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HP 5890 Series II Plus Reference Manual

Hewlett-packard reference manual.
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Reference Manual
HP 5890 Series II and
HP 5890 Series II Plus

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   Summary of Contents for HP 5890 Series II Plus

  • Page 1

    Reference Manual HP 5890 Series II and HP 5890 Series II Plus...

  • Page 2

    Third edition—Jan 1990 material. Printed In U.S.A. Fourth edition—Oct 1990 Safety Information Printed In U.S.A. The HP 5890 Series II and Fifth edition—Oct 1991 HP 5890 Series II Plus are Printed In U.S.A. IEC (International Fifth edition—Mar 1993 Electrotechnical Printed In U.S.A.

  • Page 3: Table Of Contents

    Contents Chapter 1 — Columns and Fittings Column oven ............Column placement Packed column Hewlett•Packardcapillary columns...

  • Page 4: Table Of Contents

    How do I know in which mode my GC is configured now? How do I change modes? How to convert HP 339X Integrator workfiles from 5890A to SERIES II mode: ....

  • Page 5: Table Of Contents

    Chapter 6 — Inlet Systems Packed column inlet ........... Electronic flow sensor .

  • Page 6: Table Of Contents

    Chapter 8 — Preventive Maintenance Conditioning columns ..........(Re)Packing columns .

  • Page 7: Table Of Contents

    Chapter 9 — Chromatographic Troubleshooting Introduction ............Baseline symptoms .

  • Page 8

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  • Page 9: Chapter 1 — Columns And Fittings

    Columns and Fittings...

  • Page 10

    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. Additional flexibility is gained through positions of inlets and detectors relative to each other and through the large internal volume of the oven.

  • Page 11: Column Oven

    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•drivenflaps at 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).

  • Page 12: Column Placement, Packed Column

    Columns and Fittings Column oven Column placement Generally, a column may be installed between any inlet and detector. A rigid 1/4•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.

  • Page 13: Hewlett•packardcapillary Columns

    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...

  • Page 14: Fittings

    Columns and Fittings Fittings Figure 1-4. Column Hanger Part No. 1460-1914 Installed Bracket for Hewlett-Packard Capillary Columns 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.

  • Page 15

    Columns and Fittings Fittings 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/splitless capillary inlet inserts.

  • Page 16

    Columns and Fittings Fittings Table 1-1. Typical Fittings for Columns and Inlet/Detector Liners, Adapters, and Inserts Type Description 1/4-inch swage, stainless steel, front ferrule pkg, 20 of each back ferrule 1/8-inch swage, stainless steel, front ferrule pkg, 20 of each back ferrule 1/4-inch swage, brass, pkg,...

  • Page 17: Liners/adapters And Inserts, General

    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;...

  • Page 18

    Columns and Fittings Liners/adapters and inserts, general Table 1-2. Hardware and Recommended Fittings for Packed Column Installation 1/8-inch Metal Recommended 1/8-inch Column Fittings swage-type nut and ferrules Packed Column 19243-80510 Inlet Liners 19243-80530 (requires glass insert) FID/NPD 19231-80521 Liners/Adapters TCD Liners/Adapters None ECD Liner/Adapters 19301-80530...

  • Page 19

    Columns and Fittings Liners/adapters and inserts, general Table 1-3. Hardware and Recommended Fittings for Capillary Column Installation HP Series 530 Recommended Capillary column Column Fittings nut and 1.0-mm graphite ferrule, or silicone O-ring(s) Packed Column 19244-80540 Inlet Liners (requires glass insert) Split/Splitless &...

  • Page 20: Inlet/detector Liners/adapters, Packed Column Inlet Liners

    Packed column inlet liners Figure 1-5 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. ¿...

  • Page 21

    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 No liner is used with 1/4•inchpacked glass columns. The long leg of the column fits into the inlet body, replacing the liner.

  • Page 22: Detector Liners/adapters

    Columns and Fittings Inlet/detector liners/adapters Detector liners/adapters Figure 1-6 Liner/Adapter 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.

  • Page 23: Ecd And Tcd Adapters

    The adapter must be removed for packed column applications. In addition, to install an HP Series 530 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.

  • Page 24: Liner/adapter Installation

    The single exception is the adapter to install an HP Series 530 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.

  • Page 25: Inlet Inserts, Packed Column Inlet Inserts

    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 possible. 3. Holding the liner/adapter in this position, tighten the nut finger•tight. 4.

  • Page 26

    Columns and Fittings Inlet inserts Exercise care! the oven, and/or inlet, or detector fittings may be hot WARNING enough to cause burns. Figure 1-9 Installing a Glass Insert in a Packed Column Inlet 1. In handling the insert, avoid contaminating its surface (particularly its interior).

  • Page 27: Split/splitless Or Split•onlycapillary Inlet Inserts

    Columns and Fittings Inlet inserts Note: For the liner and insert for an HP Series 530 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.

  • Page 28

    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.

  • Page 29

    Columns and Fittings Inlet inserts Figure 1-11 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.

  • Page 30: Jet Replacement, Fids Or Npds, Metal Capillary Columns

    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.

  • Page 31: Chapter 2 — Keyboard And Displays

    Keyboard and Displays...

  • Page 32

    Control STORE SIG 1 Setpoint Storage LOAD SIG 2 Control RANG Signal Definition and Control ZERO ATTN SENS HP 5890 SERIES II Keyboard and Display Panel SYSTEM OVEN FINAL TIME RATE STOP TIME TABLE DELETE INIT IINIT RATE VALUE TIME...

  • Page 33: Displaying Setpoints

    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/splitless capillary inlet is installed).

  • Page 34: Entering Setpoints

    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 is pressed to terminate the entry.

  • Page 35

    Keyboard and Displays Entering setpoints To display the function and its setpoint: Figure 2-4 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 function key Once detector A temperature is displayed by pressing new setpoint value may be entered at any time thereafter.

  • Page 36

    Keyboard and Displays Entering setpoints can be used anytime during an entry, prior to pressing CLEAR erase the entry in progress. The * disappears, and the original setpoint display is restored. Rules regarding keyboard usage are summarized below: 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.

  • Page 37: 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: 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...

  • Page 38: Protecting Setpoints

    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;...

  • Page 39: Loading Default Setpoints

    KEYBOARD 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.

  • Page 40

    Keyboard and Displays Loading default setpoints Upon pressing setpoints already present. Table 2•1lists resulting HP 5890 default setpoints. Table 2-1. HP 5890 Default Setpoints Function Inj Temp (A & B): Det Temp (A & B): Oven Temp: Oven Max Temp:...

  • Page 41

    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.

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  • Page 43: Chapter 3 — Temperature Control

    Temperature Control...

  • Page 44: 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 INIT TEMP VALUE INJ A INJ B TEMP TEMP 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.

  • Page 45

    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 C, and the oven is now heating to the new setpoint. Given sufficient time for equilibration, ACTUAL and SETPOINT values become equal.

  • Page 46: Valid Setpoint Ranges

    Temperature Control 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 OVEN TEMP INIT TEMP INIT TIME RATE FINAL TEMP FINAL TIME OVEN MAX EQUIB TIME...

  • Page 47: Cryogenic (sub•ambient)oven Control

    Temperature Control Cryogenic (sub-ambient) oven control Cryogenic (sub-ambient) oven control Liquid N or liquid CO cryogenic options are for operation at temperatures less than about 7 C above ambient. This is done through operation of a valve which opens when coolant is demanded and closes when the setpoint temperature is reached.

  • Page 48

    Temperature Control Cryogenic (sub-ambient) oven control Figure 3-4 CRYO OFF at ambient +15 (CRYO ON) Oven profile using CRYO, for operation during runs at subambient temperatures Figure 3- 5. Oven profile using CRYO BLAST, for very fast cool down between runs CRYO ON at ambient + 25 CRYO BLAST ON...

  • Page 49: Programming Oven Temperature

    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...

  • Page 50: Oven Status

    Temperature Control Oven status In isothermal operation ( (zero), the HP 5890 internally sets run time to the maximum, 650 minutes. is included in key sequences defining parameters for a second ramp; is included in key sequences defining parameters for a third ramp.

