Agilent 7697A

Headspace Sampler

Installation and First Startup

Agilent Technologies
Notices
© Agilent Technologies, Inc. 2014 Warranty Safety Notices
No part of this manual may be reproduced The material contained in this document
in any form or by any means (including is provided “as is,” and is subject to being
electronic storage and retrieval or
CAUTION
changed, without notice, in future
translation into a foreign language) without editions. Further, to the maximum extent A CAUTION notice denotes a hazard. It
prior agreement and written consent from permitted by applicable law, Agilent calls attention to an operating
Agilent Technologies, Inc. as governed by disclaims all warranties, either express
United States and international copyright procedure, practice, or the like that, if
or implied, with regard to this manual and
laws. not correctly performed or adhered to,
any information contained herein,
could result in damage to the product
including but not limited to the implied
Manual Part Number warranties of merchantability and fitness or loss of important data. Do not
for a particular purpose. Agilent shall not proceed beyond a CAUTION notice
G4556-90013 be liable for errors or for incidental or until the indicated conditions are fully
consequential damages in connection understood and met.
Edition with the furnishing, use, or performance
of this document or of any information
Fourth edition, April 2014
contained herein. Should Agilent and the WA R N I N G
Third edition, September 2012
user have a separate written agreement
Second edition, November 2011
with warranty terms covering the A WARNING notice denotes a hazard.
First edition, January 2011 It calls attention to an operating
material in this document that conflict
Printed in USA with these terms, the warranty terms in procedure, practice, or the like that, if
the separate agreement shall control. not correctly performed or adhered to,
Agilent Technologies, Inc. could result in personal injury or
2850 Centerville Road
death. Do not proceed beyond a
Wilmington, DE 19808-1610 USA
WARNING notice until the indicated
安捷伦科技 （上海）有限公司 conditions are fully understood and
上海市浦东新区外高桥保税区 met.
英伦路 412 号
联系电话：（800）820 3278
Contents
1 Installation
Before You Begin 6
Tools required for installation 6
Personnel needed for installation 6
Parts supplied with the instrument 7
Verify site preparation 8
Prepare the GC and data system 8
Determine how you will connect the headspace sampler to the GC 9
Install the GC consumables needed for HS checkout 13
Inspecting the Headspace Sampler 14
Place the Headspace Sampler on the Bench 15
Install the Configuration Plug 17
Verify the available power configuration 17
Install the configuration plug 18
Install the Vial Tray (111 Vial Model Only) 21
Connect Cabling 26
Cabling diagrams for Agilent GCs 27
Other systems 28
Connect Gas Supplies 30
Connect the vial pressurization gas 31
Connect the carrier gas (using GC inlet carrier control) 32
Connect the Transfer Line to the GC 35
Install the transfer line to the Headspace 36
Attach the transfer line to a GC inlet 45
Install the transfer line support bracket 47
Turn On the Headspace Sampler 49
Set the IP Address 50
To set the LAN address at the keyboard 50
To use a DHCP server 50
Configure the Headspace Sampler 51

2 First Startup
Tools and Materials Required 54
Load the Checkout Method in the HS 55
Make the First Connection 57
Set the Checkout Method Parameters 58

Installation and First Startup 3

 If using an Agilent data system 58
Checkout method GC parameters 58
Prepare the Checkout Sample 61
Run the Checkout Sample 62
Compare Results 64
Prepare for Your Method (Optional) 67

A Making Swagelok Connections

Making Swagelok Connections 70
Using a Swagelok Tee 73

4 Installation and First Startup

Agilent 7697A Headspace Sampler
Installation and First Startup

1
Installation
Before You Begin 6
Inspecting the Headspace Sampler 14
Place the Headspace Sampler on the Bench 15
Install the Configuration Plug 17
Install the Vial Tray (111 Vial Model Only) 21
Connect Cabling 26
Connect Gas Supplies 30
Connect the Transfer Line to the GC 35
Turn On the Headspace Sampler 49
Set the IP Address 50
Configure the Headspace Sampler 51

This guide describes how to install the Agilent 7697A

Headspace Sampler (HS). This guide assumes that the GC is
installed, configured, and operating properly, along with any
associated data system.
This chapter describes the installation steps to unpack and
install the instrument. The next chapter describes how to
start up the HS for the first time and verify it is operating
properly.

Agilent Technologies 5
1 Installation

Before You Begin

Before installing the headspace sampler (HS), review the
information below.

Tools required for installation

The following tools and parts are needed for installation.

Table 1 Tools and parts for installation

Tool Agilent part number Use

Required
Torx T-20 driver 5182-3465 Transfer line installation
Open-end wrenches: Swagelok fittings for gas connections, sample loop,
• 7/16-inch (2) 8710-0972 and transfer line
• 5/16-inch 8710-0510
Tubing cutter 8710-1709 Cut 1/8-inch gas supply plumbing
Precision tubing cutter 5190-1442 Cut 1/16-inch stainless steel tubing
Included
1/4-in. x 3/16-in. wrench 8710-2618 Transfer line installation
Column cutting wafer 5181-7487 Transfer line installation

The other necessary parts and tools are supplied with the
new instrument.

Personnel needed for installation

The instrument is heavy. When lifting or moving the
instrument, two persons are required.

6 Installation and First Startup

 Installation 1

Parts supplied with the instrument

The headspace sampler ships with consumables and
hardware sufficient for typical installation and checkout. See
Table 2 below.

Table 2 Parts supplied with the headspace sampler

Description Part number Quantity Use

Wrench, open end 3/16-in. x 1/4-in. 8710-2618 1 Transfer line connection.
LAN cable 8121-0940 1 Communications.
Cable, APG remote, 9M/9M G1530-60930 1 Communications.
Flat bottom headspace vials, 20 mL, 100/pk 5182-0837 1 Checkout.
Crimp cap, headspace, Al, PTFE/Si septum, 5183-4477 Checkout.
20 mm, 100/pk
Ergonomic manual crimper for 20 mm caps 5040-4669 Checkout.
Leak Test Kit G4556-67010 1
Vial Pressurization Connection Kit
Tubing, post-drawn, 1650 mm 1530-2239 1 Connect HS Vial Pressure fitting to the gas
supply.
Nut, stainless steel, for 1/16-in. tubing 0100-0053 1 Connect the 1/16-in. end of the post-drawn
tubing to the HS Vial Pressure fitting.
Ferrule set, stainless steel, for 1/16-in. tubing 0100-1490 1

Nut and ferrule set, 1/8-in. Swagelok, 5181-7482 1 Connect the 1/8-in. end of the tubing to the
stainless steel gas supply.
Transfer Line Connection Kit
Fused silica, deactivated, .530 mm id x 5 m 160-2535-5 1 Transfer line.
long
Fitting, internal reducer, 1/16-in. to 1/32-in. 0100-2594 1 Transfer line connection.
Ferrule, polyamide graphite 1/32-in. 0100-2595 1 Transfer line connection.
Transfer line support assembly G3504-60620 1 Support transfer line at GC inlet. Consists of
bracket, clamp, and knurled thumbscrew.
Tubing, post-drawn, 1650 mm 1530-2239 1 Connect HS Carrier fitting to the gas supply
from the GC inlet flow module.
Union SS 1/16-inch tubing 0100-0124 1 Connect the 1/16-in. end of the post-drawn
tubing to the open end of the GC inlet carrier
line.
Column cutting wafer 5181-7487 1 Trim fused silica transfer line.

