G1888-90009 Headspace Sampler
G1888-90009 Headspace Sampler
G1888-90009 Headspace Sampler
Agilent Technologies
Notices
Agilent Technologies, Inc. 2004
Warranty
The material contained in this document is provided as is, and is subject to being changed, without notice,
in future editions. Further, to the maximum extent permitted by applicable
law, Agilent disclaims all warranties,
either express or implied, with regard
to this manual and any information
contained herein, including but not
limited to the implied warranties of
merchantability and fitness for a particular purpose. Agilent shall not be
liable for errors or for incidental or
consequential damages in connection with the furnishing, use, or performance of this document or of any
information contained herein. Should
Agilent and the user have a separate
written agreement with warranty
terms covering the material in this
document that conflict with these
terms, the warranty terms in the
separate agreement shall control.
Edition
First edition, March 2004
Printed in US
Agilent Technologies, Inc.
2850 Centerville Road
Wilmington, DE 19808-1610 USA
Acknowledgements
Swagelok is a registered trademark of the
Swagelok Company.
Microsoft and Windows are registered
trademarks of the Microsoft Corporation.
Safety Notices
CAU TI O N
A CAUTION notice denotes a hazard. It calls attention to an operating procedure, practice, or the like
that, if not correctly performed or
adhered to, could result in damage
to the product or loss of important
data. Do not proceed beyond a
CAUTION notice until the indicated
conditions are fully understood and
met.
WA RN ING
A WARNING notice denotes a
hazard. It calls attention to an
operating procedure, practice, or
the like that, if not correctly performed or adhered to, could result
in personal injury or death. Do not
proceed beyond a WARNING
notice until the indicated conditions are fully understood and
met.
Manual Overview
This manual contains four chapters and one appendix.
Introduction
This chapter gives an overview of the manual and contains
safety information.
Site Preparation
This chapter provides the requirements for preparing the site
before installing the Headspace Sampler. It covers the
requirements for temperature and humidity, space, power, gas,
and venting.
Installation
Installation describes how to install the Headspace Sampler. It
includes instructions for unpacking the unit, checking the
contents, connecting the power and gas supplies, making
connections to an integrator or Agilent data system, and
connecting the unit to a GC.
Contents
1
Introduction
About this Manual 10
Video supplements 10
Important Safety Warnings 11
Many internal parts of the instrument carry dangerous
voltages 11
Electrostatic discharge is a threat to instrument
electronics 11
Many parts are dangerously hot 12
Gases 12
General warnings 13
Safety and Regulatory Certifications 14
Information 14
Symbols 15
Electromagnetic compatibility 15
Sound Emission Certification for Federal Republic of
Germany 16
Fuses
Cleaning
17
17
17
Site Preparation
Introduction to Site Preparation
20
21
Space Requirements
22
Power Requirements 23
Line voltage 23
Power line cord 23
Gas Requirements
24
External Plumbing 25
Supply tubing 25
Regulators 25
Venting Requirements
Sampler Considerations
3
28
29
Installation
Installation
32
33
34
35
50
52
40
41
56
70
71
1
Introduction
About this Manual 10
Video supplements 10
Important Safety Warnings 11
Many internal parts of the instrument carry dangerous voltages 11
Electrostatic discharge is a threat to instrument electronics 11
Many parts are dangerously hot 12
Gases 12
General warnings 13
Safety and Regulatory Certifications 14
Information 14
Symbols 15
Electromagnetic compatibility 15
Sound Emission Certification for Federal Republic of Germany 16
Fuses 17
Cleaning 17
Recycling the Product 17
Agilent Technologies
Introduction
Video supplements
Click this icon when it appears throughout the manual to view
video supplements to certain procedures.
10
Introduction
WA RN ING
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 heated zones are turned off.
WA RN ING
11
Introduction
WA RN ING
Gases
Do not use flammable carrier gases.
Do not use hydrogen as a carrier gas in the Headspace
Sampler. Hydrogen creates a potential explosion hazard due
to the venting of gases during operation and standby.
Wear eye protection when using compressed gas to avoid eye
injury.
Fasten all compressed gas cylinders securely to an
immovable structure or permanent wall.
Store and handle compressed gases in accordance with
relevant safety codes.
Do not put gas cylinders in the path of a hot air vent
(including a GC oven exhaust).
12
Introduction
General warnings
Perform periodic leak checks on supply lines, fittings, and
pneumatic plumbing to prevent a potentially hazardous
condition.
