HP 5890 II Plus, 5890 II User Manual

Reference Manual
HP 5890 Series II and HP 5890 Series II Plus
D
All Rights Reserved. Reproduction, adaptation, or translation without permission is prohibited, except as allowed under the copyright laws.
HP part number 05890-90271
First edition—Jun 1989
Printed In U.S.A. Second edition—Oct 1989 Printed In U.S.A. Third edition—Jan 1990 Printed In U.S.A. Fourth edition—Oct 1990 Printed In U.S.A. Fifth edition—Oct 1991 Printed In U.S.A. Fifth edition—Mar 1993 Printed In U.S.A. Sixth edition—Jul 1994 Printed In U.S.A.
Printed in USA
Warranty The information contained
in this document is subject to change without notice.
Hewlett-Packard makes no warranty of any kind with regard to this material, including, but not limited to, the implied warranties of merchantability and fitness for a particular purpose. Hewlett-Packard shall not be liable for errors contained herein or for incidental or consequential damages in connection with the furnishing, performance, or use of this material.
Safety Information The HP 5890 Series II and
HP 5890 Series II Plus are IEC (International Electrotechnical Commission) Safety Class 1 instruments. This unit has been designed and tested in accordance with recognized safety standards. Whenever the safety protection of the HP 5890 Series II has been compromised, disconnect the unit from all power sources and secure the unit against unintended operation.
Safety Symbols This manual contains
safety information that should be followed by the user to ensure safe operation.
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.
Important User Information for In Vitro Diagnostic Applications
This is a multipurpose product that may be used for qualitative or quantitative analyses in many applications. If used in conjunction with proven procedures (methodology) by qualifiedoperator, one of these applications may be In Vitro Diagnostic Procedures.
Generalized instrument performance characteristics and instructions are included in this manual. Specific In Vitro Diagnostic procedures and methodology remain the choice and the responsibility of the user, and are not included.
Sound Emission Certification for Federal Republic of Germany
If Test and Measurement Equipment is operated with unscreened cables and/or used for measurements in open set-ups, users have to assure that under these operating conditions the Radio Interference Limits are still met at the border of their premises.
The following information is provided to comply with the requirements of the German Sound Emission Directive dated January 18, 1991
Sound pressure Lp < 70db(A)
During normal operation At the operator position According to ISO 7779
(Type Test) When operating the HP
5890 Series II with cryo valve option, the sound pressure cryo valve operation for short burst pulses.
78 db(A) during
Schallemission Werden Meß- und
Testgeräte mit ungeschirmten Kabeln und/oder in offenen Meßaufbauten verwendet, so ist vom Betreiber sicherzustellen, daß die Funk-Entströbedingungen unter Betriebsbedingungen an seiner Grundstücksgrenze eingehalten werden.
Diese Information steht im Zusammenhang mit den Anforderungen der Maschinenl
sverordnung vom 18 Januar 1991.
Schalldruckpegel LP < 70 dB(A)
Am Arbeitsplatz Normaler Betrieb Nach DIN 45635 T. 19
(Typpr Bei Betrieb des HP 5890
Serie II mit Cryo Ventil Option treten beim Oeffnen des Ventils impulsfoermig Schalldrucke Lp bis ca. 78 dB(A) auf.
ärminformation
üfung)
Little Falls Site

Contents

Chapter 1 — Columns and Fittings 9.................
Column oven 11..........................................................
Column placement 12.................................................
Packed column 12....................................................
Hewlett•Packardcapillary columns 13..................................
Fittings 14...............................................................
Liners/adapters and inserts, general 17....................................
Inlet/detector liners/adapters 20...........................................
Packed column inlet liners 20..........................................
Detector liners/adapters 22............................................
ECD and TCD adapters 23............................................
Liner/adapter installation 24..........................................
Inlet inserts 25...........................................................
Packed column inlet inserts 25.........................................
Split/splitlessor split•onlycapillary inlet inserts 27......................
Jet replacement, FIDs or NPDs 30.........................................
Metal capillary columns 30................................................
Chapter 2 — Keyboard and Displays 31...............
Displaying setpoints 33...................................................
Entering setpoints 34.....................................................
Keyboard operation, INET control 37......................................
Protecting setpoints 38...................................................
Loading default setpoints 39..............................................
Chapter 3 — Temperature Control 43.................
Valid setpoint ranges 46..................................................
Cryogenic (sub•ambient)oven control 47...................................
Programming oven temperature 49........................................
Oven status 50...........................................................
Oven safety 51...........................................................
Fault: messages 52.......................................................
After a power failure . . . 53...............................................
Oven temperature calibration 54..........................................
Contents
Chapter 4 — Electronic Flow Sensing 57...............
Displaying gas flow rate 58...............................................
Designating gas type 59..................................................
Electronic flow sensor (EFS) calibration 60.................................
Preparation 61.......................................................
Setting the zero calibration value 61...................................
Setting the GAIN calibration value 63..................................
Entering specific ZERO and GAIN values 65............................
Chapter 5 — Signal Output 67........................
Zeroing signal output 68..................................................
Displaying current setpoint 69........................................
Self• setpoint 70......................................................
User•defined setpoint 72..............................................
Signal attenuation 72.....................................................
Displaying current
RANGE 2!()
Entering / setpoints 76..............................................
Switching off the +1 mV output 76.....................................
Test signal output 77.....................................................
Instrument network (INET) 79............................................
The controller 79.....................................................
An instrument 81.....................................................
Active workspace 82..................................................
HP 5890 INET states 82...............................................
INET operation 83....................................................
Automatic INET reconfiguration 85....................................
INET configuration 85....................................................
Switching between Global and Local 86.................................
INET/HP•ILaddresses 87.............................................
HP•ILloopback test 90...................................................
Warn: and fault: messages 92.............................................
File compatibility with data handling devices 94............................
What are the modes? 94...............................................
What is the proper mode for my data handling device? 94................
How do I know in which mode my GC is configured now? 94..............
How do I change modes? 95............................................
How to convert HP 339X Integrator workfiles from 5890A
to SERIES II mode: 97.............................................
ATTN 2!()
/
setpoints 75..............
Contents
Chapter 6 — Inlet Systems 99.........................
Packed column inlet 100...................................................
Electronic flow sensor 102..............................................
Septum•purgedpacked column inlet 103.................................
Problems at high inlet temperatures 104.................................
A thermally optimized high•temperatureinlet 104........................
Septum purge 105.....................................................
Electronic flow sensor 106..............................................
Split/splitlesscapillary inlet 107............................................
Carrier gas considerations 108..........................................
Initial column head pressure 110........................................
Split sampling 111.....................................................
Splitless sampling 114.................................................
Injection technique, split/splitless sampling 121..........................
Chapter 7 — Detector Systems 123.....................
Capillary makeup gas flow rate 124.........................................
FID and NPD jets 125.....................................................
Flame ionization detector (FID) 126.........................................
FID flameout problems 128.............................................
Nitrogen•phosphorusdetector (NPD) 129....................................
Performance considerations 132.........................................
Electron capture detector (ECD) 135........................................
Requirements for USA owners 135......................................
Temperature 140......................................................
Background level 141..................................................
Thermal conductivity detector (TCD) 143....................................
Optimizing performance 146............................................
Analyzing for hydrogen, special considerations 148.......................
TCD•to•FIDseries connection 149.......................................
Filament passivation 149...............................................
Capillary column considerations 150....................................
Flame photometric detector (FPD) 151......................................
Optimizing FPD sensitivity and selectivity 151...........................
Flame ignition problems 153............................................
Contents
Chapter 8 — Preventive Maintenance 155..............
Conditioning columns 156..................................................
(Re)Packing columns 158..................................................
Packed column inlet 159...................................................
Changing septa 159....................................................
Insert/liner care 160...................................................
Leaks 160.............................................................
Cleaning 162..........................................................
Split/splitlesscapillary inlets 163...........................................
Changing septa 163....................................................
Insert care 164........................................................
Leaks 165.............................................................
Cleaning 168..........................................................
Liner and/or insert care 169................................................
Glass inserts 169......................................................
Repacking a split insert 170............................................
Metal inserts and/or liners 171..........................................
Flame ionization detector (FID) 171.........................................
Jet exchange/replacement 172..........................................
Cleaning 173..........................................................
Ignition problems 177..................................................
Nitrogen•phosphorusdetector (NPD) 178....................................
Cleaning 178..........................................................
Removing/replacing the NPD collector 181...............................
Type B NPD transformer/collector assembly 184..........................
Reinstallation 186.....................................................
Electron capture detector (ECD) 188........................................
Frequency test 188....................................................
Carrier gas evaluation 188.............................................
Leaks 189.............................................................
Thermal cleaning 190..................................................
Packed column: 191....................................................
Capillary column: 191..................................................
Radioactivity leak test (wipe test) 192...................................
Thermal conductivity detector (TCD) 192....................................
Cleaning 192..........................................................
Flame photometric detector 193............................................
Cleaning/replacing FPD windows, filters, seals 193.......................
Cleaning/replacing the FPD jet 197.....................................
FPD leak testing (GC with electronic flow sensor) 198....................
FPD leak testing (GC without electronic flow sensor) 199.................
Conditioning chemical traps 200............................................
Contents
Chapter 9 — Chromatographic Troubleshooting 201......
Introduction 202..........................................................
Baseline symptoms 202....................................................
Position 202...........................................................
Wander and drift 203..................................................
Noise 204.............................................................
Spiking 206...........................................................
Retention time symptoms 207..............................................
Retention time drift 207................................................
Retention time wander (reproducibility) 207.............................
Peak symptoms 209.......................................................
No peaks 209..........................................................
Inverted peaks 209....................................................
Extra peaks 209.......................................................
Deformed peaks 211...................................................
Troubleshooting valve systems 214..........................................
Chromatographic symptoms 214........................................
Locating leaks 216........................................................
Pressure check 217........................................................
Electronic pressure control 218.............................................
Safety shutdown 219...................................................
Proper configuration 220...............................................
Switch setting examples 221............................................
Chapter 10 — Test Sample Chromatograms 223........
Test sample chromatograms 225............................................
Index 241.............................................
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1

Columns and Fittings

Columns and Fittings
The HP 5890 SERIES II (hereafter referred to as HP 5890) provides flexibility in choices among inlets, columns, and detectors through use of liners and adapters, allowing any standard column to be used without sacrificing performance. Additionalflexibility is gained through positions of inlets and detectors relative to each other and through the large internal volume of the oven.
This section provides information for the following:
C
The column oven.
C
Fittings.
C
Liners and inserts.
C
ECD and TCD capillary makeup gas adapters.
The first three items must be considered before a column may be installed properly at either an inlet or a detector. In addition, for an FID or NPD, and depending upon the column to be installed (packed versus capillary), the correct jet must be installed before installing the column. Jet installation is described in Chapter 8, Preventive Maintenance.
10
For specific information on ordering fittings, liners, and inserts, see
Hewlett•Packard's analytical supplies catalog.
Columns and Fittings

Column oven

Column oven
Figure 1-1
Inlet Ftg
Nut Plate
The Column Oven
The oven door latch, located beneath the lower right corner of the door, is pressed upward to open the door.
Motor•drivenflapsat the rear of the oven admit room air for cool down or
near•ambientoperation, so the door is kept closed except for access to columns (the oven cools most efficiently with its door closed).
Det Ftg
The oven can maintain temperature down to about 7
^
C above ambient without auxiliary cooling. If lower temperatures are required, a cryogenic valve (for either liquid CO
1
or liquid N1) is needed. Liquid CO permits reliable temperature control down to -50^C; liquid N1provides reliable control down to -80 450
^
C.
^
C. The maximum oven temperature is
1
11
Columns and Fittings
Column oven