  • Page 51: Oven Safety

    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.

  • Page 52: Fault: Messages

    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).

  • Page 53: After A Power Failure

    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.

  • Page 54: Oven Temperature Calibration

    Temperature Control Oven temperature calibration Figure 3-8 INITIAL TIME Message Display, Power Failure and Recovery Heated zones return to their respective setpoint values, after which the oven returns to its setpoint value. OVEN TEMP 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.

  • Page 55

    Temperature Control Oven temperature calibration The HP 5890 provides the 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...

  • Page 56

    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.

  • Page 57: Chapter 4 — Electronic Flow Sensing

    Electronic Flow Sensing...

  • Page 58: Displaying Gas Flow Rate

    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 If carrier gas flows are monitored, A implies flow through column A (nearest the instrument front);...

  • Page 59: Designating Gas Type

    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 To select one of these gases for a particular flow channel, press: FLOW...

  • Page 60: Electronic Flow Sensor (efs) Calibration

    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 , He, N , and Ar/CH , within the flow rate range of 0 to 100 ml/min.

  • Page 61: Preparation, Setting The Zero Calibration Value

    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: GAIN A is displayed, followed by two values: the observed flow rate through Channel A, and the current gain calibration value for Channel A.

  • Page 62

    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.

  • Page 63: Setting The Gain Calibration Value

    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 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.

  • Page 64

    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). Press After obtaining the desired flow rate, press: CLEAR EFS channel A is assumed.

  • Page 65: Entering Specific Zero And Gain Values

    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.

  • Page 66

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  • Page 67: Chapter 5 — Signal Output

    Signal Output...

  • Page 68: Zeroing Signal Output

    Signal Output A standard signal channel, controlled via A second signal channel, controlled via 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.

  • Page 69

    Signal Output Zeroing signal output The function of the detector signal. Background signal sources include the detector itself (background level depending upon detector type), column bleed, or contaminants in supply gas(es). Displaying current Current ZERO signal channel key ( alone, if the desired signal channel is already displayed). Typical ZERO displays are shown in Figure 5•1.

  • Page 70

    1.0 V maximum output level 0.9 V usable dynamic range ZERO ENTER pressed Constant 0.100 V detector background signal HP 5890 SERIES II electrical zero on the +1 V Analog Output ZERO ZERO ZERO function) 1.0 V usable dynamic range...

  • Page 71

    ZERO ENTER pressed Constant 0.1 mV detector background signal HP 5890 SERIES II electrical zero ZERO on the +1 mV Analog Output setpoint value is displayed for the desired signal ZERO causes the value to be changed to the current...

  • Page 72: Signal Attenuation

    Signal Output Signal attenuation Note: If a self• exceeding the maximum permitted setpoint value for User•defined and the message SIG 1 (or 2) ZERO TOO HIGH is displayed. User-defined If the self• particular application, any value from -830000.0 through 830000.0 may be entered at the keyboard.

  • Page 73

    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. RANGE 2 ATTN 2 Note: ATTN 2...

  • Page 74

    Signal Output Signal attenuation For analytical information from a detector, proper settings for ATTN 2 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.

  • Page 75

    Signal Output Signal attenuation From Table 5•3,note that for a TCD, virtually all applications since the entire linear output range of the detector is included. Likewise, the entire useful output range for an ECD. Only an FID or NPD may require use of the higher Displaying current Current setpoint value for...

  • Page 76: Switching Off The +1 Mv Output

    Signal Output Signal attenuation Note that if SIG 1 SIG 2 desired, SIG 2 SIGNAL 2 channel. Entering A new setpoint value is entered for either the key sequence: SIG 1 Once channel and function are displayed, appropriate keys for the new value are pressed, followed by Switching off the +1 mV output The +1 mV signal output can be switched off, providing no signal to the...

  • Page 77: 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 RANGE 2 about 0.13 minutes.

  • Page 78

    An oven temperature program (e.g., a setpoint value for 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...

  • Page 79: Instrument Network (inet), The Controller

    Automation of data collection, sample tracking, and report generation. Note: In default operation the HP 5890 supplies only Signal 1 data to the INET loop. That is, HP 5890 data supplied to the INET loop is defined according to the assignment made via data instead, signal reassignment is done at the HP 5890.

  • Page 80

    Instrument network (INET) Figure 5-6 Sampler 5890 HP 5890 SERIES II Gas Chromatograph Typical INET Loop 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.

  • Page 81: An Instrument

    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.

  • Page 82: Active Workspace, Hp 5890 Inet States

    HP 5890 INET states At the HP 5890, when a part of INET, the RUN LED provides indication of INET status: 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).

  • Page 83: Inet Operation

    INET controller device. Also consult appropriate manual(s) for other devices (sampler/event control module, etc) configured in the loop. Typical displays occurring when the HP 5890 is under INET control are shown in Figure 5•7. Figure 5-7...

  • Page 84

    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.

  • Page 85: Automatic Inet Reconfiguration, Inet Configuration

    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...

  • Page 86: Switching Between Global And Local

    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;...

  • Page 87: Inet/hp•iladdresses

    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).

  • Page 88

    (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.

  • Page 89

    INET Signal Definition Displays From the displays, the following may be noted: HP 5890 signal channels are designated SIG 1 or SIG 2. 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.

  • Page 90: Hp•illoopback Test

    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 RANGE 2 the detector itself. The choice of the type of data to be transmitted is set at the controller.

  • Page 91

    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.

  • Page 92: Warn: And Fault: Messages

    Signal Output Warn: and fault: messages Warn: and fault: messages Figure 5-13 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: WARN: INET TIMEOUT is displayed if information transmission on the INET loop is interrupted;...

  • Page 93

    (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.

  • Page 94: File Compatibility With Data Handling Devices, What Are The Modes

    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.

  • Page 95: How Do I Change Modes

    Signal Output File compatibility with data handling devices Figure 5-14 HP 5890A mode HP 5890 SERIES II mode 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.

  • Page 96

    GC chassis with an ESD strap, or touch an unpainted area of the oven such as the door hinge. Figure 5-17 HP 5890A mode Setting the jumper. Main PC Board HP 5890 SERIES II mode...

  • Page 97: How To Convert Hp 339x Integrator Workfiles From 5890a To Series Ii Mode

    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).

  • Page 98

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  • Page 99: Chapter 6 — Inlet Systems

    Inlet Systems...

  • Page 100: Packed Column Inlet

    Inlet Systems This chapter provides information for the following HP 5890 SERIES II (hereafter referred to as HP 5890) inlet systems: Packed column inlet Septum•purgedpacked column inlet Split/splitless capillary inlet For cool on•columninformation, see the manual Programmable Cool On•ColumnInlet. Maintenance information is provided in Chapter 8, Preventive Maintenance.

  • Page 101

    Inlet Systems Packed column inlet Figure 6-1 Liner Glass Insert Carrier Gas Column Packed Column Inlet Septum Retainer Nut Septum Graphite Ferrule Swage-type Nut and Ferrules...

  • Page 102: Electronic Flow Sensor

    Inlet Systems Packed column inlet Figure 6-2 Trap(s) Carrier Flow Diagram, Packed Column Inlet (with electronic flow sensor) Liquid sample is rapidly volatilized inside the inlet. To ensure complete volatilization, inlet temperature typically should be at least 20 ^ C greater than the highest oven temperature to be used.

  • Page 103: Septum•purgedpacked Column Inlet

    Septum-purged packed column inlet The septum•purgedpacked column inlet may be used with HP Series ¿ capillary columns, metal packed or glass packed columns. Additionally, on•columninjection is possible with 1/4•inchglass packed columns.

  • Page 104: Problems At High Inlet Temperatures, A Thermally Optimized High•temperatureinlet

    Inlet Systems Packed column inlet Problems at high inlet temperatures A common problem with conventional packed column inlets operated at high temperatures is septum bleed and the associated ghost peaks. To minimize this effect, some inlet systems are designed with steep temperature gradients throughout the entire upper length of the inlet to provide a cool septum and minimal ghost peaks.