Installation and First Startup 7

1 Installation

Table 2 Parts supplied with the headspace sampler (continued)

Description Part number Quantity Use

Cap, 1/16-in., stainless steel 0100-0050 1 Cap the cut end of the SSL or MMI inlet
carrier tubing.
Nut and ferrule set, 1/8-in. Swagelok, 5181-7482 1 Connect the 1/8-in. end of the post-drawn
stainless steel tubing to the HS.
Nut, stainless steel, for 1/16-in. tubing 0100-0053 1 Cap the cut end of the SSL or MMI inlet
carrier tubing.
Ferrule set, stainless steel, for 1/16-in. tubing 0100-1490 1
Septum retainer nut for transfer line G3452-60835 1 Support transfer line on GC SSL or MMI inlet
Liner, Direct Connect, 2 mm ID, deactivated 5181-8818 1 GC SSL or MM inlet liner for checkout.
O-Ring, 2-010, Fluoroelastomer, 10/pk 5188-5365 1 GC SSL or MM inlet liner O-ring.
Septa, 11 mm low bleed, 5/pk 5182-3413 1 GC SSL or MM inlet septum (for checkout).

Verify site preparation

Verify that the site has been prepared according to the site
preparation manual. Sufficient bench space, power supply
receptacles, supplies, gases, traps, required accessories, and
so forth must be available.

Prepare the GC and data system

If not already installed, install the gas chromatograph and
verify its performance before beginning HS installation.
• Install the GC.
• Install the data system.
• Verify GC and data system performance.
• Cool all heated zones in the GC to safe handling
temperatures, especially the column oven and the inlet.
HS installation requires carrier gas flow interruption,
which can damage a hot column. HS installation requires
contact with the GC inlet, which can be hot enough to
cause burns.
• If you purchased the add- on HS control software, install
it after installing the data system.

8 Installation and First Startup

 Installation 1

Determine how you will connect the headspace sampler to the GC

How you connect the headspace sampler to the GC depends
on:
• The GC model
• The GC inlet type
• Optional HS accessories
• Whether or not you need to also use this same GC inlet
for other injection types (ALS or manual, for example)
See Table 3. Determine the connection best suited to your
hardware and needs.

Table 3 Supported headspace sampler–GC connections and control modes

Inlet type GC models Connection type Supports HS Comments

carrier mode(s)
Recommended configurations
Split/ 7890, 7820, Transfer line through • GC controls • Standard configuration.
splitless, 6890, 6850, septum head carrier flow • Can be disconnected to support
Multimode 5975T • GC + HS autosampler or manual injection.
(additive)* • With GC control of carrier flow, HS must be
On for non-HS injections.
• Supports frequent column changes.
Optional hardware:
• G4562A Carrier Gas EPC Module
Accessory.
• G3521A 7890A S/SL MMI Weldment for
Headspace (7890A, 5975T only).
* Requires G4562A Carrier Gas EPC Module Accessory

Installation and First Startup 9

1 Installation

Table 3 Supported headspace sampler–GC connections and control modes (continued)

Inlet type GC models Connection type Supports HS Comments

carrier mode(s)
Split/ 7890 G3520A Transfer Line GC controls carrier • Allows alternating HS and ALS usage,
splitless, Interface Accessory flow without hardware changes.
Multimode • Transfer line bypasses septum, reducing
cross-contamination between runs.
• Design reduces cold spots, improves
performance for samples with analytes
such as high weight alkenes (C40).
• Best performance for widest range of
analyses.
• Supports frequent column changes.
• Reduces potential for leaks.
• With GC control of carrier flow, HS must be
On for non-HS injections.
Required hardware:
• G3520A Transfer Line Interface Accessory.
• 1/16-inch stainless steel tubing.
Optional hardware:
• G4562A Carrier Gas EPC Module
Accessory.
Volatiles 7890, 6890 Transfer line direct to GC controls carrier • No support for additive flow.
interface volatiles interface flow • High sensitivity.
• Allows small volume injections.
• Most inert choice.
• Not recommended for frequent column
changes.
• Does not support ALS or manual injections.
Required hardware:
• Strain relief adapter.
Optional configurations
Split/ 7890, 7820, Transfer line through • HS controls • Can be disconnected to support
splitless, 6890, 6850, septum head carrier flow* autosampler or manual injection.
Multimode 5975T • GC + HS • Carrier flow control not as robust as control
(additive)* available using GC.
Required hardware:
• G4562A Carrier Gas EPC Module
Accessory.
* Requires G4562A Carrier Gas EPC Module Accessory

10 Installation and First Startup

 Installation 1

Table 3 Supported headspace sampler–GC connections and control modes (continued)

Inlet type GC models Connection type Supports HS Comments

carrier mode(s)
Purged 7890, 7820, Transfer line through GC + HS (additive)* Purged packed inlet is not recommended for
packed 6890, 6850 septum head HS use. The flow rate through the transfer line
needs to be high, which broadens peaks. If
used, set only a small flow from the PP inlet
(to sweep the inlet septum). Provide the main
column flow using the HS additive flow.
• Supports frequent column changes.
• Can be disconnected to support
autosampler or manual injection.
• Users will need to experiment with flows to
optimize the analysis.
Required hardware:
• G4562A Carrier Gas EPC Module
Accessory.
Cool 7890, 6890, Transfer line through GC controls carrier Cool on-column inlet is not recommended for
on-column 6850 septum head flow HS use. For most analytes, instead use a SSL
or MMI and run the column up and through
the transfer line to the HS 6 port valve. (Use of
columns > 530 µm is not recommended in the
transfer line. Larger id columns are not
supported for this use.) If connecting the
column directly to the HS sampling valve, for
most analytes provide a small split flow so
that the inlet provides a small amount to
sweep septum, and let the HS provide most
flow, for example 0.1:1.
• The flow rate through the transfer line
needs to be high, which broadens peaks.
• Supports frequent column changes.
• Can be disconnected to support
autosampler or manual injection, but
realignment of ALS or change of inlet
hardware may be required.
• Users will need to experiment with flows to
optimize the analysis.
• With the cool on-column inlet, the transfer
line butts against column. This is not
preferred.
Required hardware:
• G4562A Carrier Gas EPC Module
Accessory.
• Cool on-column inlet hardware for transfer
line size.
* Requires G4562A Carrier Gas EPC Module Accessory

Installation and First Startup 11

1 Installation

Table 3 Supported headspace sampler–GC connections and control modes (continued)

Inlet type GC models Connection type Supports HS Comments

carrier mode(s)
Any any User must determine • GC + HS • Determine best modes and use cases
non-Agilent non-Agilent connection method (additive)* based on similar Agilent hardware.
• HS controls Required hardware:
carrier flow • G4562A Carrier Gas EPC Module
Accessory.
* Requires G4562A Carrier Gas EPC Module Accessory

12 Installation and First Startup

 Installation 1

Install the GC consumables needed for HS checkout

HS checkout requires the GC consumables listed in Table 4.
Install them before installing the HS. See your GC user
documentation for details.