Column placement

Generally, a column may be installed between any inlet and detector. A rigid1/4•inchpacked glass column, however, if installed in the B
(rear•most)inlet, can only be installed in the B (rear•most)detector. Distance relationships among inlets and detectors are shown in Figure 1•2.
Figure 1-2
Top View
(showing relationshipof inlets to detectors)
B
A
Front
Installation Restrictions, Rigid Columns
1mm
228 +
B
A
12

Packed column

Packed columns require no physical support other than that provided by proper installation at inlet and detector fittings.
Columns and Fittings
Column oven

Hewlett-Packard capillary columns

Hewlett•Packardcapillary columns are wound on wire frames which mount on a pair of brackets which slip into slots at the top of the oven interior.
Figure 1-3
Typical Hewlett-Packard Capillary Columns
13
Columns and Fittings

Fittings

Figure 1-4.
Column Hanger
Part No. 1460-1914
Installed Bracket for Hewlett-Packard Capillary Columns
Column Installed
The bracket has two positions from which to hang the column wire frame. Depending upon frame diameter, use the position which best centers the column in the oven. Column ends should come off the bottom of the frame, making smooth curves to inlet and detector fittings. Avoid allowing any section of the column itself to come in contact with oven interior surfaces.
Fittings
The following is a brief comparison of common types of fittings (nuts, ferrules, O•rings)used to install columns, and to install inlet and detector
liners and/or inserts. Each type has its own set of advantages and disadvantages:
14
Columns and Fittings
Fittings
C
C
C
Graphite O•ringsor ferrules have excellent sealing quality and long service life, can be used continuously to 400
^
C, and are generally recommended for most applications, particularly capillary and glass columns. They are also recommended for inlet and detector liners, and for split/splitlesscapillary inlet inserts.
Since they do not adhere permanently to glass or metal, they can be removed easily without damage to the column, tubing, liner, or insert. A rear metal ferrule may be needed if recommended by the manufacturer.
Commonly used with metal columns and tubing, brass nuts and ferrules on the column prevent damage to inlet and detector liners, but may develop leaks above 250
^
C or with temperature
programming. Also commonly used with metal columns and tubing, stainless steel
fittings minimize possibility of leakage at high temperature, but require care in installing columns; overtightening may damage the column end or inlet/detector fitting.
C
Teflon ferrules may be used to 250^C but are recommended only for isothermal work, because they develop leaks when temperature•programmed.
C
Commonly used with glass columns, Vespel (or graphite•filledVespel) ferrules are reusable and work well to 350
^
C. These ferrules may
leak or crack if tightened when cold.
C
Glass columns can be installed using silicone O•rings. For O•ring installation, a back metal ferrule, reversed, is necessary to provide a flat surface to seal against.
Silicone O•ringsare useful to about 250
^
C, but, due to bleed, interfere in high•sensitivitywork. They also gradually lose elasticity and crack, so they must be replaced fairly often.
15
Columns and Fittings
Fittings
Table 1-1. Typical Fittings for Columns and Inlet/Detector Liners, Adapters, and Inserts
Type Description Typical Use Part No.
1/4-inch swage, nut 1/4-inch packed metal columns 5080-8753 stainless steel, front ferrule pkg, 20 of each back ferrule
1/8-inch swage, nut 1/8-inch packed metal columns 5080-8751 stainless steel, front ferrule pkg, 20 of each back ferrule
1/4-inch swage, nut 1/4-inch packed metal columns 5080-8752 brass, pkg, front ferrule 20 of each back ferrule
1/8-inch swage, nut 1/8-inch packed metal columns 5080-8750 brass, pkg, front ferrule 20 of each back ferrule
Vespel, 1/4-inch ferrule inlet/detector liners, 5080-8774 pkg of 10 1/4-inch glass packed columns
Vespel, 1/8-inch ferrule metal columns 0100-1107 pkg of 10
graphite, 1.0-mm ferrule capillary columns 5080-8773 pkg of 10
graphite, 0.5-mm ferrule capillary columns 5080-8853 pkg of 10
graphite 6.35-mm O-ring inlet/detector liners, 0905-0767
1/4-inch glass packedcolumns,
split capillary inlet insert graphite 6.52-mm O-ring splitless capillary inlet insert (use) 0905-1004 silicone 6.0-mm O-ring inlet/detector liners 0905-0322
1/4-inch glass packedcolumns,
split/splitless capillaryinlet inserts silicone 1.0 mm O-ring capillary columns 0905-0759 Note: Dimensions given are id’s of the O-ring or ferrule.
16
Columns and Fittings

Liners/adapters and inserts, general

Liners/adapters and inserts, general
A liner/adapter is installed from below, inside the oven; it serves both as an adapter to mate the particular column to the inlet or detector and to provide correct internal volume for proper operation.
Inserts are used with inlets only, and, when required, are installed from above, at the top of the inlet; these are discussed specificallylater in this section (see Inlet inserts).
In general, the analysis to be performed determines the column to be used. The column then dictates hardware required for the inlet and detector (liner, insert, adapter, jet (FID or NPD)).
Note:
C
A correctly designed 1/4•inchpacked glass column requires no liners since the column ends themselves serve this purpose.
C
The appropriate liner/adapter, and insert if required, must be installed prior to installing a column.
Tables 1•2and 1•3summarize hardware required for various combinations of inlets, columns, and detectors.
17
Columns and Fittings
Liners/adapters and inserts, general
Table 1-2. Hardware and Recommended Fittings for Packed Column Installation
Packed Columns
1/8-inch Metal 1/4-inch Metal 1/4-inch Glass
Recommended 1/8-inch 1/4-inch 1/4-inch swage- Column Fittings swage-type nut swage-type nut type nut and
and ferrules
3
and ferrules
3
graphic ferrule or silicone O-ring(s)
Packed Column 19243-80510
1
19243-80520
1
Inlet Liners or or
19243-80530
1
19243-80540
1
(requires glass insert) (requires glass insert)
FID/NPD
2
19231-80521
1
19231-80530
1
Liners/Adapters
TCD Liners/Adapters None 19302-80020
ECD Liner/Adapters 19301-80530
1
Use 1/4-inch swage-typenut and Vespel or graphite ferrule to install liner/adapter.
2
See Chapter8 for details regardingjet exchange(if necessary).
3
See information later in this chapter regarding proper installation of swage-type fittingson packed metal columns.
1
None None
1
None
None
19302-80020 (may require altering the column)
1
18
Columns and Fittings
Liners/adapters and inserts, general
Table 1-3. Hardware and Recommended Fittings for Capillary Column Installation
Capillary Columns
HP Series 530
¿
320¿m ID 200¿m ID Metal/
Glass
Recommended Capillary column Capillary column Same as 320¿m Same as Column Fittings nut and 1.0-mm nut and 0.5-mm HP Series
graphite ferrule, or graphite or 530
¿
silicone O-ring(s) silicone O-ring(s)
Packed Column 19244-80540
1
Not Not Not
Inlet Liners (requires glass Recommended Recommended Recom-
insert) mended
Split/Splitless & 18740-60840 Same Same Same Split-Only with graphiteor Capillary Inlet silicone O-ring Split Sampling
Split/Splitless 18740-80220 Same Same Same Capillary Inlet with graphite or Insert: Splitless silicone O-ring Sampling
Programmable 19245-20580
3
19245-20520 19245-20510 19245-
On-Column 20550 Capillary Inlet Insert
FID/NPD
2
19244-80550
1
Same Same Same
Liners/Adapters TCD 18740-20950 19232-80550
1
Same Same
Liners/Adapters and
18740-20960
ECD 19244-805501,
3
3
19233-80530 Same Same
Liners/Adapters
1
Use 1/4-inch swage-typenut (if a nut is notsuppliedas part ofthe adapter) and graphite or Vespel ferrule to install liner/adapter.
2
0.11-inch jet must beused; see Chapter8 for informationregarding jet exchange (if necessary).
3
Use only if detector is not configured with capillary makeupgas adapter. If makeup adapter is provided,it is used instead (usually with makeup gas turnedoff).
19
Columns and Fittings

Inlet/detector liners/adapters

Inlet/detector liners/adapters
Interchangeable stainless steel liners/adapters, installed from inside the oven, are used with the packed column inlet, and with all detectors, depending upon the column to be installed.

Packed column inlet liners

Figure 1-5
20
Liner
Installed Liner, Packed Column Inlet
Liners for the packed column inlet are available in three sizes: one for
1/8•inchcolumns, one for 1/4•inchcolumns, and one for HP Series 530
capillary columns.
¿
Columns and Fittings
Inlet/detector liners/adapters
In addition, liners for the packed column inlet are available to accept glass inserts (discussed later) for reduced reactivity, to trap nonvolatile residues, or for use with an HP Series 530
C
No liner is used with 1/4•inchpacked glass columns. The long leg of the column fits into the inlet body, replacing the liner. Packing and glass wool plug must be below the tip of the needle for best results.
C
Metal columns are installed with a liner appropriate for the column diameter.
C
If necessary, glass columns can be installed using a metal liner (preferably those accepting a glass insert), but this is not recommended. There may be problems with dead volume in connections, and preventing contact of sample with metal surfaces.
¿
capillary column.
21
Columns and Fittings
Inlet/detector liners/adapters

Detector liners/adapters

Figure 1-6
Liner/Adapter
22
Typical Installed Detector Liner/Adapter
Detectors require a liner/adapter to be installed when used with packed metal columns (either 1/8•or 1/4•inch),and with any type of capillary
column. Normally, no liner is required with 1/4•inchpacked glass columns, since the leg of the column itself serves as the liner.
For the FID or NPD, the correct detector jet must be installed prior to installation of the liner. (If jets must be exchanged, see Chapter 8, Preventive Maintenance.)
Columns and Fittings
Inlet/detector liners/adapters

ECD and TCD adapters

A makeup gas adapter must be installed in the ECD or TCD base to install a capillary column, and to augment carrier flow through the column with additional gas flow needed for optimal detector operation. The adapter must be removed for packed column applications.
In addition, to install an HP Series 530
¿
capillary column in an ECD or TCD having no capillary makeup gas adapter, the following adapters are used: Part No. 19244•80550for the ECD, and Part No. 18740•20950and
18740•20960for the TCD. Finally, to use a 1/4•inchcolumn with the TCD (having a base designed
for 1/8•inchcolumns), a 1/8•to 1/4•inchadapter is required (Part No. 19302•80020). For the ECD (having a base designed for 1/4•inch columns), to use a 1/8•inchcolumn, a 1/4•to 1/8•inchadapter is required (Part No. 19301•80530).
23
Columns and Fittings
Inlet/detector liners/adapters

Liner/adapter installation

Figure 1-7
Liner
1/4-inch Ferrule
Liner Retainer Nut
Capillary Column Nut
WARNING
Packed Column Inlet Liner for HP Series 530 Capillary Column Use
Nut and Ferrule Installed on a Liner/Adapter
¿
1-mm Graphite Ferrule
With one exception, liners/adapters are installed in the same manner; if the liner/adapter has not been used before, a new ferrule must be installed.
¿
The single exception is the adapter to install an HP Series 530
capillary
column in a TCD without provision for capillary makeup gas (Part No.
18740•20950and 18740•20960). In this case, no ferrule is required to form a seal with the detector base.
Note: A graphite ferrule is strongly recommended; since metal ferrules tend to lock permanently onto the liner/adapter, their use may require replacing the entire liner/adapter, should a permanent leak develop.
Exercise care! The oven, and/or inlet or detector fittings may be hot enough to cause burns.
24
Note: The liner/adapter must be kept as clean as possible to prevent introducing contamination into the inlet or detector. Use a clean, lint•freecloth to remove fingerprints, etc., from the end of the liner/adapter to be inserted into the inlet or detector base. CH
2
OH
(methanol) may be used as a solvent.
Columns and Fittings

Inlet inserts

1. Assemble a brass nut and graphite ferrule onto the liner/adapter.
2. Insert the liner/adapter straight into the detector base as far as
3. Holding the liner/adapter in this position, tighten the nut finger•tight.
4. Use a wrench to tighten the nut an additional 1/4 turn.
5. Install the column; then heat the oven, inlet, and detector to desired
Inlet inserts
Inserts are used in inlets, and can be installed from the top of the particular inlet.