  • Page 105: Septum Purge

    Inlet Systems Packed column inlet Figure 6-4 Bottom of Sep- Syringe Tip Base of Injection Port Thermal Profiles This optimized thermal profile allows very reproducible results and virtually eliminates injection port discrimination against high boiling point components. When combined with fast automated injection, excellent quantitative accuracy is possible.

  • Page 106

    Inlet Systems Packed column inlet When operating the inlet with septum purge, low bleed septa are unnecessary and the selection of septa should be made primarily for good sealing and extended septa life reasons. On a periodic basis (every 1 to 2 months), the Teflon•coatedO•ring sealing the purge cavity should be replaced.

  • Page 107: Split/splitless Capillary Inlet

    Inlet Systems Split/splitless capillary inlet Split/splitless capillary inlet Figure 6-5 Sealing O-Ring Insert 1, 2, or Item Description Split Insert (packed)18740-60840 Split Insert (unpacked)18740-80190 Direct Injection Insert18740-80200 Splitless Insert 18740-80220 1/8-in. Column Insert18709-80030 1/4-in. Column Insert18745-80010 *NOTE: Not shown Split/Splitless Capillary Inlet A.

  • Page 108: Carrier Gas Considerations

    Inlet Systems Split/splitless capillary inlet The multiple•modesplit/splitless capillary inlet system may be used with any of the common types of capillary columns (fused silica, quartz, glass, metal). Specific sampling modes include: Split, for major•componentanalyses. Purged splitless, for trace•componentanalyses. Each mode requires installation of a specific inlet insert. Figure 6-6 Available Inlet Inserts Note that performance in capillary analyses is closely related to the...

  • Page 109

    Inlet Systems Split/splitless capillary inlet In general, the carrier gas is chosen to maximize component resolution and detector performance while minimizing overall analysis time. Figure 6•7,a family of van Deemter curves for common carrier gases, illustrates the effect of gas choice and linear velocity ( efficiency (HETP, Height Equivalent to a Theoretical Plate) for a particular column and analysis.

  • Page 110: Initial Column Head Pressure

    Inlet Systems Split/splitless capillary inlet Van Deemter curves demonstrate advantages of using either He or H as carrier gas. From the curves, several observations may be made: Minima for He and H velocities than N higher velocities than N or He allows shorter overall analysis times. An additional benefit in using H achieved at relatively low column head pressures.

  • Page 111: Split Sampling

    Inlet Systems Split/splitless capillary inlet Table 6-1. Nominal ID (mm) 0.20 0.32 0.53 It must be emphasized that values in this table are recommended as starting points only! Values listed are independent of carrier gas used. It is important to note that flow settings made for one particular column are not necessarily correct for any other column, or for every application.

  • Page 112

    Inlet Systems Split/splitless capillary inlet Figure 6-8 External Internal Plumbing Plumbing Trap(s) Mass Flow Controller Carrier Flow Diagram, Split Operation Due to short sample residence time inside the inlet, the technique requires rapid volatilization; thus, inlet temperature must be high enough to ensure this.

  • Page 113

    The split ratio is an indicator of the fraction of total sample entering the column: the higher the value, the less sample enters the column. For setting flow for split sampling, see Chapter 4 of the HP 5890 Operating Manual.

  • Page 114: Splitless Sampling

    Inlet Systems Split/splitless capillary inlet Splitless sampling For splitless operation, the dilute sample is vaporized inside the inlet insert. Most of the sample is then swept onto the column. For full column efficiency, vaporized sample components must reconcentrate at the head of the column prior to separation; without reconcentration, peak widths of eluting components reflect inlet insert volume rather than column efficiency.

  • Page 115

    Inlet Systems Split/splitless capillary inlet Figure 6-9 Needle Carrier Gas The Solvent Effect The solvent effect is described in great detail elsewhere: see Grob, K. and Grob, K., Jr., Journal of Chromatography, 94, page 53 (1974); Grob, K. and Grob, G., Chromatographia, 5, page 3 (1972). To reconcentrate sample components via the solvent effect, oven temperature must be low enough so solvent remains at the head of the column for a sufficiently long time period.

  • Page 116

    Inlet Systems Split/splitless capillary inlet Table 6-2. Solvent Diethyl Ether n-Pentane Methylene Chloride Carbon Disulfide Chloroform* Methanol* n-Hexane Ethyl Acetate* Acetonitrile n-Heptane i-Octane Toluene * Should be used only with cross-linked stationary phases. The best solvent for a given application is found by trial and error, depending upon sample solubility and volatility, column polarity and type of stationary phase, and detector selectivity/sensitivity.

  • Page 117

    Inlet Systems Split/splitless capillary inlet A general guideline is that components boiling at least 150 C above the column temperature will be reconcentrated by cold trapping at the head of the column. Components with lower boiling points are reconcentrated via the solvent effect. Temperature programming Multiple•rampoven temperature programming is advantageous: the oven is held at an appropriately cool temperature at injection to create...

  • Page 118

    Inlet Systems Split/splitless capillary inlet A recommended procedure is to perform a series of analyses at increasingly higher inlet temperatures using components representative of those of interest, and analyzed using the conditions for later sample analyses. The optimum temperature is where maximum area counts are obtained, and there is no evidence of thermal degradation products.

  • Page 119

    Inlet Systems Split/splitless capillary inlet Figure 6-10 Area Counts Effect of Inlet Purge Activation Time on Area Counts Noting Figure 6•10,waiting too long does not increase component peak areas, but does increase interference by the solvent tail. Purging too early risks venting light components, not allowing sufficient time for heavier components to enter the column, and/or not having sufficient solvent enter the column to ensure good reconcentration.

  • Page 120

    Inlet Systems Split/splitless capillary inlet Figure 6-11 External Internal Plumbing Plumbing Trap(s) Mass Flow Controller Carrier Flow Diagram, Splitless Operation (inlet purge) Figure 6-12 Internal External Plumbing Plumbing Trap(s) Mass Flow Controller Carrier Flow Diagram, Splitless Operation (during injection) Capil- lary Inlet Electronic...

  • Page 121: Injection Technique, Split/splitless Sampling

    Inlet Systems Split/splitless capillary inlet Noting Figures 6•1 1 and 6•12,the splitless sampling process is as follows: Before Injection: Carrier gas flow enters through the mass flow controller, into the top of the inlet. A small fraction is split off to purge the septum and insert seal, then flows on to the purge vent.

  • Page 122

    Inlet Systems Split/splitless capillary inlet 2. Wipe excess solvent from the syringe needle. 3. Without introducing air, draw in excess sample. 4. Position the syringe plunger for the required injection volume. Wipe excess sample from the needle. 5. Draw in air until the sample/solvent is entirely within the syringe barrel.

  • Page 123: Chapter 7 — Detector Systems

    Detector Systems...

  • Page 124: Capillary Makeup Gas Flow Rate

    10 and 20 ml/min. Some loss of detector sensitivity may occur at lower flow rates. For the ECD, capillary makeup gas should be used even with HP Series ¿ capillary columns, because the large cell size requires high total flow rate (at least 25 ml/min).

  • Page 125: Fid And Npd Jets

    Detector Systems FID and NPD jets Supply pressure for capillary makeup gas should be set to about 276 kPa (40 psi). FID and NPD jets Depending upon the column type to be used, and/or analyses to be performed, exchanging the jet in an FID or NPD may be necessary. Table 7•1lists available jets.

  • Page 126: Flame Ionization Detector (fid)

    Detector Systems Flame ionization detector (FID) Flame ionization detector (FID) Figure 7-1 Inlet Inlet Flame Ionization Detector (FID) The flame ionization detector (FID) responds to compounds that produce ions when burned in a H •airflame. These include all organic compounds, although a few (e.g., formic acid, acetaldehyde) exhibit poor sensitivity.

