6850/6890 GC Column Installation and Instrument Setup Guide - PPIP/TCDJuly 14, 2004

GC Setup and Capillary Column PreparationInlets:

Split/Splitless Capillary Inlet

PPIP - Purged - Packed Injection Port

PCOC - Programmable Cool on Column

PTV - Programmable Temperature Vaporization Inlet LVI - Large Volume Injection VI - Volatiles Interface

GSV - Gas Sampling Valve

GC Capillary Column PreparationCreated 5//02Ceramic Column CutterRough EdgeNew Column FerruleColumn NutSeptum to mark Column Position1) Slide a used Septum over the column as a marker 2) Slide a Column Nut onto the column 3) Slide a new Column Ferrule onto the column4) Score the column and snap off the end5) Inspect the column for a clean cut.

GC Inlet Systems - Purged Packed Injection PortMaintenance PartsSeptum Purge WeldmentO RingGlass Liner SleeveSeptum1/4 Vespel SealHeater/Sensor AssemblyColumn Nut/FerruleColumn AdapterSeptum Purge Weldment

GC Inlet Systems - Purged Packed Injection PortColumn Adapters/liners - Capillary Column InstallationCapillaryPackedGlass InsertColumn Adapters/linersCapillary Column Installation

6890 GC Inlets - Purged Packed Injection PortMaintenance: Replace Septum Replace Glass Liner Replace Septum Purge Weldment O-Ring Perform Inlet Leak Test Run Customer Sample or Agilent Checkout Replace 1/4 Vespel Ferrule

Electronic Pneumatic Control.PPIPPacked Column/Flow Control Mode - Flow can be set, Pressure readout only No Column assigned to inletCapillary/Pressure Control Mode - Pressure can be set, Flow readout only Selected by assigning a capillary column to the inlet (Config Column 1 or 2)

GC Setup and Capillary Column InstallationDetectors:

FID - Flame Ionization Detector

TCD - Thermal Conductivity Detector

NPD - Nitrogen Phosphorous Detector

ECD/uECD - (micro) Electron Capture Detector FPD - Flame Photometric Detector

6850/90 THERMAL CONDUCTIVITY DETECTORGas ConnectionsNote: The Reference/Makeup Gas must be the same as the Carrier

6890 TCD Setup - Detector Column AdaptersNew Ferrule Design-6850/90Original 6890 Design Capillary AdapterOld StyleNew StyleG1532-805400100-13325182-9677- .20/.250 5182-9676- .320 5182-9673- .5305182-3477Description Column ID mm Single part# 10 Pack#Back Ferrule for 1/8" inlet G1530-80400 5182-3477Frnt Ferr for 0.8mm OD Col 0.53 G1530-80410 5182-9673 Frnt Ferr for 0.53mm OD Col 0.32 G1530-80420 5182-9676Frnt Ferr for 0.43mm+OD Col 0.25/0.20/0.1 G1530-80430 5182-9677Front Ferrule, no hole G1530-80440 5182-9679

6850/90 Setup - TCD Column Installation - Original Capillary Adapter 6890 Operating Manual - Volume 1 Chapter 5, Part11.2.3.4.

6850/90 Setup - TCD Column Installation - New Capillary AdapterColumn Installation - from 6890N User Information1- Slide the 1/8 swagelok Column Nut, Back Ferrule and Front Ferrule onto the column. 2- Trim the end of the column 3- Insert the column into the TCD and thread the nut onto the fitting 4- Push the column all the way into the Detector and withdraw 1-2 mm. 5- Tighten the column nut 1/8 Swagelok

6850/90 TCD - Front Panel MenuTurns Filament On and OffOutput of Detector. 1 unit = 25uVTurns polarity between + and -6890 TCD OPERATION

6850/90 THERMAL CONDUCTIVITY DETECTOROptimizing Makeup and Reference Flows

6850/90 TCD - Optimizing Makeup and Reference FlowsSetting TCD Flows in Packed Mode

The Packed Mode describes using the TCD with column flow rates between 15 and 60 ml/min. The reference flow should be set to 1.5 times the combined flow rate of the column plus make-up gas. Make-up gas is recommended whenever a capillary column is used. This allows the column to be installed all the way into the detector and withdrawn one millimeter. If make-up is not used then the end of the column should be no more than three millimeters above the ferrule. Otherwise excessive tailing will occur. The minimum make-up flow is 1 ml/min.

.Example 1: 1/8 Stainless Steel Column If the column flow = 30 ml/min, then the reference flow should be set to (30ml/min) (1.5) = 45 ml/min. Therefore total detector flow is 30 + 45 = 75 ml/min.

.Example 2: 10 Meter X 530 uM column If the column flow = 15 ml/min and the make-up flow = 2 ml/min, then the reference flow should be set to (15 ml/min + 2 ml/min) (1.5) = 25.5 ml/min. Therefore the total detector flow is 17 + 25.5 = 42.5 ml/min.

6850/90 TCD - Optimizing Makeup and Reference FlowsSetting Flows in Capillary Mode

The Capillary Mode describes using the TCD with a combined column plus make-up flow of less than 15 ml/min. The combined column plus make-up flow must not be less than 5 ml/min. The reference flow rate should be set to optimize detector response. This will result in a reference flow of approximately two times the combined column plus make-up flow for a column plus make-up flow of 10-15 ml/min. For a column plus make-up flow of 5 - 10 ml/min, a multiplier of three is used. The detector output will be within 25% of the maximum response. The response can be further optimized by adjusting the reference flow. The make-up flow should not be less than 1 ml/min.

.Example 3: 2 Meter X 200 uM capillary column If the column flow rate = .75 ml/min, then the make-up flow must be at least 4.25 ml/min. Set the make-up flow to 5 ml/min. The optimum reference flow will be (5.75 ml/min) (3) = 17.25 ml/min. The total detector flow will be 5.75 + 17.25 = 22.5 ml/min.

.Example 4: 25 Meter X 320 uM capillary column if the column flow rate = 10 ml/min, then the make-up flow should be set low to minimize sample dilution. Set the make-up to 2 ml/min. The reference flow will = (12 ml/min) (2) = 24 ml/min. The total detector flow will be 12 + 24 = 36 ml/min.

6850/90 TCD Checkout Conditions

6850/90 TCD Checkout Chromatogram25 uV(Sampling Rate)010203040506070

Acronym list for GC inlet systems Parts for Maintenance and Repair The PPIP can accommodate 1/8 or 1/4 metal and 1/4 Glass packed columns. It is also compatible with 320 and 530 micron capillary columns. Acronym list for GC inlet systems