Agilent Technologies 6850 Series II Operation manual

6850 Series II GC User Information
Released: March 2004 6850 Series II GC User Information page 1 of 256
Contents
Important Information
Important safety warnings ............. 3
Safety and regulatory certifications 8
Safety symbols ............................... 10
Electromagnetic compatibility .... 11
Miscellaneous ................................. 12
Introduction
Display and keypad ....................... 13
Methods and memory ................... 14
Loading a method .......................... 15
Run control features ..................... 15
Gas connections ............................ 16
Electrical connections .................. 17
Data rates ........................................ 20
Keypad lockout .............................. 20
Columns and Traps
Opening the oven ........................... 21
Capillary column hanger ............... 22
Ferrules for capillary columns ..... 22
Ferrules for packed metal
columns ..................................... 23
Ferrules and O-rings for glass
packed columns ....................... 24
Conditioning capillary columns ... 25
Conditioning packed columns ..... 26
Conditioning chemical traps ........ 26
Installing capillary columns ......... 27
Installing packed metal columns . 43
Installing packed glass columns .. 49
Daily Operation
To start up the GC ......................... 51
To make a run ................................ 51
To shut down the GC .................... 53
Verifying Performance
Software required .......................... 54
TCD Checkout ................................ 54
FID checkout .................................. 61
µECD Checkout ............................. 67
FPD Checkout ................................ 74
Messages
Message types ................................ 81
Not Ready messages ..................... 83
Warning messages ......................... 84
Sequence warning messages ........ 86
Service warning messages ............ 88
Shutdown messages ...................... 89
Fault messages ............................... 92
Routine Maintenance:
General
General warnings ......................... 100
Maintenance schedule ................ 102
Swagelok connections ................ 103
Preparing to service the GC ....... 104

Contents
Released: March 2004 6850 Series II GC User Information page 2 of 256
Opening the oven ......................... 104
Removing the lid top cover ........ 105
Maintaining a sampling valve
(diaphragm type) ................... 106
Maintaining a sampling valve
(rotary type) ........................... 110
Maintaining the auxiliary EPC
module ................................... 116
Routine Maintenance:
Inlets
Maintaining a split/splitless inlet 120
Maintaining a purged packed
inlet .......................................... 134
Maintaining a PTV ....................... 150
Maintaining a cool on-column
inlet .......................................... 166
Routine Maintenance:
Detectors
Maintaining a thermal conductivity
detector (TCD) ....................... 184
Maintaining a flame ionization
detector (FID) ........................ 187
Maintaining a Microcell Electron
Capture Detector (µECD) ..... 200
Maintaining the flame photometric
detector (FPD) ....................... 208
Automatic Liquid Sampler
and Injector
Pre-run checklist .......................... 217
Running a sample ........................ 217
Preparing sample vials ................ 218
Preparing the solvent and waste
bottles ..................................... 220
Syringes ......................................... 221
Cool on-column injection ........... 228
The 6850 automatic liquid
sampler ................................... 229
The 6850 automatic injector ....... 236
Faults ............................................. 239
Installing a sampler or injector
on the 6850 GC ....................... 242
Installing the injector mounting
bracket and post .................... 243
Installation
Installation checklist ................... 244
Setting your IP address ............... 245
Safely route vent tubing .............. 247
Prepare the cryogenic oven
cooling system ....................... 247
Configuration ............................... 252
Site Prep Summary
Summary of GC benchtop and lab
requirements .......................... 254
Sampling Techniques
Handbook