  • Page 127

    Detector Systems Flame ionization detector (FID) Compounds producing little or no response include: Rare gases Nitrogen Oxides Silicon Halides * Measured at the jet tip. This selectivity can be advantageous: for example, H O or CS , used as solvent, do not produce large solvent peaks. The system is linear for most organic compounds, from the minimum detectable limit through concentrations greater than 10 times the minimum detectable limit.

  • Page 128: Fid Flameout Problems

    Detector Systems Flame ionization detector (FID) FID flameout problems When using pressure programming with large id columns (i.e. 530 columns) it is possible to blow the FID flame out if pressure (flow) becomes too high. If this occurs, either lower the pressure ramp or switch to a more restrictive column (longer and/or smaller id).

  • Page 129

    Detector Systems Nitrogen-phosphorus detector (NPD) Nitrogen-phosphorus detector (NPD) Figure 7-3 NPD Collector Assembly Nitrogen-Phosphorus Detector (NPD) The nitrogen•phosphorusdetector uses a jet and collector similar to the FID; however, the collector contains a small alumina cylinder coated with a rubidium salt (the active element) which is heated electrically. In the presence of this thermionic source, nitrogen•and phosphorus•containing organic molecules are efficiently ionized.

  • Page 130

    Detector Systems Nitrogen-phosphorus detector (NPD) H and air are required, but at flows significantly less than those for an FID. Normal FID•typeionizations are therefore minimal, so response to compounds not containing nitrogen or phosphorus is reduced. Thus, the detector is both sensitive to and selective toward only compounds containing nitrogen and/or phosphorus.

  • Page 131

    Detector Systems Nitrogen-phosphorus detector (NPD) Other gas flow effects of too high flow rates of the hydrogen may allow a true flame to exist around the active element. This would overheat the active element severely and destroy the specific response. Too low flow rates of air tend to quench the background response of the active element, and this results in a re•equilibrationtime that is too long to establish proper background response (negative solvent peaks killing the...

  • Page 132: Performance Considerations

    Detector Systems Nitrogen-phosphorus detector (NPD) Performance considerations Contamination Very little contamination can create serious NPD problems. Common sources include: Columns and/or glass wool treated with H PO (phosphoric acid) Phosphate•containingdetergents Cyano•substitutedsilicone columns (XE•60,OV•225,etc.) Other nitrogen•containingliquid phases Any liquid phase deactivated for analysis of basic compounds Fingerprints Leak•detectionfluids Laboratory air...

  • Page 133

    Detector Systems Nitrogen-phosphorus detector (NPD) Residual silanizing reagents from derivatization, and/or bleed from silicone columns, may coat the active element with silicon dioxide. This decreases ionization efficiency, reducing sensitivity. If silanizing is necessary, remove excess reagent before injection. Silicone columns should be well conditioned and loaded less than 5%. Active element lifetime Lifetime of the active element is reduced by the silicon dioxide coating, described above, and by irreversible loss of rubidium salt.

  • Page 134

    Detector Systems Nitrogen-phosphorus detector (NPD) Both detector baseline and sensitivity change with carrier flow rate due to change in temperature of the active element. This is the reason for the baseline drift in pressure•controlledinlet systems (capillary inlets) when temperature•programmingthe column. The amount of change in the detector response is proportional to the ratio of the total column flow change (temperature sensitive) to the makeup gas flow (not temperature sensitive), i.e., total column flow change divided by makeup gas flow.

  • Page 135: Electron Capture Detector (ecd), Requirements For Usa Owners

    Detector Systems Electron capture detector (ECD) Electron capture detector (ECD) The effluent gas stream from the detector must be vented to a fume WARNING hood to prevent possible contamination of the laboratory with radioactive material. Specific cleaning procedures are provided in Chapter 8, Preventive Maintenance.

  • Page 136

    Return the cell for exchange, following directions included with the form General License Certification (HP Pub. No. 43•5954•7621). It is unlikely, even in this very unusual situation, that radioactive material will escape the cell. Permanent damage to the within the cell is possible, however, so the cell must be returned for exchange.

  • Page 137

    Detector Systems Electron capture detector (ECD) Figure 7-5 Anode Plated Makeup Gas Adapter Electron Capture Detector (ECD) The electron capture detector (ECD) cell contains isotope emitting high•energyelectrons ( repeated collisions with carrier gas molecules, producing about 100 secondary electrons for each initial Further collisions reduce energy of these electrons into the thermal range.

  • Page 138

    Detector Systems Electron capture detector (ECD) Uncaptured electrons are collected periodically by applying short•term voltage pulses to cell electrodes. This cell current is measured and compared to a reference current, and the pulse interval is then adjusted to maintain constant cell current. Therefore, pulse rate (frequency) rises when an electron•capturing compound is passing through the cell.

  • Page 139

    Detector Systems Electron capture detector (ECD) Table 7-2. General ECD Sensitivity to Various Classes of Compounds Chemical Type Hydrocarbons Ethers, esters Aliphatic alcohols, ketones, amines; mono-Cl, mono-F compounds Mono-Br, di-Cl and di-F compounds Anhydrides and tri-Cl compounds Mono-I, di-Br and nitro compounds Di-I, tri-Br, poly-Cl and poly-F compounds These are only approximate figures;...

  • Page 140: Temperature

    Detector Systems Electron capture detector (ECD) Considerations for packed column operation Either N or Ar containing 5 or 10% CH , may be used as carrier gas. N yields somewhat higher sensitivity, but it is accompanied by higher noise; minimum detectable limit is about the same. N sometimes produces a negative solvent peak.

  • Page 141: Background Level

    Detector Systems Electron capture detector (ECD) Background level If the ECD system becomes contaminated, whether from impurities in the carrier (or makeup) gas, or from column or septum bleed, a significant fraction of detector dynamic range may be lost. In addition, the output signal becomes noisy.

  • Page 142

    Detector Systems Electron capture detector (ECD) A very clean system may produce a value below the low end of 10 (100 Hz). To correct this condition, an adjustment is made to the present potentiometer located on the ECD electronics board. ECD Potentiometer Switch ECD Potentiometer Adjustment ECD Potentiometer Switch and Adjustment...

  • Page 143: Thermal Conductivity Detector (tcd)

    Detector Systems Thermal conductivity detector (TCD) Thermal conductivity detector (TCD) Figure 7-7 0 ml/min Switching Flow 1 (off) Thermal Conductivity Detector (TCD) HP 5890 SERIES II TCD Cell VENT (60 ml/ min) 30 ml/min 30 ml/min Column Switching Flow Flow 2...

  • Page 144

    Detector Systems Thermal conductivity detector (TCD) The thermal conductivity detector (TCD) detects the difference in thermal conductivity between column effluent flow (carrier gas + sample components) and a reference flow of carrier gas alone; it produces voltage proportional to this difference. The voltage then becomes the output signal to the connected chart recording or integrating device.

  • Page 145

    Detector Systems Thermal conductivity detector (TCD) Because of its exceptionally high thermal conductivity and chemical inertness, He is the recommended carrier gas: it gives large thermal conductivity differences with all compounds except H (considerations necessary in H analyses are discussed later). With He as carrier, the TCD exhibits universal response.

  • Page 146: Optimizing Performance

    Detector Systems Thermal conductivity detector (TCD) Optimizing performance The following sections aid in choosing operating parameters to obtain optimal TCD performance. Temperature TCD sensitivity increases as the temperature difference between the detector filament (automatically set) and the surrounding detector body (chosen detector zone temperature) increases.

  • Page 147

    Detector Systems Thermal conductivity detector (TCD) As Figure 7•9shows, however, the lower the detector zone temperature, the greater is the temperature difference between the filament versus the surrounding detector body temperature. Thus, for maximum sensitivity, the detector zone should be operated at the lowest temperature possible (limited by highest boiling components condensing inside the detector).

  • Page 148: Analyzing For Hydrogen, Special Considerations

    Detector Systems Thermal conductivity detector (TCD) Note that TCD response becomes relatively flat (insensitive) to reference gas flow rates equal to, or somewhat greater than, flow rate through the column. Analyzing for hydrogen, special considerations Only H has thermal conductivity greater than He. However, binary mixtures of small amounts of H (<...