To avoid a potential shock hazard when using liquid solution
to locate leaks, turn the main power switch off and
disconnect the main power cord. Be careful not to spill leak
solution on electrical leads.
13
Introduction
Information
The Agilent Technologies Headspace Sampler 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 Agilent
Headspace Sampler has been compromised, disconnect the unit
from all power sources and secure the unit against unintended
operation.
14
Introduction
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
customers failure to comply with these requirements.
Electromagnetic compatibility
This device complies with the requirements of CISPR 11.
Operation is subject to the following two conditions:
1 This device may not cause harmful interference.
2 This device must accept any interference received, including
interference that may cause undesired operation.
15
Introduction
Schalldruckpegel
Schalldruckpegel LP < 70 dB(A) nach DIN-EN 27779
(Typprufung).
16
Introduction
Fuses
Table 1 lists the fuses required for proper operation. These
fuses should only be accessed by Agilent service personnel.
Table 1
Fuses
Fuse designation
Location
F2, F3
F3
Terminal near
transformer
F3, F4
Power board
F1
Power board
Cleaning
To clean the unit, disconnect the power and wipe down with a
damp, lint-free cloth.
17
Introduction
18
2
Site Preparation
Introduction to Site Preparation 20
Temperature and Humidity Requirements 21
Performance range 21
Optimum performance 21
Space Requirements 22
Power Requirements 23
Line voltage 23
Power line cord 23
Gas Requirements 24
External Plumbing 25
Supply tubing 25
Regulators 25
Venting Requirements 28
Sampler Considerations 29
Agilent Technologies
19
Site Preparation
20
Site Preparation
Optimum performance
The optimum temperature and humidity are 20 C to 27 C
(58 F to 80 F) and 50% to 60% relative humidity (without
condensation).
21
Site Preparation
Space Requirements
The Headspace Sampler requires a laboratory bench with an
unobstructed surface approximately 64 cm (25 inches) deep by
46 cm (18.1 inches) wide and capable of supporting at least
30 kg (102 lb.).
The unit is approximately 56 cm (22 inches) high. The area
above it must be clear. Allow enough room to open the top lid of
the Headspace Sampler. Shelves or any overhanging
obstructions limit access to the top of the instrument and
interfere with cooling.
Other devices used with the Headspace Sampler (gas
chromatographs, detectors, integrators, or workstations) will
require additional bench space. See the manual for each
instrument for the applicable space requirements. Figure 1
shows instrument footprints for a sample installation.
PC Monitor
64 cm
Headspace
Sampler
6890 GC
PC Keyboard
46 cm
190 cm
Figure 1
22
Site Preparation
Power Requirements
Line voltage
The Headspace Sampler operates from one of these line voltage
supplies:
115 VAC single phase (90 VAC to 130 VAC), 50 to 60 Hz,
750 VA max
230 VAC single phase (198 VAC to 264 VAC), 50 to 60 Hz,
750 VA max
The Headspace Sampler is shipped with the voltage set to
230 VAC. The maximum power the Headspace Sampler can
accept is 750 VA. The recommended neutral to ground level is a
maximum of 3 VAC. The Headspace Sampler should have a
dedicated ground.
23
Site Preparation
Gas Requirements
The gas entering the Headspace Sampler becomes part of the
carrier gas for the GC column. It may come from a
pressure-regulated purified source (see Figure 3 on page 27) or
from the GC itself. A gas supply connection for vial
pressurization is also required. Gas at 550 kPa (80 psi) is
recommended.
We recommend instrument or chromatographic purity
grades specifically intended for chromatographic use. The gas
purities in Table 2 are recommended for optimal
chromatographic performance.
Table 2
WA RN ING
24
Gas
Purity
Helium
99.9995% pure
Nitrogen
99.9995% pure
Site Preparation
External Plumbing
Supply tubing
The Headspace Sampler ships with plumbing kits for both
electronic and manual pressure control (EPC and MPC,
respectively). The kits contain enough tubing to reach a gas
source 3 meters from the Headspace Sampler. Extra plumbing is
needed if the gas supply is not within 3 meters.
If extra plumbing is needed, use only preconditioned copper
tubing (part number 5180-4196) to supply gases to the
instrument. Ordinary copper tubing contains oils and
contaminants. Plastic tubing is permeable to oxygen and other
contaminants that can damage columns and detectors.
The required tube diameter depends on the distance from the
supply or source to the Headspace Sampler and the total flow
rate for the particular gas. Tubing of 1/8-inch od is adequate
when the supply is less than 3 meters (10 feet) away from the
instrument. Use 1/4-inch od tubing for longer distances.