Table 4 GC consumables needed for HS performance verification

Description Part number

GC checkout column:
7890, 7820, 6890: 19091J-413
6850: 19091J-413E
If using MS or MSD:
7890, 7820, 6890: 19091S-433
6850: 19091S-433E
5975T: G3900-63001
Helium carrier gas
For split/splitless or multimode inlet
Liner 5181-8818*
Liner O-ring 5188-6405*
If using FID or NPD
Makeup gas Nitrogen or helium
If using µECD
Makeup gas Nitrogen or argon/methane
*Supplied with the HS.

Configure the column and any other items, as needed.

Installation and First Startup 13

1 Installation

Inspecting the Headspace Sampler

WA R N I N G The instrument is heavy. Use extreme caution when handling the

instrument. A two person lift is recommended. Failure to perform a
two person lift may result in personal injury.

Inspect the headspace sampler (HS) shipping container(s).

1 Inspect the shipping containers for damage. If a container
is damaged or shows signs of stress, notify both the
carrier and your local Agilent office.
Keep all shipping materials for inspection by the carrier.
2 Check the items received against the packing lists. If there
are discrepancies, notify your local Agilent office
immediately.
Keep the shipping containers until you have checked their
contents for completeness and verified instrument
performance.

14 Installation and First Startup

 Installation 1

Place the Headspace Sampler on the Bench

The HS requires a benchtop that can support its weight plus
that of other equipment you will use with it. The area must
be free of overhanging obstructions that might interfere with
cooling and limit access to the top of the instrument.

WA R N I N G The instrument is heavy. Use extreme caution when handling the

instrument. A two person lift is recommended. Failure to perform a
two person lift may result in personal injury.

1 Remove the HS from its shipping box.

• Be careful when removing the packing foam from
around the instrument. The foam also secures the
transfer line.
2 Place the HS on the benchtop. Make sure gas and power
supplies are accessible. Place other required equipment
near the HS. Install only on the right side of the GC.
3 Remove caps and packing.

Protective caps cover gas input and vent fittings on the

back of the unit.
Remove any packing tape that secures the transfer line
against the instrument.
For the 12 vial model, lift the tray cover and remove any
packing material from the tray.

Installation and First Startup 15

1 Installation

CAUTION The tray gantry in secured only by the foam packing material. Be
careful when unpacking the tray. The gantry can move when you lift
the tray.

4 Unpack the tray, if purchased.

Remove the shipping clamp (Figure 1) using a T- 20 Torx

driver. Then check the tray for shipping tape and packing
screws. Remove them. The packing screws may be labeled
with a flag or ribbon for identification. Remove any tape
or packing screws found.

Figure 1 Remove the tray shipping clamp (part number G4556-40670)

16 Installation and First Startup

 Installation 1

Install the Configuration Plug

Before use, set the HS power configuration.

Verify the available power configuration

1 Locate the configuration plug that shipped with the
headspace sampler. Compare the voltage shown on the
configuration plug label with the laboratory line voltage.
(For customers in Japan using 100 VAC, the unit is
120 VAC with an external 100 V/200 V step up
transformer.) See Table 5.

Table 5 Headspace sampler power configuration plugs

Part number Voltage Color

G4556-60390 120 VAC Brown
G4556-60400 200 VAC Red
G4556-60410 220 VAC Orange
G4556-60420 230 VAC Yellow
G4556-60430 240 VAC Violet

2 Locate the power cord that shipped with the headspace

sampler. Verify the power cord is correct for the locale
and voltage.

WA R N I N G Measuring the mains voltage can expose you to hazardous

electrical current. Only a trained technician should perform this
step.

Measure the power outlet voltage and verify it meets the

tolerance requirements listed in Table 6.

Installation and First Startup 17

1 Installation

Table 6 Power consumption

Product Line voltage (VAC) Frequency (Hz) Maximum Current rating Power outlet
continuous (amps) current rating
power
consumption
(VA)
111 Vial model 100*/120 50/60 850 6.2 15 Amp
single phase
(–10% / +10%)
111 Vial model 200/220/230/240 50/60 850 3.8/3.4/3.3/3.1 10 Amp
single/split phase
(–10% / +10%)
12 Vial model 100*/120 50/60 850 6.2 15 Amp
single phase
(–10% / +10%)
12 Vial model 200/220/230/240 50/60 850 3.8/3.4/3.3/3.1 10 Amp
single/split phase
(–10% / +10%)
* Users of 100 V power (Japan) receive the 120 V US power option with a 100 V/120 V step up transformer.

Install the configuration plug

Install the configuration plug as follows:

WA R N I N G Only an Agilent-trained technician should perform this procedure.

CAUTION Components can be damaged by static electricity: be sure to wear

an ESD strap grounded to the GC chassis while performing this
procedure.

18 Installation and First Startup

 Installation 1

1 Locate the cover plate for the AC board on the lower back
right corner of the HS.

Screw

Hole for
configuration
plug label

2 Loosen the T- 20 Torx screw in the cover plate and rotate

the cover plate to expose the AC board.

Installation and First Startup 19

1 Installation

3 Install the configuration plug into the AC board

(connector P4). See Figure 2.

Figure 2 Close up of AC board

4 Rotate the cover plate until it covers the plug. Reinstall

the screw to secure in place. The power rating label can
be seen through the cover plate.
If the plate does not close, check the configuration plug.

20 Installation and First Startup

 Installation 1

Install the Vial Tray (111 Vial Model Only)

If you did not purchase the 111 vial 7697A Headspace
Sampler model, skip to the next section.
The headspace sampler tray fits on the top right side of the
instrument. Two rollers at the back of the tray slide into
mounting clips on top of the HS chassis.

Installation and First Startup 21

1 Installation

1 Lift the tray and place onto the headspace sampler

chassis so that the two rollers at the back of the tray rest
on the HS chassis and the front of the tray is a few
centimeters above the chassis.

2 Roll the tray back until the rollers engage the clips in the
chassis. See Figure 3.

22 Installation and First Startup

 Installation 1

Figure 3 Placing the tray

3 Connect the tray control cables to the connectors in the

chassis. See Figure 4. Route the control cables through
the plastic clip on the chassis.
• Carefully remove the packing tape from the cables.
• When finished, check that the cables route through the
clip.

Installation and First Startup 23

1 Installation

Cable in clip

Cable connections

Figure 4 Connecting and routing the cables

4 Slowly lower the front of the tray. Align the vial oven
access through- hole over the raised rim of the vial oven
access port. The tray front aligns with the front of the
instrument. The tray should be level and flat against the
instrument chassis.