Packed column inlet inserts

possible.
operating temperatures and, only if necessary to stop leaks, tighten fittings further.
Figure 1-8
Flared End
Glass Insert for Packed Column Inlet Liner
Assuming the correct inlet liner is installed, a glass insert is installed as described on the next page.
25
Columns and Fittings
Inlet inserts
WARNING
Figure 1-9
Exercise care! the oven, and/or inlet, or detector fittings may be hot enough to cause burns.
Flared End
Insert
26
Installing a Glass Insert in a Packed Column Inlet
1. In handling the insert, avoid contaminating its surface (particularly
its interior).
2. Remove the septum retainer nut and septum.
3. Carefully remove the old insert (if present) by withdrawing it straight
up. A match stick or similar fibrous item may be used as an aid in lifting the insert from the inlet.
4. Install the new insert by dropping it carefully, straight into the inlet
liner, flared end up.
Columns and Fittings
Inlet inserts
Note: For the liner and insert for an HP Series 530¿capillary column, if the column is already installed, a new insert may not seat properly in the liner; the column may prevent it from dropping completely into the liner.
If the insert does not drop completely into the liner, do not force it (either the liner or the column may shatter); instead, remove the column, seat the insert, and then replace the column.
5. Replace the septum and septum retainer nut.

Split/splitless or split-only capillary inlet inserts

Figure 1-10
Viton O-ring (Preferred) Viton O-ring
Split Use Splitless Use
Split/Splitless and Split-Only Capillary Inlet and Inserts
A specific inlet insert is required, depending upon the particular sampling mode. Specific sampling modes include:
C
Split, for major•componentanalyses
C
Purged splitless, for trace•componentanalyses
27
Columns and Fittings
Inlet inserts
The split insert contains packing material (10% OV•1on 80/100 High Performance Chromosorb•W),held in place by silanized glass wool plugs, located immediately above a mixing chamber. This ensures proper volatilization and homogeneous mixing of the sample prior to its entry into the column.
WARNING
Caution
Exercise care! The oven, and/or inlet, or detector fittings may be hot enough to cause burns.
If operating in split mode, carrier gas pressure must be reduced before opening the inlet. If not done, pressure may blow insert packing out of the inlet, altering its characteristics. Pressure is reduced at the backpressure regulator for the inlet.
1. In handling the insert, avoid contaminating its surface (particularly
its interior).
2. Remove the insert retainer nut. The septum retainer nut need not be
removed from the insert retainer nut assembly.
28
Columns and Fittings
Inlet inserts
Figure 1-11
Caution
Installation, Split/Splitless Capillary Inlet Insert
3. Using tweezers, forceps, or similar tool, remove any insert already in
place.
4. Inspect the new insert to be installed: For a split mode insert, the end
with the mixing chamber and packing is inserted first into the inlet.
5. Place a graphite or silicone O•ringon the insert, about 2 to 3 mm from
its top end.
6. Install the insert, pressing it straight down, as far as possible, into
the inlet.
Do not add any seal either at the bottom of the inlet or at the bottom of the insert; to do so will damage the inlet and/or shatter the insert.
7. Replace the insert retainer nut, tightening it to firm finger•tightness
to form a leak•freeseal. Do not overtighten.
29
Columns and Fittings

Jet replacement, FIDs or NPDs

Jet replacement, FIDs or NPDs
Depending upon the column type (packed versus capillary) to be used, and/or analyses to be performed, exchanging the jet in an FID or NPD may be necessary. This must be done prior to column installation, and is particularly important in optimizing FID performance.
Exchanging the jet in either an FID or an NPD is described in Chapter 8, Preventive Maintenance.

Metal capillary columns

Most metal capillary columns (0.6 to 1.0 mm od) can be connected directly. Some metal capillaries have a large•diametersleeve soldered on
each end; this must be removed. Use a small triangular file to score the tubing behind the sleeve; then bend the sleeve back and forth until it breaks.
30
It is important to have fresh ends of the column, free of burrs, jagged edges, and/or loose particles of column, stationary phase, and/or material from a sealing ferrule or O•ring.
Therefore, whenever the column must be cut to provide fresh ends, use a suitable file to first score the column at the point at which it is to be broken. This is done normally after installing on the column the column nut and ferrule (or O•ring)required for installation.
2

Keyboard and Displays

Keyboard and Displays
Figure 2-1
HP 5890 SYSTEM READY
OVEN
RATE
Oven Status
INITIAL TIME
ACTUAL SETPOINT
STATUS
FINAL TIME
RUN
NOT
READY
Alphanumeric
Display
Instrument Status
Programmable Cool on Column Control
Setpoint Storage Control
Signal Definition and Control
STORE
LOAD
TCD
SENS
STOP START
ON
OFF
A
B
IINIT TIME
OVEN TRACK
DET A TEMP
TIME
RATE
AUX TEMP
DET B TEMP
FLOW CRYO
PARAM PARAM
FLOW TIME
ENTER
7 8 9
4
1 2 3
0
TABLE ADD DELETE PREVIOUS NEXT
OVEN TEMP
PRES PRES INJ A
TEMP
SIG 1
SIG 2
RANG E2!()
ZERO
ATTN 2!()
DET
INIT
VALUE
INJ BINJ A
INJ B TEMP
COL COMP1
COL COMP2
FINAL VALUE
OVEN
MAX
EQUIB TIME
PURGE
VALVE
.
FINAL TIME
CLEAR
65
-
Run Control
Timetable Control
Temperature Control
Miscellaneous Functions
Numeric and Modifier Keys
32
HP 5890 SERIES II Keyboard and Display Panel
Keyboard and Displays

Displaying setpoints

HP 5890 SERIES II (hereafter referred to as HP 5890) operation is monitored and controlled through its front panel keyboard, and alphanumeric and LED displays.
Some instrument functions are monitored continuously: signal levels, temperatures, carrier gas flow rates (if electronic flow sensing is installed), and inlet purge valve status (if a split/splitlesscapillaryinlet is installed).
There are two general display areas:
C
Alphanumeric Display. Echoes keys pressed at the HP 5890 keyboard show current setpoint values for instrument functions; actual values of continuously monitored instrument functions; and warning, error, information, and diagnostic messages.
C
LED Display. Consists of two parts: the left half (OVEN) displays oven status during a run; the right half (STATUS) gives overall instrument status at any given time.
Figure 2-2
Displaying setpoints
Any particular instrument current value and/or setpoint is displayed at the alphanumeric display simply by pressing the appropriate instrument function key followed possibly by additional modifier" keys necessary to
further define the function (i.e.,
TIME
). For example, pressing
A
OVEN MAX
OVEN MAXIMUM 400
Example, a Typical Alphanumeric Setpoint Display
The name of the function key pressed is always displayed, along with the current setpoint and/or measured values.
B
or
SIG 1
,
or
might give the display:
ACTUAL SETPOINT
SIG 2,ON
or
OFF
,
33
Keyboard and Displays

Entering setpoints

Examples of possible displays are provided where appropriate throughout the manual.
If a particular function is not installed in your instrument, an appropriate message is displayed when the key corresponding to the function is pressed. For example, if no heated zone controlled by
DET B TEMP
Figure 2-3
Typical Display, a Function NOT Installed in the Instrument
Entering setpoints
is installed, pressing
DET B TEMP
ACTUAL SETPOINT
DET B NOT INSTALLED
gives the display:
34
To enter a setpoint value for a particular instrument function, the function is first displayed by pressing the appropriate key(s).
Once the chosen HP 5890 function is displayed, a new setpoint value can be entered at any time by pressing appropriate keys
.
-
,
, or possibly
A
,
B,ON
,or
OFF
. For a numeric value,
0
through
9
ENTER
,
is pressed to terminate the entry. Figure 2•4summarizes the two steps
involved.
Keyboard and Displays
Entering setpoints
To display the function and its setpoint:
Figure 2-4
(Instrument Function Key) ( or )
A B
necessary for a few
instrument functions
then, EITHER
0 9
( through , , )
-
.
ENTER
to enter a new setpoint value
OR, for a few functions,
ON
(or)
OFF
to switch the function on or off
Steps in Entering a Setpoint Value
For example, to set the A detector zone to 250^C, the following sequence of keys is pressed:
DET A TEMP
2
5
0
ENTER
function key numeric key(s)
Once detector A temperature is displayed by pressing
DET A TEMP
, the
new setpoint value may be entered at any time thereafter. Note that the display shows a flashing * (asterisk) while the new
setpoint is entered, disappearing when When
ENTER
is pressed, the setpoint value is verified and, if satisfactory,
ENTER
is pressed.
becomes the new setpoint for the function. If the entered value is not satisfactory (out of range, or inconsistent with other, related setpoints), an appropriate message is displayed. A different value may be entered immediately, without again pressing the particular function key.
35
Keyboard and Displays
Entering setpoints
CLEAR
can be used anytime during an entry, prior to pressing
ENTER
,to erase the entry in progress. The * disappears, and the original setpoint display is restored.
Rules regarding keyboard usage are summarized below:
C
An instrument function key, when pressed, is shown in the display along with its current setpoint value, and actual value for continuously monitored functions: signal levels, temperatures, flow rates.
- A displayed function is also ready for entering a new setpoint value simply by pressing appropriate keys.
C
An * (asterisk) is flashed as the new value is entered, indicating an entry in progress.
ENTER
C
must terminate a numeric entry. It is also required in terminating a sequence to assign a particular detector to a given output signal channel.
In general, any display showing the flashing * must be terminated
ENTER
using
.
36
ENTER
Upon pressing
, the value is verified to ensure it is within the range permitted for the particular function, and/or that the value is internally consistent with previously defined setpoint values for other, related functions.
- If the value is accepted, * disappears from the display indicating
the new value is stored and implemented. For functions whose values are continuously monitored, * is replaced by the actual value.
- If the value is out of range, or inconsistent with another setpoint
value, an appropriate message is displayed. Another setpoint value may be entered immediately without again pressing the particular instrument function key.
The original setpoint value remains in force until an acceptable entry is made.
Keyboard and Displays

Keyboard operation, INET control

CLEAR
C
is used anytime during setpoint entry, prior to pressing
ENTER
,
to erase the entry in progress.
CLEAR
C
, if pressed when no setpoint entry is in progress, displays
HP 5890 readiness .
C
Run Control Key
START
, if pressed while a setpoint entry is in
progress, causes the entry to be aborted.
C
If a particular key is not valid, it is simply ignored if pressed during setpoint entry.
C
While an entry is in progress, other instrument function keys are ignored if pressed, until the current entry is terminated and stored (
ENTER
) or erased (
CLEAR
).
Keyboard operation, INET control
In general terms, HP 5890 operation is the same whether the instrument is under local control or INET control (controlled by a separate device). If the HP 5890 is to be controlled through INET, the following should be noted:
C
In the event communication is lost (e.g., by power lost at one or more devices on the loop, a disconnected INET cable, etc.), HP 5890
STOP
and
C
Should the HP 5890 keyboard exhibit problems (keys inactive) while
keys will be disabled.
under INET control, disconnect INET cables at their HP 5890 receptacles; then switch power to the HP 5890 off, and then on. The keyboard should behave normally (assuming the HP 5890 itself has no problems).
C
To restore INET control, check that all devices on the loop are powered on, and that all INET cables are installed properly. The system should return to normal operation automatically.
START
37
Keyboard and Displays