Important Information
Important safety warnings
Released: March 2004 6850 Series II GC User Information page 3 of 256
Important Information
About your 6850 Gas Chromatograph
© Agilent Technologies, Inc. 1998, 1999, 2000, 2002, 2004
All Rights Reserved. Reproduction, adaptation, or translation without
permission is prohibited, except as allowed under the copyright laws.
Vespel® is a registered trademark of E.I. duPont de Nemours Co., Inc.
Swagelok® is a registered trademark of Swagelok Company.
Kalrez® is a registered trademark of DuPont Dow Elastomers.
Merlin Microseal™ is a trademark of Restek Corporation.
GRAPHPACK™ is a trademark of GERSTEL GmbH & Co.KG.
Part No. G2630-90329
First edition, March 2004
Replaces Part No. G2630-90327, G62630-90328
Printed in USA
Important safety warnings
There are several important safety notices that you should always keep in mind
when using the 6850 GC.
Many internal parts of the GC carry dangerous voltages
If the GC is connected to a power source, even if the power switch is off,
potentially dangerous voltages exist on:
• The wiring between the GC power cord and the AC power supply, the AC
power supply itself, and the wiring from the AC power supply to the power
switch.
With the power switch on, potentially dangerous voltages also exist on:
• All electronics boards in the instrument
• The internal wires and cables connected to these boards.
• The wires for any heater (oven, detector, inlet, or valve box)

Important Information
Important safety warnings
Released: March 2004 6850 Series II GC User Information page 4 of 256
Warning All these parts are shielded by covers. With the covers in place, it should be
difficult to accidentally make contact with dangerous voltages. Unless
specifically instructed to, never remove a cover unless the detector, inlet, or
oven are turned off, or the power cord is unplugged.
Warning If the power cord insulation is frayed or worn, the cord must be replaced.
Contact your Agilent service representative.
Electrostatic discharge is a threat to GC electronics
The printed circuit (PC) boards in the GC can be damaged by electrostatic
discharge. Do not touch any of the boards unless it is absolutely necessary. If
you must handle them, wear a grounded wrist strap and take other antistatic
precautions.
Many parts are dangerously hot
Many parts of the GC operate at temperatures high enough to cause serious
burns. These parts include but are not limited to:
• The inlet
• The oven and its contents
• The detector
• The column nuts attaching the column to an inlet or detector
• The valve box
You should always cool these areas of the GC to room temperature before
working on them. They will cool faster if you first set the temperature of the
heated zone to room temperature. Turn the zone off after it has reached the
setpoint. If you must perform maintenance on hot parts, use a wrench and
wear gloves. Whenever possible, cool the part of the instrument that you will
be maintaining before you begin working on it.
Warning Be careful when working behind the instrument. During cool-down cycles, the
GC emits hot exhaust which can cause burns.

Important Information
Important safety warnings
Released: March 2004 6850 Series II GC User Information page 5 of 256
Insulation fibers can cause irritation
Warning The insulation around the inlets, detectors, valve box, and the insulation cups
is made of refractory ceramic fibers. To avoid inhaling fiber particles, we
recommend the following safety procedures: ventilate your work area; wear
long sleeves, gloves, safety glasses, and a disposable dust/mist respirator; dis-
pose of insulation in a sealed plastic bag; wash your hands with mild soap and
cold water after handling the insulation.
Hydrogen
Hydrogen gas may be used as carrier gas, and/or as fuel for a detector. When
mixed with air, hydrogen can form explosive mixtures.
Warning When using hydrogen (H2) as the carrier gas or fuel gas, be aware that
hydrogen gas can flow into the oven and create an explosion hazard.
Therefore, be sure that the supply is off until all connections are made, and
ensure that the inlet and detector column fittings are either connected to a
column or capped at all times when hydrogen gas is supplied to the instrument.
Warning Hydrogen is flammable. Leaks, when confined in an enclosed space, may
create a fire or explosion hazard. In any application using hydrogen, leak test
all connections, lines, and valves before operating the instrument. Always turn
off the hydrogen supply at its source before working on the instrument.
When using hydrogen gas,check the system for leaks to prevent possible fire
and explosion hazards based on local Environmental Health and Safety (EHS)
requirements. Always check for leaks after changing a tank or servicing the gas
lines. Always make sure the vent line is vented into a fume hood.
Microcell electron capture detector (µECD)
This section describes the licensing information, handling precautions and
safety requirements concerning the µECD.
The µECD contains a cell plated with 63Ni, a radioactive isotope. 63Ni releases
β particles which collide with carrier gas molecules to produce low-energy
electrons — each βparticle produces approximately 100 electrons. The free
electrons produce a small current — called the reference or standing current
— which is collected and measured.