24 Installation and First Startup

 Installation 1

5 If needed, gently slide the gantry all the way to the back
of the tray.

6 Install the 3 vial racks into the tray.

Installation and First Startup 25

1 Installation

Connect Cabling
1 Connect the power cable. See Figure 5.

G1530-60930

8121-0940

Figure 5 Back panel connections

2 Connect the LAN cable. See Figure 5.

3 Connect the APG Remote cable. See Figure 5 through
Figure 8.

26 Installation and First Startup

 Installation 1

Cabling diagrams for Agilent GCs

LAN cable 8121-0940*

G1530-60930*
LAN cable LAN cable 8121-0940 APG Remote
8121-0940 cable

GC:
7890A, 7820A, 6890
with LAN, 6850, HS
PC LAN switch 5975T LTM
or hub GC/MSD

*Included in ship kit.

Figure 6 HS–GC (LAN)–PC

LAN cable 8121-0940*

G1530-60930*
LAN cable APG Remote
8121-0940 cable

GC HS
LAN switch 6890A GPIB
PC
or hub

*Included in ship kit.

Figure 7 HS–GC (GPIB)–PC

Installation and First Startup 27

1 Installation

LAN cable 8121-0940 (4 each)

G1530-61200
APG Remote Y-cable

LAN switch
or hub GC
MS or 7890A, 7820A,
MSD 6890 with LAN, HS
PC 6850

One LAN cable 8121-0940 included in HS ship kit. If purchased as a

complete system (MS/MSD + GC + HS), one G1530-61200 is included in
the ship kit.

Figure 8 HS–GC (LAN)–PC–MS (or MSD)

Other systems
Use the Agilent general purpose remote start/stop cable,
35900- 60670, to synchronize an Agilent product and a
non- Agilent product. See Figure 9 and Figure 10.

LAN cable 8121-0940*

35900-60670
LAN cable General purpose
8121-0940 remote cable

non-Agilent HS
PC LAN switch
or hub

*Included in ship kit.

Figure 9 HS–GC (LAN)–PC–MS (or MSD)

28 Installation and First Startup

 Installation 1

Figure 10 General purpose remote start/stop cable, Agilent product to

non-Agilent product

Table 7 Cable pinouts, general purpose remote start/stop cable

Wire color Signal name

Black Ground
White Prepare (low true)
Red Start (low true)
Green Start relay
Brown Start relay
Blue Not used
Orange Ready (high true input)
Yellow Stop (low true)
Violet Not used

To ensure compatibility when connecting to a non- Agilent

product, a detailed knowledge of signal levels, driver and
receiver circuitry, and timing is necessary.

Installation and First Startup 29

1 Installation

Connect Gas Supplies

Agilent recommends installing shutoff valves (not supplied) near the vial
NOTE
pressurization and carrier gas fittings. Using the valves provides a fast way
to isolate the HS during troubleshooting and periods of inactivity.

Agilent provides hardware to plumb the instrument gases as

shown in Figure 11. In this example, the HS connects to a
7890A GC through the inlet septum. The GC provides carrier
gas control. The vial pressurization gas is connected to a
different supply than the carrier gas.

1/8-in. flare

1530-2239 Tubing, post

drawn, 1650 mm

Carrier gas from

GC inlet
1530-2239 Tubing, post
drawn, 1650 mm
1/16-inch union
0100-0124 1/8-in. flare
Vent 1/8-in.

Vial pressure 1/16-in.

Carrier 1/8-in.

Vial Carrier gas

pressurization supply
gas supply (N2, He, H2,
(N2, He) Ar/Me)

Swagelok cap at inlet

Figure 11 Standard plumbing configuration

See Table 8 for a summary of the acceptable gas types for

the HS.

30 Installation and First Startup

 Installation 1

Table 8 Acceptable gases for HS use

Gas type Vial pressurization Carrier

Helium Yes Yes
Nitrogen Yes Yes
Hydrogen No Yes
Argon (5%)/Methane (95%) No Yes

The procedures below assume the standard configuration: Plumbing as

NOTE
shown in Figure 11, with GC carrier gas control using the inlet EPC module.
These procedures also assume that the GC is already plumbed and
operating, and that the GC is plumbed for helium carrier gas.
If your setup is different, connect your gases accordingly.

Connect the vial pressurization gas

Materials needed:
• 1/8- inch Swagelok nut and ferrule set, stainless steel
• 1/16- inch Swagelok nut and ferrule set
• 1/16- inch to 1/8- inch flared stainless steel tubing,
1650 mm long
Tools required:
• 7/16- inch open- end wrenches
• 5/16- inch open- end wrenches
• Precision tubing cutter
For details on making Swagelok connections, see “Making
Swagelok Connections.”

WA R N I N G Use only helium or nitrogen as vial pressurization gas. Never use

flammable gases for vial pressurization. Flammable gases create
an explosion hazard if used for vial pressurization.

1 Turn off the vial pressurization gas supply.

2 Use the 1/8- inch Swagelok nut and ferrules to connect
the 1/8- inch flared end of the stainless steel tubing to the
gas supply.

Installation and First Startup 31

1 Installation

3 Use the 1/16- inch nut and ferrules to connect the

1/16- inch end of the stainless steel tubing to the Vial
Pressure fitting on the back of the HS.
4 Turn on the vial pressurization gas supply and set the
source pressure to 410 kPa (60 psi).
5 Check for leaks in all external fittings. Correct any leaks
before continuing.

Connect the carrier gas (using GC inlet carrier control)

Materials needed:
• 1/16- inch Swagelok union, stainless steel
• 1/16- inch Swagelok cap, stainless steel
• 1/8- inch Swagelok nut and ferrule set, stainless steel
• 1/16- inch Swagelok nut and ferrule set, stainless steel
• 1/16- inch to 1/8- inch flared stainless steel tubing,
1650 mm long
Tools required:
• 7/16- inch open- end wrenches
• 1/4- inch open- end wrenches
• Precision tubing cutter
Before beginning, make sure the GC oven is cool. You will
need to stop GC carrier gas flow. Stopping GC carrier flow
can damage a hot column.

The procedure below assumes a 7890A GC with a multimode or

NOTE
split/splitless inlet. Other instrument types are similar.

This procedure assumes that you will manually splice the HS into the
NOTE
carrier gas stream. If you have purchased accessory G3521A, 7890A S/SL
MMI Weldment for Headspace, you will skip some steps. See below. This
procedure does not discuss installation using other accessories or inlet
types.

1 If on, turn off the carrier gas supply.

2 Remove any ALS injectors and the GC detector cover from
the GC.

32 Installation and First Startup

 Installation 1

3 Remove the GC pneumatics cover. (You may need to

disconnect any vent lines.)

If you purchased the G3521A 7890A S/SL MMI Weldment for Headspace, install it
NOTE now. Skip step 4.

4 Splice into the inlet carrier gas tubing.

a Locate the inlet carrier gas line. The inlet carrier gas
line is a 1/16- inch stainless steel tube that runs from
the inlet EPC module to the inlet, usually beside the
inlet carrier cover on the oven top. For split/splitless
and multimode inlets, there is also a stainless steel
septum purge vent line. The septum purge vent line is
larger in diameter, and runs to the septum purge vent
on the EPC module.