  • Page 149: Tcd•to•fid Series Connection, Filament Passivation

    Detector Systems Thermal conductivity detector (TCD) TCD-to-FID series connection The following describes, for a TCD whose exhaust vent returns to the inside of the oven, connecting the TCD to an FID. If necessary (see NOTE below), exchange the standard FID jet for the 0.030•inchjet (Part No.

  • Page 150: Capillary Column Considerations

    Detector Systems Thermal conductivity detector (TCD) filament. The immediate symptom is a permanent change in detector sensitivity due to change in filament resistance. If possible, such offending materials should be avoided. If this is not possible, the filament may have to be replaced frequently. Capillary column considerations The TCD cell filament channel has an internal volume of about 3.5 This small cell volume makes it suitable for use with capillary columns.

  • Page 151: Flame Photometric Detector (fpd), Optimizing Fpd Sensitivity And Selectivity

    A suggested way to set near•optimalflows is to begin with recommended flow rates located in the HP 5890 Operating Manual. Then vary each gas until a local maximum is reached. Optimize hydrogen first, then air (or oxygen), and lastly the auxiliary nitrogen flows.

  • Page 152

    Detector Systems Flame photometric detector (FPD) Figure 7-11 Flow ml/min FPD Flows versus Supply Pressures B. Detector Temperature. Detector heated zone temperature can have a significant effect on sensitivity. If analyzing thermally labile or very unstable compounds, a lower heated zone temperature may give the best results.

  • Page 153: Flame Ignition Problems

    Detector Systems Flame photometric detector (FPD) Flame ignition problems Two common flame ignition problems are: A loud pop results on ignition and the flame will not light or stay lit. If a loud pop occurs on ignition, it is usually caused by an incorrect ignition sequence.

  • Page 154

    Detector Systems Flame photometric detector (FPD) 3. Under some operating conditions, it is important to continue to hold the ignitor switch in for several seconds after opening the hydrogen valve fully counterclockwise. 4. Under some operating conditions, the flame may be more easily lit with the rubber drip tube removed.

  • Page 155: Chapter 8 — Preventive Maintenance

    Preventive Maintenance...

  • Page 156: Conditioning Columns

    Preventive Maintenance This chapter includes maintenance, cleaning, and leak•testingHP 5890 SERIES II (hereafter referred to as HP 5890) inlet and detector systems. Conditioning columns Columns may contain contaminants; conditioning drives off unwanted volatiles, making the column fit for analytical use.

  • Page 157

    Preventive Maintenance Conditioning columns back of nut). Adjust the septum purge flow rate to no more than 6 ml/min. c. Cap inlet fittings into detector(s) to prevent entry of air and/or contaminants. 3. Establish a stable flow of carrier gas through the column. He is preferred;...

  • Page 158: Re)packing Columns

    Preventive Maintenance (Re)Packing columns (Re)Packing columns In packing columns (particularly 1/4•inchglass columns), one must consider the type of packing, column bore, and type (metal or glass), the method of sample introduction (flash vaporization or on•column),inlet or detector base requirements. The method of sample introduction and/or the inlet/detector configuration determines the distance from the column end at which packing should start.

  • Page 159: Changing Septa, Packed Column Inlet

    Preventive Maintenance Packed column inlet Packed column inlet Changing septa Septum lifetime is dependent upon frequency of use and upon needle quality; burrs, sharp edges, rough surfaces, or a blunt end on the needle decreases septum lifetime. A leaking septum is evidenced by longer retention times, loss of response, and/or loss of column head pressure as well as degradation in detector signal quality (the signal becoming increasingly noisy).

  • Page 160: Insert/liner Care, Leaks

    Preventive Maintenance Packed column inlet Caution Column flow is interrupted while changing septa; since some columns may be damaged at elevated temperature without carrier flow, cool the oven to ambient before proceeding. Exercise care! The oven and/or inlet or detector fittings may be hot WARNING enough to cause burns.

  • Page 161

    Preventive Maintenance Packed column inlet 4. Fully open the mass flow controller counterclockwise and wait 1 to 2 minutes to ensure equilibrium. 5. Turn off gas to the inlet at its source. 6. Wait 10 minutes while observing carrier source pressure. If it drops less than 7 to 14 kPa (1 to 2 psi), the system (through the inlet column fitting) is considered leak free.

  • Page 162: Cleaning

    Preventive Maintenance Packed column inlet Figure 8-3 Packed Column Inlet, Leak-Checking the Septum Cleaning Turn off the heated zone for the inlet and allow it to cool. Remove the septum retainer nut and septum; remove also the column and inlet liner. Using a suitable light source, illuminate the inside of the inlet from inside the oven while looking through the inlet from the top.

  • Page 163: Split/splitless Capillary Inlets, Changing Septa

    Preventive Maintenance Split/splitless capillary inlets Split/splitless capillary inlets Changing septa For a conventional disk•typeseptum, lifetime is dependent upon needle quality; needles should be sharply pointed and free of burrs or rough surfaces. Choice of septum material is less critical than with a packed column inlet since the septum is continually purged.

  • Page 164: Insert Care

    Preventive Maintenance Split/splitless capillary inlets 1. Loosen and remove the septum retainer nut. Remove and discard the old septum, found either in the top of the inlet or inside the septum retainer nut. Figure 8-4 Septum Replacement, Split/Splitless and Split-Only Capillary Inlet 2.

  • Page 165: Leaks

    Preventive Maintenance Split/splitless capillary inlets Leaks For proper inlet operation, it is essential the entire system be leak•tight. The following procedure should be performed in initial checkout, or any time a leak is suspected. 1. Switch off detector! 2. Install an inlet plug (a paper clip or similar•gaugewire) in the same manner as a capillary column.

  • Page 166

    Preventive Maintenance Split/splitless capillary inlets 6. Turn off flow to the inlet by turning off carrier gas at the flow controller (fully clockwise, turning it only until it bottoms, and then no further). 7. Adjust the back pressure regulator clockwise, an additional 1/4•turn or set the electronic pressure control to 145 kPa (21 psi) and observe column pressure at the gauge for about ten minutes.

  • Page 167

    Preventive Maintenance Split/splitless capillary inlets Use leak detection fluid to check for leakage at the column nut. If leakage is observed, try tightening the nut first. If leakage continues, replace the ferrule. Note that if the inlet is hot, leak detection fluid may boil, giving false indication of a leak.

  • Page 168

    Preventive Maintenance Split/splitless capillary inlets Figure 8-7 Solenoid Valve, Split/Splitless Capillary Inlet Cleaning Turn off the heated zone for the inlet and allow it to cool. Remove septum retainer nut, septum, insert retainer nut, and inlet insert; also remove the column. Using a suitable light source, illuminate the inside of the inlet.

  • Page 169: Liner And/or Insert Care, Glass Inserts

    Preventive Maintenance Liner and/or insert care Liner and/or insert care Regardless of the inlet system, inlet inserts and/or liners must be kept clean for optimum performance, particularly their interiors from which contamination may enter the column and/or interact with sample components.

  • Page 170: Repacking A Split Insert

    If they must be used, thorough cleaning (chemical and physical) is required. Use a fresh, small amount of a conventional coated packing such as 2% OV•1on 100/120 mesh, Chromosorb W•HP . Packing is held in place between plugs of silanized glass wool (Part No. 8500•1572).

  • Page 171: Metal Inserts And/or Liners, Flame Ionization Detector (fid)

    Preventive Maintenance Flame ionization detector (FID) Metal inserts and/or liners Do not use concentrated acid(s) on metal inserts or liners! The insert is washed with noncorrosive solvents (H O, CH OH (methanol), (CH ) CO (acetone), CH Cl (methylene chloride), etc), and then dried thoroughly in an oven at 105 C.

  • Page 172: Jet Exchange/replacement

    Preventive Maintenance Flame ionization detector (FID) Jet exchange/replacement Depending upon the column type to be used, and/or analyses to be performed, exchanging the jet in an FID may be necessary. Figure 8-9 Flame Ionization Detector Note: The proper jet must be installed prior to column installation. If switching from packed column operation to capillary operation, the jet for capillary use must be installed prior to column installation.