Protecting setpoints

Additional information regarding INET control is available in Chapter 5, Signal Output. Servicing may be required for one or more devices on the INET loop if communication cannot be established.
Protecting setpoints
The HP 5890 provides a keyboard lock feature to minimize possibility of stored setpoints being altered unintentionally. When the HP 5890 keyboard is locked, setpoint values (numeric values, A, B, OFF, and ON) may only be displayed; they cannot be altered. remain functional, so runs may be started or stopped.
To lock instrument setpoints, first enter the key sequence:
START
and
STOP
Figure 2-5
CLEAR
Then press
.
ON
ENTER
-
to lock the keyboard, or
OFF
to unlock the keyboard.
Figure 2•5shows displays occurring during this process.
ACTUAL SETPOINT
CALIB AND TEST [0-0]
ACTUAL SETPOINT
KEYBOARD LOCK ON
ACTUAL SETPOINT
KEYBOARD LOCK OFF
Keyboard Lock Displays
38
Keyboard and Displays

Loading default setpoints

With the keyboard locked, Figure 2•6shows the display occurring if a setpoint entry is attempted:
Figure 2-6
KEYBOARD LOCKED Message Display
If the HP 5890 keyboard is locked while the instrument is under INET control, a setpoint file may be loaded into HP 5890 memory from the controller, but the loaded setpoints cannot then be edited at the HP 5890 keyboard until it is unlocked.
After locking or unlocking the keyboard, return to operation by pressing any function key (e.g.,
KEYBOARD LOCKED
OVEN TEMP
).
ACTUAL SETPOINT
Loading default setpoints
This function permits resetting HP 5890 operating setpoints to a standard set of values. Only the following information is retained:
C
Calibration constants for oven temperature control
C
All gas flow rate monitoring information (gas types and calibration constants)
C
Column compensation data, including detector assignments
Note: Since user•definedsetpoints are lost in the process, any critical HP 5890 setpoints should be recorded for later reentry before proceeding.
Through the keyboard, select CALIB AND TEST mode, function 6:
CLEAR
.
6
39
Keyboard and Displays
Loading default setpoints
Upon pressing
ENTER
, default setpoints are loaded into memory, erasing
setpoints already present. Table 2•1lists resulting HP 5890 default
setpoints.
Table 2-1. HP 5890 Default Setpoints
Function Default Setpoint
^
Inj Temp (A & B): 50 Det Temp (A & B): 50 Oven Temp: 50 Oven Max Temp: 400 Cryo Cooling: OFF Cryo Blast OFF Equib Time: 3 min Init Temp: 50 Init Time: 650 min Oven Prog Rates: 0 Final Temp: 0 Final Time: 0 min Inlet Purge: ON Purge Time: 0 min Detector (A & B): OFF Signal 1 Det: Detector A Signal 2 Det: Detector B if BOTH detectors A and
Range (1 & 2): 0 Attn (1 & 2): 0, ON Zero (1 & 2): 0, ON HP-IL (INET): Address- 31 INET: Global (unconfigured) Keyboard Lock: OFF Timetable Empty Inj A Pres OFF Inj B Pres OFF TCD Sens HIGH Oven Track ON Constant Flow OFF
C, OFF
^
C, OFF
^
C, OFF
^
C
^
C
^
C/min
^
C
B are installed; otherwise,detector A.
40
Keyboard and Displays
Loading default setpoints
Note that if the battery protecting memory should fail when main power is turned off, the default setpoints are loaded into memory when the battery is replaced. In addition, calibration constants for oven temperature control and gas flow rate monitoring are also reset to default values.
41
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3

Temperature Control

Temperature Control
Oven temperature, and temperatures of up to five separate heated zones (detectors, inlets, and/or heated valves), are controlled through keys shown in Figure 3•1.
Figure 3-1
Oven Control
Figure 3-2
OVEN TEMP
INJ A TEMP
INIT VALUE
INJ B TEMP
INIT TIME
DET A TEMP
RATE
AUX TEMP
DET B TEMP
FINAL VALUE
OVEN MAX
EQUIB TIME
FINAL TIME
Heated Zone Control
Temperature Control Keys
In these cases, both current setpoint value and current monitored value are displayed by pressing the appropriate temperature control key. For example, Figure 3•2shows typical displays obtained by pressing
OVEN TEMP
.
ACTUAL SETPOINT
OVEN TEMP 279 350
44
Typical Display, Setpoint and Current Value
Temperature Control
Note that the ACTUAL value is a measured quantity, while the SETPOINT value is user•defined:in this example, the setpoint value for
oven temperature might recently have been changed from 250 to 350 and the oven is now heating to the new setpoint. Given sufficient time for equilibration, ACTUAL and SETPOINT values become equal.
In addition to keys defining setpoint values, specific key sequences:
0
through
ON,OFF,A
^
C,
.
-
9
,
,
, and
CLEAR
,
B
, and
are used in certain
ENTER
used in
ON
C
and
OFF
add convenience in being able to switch on or off the oven, and/or heated zones, without losing their current setpoint values.
A
C
and temperature program: parameters for the second ramp;
B
are used in key sequences defining a multiple•rampoven
A
as part of key sequences defining
B
as part of key sequences
defining parameters for the third ramp.
45
Temperature Control
e

Valid setpoint ranges

Valid setpoint ranges
Table 3•1lists valid setpoint ranges for the 13 keys controlling oven and
heated zone temperatures.
Table 3-1. Valid Setpoint Ranges For Temperature Control Keys
Key
OVEN TEMP
INIT TEMP
INIT TIME
RATE
FINAL TEMP
FINAL TIME
OVEN MAX
EQUIB TIME
INJ A TEMP
INJ B TEMP
DET A TEMP
DET B TEMP
AUX TEMP
Valid
Setpoint Range
In
Increments Of Function
-80 to 450 1^C Oven Control
-80 to 450 1
^
C Oven Control 0 to 650.00 0.01 minute Oven Control 0 to 70 0.1 /minute Oven Control
-80 to 450 1
^
C Oven Control 0 to 650.00 0.01 minute Oven Control 70 to 450 1
^
C Oven Control 0 to 200.00 0.01 minute Oven Control 0 to 400 1 0 to 400 1
^
C Zone Control
^
C Zone Control 0 to 400* 1^C Zone Control 0 to 400* 1
^
C Zone Control 0 to 400 1^C Zone Control
NOTE: TOTAL run time will not exceed 650.00 minutes regardless of values enter
INIT TIME
RATE FINALTIME
, , and .
*The valid setpoint range for a Flame Ionization Detector is 0 to 450^C.
46
Temperature Control

Cryogenic (sub-ambient) oven control

Cryogenic (sub-ambient) oven control
Liquid N1or liquid CO1cryogenic options are for operation at temperatures less than about 7 operation of a valve which opens when coolant is demanded and closes when the setpoint temperature is reached.
^
C above ambient. This is done through
Figure 3-3
When you press
gold CRYO PARAM CRYO PARAM CRYO PARAM
you scroll through a series of displays for choosing cryogenic options. These options include CRYO for operation during the entire run, CRYO BLAST, for very fast cool down between runs, and AMBIENT to regulate on and off times to optimize coolant use.
ACTUAL SETPOINT
CRYO ON
ACTUAL SETPOINT
CRYO BLAST ON
ACTUAL SETPOINT
AMBIENT 25
Cryogenic options
For operation duringruns at subambient temperatures.
For very fast cool down between runs.
Lets you regulate Cryo and Cryo Blast on and off times to optimize coolant use. Default is 25
^
C and need not be changed unless ambient differs by 10
^
.
The following figures show the oven temperature profile for a typical run, showing the on and off times for CRYO and CRYO BLAST.
47
Temperature Control
Cryogenic (sub-ambient) oven control
Figure 3-4
75
50
25
Figure 3- 5.
120
80
40
CRYO OFF at ambient +15
^
9
(CRYO ON)
Oven profile using CRYO, for operation during runs at subambient temperatures
9
CRYO BLAST ON
ambient + 50
9
CRYO ON at ambient + 25
^
CRYO BLAST OFF
9
(30 sec. modulation)
^
48
Oven profile using CRYO BLAST, for very fast cool down between runs
Temperature Control

Programming oven temperature

Programming oven temperature
HP 5890 oven temperature programming allows up to three ramps, in any combination of heating or cooling. Keys defining an oven temperature program include:
INIT TEMP
INIT TIME
RATE
FINAL TEMP
FINAL TIME
A setpoint temperature value at which the oven is maintained at the beginning of a temperature•programmed
run. This is also the temperature to which the oven returns at termination of the temperature•programmedrun.
When not in a run, the setpoint value for equals
OVEN TEMP
.
Time for which oven temperature is held at
INIT TEMP
INIT TEMP
. Rate at which the oven is to be heated or cooled. Temperature the oven attains at the end of a heating or
cooling ramp. In a multiple•ramptemperature program, final
temperature for one ramp is also the initial temperature for the next ramp.
Time period over which oven temperature is held at
FINAL TEMP
.
In a multiple•ramptemperature program, final time for one ramp is also the initial time for the next ramp.
total elapsed time for a run cannot exceed 650 minutes: at 650 minutes, the run terminates and oven temperature recycles to calculated total length of time anticipated for a run,
INIT TEMP
TIME
. To know
is pressed
repeatedly until a NEXT RUN display is obtained.
49
Temperature Control

Oven status

In isothermal operation (
RATE
= 0 ), if
INIT TIME
is set equal to 0 (zero), the HP 5890 internally sets run time to the maximum, 650 minutes.
A
is included in key sequences defining parameters for a second ramp;
B
is included in key sequences defining parameters for a third ramp.
In isothermal operation, and in one•or two•ramptemperature programs,
rate for the next ramp must be set to 0 (zero) to prevent further programming.
In oven temperature programming, once any one of the five temperature programming functions (
FINAL TIME
) is displayed, pressing
INIT TEMP
INIT TIME
,
ENTER
, without entering a new
RATE
,
FINAL TEMP
,
, and
setpoint value, rolls the display successively through the entire group, (including A and B displays for second and third ramps).
This is an efficient way in which to review and, if necessary, change oven temperature program setpoints.
Oven status
50
During a temperature•programmedrun, the LED OVEN display provides indication of oven status at any given time:
C
Isothermal Run: Assuming than 0, and that
RATE
=0,only the INITIAL TIME LED is lit. It
INIT TIME
is assigned a value greater
remains lit throughout the run.
C
Single•Ramp Temperature Program: The three LEDs, INITIAL TIME, RATE, and FINAL TIME, successively light to indicate position
in the temperature program.
C
Multiple•Ramp Temperature Program: The three LEDs, INITIAL TIME, RATE, and FINAL TIME, successively light to indicate position
in the first temperature program ramp. Then RATE and FINAL TIME LEDs light alternately as the program
proceeds through the second (and third) ramp(s).
Temperature Control

Oven safety

In complex two•or three•rampoven temperature programs, information as to the part of the program in progress is monitored by pressing
OVEN TEMP
Note that, during a ramp, the SETPOINT value displayed is that
calculated to be the correct temperature, based upon specified heating/cooling rate, and initial and final oven temperatures.
Also, note that if the RATE LED is observed to blink during oven heating, this indicates the particular given operating conditions: the oven heater is operating at full power and may not be able to deliver the desired temperature program rate. Such a situation compromises accuracy in repeating the heating ramp from run to run.
Oven safety
.
RATE
value entered is too aggressive for the
WARNING
Normally, the oven should be switched off (
OVEN TEMP
OFF
) prior to accessing the oven interior (e.g., to change columns, check for leaks, etc.). For safety, this turns off power to the oven heater, fan, and cryogenic valve (if installed), but maintains the setpoint value in memory.
The oven is equipped with a shut•offfeature to protect against unintentional opening of the oven door, and/or the possibility of mechanical and/or electronic failure affecting oven operation.
At any time during normal above•ambientoperation, if the oven cannot attain and/or maintain an entered setpoint temperature, a problem is assumed and the oven is automatically switched off. Examples of possible problems include the oven door open (or closed but not properly latched), inoperative oven vent flaps, failure of the oven fan, heater, or temperature sensor, or electronic problem.
If the oven door is opened, a time delay may be observed before the oven shuts itself off. The closer the oven is to ambient temperature, the longer the delay will be.
51
Temperature Control

Fault: messages

The message displayed when this occurs is shown in Figure 3•6.
Figure 3-6
Message, Oven SHUT DOWN
The oven remains off until switched on again via the keyboard
OVEN TEMP
( Fault: messages). Power to the instrument must be switched off, and then on again to restore operation (setpoints are maintained).
Fault: messages
Figure 3•7shows possible FAULT: messages associated with heated zones or the oven. In general, the following problems are indicated when a
FAULT: message appears:
ACTUAL SETPOINT
WARN: OVEN SHUT OFF
ON
), unless a FAULT: message is displayed (see below,
52
C
ADC OFFSET indicates a problem with one or more electronic components in circuitry associated with temperature control.
C
LINE SENSE indicates a problem with AC power to the instrument (an excessively high source voltage).
C
Any of the TEMP RDG messages indicate an inoperative temperature sensor for the indicated zone or oven.
C
OVEN > MAX + 20 indicates oven temperature exceeds the current
OVEN MAX
setpoint value by more than 20^C. Thermal run•awayis
the likely cause.
Note: In case multiple problems exist simultaneously, press
CLEAR
roll through all message displays.
to
Temperature Control

After a power failure . . .