Important Information
Important safety warnings
Released: March 2004 6850 Series II GC User Information page 6 of 256
The 63Ni isotope
The radioactive isotope used in the cell is 63Ni. It is plated onto the inner
surface of the cell body and is solid at temperatures used in chromatography.
Some other properties are listed in Table 1.
Table 1. Properties of 63Ni
µECD licenses
Customers in the United States can purchase a µECD under either a General
License or a Specific License. Customers outside the United States should
contact their local Agilent sales office for information.
The license details below reflect U.S. regulations.
Specific license
Specific license µECDs require you to obtain a Materials License from the
Nuclear Regulatory Commission (NRC) or local state agency, permitting you to
possess the amount and kind of radioisotope used in the detector. You can
typically ship, sell, or transfer the µECD to other Specific Licensees. If the
license permits, you may also open the µECD for cleaning.
General license
General license µECDs do not require a Materials License. You become a
General Licensee automatically when you purchase a µECD directly from Agi-
lent Technologies. Some states may require that you register the µECD with a
state agency.
Certain restrictions apply to General Licenses:
• Owners may not open the µECD cell.
• Owners shall not modify the cell in any manner.
• Owners shall not use any solvent, including water, to internally clean the
cell.
Half-life: 101.1 years
Emission: 65.87 keV max., beta radiation
Melting point: 1453 °C
Dimensions of the active part
of the µECD:
Inside diameter: 6 mm
Height: 4.2 mm
Total activity (µECD cell): 555 MBq (15 millicuries) maximum

Important Information
Important safety warnings
Released: March 2004 6850 Series II GC User Information page 7 of 256
• Owners shall not interfere with or attempt to defeat the overheat circuitry
that may be supplied with the µECD.
• Owners shall not transfer the µECD to another person or another location
except as described in the applicable Regulations.
• Owners must perform a radioactive leak test at least every 6 months or as
required by your local Agency.
• Owners must maintain records as required by your local Agency (the NRC
or, in certain states, a state agency).
• Owners must notify the Agency in case of incidents or failures that might
lead to a hazardous condition.
Additional information is available in the publication “Information for General
Licensees,” part no. 5961-5664.
µECD warnings
Although beta particles at this energy level have little penetrating power —the
surface layer of the skin or a few sheets of paper will stop most of them—they
may be hazardous if the isotope is ingested or inhaled. For this reason the cell
must be handled with care: radioactive leak tests must be performed at the
required intervals, the inlet and outlet fittings must be capped when the
detector is not in use, corrosive chemicals must not be introduced into the
detector, and the effluent from the detector must be vented outside the
laboratory environment.
Warning Materials that may react with the 63Ni source, either to form volatile products
or to cause physical degradation of the plated film, must be avoided. These
materials include oxidizing compounds, acids, wet halogens, wet nitric acid,
ammonium hydroxide, hydrogen sulfide, PCBs, and carbon monoxide. This list
is not exhaustive but indicates the kinds of compounds that may cause damage
to 63Ni detectors.
Warning In the extremely unlikely event that both the oven and the detector heated zone
should go into thermal runaway (maximum, uncontrolled heating in excess of
400 °C) at the same time, and that the detector remains exposed to this
condition for more than 12 hours, take the following steps:

Important Information
Safety and regulatory certifications
Released: March 2004 6850 Series II GC User Information page 8 of 256
• After turning off the main power and allowing the instrument to cool, cap
the detector inlet and exhaust vent openings. Wear disposable plastic
gloves and observe normal laboratory safety precautions.
• Return the cell for exchange. Contact your local sales office for details.
• Include a letter stating the condition of abuse.
It is unlikely, even in this very unusual situation, that radioactive material will
escape the cell. However, permanent damage to the 63Ni plating within the cell
is possible, and therefore, the cell must be returned for exchange.
Warning Do not use solvents to clean the µECD.
You may not open the µECD cell unless authorized to do so by your local
nuclear regulatory agency. Do not disturb the four socket-head bolts. These
hold the cell halves together. Removing or disturbing them is a violation of the
terms of the General License and could create a safety hazard.
Safety precautions when handling µECDs
Always observe the following precautions:
• Never eat, drink, or smoke when handling µECDs.
• Always wear safety glasses when working with or near open µECDs.
• Wear protective clothing such as laboratory jackets, safety glasses, and
gloves, and follow good laboratory practices. Wash hands thoroughly with
a mild non-abrasive cleaner after handling µECDs.
• Cap the inlet and outlet fittings when the µECD is not in use.
• Connect the µECD exhaust vent to a fume hood or vent it to the outside.
Agilent Technologies recommends a vent line inside diameter of 6 mm
(1/4-inch) or greater. With a line of this diameter, the length is not critical.
Safety and regulatory certifications
The 6850 GC conforms to the following safety standards:
• Canadian Standards Association (CSA): C22.2 No. 1010.1
• CSA/Nationally Recognized Test Laboratory (NRTL): UL 61010A–1
• International Electrotechnical Commission (IEC): 61010–1
• EuroNorm (EN): 61010–1

Important Information
Safety and regulatory certifications
Released: March 2004 6850 Series II GC User Information page 9 of 256
The 6850 GC conforms to the following regulations on Electromagnetic
Compatibility (EMC) and Radio Frequency Interference (RFI):
• CISPR 11/EN 55011: Group 1, Class A
• IEC/EN 61326
• AUS/NZ
This ISM device complies with Canadian ICES-001. Cet appareil ISM est
conforme a la norme NMB—001 du Canada.
The 6850 GC is designed and manufactured under a quality system registered
to ISO 9001.
Information
The Agilent Technologies 6850 Gas Chromatograph meets the following IEC
(International Electro-technical Commission) classifications: Safety Class I,
Transient Overvoltage Category II, Pollution Degree 2.
This unit has been designed and tested in accordance with recognized safety
standards and is designed for use indoors. If the instrument is used in a manner
not specified by the manufacturer, the protection provided by the instrument
may be impaired. Whenever the safety protection of the 6850 Gas Chromato-
graph has been compromised, disconnect the unit from all power sources and
secure the unit against unintended operation.
Refer servicing to qualified service personnel. Substituting parts or performing
any unauthorized modification to the instrument may result in a safety hazard.
The instrument weighs approximately 23 kg (50 lbs) and therefore should be
moved in an upright position by two people supporting the bottom of the unit.
Sound Emission Certification for Federal Republic of Germany
Sound pressure
Sound pressure Lp < 48 dB(A) according to DIN-EN 27779.
When operating the 6850 with cryo valve option, the sound pressure 92.5 dB(A)
during cryo valve operation for short burst pulses.

Important Information
Safety symbols
Released: March 2004 6850 Series II GC User Information page 10 of 256
Schalldruckpegel
Schalldruckpegel LP < 48 dB(A) nach DIN-EN 27779.
Bei Betrieb des 6850 mit Cryo Ventil Option treten beim Oeffnen des Ventils
impulsfoermig Schalldrucke Lp bis ca. 92.5 dB(A) auf.
Safety symbols
Warnings in the manual or on the instrument must be observed during all
phases of operation, service, and repair of this instrument. Failure to comply
with these precautions violates safety standards of design and the intended use
of the instrument. Agilent Technologies assumes no liability for the customer’s
failure to comply with these requirements.
In the manual
Warning A warning calls attention to a condition or possible situation that could cause
injury to the user.
Caution A caution calls attention to a condition or possible situation that could damage
or destroy the product or the user's work.