample should be representative of the bulk, and unless specifically desired should be inserted without chemical change.
Inlet Type Split/Splitless Purged Pack Cool on-column Volatiles Interface Gas Control EPC and non-EPC EPC and non-EPC EPC only EPC only
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Programmed Temperature Vaporization EPC only

Flow System: Purged Packed Inlet

Flow controlled mode (recommended for packed columns)

Pressure controlled mode (recommended for capillary columns)

Exploded View of Purged Packed Inlet

Insulation Septum nut Septum O-ring Knurled nut Heater/sensor assembly

Purged Packed Inlet body Insulation Insulation Insulation cup Ferrule Column nut
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Liners/Adapters
1/4-Inch Metal Column, Packed Inlet 1/8-Inch Metal Column,

Packed Inlet
Inlet Fitting

Inlet Fitting 1/4-Inch Ferrule 1/4-Inch Metal Ferrule 1/4-Inch Nut

There are a variety of liners and adapters for different columns, inlets and detectors.

Back Ferrule

1/4-Inch Nut 1/8-Inch Liner

1/4-Inch Column

Front Ferrule Back Ferrule 1/8-Inch Nut 1/8-Inch Column

Using Two Wrenches in Opposition to Tighten Column Fittings

Split/Splitless Inlet

Split Mode for

Pulsed Split

Major Component Analyses

Allows for larger injection volume.

Splitless Mode for

Pulsed Splitless

Trace Component Analyses

Allows for larger injection volume

Split/Splitless Flow System

Split Flow Diagram: Pre-Injection

SEPTUM 2 mL/min TOTAL FLOW (SEPTUM) PURGE VENT

50 mL/min SPLIT VENT

48 mL/min 47.4 mL/min

(INLET) PURGE VALVE

CARRIER GAS LINER

0.6 mL/min
COLUMN

SEAL

Split Flow Diagram: Sample Injection

(SEPTUM) PURGE VENT TOTAL FLOW

SPLIT VENT

(INLET) PURGE VALVE

= CARRIER GAS = LIQUID SAMPLE MOLECULES

SPLIT RATIO = COLUMN + SPLIT VENT FLOW COLUMN FLOW COLUMN

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Split Flow Diagram: Sample Vaporization

(SEPTUM) PURGE VENT TOTAL FLOW

SPLIT VENT = CARRIER GAS = SAMPLE MOLECULES = SOLVENT MOLECULES (INLET) PURGE VALVE

Vaporization takes place when sufficient thermal energy is transferred to the sample. This can occur in the carrier gas, but is more likely upon contact with a solid surface, such as the liner or mixing medium.

COLUMN

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Split Flow Diagram: Sample/Carrier Mixing

(SEPTUM) PURGE VENT TOTAL FLOW

= CARRIER GAS = SAMPLE MOLECULES = SOLVENT MOLECULES

SPLIT VENT

(INLET) PURGE VALVE

For the concept of SPLIT RATIO to be valid, the sample (solvent + analyte) must be mixed with the carrier gas to give a homogeneous mixture. At the bottom of the injection port a small part of this mixture will transfer to the column, while the bulk of the mixture will leave the chromatograph via the SPLIT VENT.
COLUMN

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Split Flow Diagram: Liner Overload

(SEPTUM) PURGE VENT TOTAL FLOW

= CARRIER GAS = SAMPLE MOLECULES = SOLVENT MOLECULES

SPLIT VENT

(INLET) PURGE VALVE

A large injection of a solvent with a large expansion volume can cause an overload of the injection port liner. This can result in loss of sample out the PURGE VENT as well as contamination of the in-coming carrier gas line.

COLUMN

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Split Ratio Calculations

Split Ratio = Split Vent Flow + Column Flow Column Flow

A Column I.D. (m) Total Flow 200 320 530 100 100 100

B Column Flow 0.5 1.0 3.0

C Septum Purge 2.0 2.0 2.0

D Split Flow SplitRatio 97.5 97 95 196:1 98:1 33:1

Split Vent Flow = (Split Ratio)(Column Flow) - Column Flow

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Gas Saver
Gas Saver reduces the carrier gas flow from the split vent after the sample is on the column. Column head pressure and the column flow rate are maintained, while the purge/split vent flows decreases. Can be used in split and splitless modes. Gas Saver time is set to activate during the run after the sample is on the column.
Start Gas saver time set to 2.5 min. Run ends

200 175 Split vent 150 100 flow (mL/min) 75 50 25

Gas Saver Flow

-2 -1 0

Regular Flow

Gas saver flow

9 10

Prep Run

Time
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Splitless Flow Diagram

Purge valve closed during injection (no split vent flow). At a specified time after injection, the purge valve opens to sweep remaining vapors out of inlet.