Figure 3-7
Thermal Control FAULT: Messages
ACTUAL SETPOINT
FAULT: ADC OFFSET
ACTUAL SETPOINT
FAULT: LINE SENSE
ACTUAL SETPOINT
FAULT: INJA TEMP RDG
ACTUAL SETPOINT
FAULT: DETA TEMP RDG
ACTUAL SETPOINT
FAULT: OVEN TEMP RDG
ACTUAL SETPOINT
FAULT: OVEN > MAX+20
In addition to the message, the red NOT READY LED blinks. All zones and the oven are turned off and made inoperative until power is switched off, and then on again (setpoints are maintained).
After a power failure . . .
Setpoint values are protected during a power failure (even if intentional, by disconnecting the power cord, or by switching off the HP 5890 at its main power switch) by a lithium battery (10•yearnominal life) which
maintains power to HP 5890 memory. After power is restored, a message is displayed, as shown in Figure 3•8.
53
Temperature Control

Oven temperature calibration

Figure 3-8
ACTUAL SETPOINT
PASSED SELF TEST
INITIAL TIME
RATE
OVEN
FINAL TIME
STATUS
RUN
NOT
READY
Message Display, Power Failure and Recovery
Heated zones return to their respective setpoint values, after which the oven returns to its setpoint value.
If
OVEN TEMP
is displayed after recovery from a power failure, and if
C
the oven was ON before the power failure, the oven display shows the actual oven temperature value, and cycles between showing the setpoint value and OFF until other zones achieve their respective setpoint temperatures.
C
The oven can be switched ON through the keyboard at any time, without waiting for heated zones to first come to correct temperature.
C
An analytical or column compensation run in progress at the time of a power failure is aborted; similarly, a keyboard entry in progress is aborted.
54
Oven temperature calibration
To maximize precision with respect to retention time information, particularly if retention times are to be compared between chromatographs, it may be necessary to calibrate oven temperature in the range of interest using an independent temperature•measuringdevice.
With the factory•setcalibration difference value of 0 (zero), displayed oven temperature is accurate to within 1% of the actual temperature, expressed in
^
K (Kelvin).
Temperature Control
Oven temperature calibration
The HP 5890 providesthe means to (if necessary) reset oven temperature monitoring so the displayed ACTUAL value accurately represents the correct temperature.
Oven temperature calibration requires entering the difference (delta)
^
value (in
C) between an independently measured temperature value
versus the corresponding displayed oven temperature value:
Correction Value =
Measured Temperature (
For example, if actual measured oven temperature were found to be
148.73
^
C, while the corresponding displayed value was 150.00, the
calibration difference value to be entered would be -1.27.
Setting the oven calibration value
An oven temperature calibration measurement should be made at a temperature in the middle of the range of interest. Allow ample time (up to 1/2•hour)for thermal equilibration at the selected temperature; no
drift should be observed. The temperature•sensingprobe should be placed in the region of the oven occupied by the column(s).
^
C) - Displayed Temperature (^C)
1. Through the keyboard, select CALIB AND TEST mode, function 1:
CLEAR
.
ENTER
1
CALIB is displayed, followed by two values: the observed oven
temperature (to 0.01
^
C), and the current difference (delta)
calibration value.
Note: Record the displayed calibration delta value! If problems are encountered in recalibration, the value may be reentered.
2. Assuming no drift in temperature, the new difference (delta) value is
then entered by pressing appropriate number keys, followed by
appropriatevalue
ENTER
ENTER
:
55
Temperature Control
Oven temperature calibration
3. CALIB DELTA is displayed until
ENTER
is pressed; then oven temperature recalibration occurs. Note that, after calibration, the displayed oven temperature value should match closely the measured value.
Any delta value within the range -10.00 through +10.00
^
C may be entered. If a value outside this range is entered, the message CORRECTION TOO HIGH is displayed.
Assuming the battery protecting HP 5890 memory is operational, a new calibration constant remains in effect even if the instrument is switched off, or disconnected from its power source, or if power fails.
56
4

Electronic Flow Sensing

Electronic Flow Sensing
Two channels of electronic flow rate sensing continuously monitor gas flow rates (usually carrier) in the HP 5890 SERIES II. Proper scaling of displayed values for different commonly used gases is defined through keyboard entries. The two flow channels are distinguished through and
If carrier gas flows are monitored, A implies flow through column A (nearest the instrument front); B implies flow through column B (nearest the instrument rear).
Displayed flow rate values are in ml/minute.

Displaying gas flow rate

Current flow rate is displayed by pressing:
B
.
A
Figure 4-1
58
FLOW A
(or
B
)
Typical gas flow rate displays are shown in Figure 4•1:
ACTUAL SETPOINT
FLOW A 25.4 N2
ACTUAL SETPOINT
NO FLOW SENSOR
Typical Electronic Flow Rate Sensor Displays
Electronic Flow Sensing

Designating gas type

Designating gas type
To scale the displayed flow rate value properly, one of four commonly used gases must be designated. The appropriate gas type is selected according to Table 4•1:
Table 4-1. Defining Type of Gas to be Monitored
Number Gas Type Preferred Use
1 He (Helium) TCD 2N 3H 4 Ar/CH
(Nitrogen) General
2
(Hydrogen) Capillary
2
(Methane in Argon) ECD
4
To select one of these gases for a particular flow channel, press:
FLOW
1
2
,
ENTER
, the current flow rate is displayed, scaled appropriately for the
B
(
) to display FLOW A (or FLOW B).
3
,
,or
4
is then pressed, followed by
ENTER
. Upon pressing
chosen gas type. If a gas other than one of the above standard four is used, select He,
N
1,H1
, or Ar/CH3according to which one is closestin thermal conductivity to the gas being used. Under no circumstances should any corrosive gas be passed through the EFS.
The maximum usable range for H ( >100 ml/min), where a gas other than He, N
1
is 100 ml/minute. At higher flow rates
1
, or Ar/CH3is being used, or to ensure maximum accuracy in displayed flow rate, calibration of the EFS may be necessary.
59
Electronic Flow Sensing

Electronic flow sensor (EFS) calibration

Electronic flow sensor (EFS) calibration
Electronic flow sensor (EFS) calibration may be performed any time to ensure displayed flow rate accurately represents real gas flow rate through the sensor. The EFS is factory•calibratedfor four standard
gases, H ml/min. This covers the majority of chromatographic applications.
Two situations where it would be appropriate to perform recalibration would be where a nonstandard gas is to be used (e.g., something other than H to be used.
EFS calibration requires setting two values for a given flow channel•first, the zero value (defined with no flow through the given flow channel) and then the gain value (calculated, based upon a measured flow rate value).
1
, He, N1, and Ar/CH3, within the flow rate range of 0 to 100
1
, He, N1, or Ar/CH3), or if flow rates in excess of 100 ml/min are
WARNING
60
If calibration is being performed for H2, observe proper safety precautions to prevent fire or explosion hazard.
Prior to performing the calibration procedure, the following must be done:
C
The instrument must be on for at least one hour for thermal equilibration of the EFS.
C
Since gas flow through the channel to be calibrated will be interrupted, detectors should be turned off (particularly an NPD or TCD! ), and the oven cooled to ambient temperature (to protect columns).
C
A flow•measuringdevice is required, accurate to better than 1 ml/min.
C
The EFS is calibrated to measure volumetric flow at standard temperature and pressure. Flows measured at ambient temperature with a bubble flow meter will have to be converted from ambient temperature and pressure to standard temperature and pressure.
Electronic Flow Sensing
Electronic flow sensor (EFS) calibration

Preparation

1. Access the EFS by removing the left side panel; remove two screws
along its lower edge, slide the panel toward the rear of the instrument, and then lift.
2. Through the keyboard, select CALIB AND TEST mode, function 2:
CLEAR
.
ENTER
2
GAIN A is displayed, followed by two values: the observed flow rate
through Channel A, and the current gain calibration value for Channel A.

Setting the zero calibration value

The zero calibration value must be set with no gas flow through the channel being calibrated.
ZERO
1. Press
current zero calibration value for EFS Channel A). Note that Channel A is assumed by default; if channel B is to be calibrated instead, press
2. Disconnect the gas source to the particular flow channel being
calibrated. Do not trust an on/off valve, pressure regulator, or mass flow controller to be an effective shutoff device; any gas flowing through the EFS will invalidate the zero calibration value. Disconnect the source at any convenient point (e.g., at the connection of the supply line into the instrument).
: FLOW A ZERO is displayed, followed by a value (the
B
.
61
Electronic Flow Sensing
Electronic flow sensor (EFS) calibration
3. Locate the EFS module and note its labelling: CHANNEL A/
CHANNEL B, IN/OUT. For the channel being calibrated, locate and
disconnect its OUT fitting; use two wrenches in opposition to prevent twisting the tubes.
Figure 4-2
Outlet Line, Channel B
EFS Module
Detail, Electronic Flow Sensor (EFS) Module
Outlet Line, Channel
A
4. Install the EFS flow•measuringadapter (Part No. 05890•80620)into
the female OUT fitting to the EFS module. Connect a bubble flow meter to the adapter.
62
Allow ample time (up to 1/2•hour)for residual gas within connected plumbing to bleed off. Verify that absolutely no flow is observed at the connected bubble flow meter.
Electronic Flow Sensing
Electronic flow sensor (EFS) calibration
Figure 4-3
EFS Flow-Measuring Adapter (Part No. 05890-80620)
5. Assuming there is no gas flow through the channel being calibrated,
press
ENTER
at the keyboard. This updates the zero calibration value.

