Agilent Technologies 6850 Series II Manual de operación

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

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.

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