Gas connection to the Headspace Sampler is made with 1/8-inch
Swagelok bulkhead fittings. Never use Teflon tape on
Swagelok-type fittings.
Do not use pipe dope or liquid thread sealant on any pipe
threads. Use only PTFE plumbing tape for these fittings.
Regulators
Two-stage regulators are recommended. Consult a local gas
supplier for the type and size of cylinder valve connections. If
possible, obtain Compressed Gas Association (CGA) numbers.
Suitable two-stage regulators are also available from Agilent.
If cylinders and regulators are stored outdoors where
temperature fluctuates, use an additional single-stage regulator
at the back of the instrument.
25
Site Preparation
Gas supply
source
Figure 2
550-830 kPa
80-120 psig
410-690 kPa
60-100 psig
Headspace
unit
Set regulators to deliver 410 to 690 kPa (60 to 100 psi) to the
instrument. Flow and pressure regulators require at least
140 kPa (20 psi) pressure drop across them to maintain
regulation. See Table 3 for the correct regulator to use with each
outlet fitting.
Table 3
26
346
5183-4641
540
5183-4643
580
5183-4644
590
5183-4645
Site Preparation
On/Off valve
Moisture trap
Hydrocarbon trap
To Headspace
Sampler
Oxygen trap
Gas supply
Figure 3
27
Site Preparation
Venting Requirements
During normal operation, some of the vial headspace gas is
vented to the outside of the Headspace Sampler. If the
components of this gas are expected to be toxic or noxious,
place the unit within a fume hood or attach a vent system, at
atmospheric pressure, to the port on the sampler unit. Use a
1/8-inch Swagelok fitting for the connection. See Figure 4 for
the location of the vent line.
Vent line
Figure 4
28
Site Preparation
Sampler Considerations
One or more optional parts and kits may be required for the
installation, depending on the intended use.
The Headspace Sampler ships with a deactivated flowpath
and a 1-mL sample loop. A 3-mL sample loop (part number
2321700004) can be ordered separately.
To enable software method control of the Headspace Sampler
flows and pressures, an Agilent 6890 or Agilent 6850 GC
must have an auxiliary electronic pressure control (EPC)
module. Order kit G1888-60705. The kit contains the EPC
module, the bleeder weldment, and the interface kit.
To splice the transfer line into the inlet, order the Manual
Pressure Control Interface Kit G1290-60515.
There is an optional wire support for the transfer line for use
on an Agilent 6890 GC. Order Transfer Line Support Kit
G2319-60600.
29
Site Preparation
30
3
Installation
Installation 32
Unpack the Unit and Check the Contents 33
Place the Unit in Position 34
Connect the Power Cord 35
Connect the Plumbing and Transfer Line 37
Flow modes 37
Typical installation procedures 39
Set the flow mode on the Headspace Sampler 40
Connect on/off valves to the gas input fittings 41
MPC connections 42
EPC connections 46
Connect the control cables 50
Set communication options 52
Control Setup 50
Agilent Technologies
31
Installation
Installation
CAU TI O N
32
Installation
33
Installation
CAU TI O N
Release tab
Figure 5
34
Installation
Voltage selector
Fuses
Figure 6
Power connection
35
Installation
Shutter:
OK
Tray
OK
Carousel
OK
Oven Sensor
OK
Loop Sensor
OK
Figure 7
DIAGNOSTIC
SELF TEST
NOT READY
Self-test screen
36
Installation
Figure 8
37
Installation
EPC connections
Direct connection to a split/splitless inlet The sampler is
inserted between the inlet flow module and the inlet, allowing
real method control, via the GC, of flows and pressures for
consistent results between setups. The system is easy to
duplicate and monitor but requires time to convert back to
normal inlet injection for nonheadspace samples.
Direct connection to a volatiles interface The transfer line from
the sampler is connected to the volatiles interface. See the
6890 GCs user information for instructions.
MPC connections
Needle connection to a split/splitless inlet The transfer line
from the sampler ends in a needle (part no. 2322590005) that is
inserted through the inlet septum. Conversion to normal
injection is rapid and simple.
Needle connection to a cool on-column inlet The transfer line
from the sampler ends in a small od needle (part no.
2322590004) that is inserted through the inlet septum.
38
Installation
Alternative installations
To install the Headspace Sampler on a 4890D or 5890 Series II
GC, contact Agilent Service.