Setting the GAIN calibration value

After the zero calibration value is set at zero flow rate through the given channel, the gain calibration value must be set, based upon a measured flow rate.
1. At the keyboard, press
FLOW
: GAIN A (or GAIN B) is displayed, followed by two values (the observed flow rate through the channel, and the current gain calibration value for the channel).
2. Reconnect the gas supply to the channel being calibrated. Do not reconnect the OUT fitting for the particular channel.
3. Using a suitable flow•measuringdevice (accurate to better than
1 ml/min) connected at the OUT fitting for the given channel, adjust flow through the channel so measured flow rate is approximately in the middle of the range to be used. For example, if the range of flow rates to be used is between 50 and 150 ml/min, measured flow rate should be adjusted to about 100 ml/min.
63
Electronic Flow Sensing
Electronic flow sensor (EFS) calibration
Note: The HP 5890 has a timer function that may be used as an aid in measuring flow rate (see the Operating Manual, Chapter 4).
C
Press
C
After obtaining the desired flow rate, press:
CLEAR
C
EFS channel A is assumed. Press
TIME
.
to access the timer function.
ENTER
2
to return to setting the gain value.
B
if Channel B is being
calibrated.
4. Allow ample time for flow rate to equilibrate (no drift should be observed).
5. Assuming no drift in measured flow rate, note the flow rate value at the connected flow•measuringdevice. Enter this measured value
through the keyboard:
Measured Value
Upon pressing
ENTER
ENTER
, CALIBRATING is displayed.
6. After a short time, GAIN A (or GAIN B) is again displayed, followed by the observed flow rate and a new gain calibration value based upon the measured flow rate.
Note that the displayed flow rate value now should be quite close to the measured flow rate value. If not, drift may have occurred, so the process should be repeated.
64
7. This completes EFS calibration. Remove the flow•measuringadapter, reconnect channel OUT fittings (use two wrenches in opposition to avoid twisting tubes), replace the left side panel, and restore the instrument to service.
Electronic Flow Sensing
Electronic flow sensor (EFS) calibration

Entering specific ZERO and GAIN values

Calibration values for zero and gain should be recorded when a particular channel is calibrated. They can then be reentered through the keyboard if necessary, without repeating the entire calibration procedure.
To enter specific zero and gain calibration values:
1. Select CALIB AND TEST mode, function 2:
CLEAR
.
ENTER
2
GAIN A (or GAIN B) is displayed, followed by two values (the observed
flow rate through the channel and the current gain calibration value for the channel).
Note that Channel A is assumed by default. If Channel B is to be calibrated instead, press
2. Enter the desired gain calibration value, preceded by
-
Numeric Value
-
is necessary to signify entry of a gain calibration value, rather
B
.
-
:
ENTER
than a measured flow rate.
ZERO
3. Press
: FLOW A ZERO is displayed, followed by a value (the
current zero calibration value for EFS Channel A). Note that Channel A is assumed by default. If Channel B is to be
B
calibrated instead, press
.
4. Enter the desired zero calibration value:
ZERO
ENTER
or
FLOW
displays either the zero
Numeric Value
Note that alternately pressing calibration value or the gain calibration value for the given channel (A or B).
65
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5

Signal Output

Signal Output
A standard signal channel, controlled via A second signal channel, controlled via
SIG 1
, always is provided.
SIG 2
, is provided if Option 550/ Accessory 19242A (Communications Interface Board ), or Option 560/ Accessory 19254A (RS•232), is installed.
Output sources include detector signal(s), heated zone or oven temperatures, carrier gas flow rates, column compensation run data, or test chromatographic data. If both signal channels are present, each may output information simultaneously from the same source, or from two different sources.
For either channel, two separate levels of ANALOG output are provided, depending upon the analog signal cable used: +1 V or 1 mV.
0 to +1 mV: for strip chart recorders.
-0.01 to +1 V: for electronic integrators with analog inputs.
The two output levels are independent, and may be connected simultaneously to separate data•receivingdevices.
Note: A tick mark (electrical pulse) is produced at the +1 mV analog output when either
START
or
STOP
is pressed, and when a run timesout (run time elapses). These marks locate beginning and ending points in a chromatogram plotted at a continuously running strip chart recorder.
68

Zeroing signal output

Acting on +1 mV and +1 V analog outputs, offset which is then subtracted from the output signal (prior to signal attenuation by
RANGE 2!()
or
ATTN 2!()
ZERO
defines a constant
).
Signal Output
Zeroing signal output
Figure 5-1
The function of
ZERO
is to subtract a constant background signal from the detector signal. Background signal sources include the detector itself (background level depending upon detector type), column bleed, or contaminants in supply gas(es).
SIG 1
ZERO
setpoint
SIG 2
or
), followed by
ZERO
(or simply press
Displaying current
Current signal channel key (
ZERO
ZERO
setpoint value is displayed by pressing the appropriate
alone, if the desired signal channel is already displayed). Typical
displays are shown in Figure 5•1.
ACTUAL SETPOINT
SIG 1 ZERO 104.5
ACTUAL SETPOINT
SIG 2 NOT INSTALLED
ACTUAL SETPOINT
ZERO 1 104.5 OFF
ACTUAL SETPOINT
ZERO LIMIT = 83000
Typical Displays
ZERO
Table 5•1lists conversions between detector units and the scale used for
ZERO
setpoint values.
-12
ZERO
A)
Table 5-1. Conversions from Detector Units to Setpoint Val­ues
Detector
Conversion
ZERO
(1.0 unit = )
FID & NPD 1.0 pA (1.0}10
¿
TCD 25
V (2.5}10-5V)
ECD 10 Hz
69
Signal Output
Zeroing signal output
Figure 5-2
O U
T P
U T
V O L T A
G E
Self-
Referencing Figure 5•2for the +1 V output, note that using
ZERO
setpoint
ZERO
increase dynamic range available for signal output by shifting an existing constant offset signal to a lower level (usually electrical zero). There are limits to this, however, so it is good practice to have background reduced as much as possible by minimizing column bleed, using clean supply gases, and by performing proper detector maintenance.
ZERO
1.0 V usable
dynamic range
+ 1.000 V
+ 0.100 V
0V
1 V Output: Canceling BaselineOffset (the self- function)
1.0 V maximumoutput level
0.9 V usable
dynamic range
ENTERZERO
pressed
Constant 0.100 V
detector background
signal
HP 5890 SERIES II electrical zero
can
70
-0.010 V
Effect of on the +1 V Analog Output
ZERO
Signal Output
Zeroing signal output
Figure 5-3
O
+ 1.000 mV
U
T P
U
T V
O
L T
+ 0.100 mV
A G E
+ 0.006 mV
1 mV Output: CancelingBaseline Offset (the self- function)
1.0 mV maximum output level
0.9 mV usable
dynamic range
ENTERZERO
pressed
Constant 0.1 mV
detector background
signal
HP 5890 SERIES II electrical zero
0mV
Effect of on the +1 mV Analog Output
ZERO
ZERO
1.0 mV usable
dynamic range
The example in Figure 5•2is in terms of the +1 V analog output. In Figure 5•3,identical treatment is made for the +1 mV output, except that the signal is shifted to an offset somewhat above electrical zero. This ensures a small positive offset (about 6% of full scale) in pen position at a connected chart recorder, and permits uninterrupted plotting, even if a small negative baseline drift occurs.
Once current channel, pressing
ZERO
setpoint value is displayed for the desired signal
ENTER
causes the value to be changed to the current
signal value. Self•
ZERO
should be done only at times of quiet chromatographic activity (i.e., not during a run). To do so during an active run may cause a baseline shift at the recording/integrating device.
71
Signal Output

Signal attenuation

Note: If a self• exceeding the maximum permitted setpoint value for
User•defined
ZERO
determination is performed on an active signal
ZERO
ZERO
setpoint), the maximum setpoint value is assigned
(see
and the message SIG 1 (or 2) ZERO TOO HIGH is displayed.
User-defined
If the self•
ZERO
setpoint
ZERO
setpoint value determination is not appropriate for a particular application, any value from -830000.0 through 830000.0 may be entered at the keyboard.
Entering a value less than the self•
ZERO
value shifts background baseline upward (but at the expense of available output range); for example, to capture negative peaks, or to compensate for negative baseline drift.
Signal attenuation
Analog signal output levels (+1mV or +1 V outputs) for either signal channel (controlled by
SIG 1
, and by
19242A or Option 560/Accessory 19254A is installed) are attenuated via
RANGE 2!()
and
ATTN 2!()
.
SIG 2
if Option 550/Accessory
72
RANGE 2!()
For signal level by a factor of 2 (half the previous level). Also,
, each step to a higher setpoint value decreases the output
RANGE 2!()
affects signal level at both the +1 V and +1 mV analog outputs.
Signal
+1 V Output Level =
ATTN 2!()
affects only the +1 mV analog output: each step to a higher
value reduces the output signal level (as defined by
+1 mV Output Level =
RANGE 2!()
2
RANGE 2!()
2
Signal
}
RANGE 2!()
ATTN 2!()
2
) by half.
Signal Output
Signal attenuation
Thus, signal output level at the +1 mV analog output may be set separately from that at the +1 V output.
Table 5•2gives values permitted for either function, and the output
affected.
Table 5-2. Valid Setpoints for and
RANGE 2!() ATTN 2!()
Permitted SetpointsKey
RANGE 2!()
ATTN 2!()
Note:
ATTN 2!()
0 to 13 Both +1 mV & +1 V 0 TO 10 Only +1 mV
OFF
ON
,
functions only for the +1mV output, and acts on the
signal after it has been ranged by
RANGE 2!()
Affected Output
.
Generally, if both an integrator or A/D converter (+1 V output) and chart recorder (+1mV output) are connected to the same signal channel,
RANGE 2!()
then
should be set properly first for the integrator or computer,
ATTN 2!()
set appropriately for the chart recorder.
To minimize integration error for an integrator or A/D converter,
RANGE 2!()
normally should be set to the lowest value possible, provided the largest peaks of interest do not exceed 1 volt. Attenuation functions at the integrating device or computer are then used to ensure that plotted peaks remain on scale.
RANGE 2!()
selects and sizes a portion of the full dynamic range for the signal source assigned to an output channel. The portion selected is sized such that the highest possible value for the portion does not exceed maximum output voltage allowed for the given output (+1 mV or +1 V).
ATTN 2!()
further selects and sizes a portion of the ranged signal for the +1 mV output to ensure that the signal does not exceed +1 mV.
73
Signal Output
Signal attenuation
For analytical information from a detector, proper settings for
ATTN 2!()
and
are determined such that peaks of interest are on scale at the integrator or chart recorder: peaks of interest must neither flat top by exceeding the allowed maximum output level, nor be too small to be measured. Table 5•3lists maximum detector output producing +1 volt
at the +1V output for each
Table 5-3. Detector Output Producing a 1 V Signal
Maximum Detector Signal
Producing +1 V Output
RANGE 2!()
0 1.0}10 1 2.0 2 4.0}10 3 8.0 4 1.6}10 5 3.2
FID & NPD (pA)
3
3
}
10
3
3
}
10
4
4
}
10
(mV, High Gain)
RANGE 2!()
TCD
25 800 10 50
CC
CC
CC
CC
setpoint value.
TCD
(mV, Low Gain)
C
RANGE 2!()
ECD (kHz)
20 40
80 160 320
6 6.4}10 7 1.3}10 8 2.6}10
9 5.1}10 10 1.0}10 11 2.0}10 12 4.1}10 13 8.2}10
74
4
5
5
5
6
6
6
6
CCC
CCC
CCC
CCC
CCC
CCC
CCC
CCC
Signal Output
Signal attenuation
Figure 5-4
From Table 5•3,note that for a TCD,
RANGE 2!()
= 0 is suitable for virtually all applications since the entire linear output range of the detector is included. Likewise,
RANGE 2!()
settings from 0 through 5cover
the entire useful output range for an ECD. Only an FID or NPD may
RANGE 2!()
ATTN 2!()
or
RANGE 2!()
RANGE 2!()
settings.
ATTN 2!()
/
ATTN 2!()
or
(or simply press
setpoints
is displayed by
SIG 1
or
RANGE 2!()
SIG 2
), followed
or
require use of the higher
Displaying current
Current setpoint value for pressing the appropriate signal channel key ( by either
ATTN 2!()
RANGE 2!()
alone, if the desired signal channel is already displayed).
For example, the following key sequence displays current setpoint for
RANGE 2!()
for the
SIG 2
output channel:
SIG 2
RANGE 2!()
Typical displays that occur are shown in Figure 5•4.
ACTUAL SETPOINT
SIGNAL 1 RANGE 10
SIGNAL 1 ATTN 10
SIGNAL 1 ATTN 10 OFF
SIG 2 NOT INSTALLED
Typical Signal Channel Displays
ACTUAL SETPOINT
ACTUAL SETPOINT
ACTUAL SETPOINT
75
Signal Output
Signal attenuation
Note that if
SIG 1
or
desired,
SIG 2
RANGE 2!()
SIG 2
, SIGNAL 1 channel is assumed (and displayed). If
can then be pressed to display the same function for the
or
ATTN 2!()
is pressed without first pressing
SIGNAL 2 channel.
Entering
RANGE 2!()
A new setpoint value is entered for either
ATTN 2!()
/
setpoints
RANGE 2!()
or
ATTN 2!()
using
the key sequence:
SIG 1
(or
SIG 2
RANGE 2!()
)
(or
ATTN 2!()
)Numeric Value
ENTER
Once channel and function are displayed, appropriate keys for the new value are pressed, followed by
ENTER
to terminate the entry.
Switching off the +1 mV output
The +1 mV signal output can be switched off, providing no signal to the
data•receivingdevice. This is often useful in setting the zero position at a connected strip chart recorder.
This is done through the following key sequence:
76
SIG 1
The third example display in Figure 5•4is typical after pressing
(or
SIG 2
)
ATTN 2!()
OFF
OFF
.
After setting the pen to the desired zero position at the connected chart
ON
recorder, the current attenuation value is restored by pressing Entering a new
ATTN 2!()
value overrides OFF.
.
Signal Output