Carrier gas line is 1/16-inch id.

It is always slightly smaller than
the septum purge line.

Septum purge gas line is slightly

larger than the carrier gas line.

7890A Multimode inlet shown. Other inlets similar.

b Using the precision tubing cutter, cut the carrier gas

line leading into the inlet at approximately 3 to 5 cm
from the septum head.

CAUTION Cut the tubing as square as possible. Be careful to avoid kinks in the
tubing. Avoid deforming the tubing. The cut should not be beveled or
angled.

Installation and First Startup 33

1 Installation

c Plug the inlet carrier line at the septum head using the
1/16- inch Swagelok nut, ferrules, and cap assembly
provided in the ship kit.

5 Install the male half of a 1/16- inch union onto the open
end of the carrier gas tubing coming from the inlet EPC
module.

When completed, you should be able to reassemble the original carrier

NOTE
flow path by removing the cap from the plug, then connecting the two
ends of the tubing.

6 Use the other half of the 1/16- inch Swagelok union to

connect the carrier gas tubing from the EPC module
(prepared in step 5) to the smaller (1/16- inch) end of the
flared stainless steel tubing.
7 Use a 1/8- inch Swagelok nut and ferrules to connect the
larger end of the flared stainless steel tubing to the
Carrier fitting on the HS.
8 Turn on the carrier gas supply. Set the delivery pressure
to 550 kPa (80 psi).
9 Check for leaks in all external fittings. Correct any leaks
before continuing.

34 Installation and First Startup

 Installation 1

Connect the Transfer Line to the GC

This procedure describes installation of the fused silica
transfer line provided with the instrument. If you have
purchased a different transfer line, you can install it instead
of the 530 µm line listed below. Refer to the Maintenance
manual for part numbers and procedures.
Materials needed:
• 1/16- inch internal reducer union
• 530- µm fused silica column
• 11- mm septum
• Septum nut adapter (G3452- 60835)
Tools needed:
• 3/16- inch open end wrench
• 1/4- inch open end wrench
• Column cutting wafer

Installation and First Startup 35

1 Installation

Install the transfer line to the Headspace

CAUTION Wear clean, lint-free gloves to prevent contamination of parts with

dirt and skin oils.

1 Remove the front pneumatics cover.

a Remove the T- 20 screw that secures the cover in place.

Front pneumatics cover

b Pull the cover away from the chassis, then lift to

remove.

36 Installation and First Startup

 Installation 1

2 Lift the valve thermal enclosure straight up from the HS.

Installation and First Startup 37

1 Installation

3 Depending on your hardware configuration, do one of the

following:
• Remove the valve cover (Figure 12). Completely loosen
the two T- 20 Torx screws, and remove the valve cover.
• Remove the valve/loop cover (Figure 13). Completely
loosen the three T- 20 Torx screws, and remove the
valve/loop cover.

Valve cover

Figure 12 The valve cover

Figure 13 The valve/loop cover

38 Installation and First Startup

 Installation 1

4 The transfer line will install in the valve port at the

10 O’clock position, as shown in the figure below (valve
port 3). Remove the 1/16- inch plug. Save the plug for
future use.

6 port valve Sample loop

Sample probe
10 O’Clock
position Vial pressurization gas
line
Carrier gas line
Sample loop

5 Disassemble the 1/16- inch internal reducer provided in

the HS ship kit.

3/16-inch nut 1/4-inch nut 1/16-inch tube

Polyimide ferrule Stainless steel ferrule

Figure 14 Internal reducer parts

Installation and First Startup 39

1 Installation

WA R N I N G Wear safety glasses to protect your eyes from flying particles

while handling, cutting, or installing glass or fused silica capillary
columns. Use care in handling these columns to prevent puncture
wounds.

6 Slide the stainless steel ferrule over the 1/16- inch tube
end of the reducer, then install into the open valve port
(at 10 O’clock). Finger- tighten, then tighten 1/4- turn
more.

40 Installation and First Startup

 Installation 1

7 Remove the protective cap from the transfer line.

8 Depending on the type of tubing you are using in the

transfer line, do the following:
Uncoated deactivated fused silica tubing: Uncoil about
1 m of the 530 µm uncoated deactivated fused silica
tubing.
ProSteel tubing: Cut a ProSteel metal capillary (0.53 mm
ID with maximum OD of 0.67 mm) to approximately 1 m
in length using a precision tubing cutter.
9 If using ProSteel tubing and you intend to operate at
temperatures 200 °C and higher, you must use the
ProSteel protective sleeve with the ProSteel tubing.
Without the ProSteel protective sleeve, the ProSteel tubing
can permanently bind to the heated conduit tube. If using
fused silica tubing, skip this step.
To install the ProSteel protective sleeve:
a Trim the ProSteel protective sleeve to match the length
of the transfer line (approximately 1 m), plus or minus
a few millimeters.
b Straighten the ProSteel tubing and protective sleeve.
c Slide the ProSteel tubing into the protective sleeve.

Installation and First Startup 41

1 Installation

10 Working from the open end that will connect to the GC

(not the end near the 6 port valve), gently slide the
tubing through the transfer line until it appears out the
end near the 6 port valve.
If using ProSteel tubing with protective sleeve, make sure
the protective sleeve protrudes a few millimeters from
both ends of the transfer line for easy removal.

11 Gently grasp the tubing at the HS end and gently push

and pull the tubing to verify that it is unbroken in the
transfer line. The tubing should move back and forth.
12 Assemble the 3/16- inch nut and polyimide ferrule onto
the tubing as shown below. Be sure to use the appropriate
nut and ferrule supplied with the capillary in use.

3/16-inch nut Tubing

Polyimide ferrule

42 Installation and First Startup

 Installation 1

13 Use a column cutter to trim approximately 1 cm from the

leading edge of the tubing.

For detailed instructions on how to trim a fused silica column, refer to your
NOTE
HS maintenance manual or the GC maintenance manual.

14 Insert the tubing into the internal reducer and loosely

install the 3/16- inch nut. Do not tighten yet.

Installation and First Startup 43

1 Installation

15 Gently slide the tubing into the internal reducer until it

bottoms. Tighten the 3/16- inch nut finger tight, then an
additional 1/4- turn. Test the connection by gently pulling
on the transfer line. The transfer line should not slide out
of the newly- made fittings. See Figure 15.

Figure 15 Transfer line installed into 6 port valve

44 Installation and First Startup

 Installation 1

Attach the transfer line to a GC inlet

CAUTION Wear clean, lint-free gloves to prevent contamination of parts with

dirt and skin oils.

WA R N I N G Be careful! The oven and/or inlet may be hot enough to cause

burns. If either is hot, wear heat-resistant gloves to protect your
hands.