  • Page 173

    Preventive Maintenance Flame ionization detector (FID) Table 8-1. Available FID/NPD Jets Part No. 18789-80070 18710-20119 19244-80560 * Measured at the jet tip. NOTE: The 0.011-inch jet optimizes performance with capillary columns. If used with packed columns, FID flame-out may occur with solvent peaks. Because jet exchange requires disassembling the collector assembly from the detector base, it is also a convenient opportunity to inspect the detector collector and base for contaminating deposits.

  • Page 174

    Preventive Maintenance Flame ionization detector (FID) Figure 8-10 Cover Removed, Flame Ionization Detector (FID) Turn off the detector and its heated zone; also turn off gases to the detector (particularly H !). Allow time for the detector zone to cool. Open the top cover at its front edge to access the detector.

  • Page 175

    Preventive Maintenance Flame ionization detector (FID) Wash the collector in distilled water, hexane, and/or CH OH (methanol). Dry in an oven at 70 C for at least 1/2•hour . Figure 8-11 FID Collector Assembly 4. Using a 1/4•inchhex nut driver, unscrew (counterclockwise) and remove the jet from the detector base.

  • Page 176

    Preventive Maintenance Flame ionization detector (FID) Figure 8-12 FID Jet 5. The jet exists in three sizes: 0.030•,0.018•,or 0.011•inch.Use a cleaning wire (0.016•inchod, 12•inchlength, Part No. 18765•20070)to loosen/remove internal deposits. Be careful in using the wire with the 0.011•inchjet. Wash both the internal bore and exterior of the jet with a 1:1 (V/V) solution of CH OH (methanol) and (CH ) CO (acetone).

  • Page 177: Ignition Problems

    Preventive Maintenance Flame ionization detector (FID) Figure 8-13 FID Signal Board Interconnect 9. Reassemble the detector cover. Ignition problems Before proceeding, make sure that gases are plumbed correctly, the system is leak•free,flow rates are set correctly, and external lines have been well purged.

  • Page 178

    Preventive Maintenance Nitrogen-phosphorus detector (NPD) is best to have a new jet on hand to exchange if a damaged jet is suspected. Nitrogen-phosphorus detector (NPD) In addition to the detector itself, other systems associated with the detector may also require routine maintenance. Nitrogen•phosphorusdetectors use H WARNING no column is connected to the detector inlet fitting, H...

  • Page 179

    Preventive Maintenance Nitrogen-phosphorus detector (NPD) Turn off the detector and its heated zone; also turn off gases to the detector (particularly H ! ). Allow time for the detector zone to cool. Open the top cover at its front edge to access the detector. 1.

  • Page 180

    Preventive Maintenance Nitrogen-phosphorus detector (NPD) 2. a. Using compressed air or N , blow out loose material from inside the collector. Do this carefully so as not to disturb the active element. Do not attempt to clean the inside of the collector by inserting objects Caution such as wires or brushes;...

  • Page 181: Removing/replacing The Npd Collector

    Preventive Maintenance Nitrogen-phosphorus detector (NPD) Caution Do not overtighten the jet! Overtightening may permanently deform and damage the jet, the detector base, or both. 8. Replace the NPD collector, and transformer and cover assembly. Be certain the spring contact to the signal board is in good contact with the groove on the collector (see Figure 8•13).During reassembly do not touch the lower portion of the collector assembly because fingerprints and/or other contamination may (will) cause baseline...

  • Page 182

    Note: During disassembly do not touch the lower portion of the collector assembly. Use clean, lint•freegloves to prevent contamination of the assembly. Suitable gloves (HP Part No. 8650•0030)are available. 1. Following the procedure under Cleaning, remove the collector assembly from the detector base. A 1.5•mmhex wrench is required for disassembly.

  • Page 183

    Preventive Maintenance Nitrogen-phosphorus detector (NPD) 3. Remove the Teflon spacer and stainless steel spring spacer from the top of the collector body. 4. Loosen the setscrew in the Teflon portion of the collector body. 5. Grasping the collector at its top end (to avoid contaminating its detecting end), withdraw it from the collector body.

  • Page 184: Type B Npd Transformer/collector Assembly

    Caution assembly. Use clean, lint•freegloves to prevent contamination of the assembly. Suitable gloves (HP Part No. 8650•0030)are available. 1. Remove the two screws holding the transformer inside the cover. 2. Remove the two screws holding the collector insulator to the cover.

  • Page 185

    Preventive Maintenance Nitrogen-phosphorus detector (NPD) 4. Remove the collector from the collector assembly as follows: Loosen the 1.5•mmscrew holding the transformer secondary wire to the top of the collector and disconnect the wire. The hex key wrench required is a 1.5•mmsize and was provided with the instrument. Loosen the 1.5 hex key screw holding the brass connector to the collector top and remove the brass connector.

  • Page 186: Reinstallation

    Preventive Maintenance Nitrogen-phosphorus detector (NPD) Reinstallation 1. Reinstall the jet in the detector base (using a 1/4•inchnut driver). Make sure that the threads are clean and free of burrs that could cause damage. If there is any binding, the cause should be determined and corrected before proceeding.

  • Page 187

    Preventive Maintenance Nitrogen-phosphorus detector (NPD) All collectors should be washed off with GE grade hexane or a similar solvent before reinstalling in the instrument to remove any grease, fingerprints, or other contaminants. Soak the entire collector in a vial of hexane for several minutes (2-10).

  • Page 188: Frequency Test, Electron Capture Detector (ecd), Carrier Gas Evaluation

    Preventive Maintenance Electron capture detector (ECD) Electron capture detector (ECD) Frequency test Note: For high sensitivity operation, and starting from a cold system, 24 hours may be necessary before baseline is completely stabilized. Use low•bleedsepta and condition a new septum prior to use in an unused inlet for several hours with 1 to 5 ml/min carrier flow rate.

  • Page 189

    ECD. If a capillary column was installed, remove also the makeup gas adapter in the detector base. 2. Disconnect the carrier gas source line at its fitting on the HP 5890. 3. Using a Vespel ferrule, and adapters as necessary, connect the carrier source line to the detector base, including any traps in the line.

  • Page 190: Thermal Cleaning

    Preventive Maintenance Electron capture detector (ECD) flow through the system is available. Allow time for the system to become fully pressurized. 4. Close carrier gas flow at its source and monitor system pressure. 5. The system may be assumed to be leak•freeif no pressure drop is observed over a 10•minuteperiod.

  • Page 191: Packed Column, Capillary Column

    Preventive Maintenance Electron capture detector (ECD) Packed column: 1. Close the anode purge on/off valve. 2. Remove the column from the detector; install in its place an empty glass column. 3. Establish normal carrier gas flow rate (20 to 30 ml/min); set oven temperature to 250 C.

  • Page 192: Radioactivity Leak Test (wipe Test), Thermal Conductivity Detector (tcd), Cleaning

    More frequent tests may be conducted when necessary. The procedure used is the wipe test. A wipe test kit (Part No. 18713•60050)is supplied with each new ECD. Its contents are listed in Table 8•2: Table 8-2. HP 5890 Radioactivity Leak Test (Wipe Test) Kit Item Description Envelope...

  • Page 193: Flame Photometric Detector, Cleaning/replacing Fpd Windows, Filters, Seals

    Preventive Maintenance Flame photometric detector Caution Failure to turn off the TCD and to cap the detector column fitting may cause irreparable damage to the filament due to O detector. 3. Establish normal reference gas flow rate (20 to 30 ml/min) through the detector (set oven temperature to 250 C).

  • Page 194

    Preventive Maintenance Flame photometric detector Likewise, damage to the PMT window cannot be tolerated; if necessary, replace the PMT or call Hewlett•Packardsupport. 1. Remove four screws to remove the PMT adapter flange. Remove the adapter carefully; a quartz window is exposed and may fall out. The window is cleaned in a manner similar to the filter.