Test signal output

Test signal output
A test chromatogram, consisting of three peaks, is permanently stored in the HP 5890. Each peak is approximately 1/10 the height of the previous peak, with the first (tallest) peak having a height value of about 125 mV at
about 0.13 minutes.
Figure 5-5
RANGE 2!()
=0(+1Vanalog output); half•heightwidth of this peak is
LIST: LIST PEAK CAPACITY: 1159
HP 5890:
RANGE 2 ”()
ATTN 2”()
1 V Analog Output
=0
=0
ZERO =
ATT 2 CHT SP = 1. PK WD =3.13 THRSH = AR REJ =
START
1.25
STOP
RUN # 8
AREA%
RT AREA TYPE AR/HT AREA%
3
.25 79394
3
.75 79353
1.25 79
TOTAL AREA = 88121 MUL FACTOR = 1.
!
3
, •1.5
=7
3
3 3
.75
33
3
3
94 BB3.134
3333E+33
BB PB
3
.135 93.397
3
.135 9.335
33
3
.898
.25
Typical HP 5890 Test Chromatogram (using an HP 3390A Reporting Integrator)
77
Signal Output
Test signal output
To access this function, the following key sequence is entered:
SIG 1
(or
SIG 2
ENTER
9
)
Test plot mode is confirmed by the display SIGNAL 1 (or 2) TEST
PLOT. Pressing
SIG 1
(or
SIG 2
) a second time displays the current signal level value (which is 0.0 initially). This permits monitoring the output signal.
START
The chromatogram is initiated by pressing continues to cycle until
STOP
is pressed. Each cycle is about 1•1/2
. The chromatogram
minutes in length.
Note:
C
Setpoint values assigned to
RANGE 2!()
and
ATTN 2!()
affect level of the test signal output, as do equivalent functions on the receiving device.
C
An oven temperature program (e.g., a setpoint value for
RATE
other
than 0) must be set up at the HP 5890 for the test plot to function.
The test chromatogram is useful as a troubleshooting aid in deciding whether a lost or noisy signal observed at a connected integrating or chart recording device is due to a chromatographic problem (lost sample due to leaks, noise due to a dirty detector, etc.), versus problems either with the integrating/recording device itself, or in its connecting cables.
78
If the test chromatogram does not exhibit any problems at the integrating/recording device, a chromatographic problem is likely to exist; if the test chromatogram exhibits noise, or does not appear at all, the problem is not likely to be chromatographic.
Signal Output

Instrument network (INET)

Instrument network (INET)
The Instrument Network (INET) is a path for various devices to communicate with each other (data and/or commands). INET permits a group of devices (consisting of a controller, and some number of data Producers and data Consumers) to function as a single, unified system.
INET permits:
C
Management of active workspace (described below) among instruments, a controller, and storage and print media.
C
Sharing of run and readiness conditions among INET instruments.
C
Sharing of setpoint and parameter information among INET instruments.
C
Automation of data collection, sample tracking, and report generation.
Note: In default operation the HP 5890 supplies only Signal 1data to the INET loop. That is, HP 5890 data supplied to the INET loop is defined according to the assignment made via
SIG 1
. To use Signal 2
data instead, signal reassignment is done at the HP 5890.

The controller

INET is a series•connectedloop of devices, with the output of each device
connected to the input of the next. A message sent from a particular device travels around the loop, returning to the same instrument as confirmation of transmission. Thus, the loop must be continuous, and all devices must be on for the loop to function.
79
Signal Output
Instrument network (INET)
Figure 5-6
Sampler
5890
IN OUT
S/ECM
OUT IN
OUT IN
80
HP 5890 SERIES II Gas Chromatograph
Typical INET Loop
Controller & Integrator
Each INET must have one (and only one) device defined as the controller. The controller is responsible for network configuration when the network is first connected and powered on.
The controller then retains this status for subsequent loop operations, maintaining its responsibility as network traffic manager. Note that the device defined as controller usually has other capabilities.
The controller assigns addresses to each device on the loop, and configures them to operate in orderly fashion. In addition, the controller provides user access to the network configuration so desired changes can be made.
For a typical analytical system, the default, automatic configuration should be acceptable in most cases. For specific information regarding
Signal Output
Instrument network (INET)
configuration, consult appropriate manual(s) for the controller device (the HP 5890 is never a controller).

An instrument

Addresses
An instrument is a device, housing together a collection of functions, and having a single model number. It has a single pair (IN and OUT)of INET cable connections.
The INET controller assigns each instrument a unique address, in order, around the loop. Thus, addresses correspond to the physical order of connections around the loop.
Note that the controller usually is also an instrument in that it has capability of performing various analytical tasks (for example, integration).
Data or a command message destined for a particular instrument is labelled with the corresponding address for the instrument.
Setpoints
The controller passes setpoints among INET instruments (including itself), and to and from local storage. Setpoints are grouped according to the instrument to which they belong, and labelled with the corresponding INET address. Setpoint traffic is automatic, once appropriate commands are entered at the controller.
If an instrument receives setpoints intended for a different instrument because of an address error, it rejects them, causing the controller to print an error message.
Generally, each instrument provides a means for entering its own setpoints (i.e., a keyboard or control panel). The HP 19405A S/ECM is an exception: its setpoints are defined through the controller.
81
Signal Output
Instrument network (INET)
Except for the controller, each instrument handles setpoints for instrument(s) other than itself only as blocks of data to be transmitted, but not altered.

Active workspace

Each device in an INET loop provides storage area for its own setpoints and parameters. These individual storage areas (each containing setpoints and parameters for the specific instrument) are also available to any other device in the loop. For example, the controller may access them for listing and/or storage.

HP 5890 INET states

At the HP 5890, when a part of INET, the RUN LED provides indication of INET status:
C
If the RUN LED is off, the INET system is in its idle state, waiting for initiation of some action (e.g., starting a run, listing information, etc). In this state, the HP 5890 NOT READY LED is turned on if the HP 5890 is not ready, and/or if the INET system itself is not ready (e.g., if a device on the loop is busy). A message SYSTEM NOT READY will appear on the HP 5890 if some other device on the INET loop reports not ready, and the HP 5890 is itself ready.
82
CLEAR
C
If the RUN LED is blinking, the INET system is in pre•runor
may be pressed to display things that are not ready.
post•runoperation (e.g., a sampler cycling, a report in progress, etc). In addition, either SYSTEM IN PRE-RUN or SYSTEM IN POST-RUN is displayed if
CLEAR
is pressed. The NOT READY LED is on only if
the HP 5890 itself is not ready.
C
If the RUN LED is on, a run is in progress. The NOT READY LED is turned on only if the HP 5890 itself should become not ready.
Signal Output
Instrument network (INET)

INET operation

In using the INET function, chromatographic parameters are entered normally through the HP 5890 keyboard. Integration parameters are entered at the controller. Parameters for other devices on the INET loop may be entered at the controller, or at their own keyboards. Collectively, the separate sets of parameters constitute a single set of parameters for an analysis.
The intent here is to discuss INET operation only from the point of view of the HP 5890. For specificinformationregarding INET loop control (configuration, workfile storage and recall, etc), consult the appropriate operation manuals for the INET controller device. Also consult appropriate manual(s) for other devices (sampler/event control module, etc) configured in the loop.
Typical displays occurringwhen the HP 5890 is under INET control are shown in Figure 5•7.
Figure 5-7
INET Displays
ACTUAL SETPOINT
UNDER REMOTE CONTROL
ACTUAL SETPOINT
SYSTEM NOT READY
ACTUAL SETPOINT
SETPOINT FILE LOADED
Typical INET Loop Displays
C
Keyboard setpoint entry is not allowed at the HP 5890 while a workfile or method is stored or listed at the controller: UNDER
REMOTE CONTROL is displayed if an entry is attempted.
83
Signal Output
Instrument network (INET)
If a setpoint entry at the HP 5890 keyboard is in progress when a workfile or method is stored or listed at the controller, the entry is aborted. After the operation finishes, the HP 5890 returns to the same setpoint display.
C
When a stored workfile or method is recalled to active workspace at the controller, its setpoints are automatically downloaded into devices on the INET loop, including the HP 5890. Successful download at the HP 5890 is confirmed by the display, SETPOINT FILE LOADED. Any instrument function key (e.g., message.
If a setpoint entry at the HP 5890 keyboard is in progress when a workfile or method is recalled, the entry is aborted.
C
If problems occur in transferring chromatographic setpoints to the HP 5890, the HP 5890 retains its present setpoints, so there is no indication at the HP 5890 that transfer was attempted. Appropriate error messages are printed at the controller device.
OVEN TEMP
), or
CLEAR
, erases the
84
C
SYSTEM NOT READY, if displayed, indicates one or more devices on the INET loop report not ready.
C
UNDER REMOTE CONTROL is displayed if, from a host computer system, a command has been entered to lock the HP 5890 keyboard to prevent alteration of setpoints, and entry of a setpoint value is attempted at the HP 5890.
C
In case of INET system failure, the HP 5890 may be operated by itself (INET cables should be disconnected at the HP 5890). If, as a result of the failure, the HP 5890 keyboard does not respond normally to key presses, switch off the instrument at its main power switch. Upon restoring power, the keyboard should be active.
Signal Output

INET configuration

Automatic INET reconfiguration

In the following circumstances, INET automatically reconfigures under direction of the controller:
C
C
C
Consult appropriate manuals for the controller in the event of problems arising from any of these circumstances.
INET configuration
The CONFIGURE NETWORK function provides four features: verifying the INET address for the HP 5890 (as determined through automatic loop configuration), setting the default HP•ILaddress to be used when the
HP 5890 is connected to some device where addresses must be set manually (i.e., no automatic loop configuration), switching the INET function at the HP 5890 between global or local, and verifying INET signal definitions. Each feature is discussed separately.
Recovery from a power failure. Recovery from any particular device on the loop being switched off,
then on again. Recovery from a disconnected (then reconnected) loop cable.
Figure 5-8
ACTUAL SETPOINT
CONFIGURE NETWORK
ACTUAL SETPOINT
GLOBAL ADDR: 8,31
ACTUAL SETPOINT
LOCAL ADDR: 8,31
CONFIGURE NETWORK Displays
85
Signal Output
INET configuration
Figure 5•8shows displays resulting from the key sequence:
Figure 5-9
CLEAR
.
ENTER
3

Switching between Global and Local

With regard to the INET function at the HP 5890, there are two operating modes: global or local.Inglobal mode (default mode), HP 5890
START
INET loop. In local mode, however, pressing HP 5890 affects only the HP 5890. A run may be started or stopped at the HP 5890 without affecting other devices on the INET loop.
In local mode, note that the HP 5890 remains part of the INET system; it reports its readiness to the system and pressing keys on other devices on the INET loop (e.g., the controller) will affect HP 5890 operation.
Once in CONFIGURE NETWORK, pressing respectively, between global or local mode shows resulting displays as in Figure 5•9.
and
STOP
keys, when pressed, affect other devices on the
ON
START
or
OFF
or
START
switches,
STOP
and
at the
STOP
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ACTUAL SETPOINT
GLOBAL ADDR: 8,31
ACTUAL SETPOINT
LOCAL ADDR: 8,31
INET GLOBAL/LOCAL Displays
An example of where having the HP 5890 in local mode might be useful is in the case of conditioning a column: the HP 5890 may be started or stopped as desired without affecting other devices on the INET loop.
Signal Output
INET configuration
Note that global mode has two states: if GLOBAL flashes (default mode) when displayed, the HP 5890 is in global mode, but not configured into the INET system. When the HP 5890 is properly configured into the INET system, GLOBAL is displayed continuously. This feature provides a convenient diagnostic to determine if system configuration has occurred (at least as far as the HP 5890 is concerned).