39
Installation
MPC
EPC
Carrier gas
Figure 9
40
Installation
For EPC
For MPC
Carrier gas in
Vial pressurization gas in
On/Off valves
for leak testing
Figure 10
41
Installation
MPC connections
Carrier gas and vial pressurization gas connections
If both the carrier gas and vial pressurization gas are MPC,
Install a T-fitting to the on/off valves. Run a line from a
pressure-regulated gas source to the T-fitting as shown in
Figure 11.
To pressure
regulated
gas source
Carrier gas in
Vial pressure
T-fitting
On/Off valves
Figure 11
42
Installation
43
Installation
Top of inlet
Figure 12
44
Installation
6 Insert the tip of the needle into the inlet. Force the septum (it
is oversized) into the recess in the top of the inlet. See
Figure 13 for the assembled view.
Figure 13
45
Installation
EPC connections
Connect the vial pressurization gas for an EPC setup
An Auxiliary gas channel in the GC supplies vial pressurization
gas. The following steps describe installation for a 6890 GC with
EPC control of headspace. The installation procedure is similar
for a 6850 GC.
1 If the GC does not have an Auxiliary EPC module, install the
G1940A Headspace Interface Kit. Follow the instructions
provided with that kit.
2 Install the external sampler interface kit (part no.
G1888-60705) into the GC. Follow the procedure for
installing onto a back-pressure regulated system.
3 Locate the block on the Auxiliary EPC module that connects
the three gas outlet tubes for the auxiliary channels to the
pneumatics module.
4 Remove the screw that holds the block to the pneumatics
module. Pull the block free of the module and rotate it so that
the frits are on top. See Figure 14.
Frits
Aux 4
Aux 3
Aux 5
Aux 3
Outputs
Aux 4
Aux 5
Figure 14
46
Installation
Headspace Sampler
Vial pressure fitting
Bleed weldment
Brass end
Figure 15
47
Installation
Figure 16
48
Installation
ZDV union
Carrier line
Ferrule
Nut
Figure 17
Transfer line
ZDV union
Figure 18
7 Use the other ZDV union to connect the free end of the
carrier gas line to the length of tubing provided in the
shipping kit. Route the tubing out the back of the GC to the
rear panel of the sampler.
8 Connect the tubing to the CARRIER fitting on the sampler.
49
Installation
Control Setup
Connect the control cables
Connect the remote start/stop cable to the back of the sampler.
Be sure to connect the spade lug to the ground screw. Connect
the free end of the cable to the GC.
Depending on the setup, other cable connections may be
needed. Refer to Table 4 for an overview of cable connections
used with the Headspace Samplers.
Table 4
Sampler port
Connect to
Part number
LAN*
Hub*
8121-0940
Remote
G1530-60930
APG Y-cable
G1530-61200
Serial (RS-232)
PC
G1530-60600
Remote
35900-60700
50
Installation
Cables
1.
2.
3.
1
1
Workstation
Hub or switch
Printer
6890N
1
1
G1530-61200, 2-m
APG Y-cable, two
9-pin male, one
9-pin female
Workstation
Hub or switch
BNC
BNC
4.
G1888A
Local Talk
8121-1013,
USB-DB9 RS-232
adapter cable
Local Talk
5.
Printer
G1888A
5
6850
Workstation
Printer
G1888A
6820
1
1
1
1
Workstation
Hub or switch
Printer
G1888A
Figure 19
5973N
6890N
51
Installation
LAN settings
If the Headspace Sampler is connected to a LAN, set the IP
Address, subnet mask, and gateway using the Advanced
Functions menu.
1 Press the Menu key.
2 Scroll down to Advanced Functions. Press Enter.
3 Scroll down to LAN Config. and press Enter or
press . followed by 4 on the numeric keypad.
4 The LAN Config. screen is shown in Figure 20. Use the cursor
and keypad to enter new values. Press Enter to set the value.
SET
IP Address
10 .1 .1 .105
Sub Mask
Gateway
10 .1 .1 .1
Figure 20
LAN Config.
Running
52
Installation
ADV. FUNCTION
No
Figure 21
53
Installation
ADV. FUNCTION
No
Figure 22
54
4
Running Checkout Samples
Running Checkout Samples 56
Prepare the checkout sample 56
Run the sample 57
6850/6890 GC checkout method 58
Agilent Technologies
55
1. Grasp
Figure 23
2. Fill
3. Wipe
Filling a pipette
56
NO TE
57
Electronic flow
meter
Split vent
68
GC50 S
S y e ri e
s te s
m
Figure 24
6850 GC shown
The electronic flow meter connected
58
DIAGNOSTIC
STORED METH.