Split Splitless or Multimode Inlet

1 Slide the one- piece septum nut and strain relief coupling
onto the tubing until the inner metal sleeve of the
transfer line bottoms- out on the strain relief.
2 Slide the septum onto the tubing until the septum is
against the bottom of the one- piece septum nut and
strain relief coupling.
3 Trim the tubing 42 +/- 5 mm past the end of the septum.
4 Install the inlet liner (with o- ring) that is appropriate for
your application.
5 Insert the tip of the transfer line into the inlet.
6 Finger- tighten the strain relief coupling.

Purged Packed Inlet

1 Slide the one- piece septum nut and strain relief coupling
onto the tubing until the inner metal sleeve of the
transfer line bottoms- out on the strain relief.
2 Slide the septum onto the tubing until the septum is
against the bottom of the one- piece septum nut and
strain relief coupling.
3 Trim the tubing 2 mm past the end of the septum.
4 Install the inlet liner (with o- ring) that is appropriate for
your application.
5 Insert the tip of the transfer line into the inlet.
6 Finger- tighten the strain relief coupling.

Installation and First Startup 45

1 Installation

Volatiles Interface
1 Slide the transfer line nut (G2319- 20210) onto the tubing.
2 Install a SilTite ferrule and make a SilTite connection as
described below. Refer to Table 9 and use the SilTite
ferrule appropriate for your transfer line.

Table 9 SilTite ferrules

Transfer line id Use SilTite ferrule part number:

0.25 mm 5188-5361
0.32 mm 5188-5362
0.53 mm 5188-5363

CAUTION The SilTite ferrules are delicate. Follow the instructions in the next
steps very carefully to avoid overtightening.

a Pass the transfer line tubing end through the SilTite

ferrule leaving approximately 1 cm of tubing
protruding beyond the ferrule. Thread the pre- swaging
tool onto the transfer line nut (Figure 16) with the
tubing protruding through the tool.

Nut
Pre-swaging tool

Figure 16 Volatiles interface nut and pre-swaging tool (G4556-67018)

b Using a wrench and ferrule pre- swaging tool, tighten

the nut a little at a time, occasionally checking to see
if the ferrule is gripping the tube. When the ferrule
just starts to grip, notice position of the nut and then
tighten by turning 45 to 60 degrees of rotation, but no

46 Installation and First Startup

 Installation 1

more than 60 degrees (one flat). If you can pull the

transfer line tubing free, it is not tight enough.
c Remove the pre- swaging tool.
d Using a ceramic column cutter, trim the tubing at the
small end of the ferrule leaving approximately 0.3 mm
of tubing extending beyond the ferrule.

It is important that the tube end does not extend

beyond 0.5 mm from the end of the ferrule.
e Check the end of the tube with a magnifier. The end of
the tube need not be perfectly square, but should not
have cracks which extend under the ferrule.
3 Screw the nut onto the volatiles interface.

Cool On-Column Inlet

1 Trim the tubing so that it extends 42 mm out of the inner
metal sleeve on the transfer line.
2 Slide the tubing through the retaining nut on the cool
on- column inlet.
3 Finger- tighten the retaining nut. Pull the transfer line
gently to be sure the ferrule has formed a tight seal with
the transfer line. Tighten the retaining nut further, if
necessary.

Install the transfer line support bracket

Install the transfer line support bracket as described below.
Use this bracket in all configurations, and for all Agilent
inlet types and GCs.
1 If necessary, remove any existing ALS post from the
mounting hole next to the transfer line.
2 Place the transfer line support bracket on the inlet carrier
cover. The locator holes in the support bracket should
align over the holes for the inlet ALS injector post and
the raised mounting detail. See the figures below.

Installation and First Startup 47

1 Installation

Back mounting
post hole

Back mounting
detail
Front mounting
post hole

Front mounting
detail

Figure 17 Mounting location for support bracket, 7890A inlet carrier

cover shown

Transfer line

Clamp

Support bracket

Knurled thumbscrew

Figure 18 Transfer line installed onto 7890A inlet

3 Locate the knurled thumbscrew provided in the HS ship

kit transfer line support assembly.
4 Install the knurled thumbscrew into the inlet cover
through the transfer line support bracket.
5 Install the clamp onto the bracket. Align the clamp so
that it supports the transfer line as high as possible above
the GC as shown in Figure 18.

48 Installation and First Startup

 Installation 1

Turn On the Headspace Sampler

1 Turn on the gas supplies.
2 Turn on the headspace sampler.

After power up, the display should be similar to the

following:

Agilent 7697A
A.01.01

Power on successful

Now that the gases and HS are turned on, the vial
pressurization gas will begin to purge the HS sampling
system.

Installation and First Startup 49

1 Installation

Set the IP Address

For network (LAN) operation, the HS needs an IP address.
Typically enter the IP address using the HS keyboard. See
your LAN administrator.

To set the LAN address at the keyboard

1 Press [Options]. Scroll to Communications and press [Enter].
2 Scroll to IP. Enter the numbers of the HS IP address,
separated by dots, and press [Enter]. A message tells you
to power cycle the instrument. Do not power cycle yet.
Press [Clear].
3 Scroll to GW. Enter the Gateway number and press [Enter].
A message tells you to power cycle the instrument. Do not
power cycle yet. Press [Clear].
4 Scroll to SM and press [Mode/Type]. Scroll to the
appropriate subnet mask from the list given and press
[Enter]. A message tells you to power cycle the instrument.
Do not power cycle yet. Press [Clear].
5 Scroll to Reboot instrument. Press [On/Yes] and [On/Yes] to
power cycle the instrument and apply the LAN setpoints.

To use a DHCP server

Note that DHCP is not supported by all Agilent data
systems.
1 Press [Options]. Scroll to Communications and press [Enter].
2 Scroll to Enable DHCP and press [On/Yes]. When prompted,
turn the instrument off and then on again.

50 Installation and First Startup

 Installation 1

Configure the Headspace Sampler

Next, enter details that describe the gas types, vial sizes,
sample loop size, and other important information.
1 Press [Config].
2 Use   to scroll to Vial Gas type and press [Mode/Type].
3 Use   to select the vial pressurization gas type from the
list, then press [Enter].
4 Scroll to Loop Volume (mL). Press [Mode/Type]. Select 1.0 as
the sample loop volume, in mL, then press [Enter]. (All
headspace samplers ship with a 1 mL sample loop
installed.)
5 If you ordered the optional G4562A Carrier Gas EPC
Module Accessory, scroll to Carrier. Press [Mode/Type].
Select the correct control mode for checkout:
• If the HS will provide all carrier gas to the GC, select
GC Control. (For example, you did not plumb carrier gas
to the GC.)
• If the GC will provide its own carrier gas flow, select
GC + HS Control. In this case, the HS will provide enough
additional carrier gas flow during injection to push the
checkout sample into the GC inlet.
6 Scroll to APG polarity. If needed, press [Mode/Type] to
change.
• For Agilent GCs, use Active high.
• For non- Agilent GCs, refer to the GC documentation.