INET/HP-IL addresses

Figure 5•10shows displays occurring either in verifying an INET address
set through automatic loop configuration or in entering a specific HP•IL default address used when the HP 5890 is included in an HP•ILloop without automatic configuration. The address is maintained in battery•protectedmemory along with other instrument setpoints.
Figure 5-10
ACTUAL SETPOINT
GLOBAL ADDR: 8,31
ACTUAL SETPOINT
DEFAULT ADDRESS * 25
ACTUAL SETPOINT
GLOBAL ADDR: 8,25
ACTUAL SETPOINT
ADDRESS LIMIT = 31
INET/HP-IL ADDR: Displays
Verifying the HP 5890 INET address
In Figure 5•10,note the two numeric values following ADDR:. The first of these numbers is the INET address for the HP 5890, determined via automatic loop configuration.
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Signal Output
INET configuration
The specific number shown depends upon how INET cables are connected among devices included in the loop. The value shown in the example (8) implies the HP 5890 is the first instrument on the loop, starting from the OUT receptacle on the controller device (the controller is always defined as 0). A 9 indicates the HP 5890 is the second device on the loop, etc, to a maximum value of 31.
If cabling is altered, or if one or more devices are powered off and then on again, automatic loop configuration, initiated by the controller, updates the displayed value accordingly.
Setting the default HP-IL address
Remaining displays in Figure 5•10show the process of defining a specific
HP•ILaddress for the HP 5890. Entry of any value from 8 through 31 is permitted. An attempt to enter an invalid value results in the ADDRESS LIMIT message shown.
INET-HP 5890 signal definition
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INET signal definition (defined at the controller) may be verified at the HP 5890. To display the definitions, enter:
CLEAR
.
SIG 1
(
or
ENTER
3
SIG 2
)
Signal Output
INET configuration
Figure 5•11 shows resulting displays.
Figure 5-11
INET-HP 5890
Signal Definition
ACTUAL SETPOINT
GLOBAL ADDR: 8,31
ACTUAL SETPOINT
SIG 1 ON RANGED
ACTUAL SETPOINT
SIG 1 ON FULL RANGE
ACTUAL SETPOINT
SIG 2 OFF
INET Signal Definition Displays
From the displays, the following may be noted:
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HP 5890 signal channels are designated SIG 1 or SIG 2.
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ON indicates the given signal channel is considered active by the controller; data from this signal channel is transmitted to other devices on the INET loop.
Similarly, OFF indicates the channel is considered inactive; no data from this signal channel is transmitted to other devices on the loop.
It is important to note that ON or OFF in this context are strictly INET definitions, defined at the system controller. They do not, for example, bear any relationship to whether or not a given detector assigned to the signal channel is turned on or off.
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Signal Output

HP-IL loopback test

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RANGED versus FULL RANGE indicates the dynamic range for the data to be transmitted to other devices on the loop; dynamic range for RANGED data is set at the HP 5890 according to the setpoint for
the detector itself. The choice of the type of data to be transmitted is set at the controller.
HP-IL loopback test
The HPIL LOOPBACK TEST may be performed any time to verify that HP 5890 INET communication is performing satisfactorily. Testing involves setting up the HP 5890 to send an INET message directly to itself by connecting its INET output to its INET input. The following procedure is used:
1. Disconnect INET cables at their respective INSTRUMENT NETWORK IN and OUT receptacles on the HP 5890 (located beneath the top right cover panel).
RANGE 2!()
. Dynamic range for FULL RANGE data is limited only by
90
2. Choose either one of the cables and disconnect it at the next device on the INET loop.
3. Connect this free cable to both IN and OUT INSTRUMENT NETWORK receptacles on the HP 5890.
4. Enter the following key sequence:
.
ENTER
7
Upon pressing
ENTER
CLEAR
, the test is performed: the HP 5890 both sends and verifies a diagnostic message to itself through the connected cable. Each press of
ENTER
repeats the test. Each test requires about one
second. Figure 5•12shows displays to be expected.
Signal Output
HP-IL loopback test
Figure 5-12
ACTUAL SETPOINT
HPIL LOOPBACK TEST
ACTUAL SETPOINT
PASSED SELF TEST
ACTUAL SETPOINT
FAILED SELF TEST
HPIL LOOPBACK TEST Displays
The message PASSED SELF TEST indicates INET, at least with respect to the HP 5890, is performing satisfactorily. If FAILED SELF-TEST is displayed, a bad cable may be indicated; install a different INET cable and repeat the test. If FAILED SELF-TEST is displayed again for a second cable, electronic problems within the HP 5890 are indicated.
Note: The loopback testmay be used to check for continuity in an INET cable; an open cable causes test failure. Verify that the cable is at fault (rather than the HP 5890) by testing a second cable.
If an intermittent cable problem is suspected, the test may be repeated as necessary while flexing the cable (particularly at its plugs). An ohmmeter should also be used to test for problems; it is a reliable method for testing continuity.
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Signal Output

Warn: and fault: messages

Warn: and fault: messages
Figure 5-13
ACTUAL SETPOINT
WARN: INET TIMEOUT
ACTUAL SETPOINT
WARN: SIGNAL CHANGED
ACTUAL SETPOINT
WARN: NO DETECTORS
ACTUAL SETPOINT
FAULT: INET CPU
ACTUAL SETPOINT
FAULT: INET CPU RAM
ACTUAL SETPOINT
FAULT: INET RAM TEST
ACTUAL SETPOINT
FAULT: INET ROM TEST
ACTUAL SETPOINT
FAULT: ATTN1 TEST
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ACTUAL SETPOINT
FAULT: DAO1 TEST
Signal Control WARN: and FAULT: Messages
Figure 5•13shows possible WARN: and FAULT: messages associated with signal functions. In general, the following problems are indicated if the following messages appear:
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WARN: INET TIMEOUT is displayed if information transmission on the INET loop is interrupted; for example, if an INET loop cable is accidentally disconnected.
Signal Output
Warn: and fault: messages
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WARN: SIGNAL CHANGED and/or WARN: NO DETECTORS is displayed if a detector previously assigned to a particular signal channel is found to be absent; for example, if the signal board for a given detector should fail or be removed for service.
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FAULT: INET CPU is displayed if the processor (and/or its associated circuitry) for HP 5890 INET operations should fail.
HP 5890 diagnostics generating the above message displays are active at all times in normal operation. The next group appears only if a problem is found to exist at HP 5890 power•on:
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Remaining FAULT: INET messages are displayed if problems are diagnosed in INET circuitry.
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FAULT: ATTN1 TEST and/or FAULT: DAC1 TEST occur if problems are diagnosed in signal path circuitry for a particular signal channel (channel 1, in the example displays).
In general, if signal problems are suspected, power to the HP 5890 may be turned off, and then on again to perform internal self•testing. Appropriate message displays occur if problems are found to exist.
Note: In case multiple problems exist simultaneously, press
CLEAR
to
roll through NOT READY and/or FAULT: displays. Note that, with exception of WARN: OVEN SHUT OFF,
CLEAR
erases any
displayed WARN: message. For WARN: messages, the instrument remains operational, except for
the function indicated by the message: the message is erased upon pressing any instrument function key (e.g.,
OVEN TEMP
). For FAULT: messages, in addition to the message, the red NOT READY LED blinks: the instrument CANNOT be operated until the problem is corrected.
If a WARN: or FAULT: message occurs in normal operation, try switching power to the instrument off, and then on again. If the problem recurs when power is restored, service procedures are indicated.
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Signal Output

File compatibility with data handling devices

File compatibility with data handling devices
You must have the HP 5890 SERIES II in the proper mode for file compatibility with your data handling device.

What are the modes?

There are 2 file transfer modes: HP 5890A and HP 5890 SERIES II.
HP 5890A File Transfer Mode HP 5890 SERIES II File Transfer Mode
Transmits HP 5890 setpoints: Transmits HP 5890 setpoints plus:
Timetable events Inlet pressure and temperaturepro-
grams
^
Up to 450 Cryo Blast and Ambient setpoints TCD sensitivity Aux temperature setpoint
oven and FID temperature
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What is the proper mode for my data handling device?

Selection of the proper mode depends on the product and version of your software.

How do I know in which mode my GC is configured now?

1. Turn power off, then on.
2. Check the GC display.
Signal Output
File compatibility with data handling devices
Figure 5-14
GC Displays for File Transfer Modes

How do I change modes?

1. Turn power off.
2. Remove the GC side panel, and locate the main PC board.
Figure 5-15
Top Hinge for Grounding
HP 5890A mode
HP 5890 SERIES II mode
ACTUAL SETPOINT
EMULATION MODE OK
ACTUAL SETPOINT
PASSED SELF TEST
Finding the Main PC Board.
3. Find component P15 on the main PC board.
Main PC Board
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Signal Output
File compatibility with data handling devices
Figure 5-16
Figure 5-17
P5
P6
P15
P2
P3
P13 P12
Main PC Board
Finding component P15 on the Main PC Board.
4. Set the jumper (Part No. 1258•0141)for the proper mode. To avoid
electrostatic damage to the main board, ground yourself to the GC chassis with an ESD strap, or touch an unpainted area of the oven such as the door hinge.
HP 5890A mode
HP 5890 SERIES II mode
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Setting the jumper.
Signal Output
File compatibility with data handling devices

How to convert HP 339X Integrator workfiles from 5890A to SERIES II mode:

1. Turn the GC off.
2. Follow the previous instructions to set the GC for 5890A mode (use
proper grounding).
3. Download the workfile from the integrator.
4. Turn GC power off.
5. Remove the P15 jumper. (Now the GC is in SERIES II mode.)
6. Turn GC power on.
7. Add SERIES II setpoints (time table, etc).
8. Store the workfile at the integrator.
STORE
Note: Using workfiles can be converted with each jumper change sequence.
on the HP 5890 SERIES II, up to 4 integrator
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6

Inlet Systems

Inlet Systems
This chapter provides information for the following HP 5890 SERIES II (hereafter referred to as HP 5890) inlet systems:
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Packed column inlet

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Septum•purgedpacked column inlet
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Split/splitlesscapillary inlet
For cool on•columninformation, see the manual Programmable Cool
On•ColumnInlet. Maintenance information is provided in Chapter 8, Preventive Maintenance.
Packed column inlet
The packed column inlet may be used with HP Series 530¿capillary columns, metal packed or glass packed columns. Additionally, on•column
injection is possible with 1/4•inchglass packed columns. The packed column inlet is optimized for low to intermediate temperatures (200-300
^
C).
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