Default
Checkout
OQ/PV
READY
MeOH in H2O
Figure 25
Headspace method
Oven temperature
100 C
Valve temperature
110 C
115 C
Loop volume
1 mL
Vial pressure
GC cycle time
5.5 min
7.0 min
Pressurization time
0.08 min
59
Table 5
Headspace method
60
0.5 min
0.05 min
Injection time
1.0 min
Table 6
GC oven settings
Oven
Initial temperature
100 C
Initial time
4.00 min
Rate
0 (Off)
Maximum temperature
300 C
Equilibration time
1.00 min
Run time
4.00 min
Table 7
Inlet settings
Mode
Split
Initial temperature
250 C (On)
Pressure
Split ratio
20:1 (G1289)
Split flow
80 mL/min (G1289)
Total flow
87 mL/min (G1289)
Gas saver
Off
Gas type
Helium
Liner
5181-8818
61
Table 8
Column settings
Column
62
Model number
Maximum temperature
325 C
Length
30 m
Diameter
320 m
Film thickness
0.25 m
Mode
Constant flow
Initial flow
4.0 mL/min
Initial pressure
19.5 psi
Average velocity
60 cm/s
Outlet pressure
Ambient
Table 9
Detector
parameters
FID
NPD
Temperature
300 C
300 C
Hydrogen flow
30 mL/min
2.0 mL/min
Air flow
400 mL/min
60 mL/min
Constant makeup
Mode
Constant makeup
Constant
makeup
30 mL/min
Makeup flow
25 mL/min
8 mL/min
Nitrogen or
argon/methane
Makeup gas
type
Nitrogen or helium
Nitrogen or
helium
Flame
On
Electrometer
On
Lit offset
2.0
ECD
On
On
Adjust offset
30
Bead
On
Equilibration
time
63
Table 10
Solvent delay
3 min
Run time
6.5 min
7 min
Scan range
45 to 300
Method used
Atune file
Inlet pressure
12 psi
Column flow
Split ratio
80:1
Injector
External device
64
Gas type
Helium
Initial pressure
15 psi (On)
Initial time
0 min
Rate
0 (Off)
Table 12
Checkout sample
Checkout sample
Headspace OQ/PV Standard
Part number
5182-9733
Size
2.037
Type
pA
160
2.476
0.880
FID1 A, (HS_ECD\HSVI0004.D)
Ethanol
Nitrobenzene
2.825
140
120
Dichlorobenzene
t-Butyl disulfide
100
80
60
0.858
40
20
0.0
Figure 26
0.5
1.0
1.5
2.0
2.5
3.0
3.5
4.0
min
65
2.384
NPD1 B, (HS_NPD\HSNPD002.D)
pA
Nitrobenzene
250
200
150
100
Ethanol
50
0.0
Figure 27
66
0.5
1.0
1.5
2.0
2.5
3.0
3.5
min
ECD1 A, (HS_ECD\HSEC0000.D)
Hz
2.021
Dichlorobenzene
120000
2.461
100000
80000
60000
0.850
2.810
Ethanol
40000
20000
0
0
Figure 28
min
67
Dichlorobenzene
1000000
TIC: 0201002.D
Abundance
800000
600000
Nitrobenzene
t-Butyl disulfide
400000
200000
0
3.20
3.60
4.00
4.40
4.80
5.20
5.60
6.00
6.40
Time
Figure 29
68
A
Connecting a Swagelok Fitting
Preparation 70
Procedure 71
Agilent Technologies
69
Preparation
Objective
To make a leak-free tubing connection 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
70
Procedure
1 Place a Swagelok nut, back ferrule, and front ferrule to the
tubing as shown in Figure 30.
Front ferrule
Back ferrule
IMPORTANT!
The narrow end of the back
ferrule fits into the rear of
the front ferrule.
Nut
Tubing
Figure 30
CAU TI O N
Do not
3 Push the tubing into the stainless steel plug (Figure 31).
4 Make sure that the front ferrule is touching the plug. Slide
the Swagelok nut over the ferrule and thread it onto the plug.
Nut and ferrules
Plug or fitting
held in a vise
Figure 31
Tubing
71
Nut
Front
ferrule
Tighten nut
Figure 32
Pencil line
Figure 33
Figure 34
Final tightening
8 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 of a turn (1/8-inch
fittings) or 1-1/4 of a turn (1/4-inch fittings).
9 A correctly-swaged connection is shown in Figure 35. 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 35
Completed fitting
73
Agilent Technologies