  • Page 195

    Preventive Maintenance Flame photometric detector Figure 8-20. Subassembly Parts Identification O-ring 3 to 6 mm 4 Places...

  • Page 196

    Preventive Maintenance Flame photometric detector Figure 8-21. Item Description Weldment, Base Gigabore Liner/Ferrule Assembly (see note) Lockwasher Lower Heater Block Weldment, Transfer Tube Nut, Brass, 1/4-inch id Ferrule, Vespel, 1/4-inch id O-ring-Kalrez, Transfer Tube Weldment, Jet O-ring-Kalrez, Jet Cartridge Heater/Sensor Assembly Spacer, Ignitor Glow Plug O-ring-Kalrez, Ignitor...

  • Page 197: Cleaning/replacing The Fpd Jet

    Preventive Maintenance Flame photometric detector NOTE: Once installed, the ferrule cannot be removed from the liner for reuse unless both parts are still warm. Cleaning/replacing the FPD jet If a response problem is encountered (sensitivity, noise, selectivity), the FPD jet should be inspected for deposits and, if necessary, cleaned or replaced.

  • Page 198: Fpd Leak Testing (gc With Electronic Flow Sensor)

    Preventive Maintenance Flame photometric detector 6. Use compressed gas, air, or N and/or detector module body. 7. Inspect and clean deposits from the jet bore and from the threads using a suitable wire. If the jet is damaged in any way, it should be replaced.

  • Page 199: Fpd Leak Testing (gc Without Electronic Flow Sensor)

    Preventive Maintenance Flame photometric detector this indicates a leak in the system. Begin checking possible leak sources and monitor the EFS to determine when the leak has been eliminated. Possible leak sources, in order of probability are: 1. septum 2. column fittings 3.

  • Page 200: Conditioning Chemical Traps

    Preventive Maintenance Conditioning chemical traps Conditioning chemical traps Remove the trap from its installed location and attach it to a clean, dry gas source (helium or nitrogen). Attach the 1/8•inchend (male) of the chemical trap assembly to the reconditioning gas source using a graphite or a graphitized Vespel ferrule (Part No.

  • Page 201: Chapter 9 — Chromatographic Troubleshooting

    Chromatographic Troubleshooting...

  • Page 202: Introduction, Baseline Symptoms, Position

    Introduction This chapter is concerned with diagnosis: the process of going from unexpected behavior of the HP 5890 SERIES II (hereafter referred to as HP 5890) (symptoms) to the probable location of the difficulty (causes). Problems arise from many causes. Some of these are:...

  • Page 203: Wander And Drift

    Chromatographic Troubleshooting Baseline symptoms It can also result from valve operations: If valves are being switched during a run, examine the valve time program to see if the change coincides with a valve operation. This symptom also can occur if the septum suddenly begins to leak;...

  • Page 204: Noise

    Chromatographic Troubleshooting Baseline symptoms 2. Baseline is erratic, moves up and down (wander): Suspect a leak in the system: Check septum condition and replace if necessary. Check column connections. If the leak is at the detector end of the column, retention times are stable from run to run, but sensitivity is reduced.

  • Page 205

    Chromatographic Troubleshooting Baseline symptoms Contaminated detector gases (hydrogen and air). Air currents from a fan or air conditioner blowing across the top of the instrument may interfere with gas exiting from the detector. This is a possible, though not very likely, cause of noise since detectors are well protected.

  • Page 206: Spiking

    Loose or dirty contacts between printed circuit boards and their connectors may be responsible. Read appropriate sections regarding servicing boards and connectors for the HP 5890. 2. Spikes appear on chromatograms but not when the recorder is isolated (no input signal):...

  • Page 207: Retention Time Symptoms, Retention Time Drift, Retention Time Wander (reproducibility)

    Chromatographic Troubleshooting Retention time symptoms Retention time symptoms Retention time drift Retention time drift is a steady increase or decrease of retention times in successive runs. Erratic times (both directions) are discussed below as retention time wander. 1. In a series of runs, retention times suddenly increase: This may be due to an oven temperature change or to change in flow;...

  • Page 208

    Chromatographic Troubleshooting Retention time symptoms 2. Reproducibility is good early in the run but not toward the end: This may occur in temperature•programminga very densely packed column; as column contents expand with heating, resistance to flow may be so great that a mass flow controller cannot maintain constant flow.

  • Page 209: Peak Symptoms, No Peaks, Inverted Peaks, Extra Peaks

    Chromatographic Troubleshooting Peak symptoms Peak symptoms No peaks This is usually due to operator error; possibilities include injection on the wrong column, incorrect signal assignment, attenuation too high (peaks are present but not visible), a bent syringe needle in an automatic sampler, etc.

  • Page 210

    Chromatographic Troubleshooting Peak symptoms stationary phase with trace levels of O , H O, and/or other materials present in the carrier gas. A contaminated inlet may also produce ghost peaks. Residues in the inlet are volatilized or pyrolyzed and swept onto the head of the column.

  • Page 211: Deformed Peaks

    Chromatographic Troubleshooting Peak symptoms Deformed peaks The ideal peak, rarely occurring in chromatography, is a pure Gaussian shape. In practice, some asymmetry is always present, particularly near the baseline. 1. The peak rises normally, then drops sharply to baseline: Figure 9-1. Overloaded Peak The most likely cause is column overload;...

  • Page 212

    Chromatographic Troubleshooting Peak symptoms Interaction with column material is a frequent cause. Silanized support may help. An all•glasssystem may be required if metal column tubing is the source. Column overload with a gas sample often shows this effect; try injecting less. This may be a merged peak situation: Running at lower (30 C) oven temperature will increase resolution, perhaps enough to reveal merged peaks.

  • Page 213

    Chromatographic Troubleshooting Peak symptoms 4. Top (apex) of the peak is split: Figure 9-4. FID/NPD Flameout, or TCD with H (in He Carrier) Verify that this is not a merged peak situation: Reduce oven temperature 30 C and repeat the run. If the split peak becomes better resolved, it is probably a merged pair.

  • Page 214: Troubleshooting Valve Systems, Chromatographic Symptoms

    Chromatographic Troubleshooting Troubleshooting valve systems Troubleshooting valve systems Chromatographic symptoms Troubleshooting valves and their related plumbing is primarily a matter of systematic checking and verification of unimpaired mechanical operation of any moving part. This requires an understanding of how the valve functions internally and how the plumbing is configured.

  • Page 215

    Chromatographic Troubleshooting Troubleshooting valve systems Loss of peaks in specific areas of the chromatogram Entire sections of chromatographic data can be lost due to a valve that does not rotate or one that rotates improperly. Other than obvious component failures (i.e., solenoid, actuator, etc.), generally improper adjustments and misalignments cause most problems.

  • Page 216: Locating Leaks

    Chromatographic Troubleshooting Locating leaks Extraneous peaks Air peaks are sometimes seen in a chromatogram when leakage occurs because the valve rotor does not seal properly. These leaks may not be detectable by using the soap•bubblemethod. The leak test procedure is described in the Site Prep and Installation Manual.

  • Page 217: Pressure Check

    Chromatographic Troubleshooting Pressure check Pressure check The pressure•checkmethod will indicate, but sometimes not isolate, a leak in the flow path. Since this method does not necessarily isolate the leak, one of the leak•checkmethods may be needed to locate the leak specifically.

  • Page 218: Electronic Pressure Control

    Not Ready light flickers (oscillating pressure) Pressure not controllable If you have checked these possible causes and still have a problem, call HP Service. Possible Cause 1. Septum leaks or is missing 2. Column is broken 3. Column ferrule seal leaks 4.

  • Page 219: Safety Shutdown

    Chromatographic Troubleshooting Electronic pressure control Safety shutdown Systems equipped with electronic pressure programming have a safety shutdown feature to prevent gas leaks from creating a safety hazard. If the system cannot reach a pressure setpoint it beeps. After about 45 seconds the beep will stop and the message: will appear on the display, and the system will shut down by turning off all electronic pressure and heated zones, and locking the keyboard.