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Split/Splitless Capillary Inlet Exploded View

Septum retainer nut Septum O-ring Split vent line Insulation Split/splitless inlet body Retaining nut Inlet base seal Washer Reducing Nut

Insert Assembly Liner

Insulation

Insulation cup Ferrule Column Nut

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Capillary Injection Port Consumables

Septum: 5182 - 0739 High-temperature 11 mm DIAMETER Liner Seal: Viton: 5180 - 4182 Graphite: 5180 - 4168 5180 - 4173 CHANGE WITH LINER

BELOW 300 C SPLIT LINER ABOVE 300 C SPLITLESS LINER ABOVE 300 C

Seal: 18740 - 20885, new with 2 slits 5182-9652 GOLD PLATED, STAINLESS STEEL MUST BE KEPT CLEAN CAN BE DEACTIVATED Washer obsolete

Ferrule: GRAPHITE: Good seal easily VESPEL: Excellent seal - hard GRAPHITE/VESPEL: Very good seal with some difficulty Column Nut: 5181 - 8830 5020 - 8292 Finger-tight 5020 - 8293 530 um Finger-tight 19258-20920 spring loaded -Vespel

3 - 6 mm APPLICATION DEPENDENT

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Most Commonly Used Liners

Liners: Deactivated
Type
Packed, tapered

Configuration

Recommended Use

Part No.
5062-3587

4-mm id, nominal volume Split and splitless 900 ul, boroscilicate modes. glass (deactivated), Can be self-packed. silanized glass wool plug (deactivated) 4-mm id, nominal volume 900 ul, boroscilicate glass (deactivated) Split and splitless modes. Can be self-packed.

Unpacked, tapered

5181-3316

Liners: Untreated
Split/Splitless 4-mm id 1000-ul nominal volume, borosilicate glass (untreated) silanized glass wool plug 19251-60540 Split and splitless modes, especially recommended for rapid injections with the 7673 Automatic Sampler 5183-4647

!!New Deactivated Split Liner!!

See the HP Analytical Columns and Supplies Catalog for the complete list of liners.

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Capillary Liner Maintenance

General Purpose, Non-Deactivated Liners

CLEANING PROCEDURE: 1. Remove glass wool 2. Sonicate in solvent or acid bath 3. Rinse & dry 4. Replace deactivated glass wool 5. Deactivate Silylate* 6. Dry *Silanizing agents available from column suppliers.

Factory Deactivated (Pesticide Liners)

CLEANING PROCEDURE: 1. Remove glass wool 2. Sonicate in solvent(s) 3. Dry 4. Care should be taken to avoid scratching the inner surface of the liner.
TREAT AS ULTRA CLEAN PART
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Injection Port Seal: Maintenance

Sonicate in Solvent Deactivate with Non-Chlorinated Reagent

HMDS BSTFA BSA TSIM Bake Dry

Wash with Solvents Bake Dry

Inert First Wash - Toluene Alcohol Second Wash - Methanol

TREAT AS ULTRA CLEAN PART

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Injection Port Problems

Non-Representative sample Incorrect Temperature Blockage Contamination Leaks

Detecting Leaks Snoop Electronic Leak Detector Pressure test Chromatographic Changes (compare shifts in retention time and area counts)

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Injection Port Maintenance

Change the septum regularly. Use the lowest practical temperature. Purge with flow. Use clean liners. Solvent clean the seal. Use clean syringes.

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Other Inlets

Programmed Temperature Vaporization Inlet: Large Volume Injection (LVI) with PTV for trace analysis of later eluting solutes and dirty samples. Multiple injections are made in a cool inlet and then the temperature is ramped. Inlet uses Septum-less head. Volatiles Interface: Introduce a gas sample from an external device such as the headspace, purge and trap, or air toxics samplers.

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