Installation and First Startup 51

1 Installation

52 Installation and First Startup

Agilent 7697A Headspace Sampler
Installation and First Startup

2
First Startup
Load the Checkout Method in the HS 55
Make the First Connection 57
Set the Checkout Method Parameters 58
If using an Agilent data system 58
Checkout method GC parameters 58
Prepare the Checkout Sample 61
Run the Checkout Sample 62
Compare Results 64
Prepare for Your Method (Optional) 67

This section describes how to start up the Agilent 7697A

Headspace Sampler for the first time and verify its
performance. This section describes how to get started using
both the front panel and an Agilent data system. While the
specific software described is the Agilent ChemStation,
version B.04.03, the instructions apply generally to any
Agilent data system. Refer to the data system’s help.
Only perform the sections that apply to your setup.

Agilent Technologies 53
2 First Startup

Tools and Materials Required

Materials needed:
• Headspace checkout sample, 5182- 9733
• Flat bottom headspace vial, 20 mL
• Crimp cap, headspace, 20 mm septum
Tools required:
• Ergonomic manual crimper for 20 mm caps
• Forceps or tweezers
The checkout sample kit, part number 5182- 9733, contains
5 mL of sample and a box of 5- µL micropipettes.
The sample composition is:
• 9.59 ± 0.05% n- nonane (w/w)
• 0.348 ± 0.002% 1,2- dichlorobenzene (w/w)
• 0.322 ± 0.002% nitrobenzene (w/w)
• 0.241 ± 0.001% tert- butyldisulfide (w/w)
in dodecane matrix.

54 Installation and First Startup

 First Startup 2

Load the Checkout Method in the HS

Using the HS front panel, load the checkout method.
1 Press [Load][Method].
2 Scroll to select Checkout, then press [Enter].

The checkout method will load. The HS will begin heating

and adjusting flows to the initial conditions.
Once the front display reads Ready, let he HS sampler
stabilize for 25 to 30 minutes before running the checkout
sample. This hold time ensures thermal stability and that
any residual moisture or other contaminants are swept from
the system.
For reference, Table 10 lists the headspace sampler checkout
setpoints and configuration.

Table 10 Headspace checkout parameters

Configuration
Vial Gas type He
Loop Volume (mL) 1
Advanced Functions
Extraction mode Single
Purge flow 100.0
Purge time 1.000
Temperature
Oven 100.0 °C
Loop/Valve 110 °C
Transfer line 115 °C
Time
GC cycle time 4 min. (FID, NPD)
5 min. (µECD)
6.5 min. (MS, MSD)
Vial equib time 7 min.
Pres equib time 0.1 min.
Inject time 0.5 min
Vial

Installation and First Startup 55

2 First Startup

Table 10 Headspace checkout parameters (continued)

Fill mode Flow to pressure

Fill pressure 103.4 kPa (15 psi)
Fill flow 50 mL/min
Loop fill mode Default
Vent after extraction Yes
Vial size 20 mL
Shaking 1

56 Installation and First Startup

 First Startup 2

Make the First Connection

If using an Agilent data system, perform this step. If
operating the HS in standalone mode, skip this section.
1 Open the online session for the GC.
2 As the GC session opens, you will be prompted to
configure the instrument. Select Yes. The instrument
configuration utility opens.
If not prompted, open the utility from the Instrument
menu.
3 In the left pane, double- click on the 7697A instrument.
The instrument icon moves to the right hand list.
4 Click Configure. In the dialog that opens, enter the
following:
• In the Connect Info group, enter the Instrument Name,
then enter the instrument IP address or host name.
• Enter your license key in the Instrument License field.
You will see the Version Information for the instrument
appear (instrument serial number, firmware version,
software version, and so forth).
• Enter any Notes as desired.

Installation and First Startup 57

2 First Startup

Set the Checkout Method Parameters

Next, set the rest of the checkout parameters.

If using an Agilent data system

If using an Agilent data system, upload the current HS
parameters into the data system method. In the
ChemStation, select Method and Run Control view.
1 Select Instrument > Upload method from Agilent 7697A.
2 Save the method using a new name.
3 Select Instrument > Edit Parameters, then enter the GC
parameters listed in the next section.
Apply the method to the GC and save it.

Checkout method GC parameters

Enter the following GC setpoints, either in the data system
(if used) or at the GC using the keypad.

The table lists the settings for a 7890A GC. Other GC types use similar
NOTE
settings.

Table 11 GC checkout method

Oven
Initial temperature 100 °C
Initial time 4.00 min
Rate 0 (Off)
Equilibration time 1.00 min
Run time 4.00 min
Inlet (multimode, volatiles interface, or split/splitless)
Mode Split
Initial temperature 250 °C (On)
Pressure 134.4 kPa (19.5 psi)
Split ratio 20:1
Split flow 80 mL/min

58 Installation and First Startup

 First Startup 2

Table 11 GC checkout method (continued)

Total flow 87 mL/min

Gas saver Off
Column
Mode Constant flow
Initial flow 4.0 mL/min
Initial pressure 134.4 kPa (19.5 psi)
Average velocity 60 cm/s
Detector parameters–FID
Temperature 300 °C
Hydrogen (fuel) flow 30 mL/min
Air flow 400 mL/min
Makeup mode Constant makeup
Makeup flow 25 mL/min
Detector parameters–NPD
Temperature 300 °C
Hydrogen (fuel) flow 2.0 mL/min
Air flow 60 mL/min
Makeup mode Constant makeup
Makeup flow 8 mL/min
Detector parameters–µECD
Temperature 250 °C
Makeup mode Constant makeup
Makeup flow 30 mL/min
MS or MSD
Solvent delay 3 min
Run time 6.5 min
Headspace event time for GC cycle 7 min
time
Scan range 45 to 300
Method used Atune file
Inlet pressure 82.8 kPa (12 psi)
Column flow 1.1 mL/min

Installation and First Startup 59

2 First Startup

Table 11 GC checkout method (continued)

Split ratio 80:1

Injection source Headspace sampler (front)
Injection volume 5 µL

60 Installation and First Startup

 First Startup 2

Prepare the Checkout Sample

While the instrument comes to equilibrium, prepare the
checkout sample. The checkout method calls for a 5- µL
sample in a 20- mL headspace vial.
1 Snap the top off the checkout sample ampoule. Transfer
the contents to a screw- cap bottle.
2 Dispense one capillary pipette.
3 Hold the pipette with clean tweezers. With the checkout
sample bottle and the pipette as close to horizontal as
practical, dip the end of the pipette into the sample. See
Figure 19.

(1) Grasp (2) Fill (3) Wipe

Figure 19 Filling the pipette

4 The pipette will fill by capillary action. When it has filled

completely, pull the pipette out of the sample. Wipe the
bottom edge of the pipette against the edge of the vial to
remove any droplets on the outside.
5 Drop the filled pipette into a 20- mL headspace vial.
Crimp a cap on the vial.
6 Cap the checkout sample vial.

Installation and First Startup 61

2 First Startup

Run the Checkout Sample

After the HS has been Ready for 25–30 minutes, it has been
purged and is sufficiently stable to run the checkout sample.
1 Load the checkout sample into the HS.