  • Page 220: Proper Configuration

    Chromatographic Troubleshooting Electronic pressure control Proper configuration If the inlet is not working at all, there may be a configuration problem. 1. Turn GC power off, and remove the side panel of the GC. 2. Check if the red switches on the inlet controller board are set for your configuration.

  • Page 221: Switch Setting Examples

    Chromatographic Troubleshooting Electronic pressure control Switch setting examples IN A1 or IN B1 IN A0 or IN B0 MODE A or MODE B EPC A or EPC B EXAMPLE INLET B = Split/Splitless Inlet with Electronic Pressure Control INLET A = Any Non-Electronic Pressure Controlled Inlet LEFT = OPEN RIGHT = CLOSED IN B1...

  • Page 222

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  • Page 223: Chapter 10 — Test Sample Chromatograms

    Test Sample Chromatograms...

  • Page 224: Test Sample Chromatograms

    If not, consult the HP 5890 SERIES II Operating Manual as necessary before proceeding with test chromatogram procedures. Note that injection volumes listed with operating conditions in the following chromatograms do not necessarily indicate total absolute volume injected.

  • Page 225: Test Sample Chromatograms

    Fin Temp Fin Time Range 8 COLUMN: Part No. 19095(#100) Dimensions Sta Phase Methyl Silicone START Flame Ionization Detector (FID) HP 5890 Test Sample Operating Conditions FLOW RATES Carrier (He) Hydrogen Makeup (N2) Split Vent Septum Purge DEGREES C SAMPLE: Type Inj Volume Part No.

  • Page 226

    Test Sample Chromatograms Test sample chromatograms Figure 10-2. HP 5890 Test Sample Operating Conditions Detector Type NPD (or NPDw/MUG) Temp 220 DEGREES C Inlet Type PACKED (OR PURGED PACKED). Temp 170 DEGREES C Operating Mode Purge Time On Purge Time Off...

  • Page 227

    Range 2 COLUMN: Part No. 19095S(#100) Dimensions Sta Phase Methyl Silicone START STOP Electron Capture Detector (ECD) HP 5890 Test Sample Operating Conditions FLOW RATES Carrier (N2) Hydrogen Makeup (N2) Split Vent Septum Purge DEGREES C SAMPLE: Type Inj Volume Part No.

  • Page 228

    Test Sample Chromatograms Test sample chromatograms Figure 10-4. HP 5890 Test Sample Operating Conditions Detector Type TCD(or TCDw/MUG) Temp 300 DEGREES C Inlet Type PACKED (OR PURGED PACKED). Temp 250 DEGREES C Operating Mode Purge Time On Purge Time Off...

  • Page 229

    Test Sample Chromatograms Test sample chromatograms Figure 10-5. HP 5890 Test Sample Operating Conditions Detector Type FIDw/MUG Temp 250 DEGREES C Inlet Type Ded On-Col Cap Oven Track Temp N/A Operating Mode Purge Time On Purge Time Off Oven Temp Temp Programmed (1...

  • Page 230

    Test Sample Chromatograms Test sample chromatograms Figure 10-6. HP 5890 Test Sample Operating Conditions Detector Type FIDw/MUG Temp 250 DEGREES C Inlet Type SPLIT ONLY OR SPLIT/SPLITLESS Temp Operating Mode SPLIT(PURGE ON) Purge Time On Purge Time Off Oven Temp Programmed (1 ramp)

  • Page 231

    Test Sample Chromatograms Test sample chromatograms Figure 10-7. HP 5890 Test Sample Operating Conditions Detector Type NPD w/MUG Temp 220 DEGREES C Inlet Type Split only or split/splitless Temp 200 DEGREES C Operating Mode Split(Purge on) Purge Time On Purge Time Off...

  • Page 232

    Test Sample Chromatograms Test sample chromatograms Figure 10-8. HP 5890 Test Sample Operating Conditions Detector Type ECDw/MUG Temp 300 DEGREES C Inlet Type Split only or splitless Temp 200 DEGREES C Operating Mode Split(Purge on) Purge Time On Purge Time Off...

  • Page 233

    Test Sample Chromatograms Test sample chromatograms Figure 10-9. HP 5890 Test Sample Operating Conditions Detector Type TCDw/MUG Temp 300 DEGREES C Inlet Type Split only or split/splitless Temp 250 DEG C Operating Mode Split(Purge on) Purge Time On Purge Time Off...

  • Page 234

    Test Sample Chromatograms Test sample chromatograms Figure 10-10. HP 5890 Test Sample Operating Conditions Detector Type NPD w/MUG) Temp 220 DEGREES C Inlet Type Ded On-Col Cap Oven Track Temp N/A Operating Mode N/A Purge Time On Purge Time Off...

  • Page 235

    Test Sample Chromatograms Test sample chromatograms Figure 10-11. HP 5890 Test Sample Operating Conditions Detector Type TCDw/MUG Temp 300 DEGREES C Inlet Type Ded On-Col Oven Track Temp N/A Operating Mode Purge Time On Purge Time Off Oven Temp Programmed (1 ramp)

  • Page 236

    Test Sample Chromatograms Test sample chromatograms Figure 10-12. HP 5890 Test Sample Operating Conditions Detector Type ECDw/MUG Temp 300 DEGREES C Inlet Type Ded On-Column Oven Track Temp Operating Mode Purge Time On Purge Time Off Oven Isothermal Init Temp...

  • Page 237

    Test Sample Chromatograms Test sample chromatograms Figure 10-13. HP 5890 Test Sample Operating Conditions Detector Type FPD Temp 200 DEGREES C Inlet Type PACKED OR PURGED PACKED Temp 200 Operating Mode Purge Time On Purge Time Off Oven Temp Programmed (1 ramp)

  • Page 238

    Test Sample Chromatograms Test sample chromatograms Figure 10-14. HP 5890 Test Sample Operating Conditions Detector Type FPD Temp 200 DEGREES C Inlet Type SPLIT ONLY OR SPLIT/SPLITLESS Temp 200 Operating Mode Purge Time On Purge Time Off Oven Temp Programmed (1 ramp)

  • Page 239

    Test Sample Chromatograms Test sample chromatograms Figure 10-15. HP 5890 Test Sample Operating Conditions Detector Type FPD Temp 200 DEGREES C Inlet Type DED ON-COL CAP Oven Track Temp Operating Mode Purge Time On Purge Time Off Oven Temp Programmed (1 ramp)

  • Page 240

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  • Page 241: Index

    Index adapters, 17 detector, 22 ECD, 23 installation, 24 TCD, 23 alphanumeric display, 33 baseline problems noise, 204 position, 202 spiking, 206 wander and drift, 203 calibration electronic flow sensor, 60 oven temperature, 54 capillary columns, metal, 30 clear dot function, 39 cold trapping, 116 collector replacing NPD, 181...

  • Page 242

    Index electronic flow sensor (EFS) calibration, 60 packed inlet, 102, 106 electronic pressure control troubleshooting, entering setpoints, 34 fault: messages, 52 ferrules, 14 FID, 171 ignition problems, 177 jet replacement, 30, 172, 173 on•columntest chromatogram, 229 split inlet test chromatogram, 230 test chromatogram, 225 FID flameout problems, 128 fittings, 14...

  • Page 243

    Index leaks ECD, 189 FPD with EFS, 198 FPD without EFS, 199 packed column inlet, 160 pressure checking, 217 split/splitless capillary inlet, 165 valves, 216 LED display, 33 lighting problems, FID, 177 liners, 17 care of, 169 detector, 22 installation, 24 metal, 171 lock keyboard, 38 metal capillary columns, 30...

  • Page 244

    Index septum, changing packed column inlet, 159 split/splitless capillary inlet, 163 septum purge, packed inlet, 105 septum purged packed column inlet, 103 setpoint protection, 38 setpoints displaying, 33 entering, 34 ranges, 46 solvent effect, 114 solvent purity, 118 spiking problems, 206 split capillary inlet inserts, 27 split ratio, 112 split sampling, 111...

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5890 series ii

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