For the 111 vial model:

a Press [Tray Park/Carousel Advance] to “park” the tray
(move the gantry to a rest position for easy access to
the vial racks).
b Place the capped sample vial in position 1.

5
1

4 1
3

Figure 20 Tray vial position 1

c Press [Tray Park/Carousel Advance] to prepare the tray for

use.
For the 12 vial model:
a Open the tray cover. A label to the left of each vial
position denotes the number of that position. See
Figure 20 and Figure 21.
b If vial position 1 is not available, press [Tray
Park/Carousel Advance] to rotate the tray.
c Place the capped sample vial in position 1.

62 Installation and First Startup

 First Startup 2

Figure 21 Opening the tray cover

2 Start the sample run.

If using an Agilent data system:

a Set the injection source to be the HS.
b Create a 1 line sequence to run the checkout sample
(vial 1) once, using the checkout method.
c Set up the report so that the correct signal output
becomes part of the report.
d Start the sequence.

If using the HS standalone:

a Press [Sequence][Load/Append]. This creates the first
line of the sequence. Note that the default new
sequence line selects the current method, vial range 1
to 1, and 1 injection per vial. The sequence is
complete.
b When the GC is ready, press [Start] on the HS
keyboard.

Installation and First Startup 63

2 First Startup

Compare Results
When the run completes, compare the output chromatogram
against the examples below. Is correctly installed and
operating properly, the output chromatogram should be
similar to the example here.

2.037
FID1 A, (HS_ECD\HSVI0004.D)
0.880

pA

2.476
160

Ethanol Nitrobenzene
140 (40,000 counts

2.825
typical)
120

100 Dichlorobenzene t-Butyl disulfide

80

60

40
0.858

20

0.0 0.5 1.0 1.5 2.0 2.5 3.0 3.5 4.0 min

Figure 22 FID checkout chromatogram

64 Installation and First Startup

 First Startup 2

2.384
NPD1 B, (HS_NPD\HSNPD002.D)
pA

Nitrobenzene
250

200

150

100

Ethanol
50

0.0 0.5 1.0 1.5 2.0 2.5 3.0 3.5 min

Figure 23 NPD checkout chromatogram

2.021

ECD1 A, (HS_ECD\HSEC0000.D)
Hz

Dichlorobenzene
120000

100000
2.461

80000

60000

Ethanol
2.810

40000
0.850

20000

0 1 2 3 4 min

Figure 24 µECD checkout chromatogram

Installation and First Startup 65

2 First Startup

Dichlorobenzene
1000000
TIC: 0201002.D
800000
Abundance

600000

t-Butyl disulfide
400000 Nitrobenzene

200000

0
3.20 3.60 4.00 4.40 4.80 5.20 5.60 6.00 6.40
Time

Figure 25 MS and MSD checkout chromatogram

66 Installation and First Startup

 First Startup 2

Prepare for Your Method (Optional)

At this point, installation is complete. However, if you have
purchased an optional sample loop, install it now before
continuing. See the Maintenance guide for details.
Also consider your method’s vial pressures and carrier gas
pressures. Make sure that the gas supplies are set to provide
at least 138 kPa (20 psi) higher than the highest pressure
needed (for vial pressurization or for the GC column carrier
flow during temperature programming), up to the maximum
input pressure of 828 kPa (120 psi).

Installation and First Startup 67

2 First Startup

68 Installation and First Startup

Agilent 7697A Headspace Sampler
Installation and First Startup

A
Making Swagelok Connections
Making Swagelok Connections 70
Using a Swagelok Tee 73

The gas supply tubing is attached with Swagelok fittings. If

you are not familiar with Swagelok connections, review the
following procedures.

Agilent Technologies 69
A Making Swagelok Connections

Making Swagelok Connections

Objective
To make a tubing connection that does not leak and that can
be taken apart without damaging the fitting.
Materials needed:
• 1/8- inch (or 1/4- inch, if used) preconditioned copper
tubing
• 1/8- inch (or 1/4- inch, if used) Swagelok nuts
• Front and back ferrules
• Two 7/16- inch (for 1/8- inch nuts) or 9/16- inch (for
1/4- inch nuts) wrenches
1 Place a Swagelok nut, back ferrule, and front ferrule to
the tubing as shown in Figure 26.

Front ferrule
Important!
Back ferrule
The narrow end of the
Nut back ferrule fits into
the rear of the front
ferrule.

Tubing

Figure 26 Swagelok nuts and ferrules

2 Clamp a stainless steel plug or similar fitting in a bench

vise.

CAUTION Use a separate stainless steel fitting in a vise for initial tightening of
the nut. Do not use an inlet or detector fitting. Strong forces are
Do not

required to properly set the ferrules, and damage to an inlet or

detector fitting is very costly to repair.

3 Push the tubing into the stainless steel plug (see

Figure 27).
4 Make sure that the front ferrule is touching the plug.
Slide the Swagelok nut over the ferrule and thread it onto
the plug.

70 Installation and First Startup

 Making Swagelok Connections A

Nut and ferrules

Plug or
fitting held Tubing
in vise

Figure 27 Assembling the fitting

5 Push the tube fully into the plug, then withdraw it

approximately 1 to 2 mm (see Figure 28).
6
Front Nut
ferrule
Insert
tubing fully

Back
ferrule

Withdraw tubing
1-2 mm

Tighten nut

Figure 28 Insert the tubing

7 Finger- tighten the nut.

8 Mark the nut with a pencil line (see Figure 29).

Installation and First Startup 71

A Making Swagelok Connections

Pencil line

Figure 29 Marking the fitting

9 For 1/8- inch Swagelok fittings, use a pair of wrenches to

tighten the fitting 3/4 of a turn (see Figure 30).

Figure 30 Final tightening

10 Remove the plug from the fitting. To connect the tubing,

with nut and ferrules, to another fitting, finger- tighten the
nut, then use a wrench to tighten it 3/4 (1/8- inch fittings)
of a turn.
11 Both correctly- and incorrectly- swaged connections are
shown in Figure 31. Note that the end of the tubing in a
correctly- swaged fitting is not crushed and does not
interfere with the action of the ferrules.

Figure 31 Completed fitting

72 Installation and First Startup

 Making Swagelok Connections A

Using a Swagelok Tee

To supply gas from a single source to more than one input,
use a Swagelok Tee.

Do not combine valve actuator air with flame ionization air. The valve
NOTE
action will cause major upsets in the detector signal.

Materials needed:
• 1/8- inch preconditioned copper tubing
• Tubing cutter
• 1/8- inch Swagelok nuts and front and back ferrules
• 1/8- inch Swagelok Tee
• Two 7/16- inch wrenches
• 1/8- inch Swagelok cap (optional)
1 Cut the tubing where you want to install the Tee. Connect
the tubing and Tee with a Swagelok fitting. See Figure 32.

Cap

Tee fitting

Nut and
ferrules

Figure 32 Swagelok tee

2 Measure the distance from the Tee to the instrument

fittings. Attach copper tubing to the open Tee ends with
Swagelok fittings.

Installation and First Startup 73

Agilent Technologies

© Agilent Technologies, Inc. 2014