Benutzeranleitung / Produktwartung 5890 II Plus des Produzenten HP
Zur Seite of 244
Reference Manual HP 5890 Series II and HP 5890 Series II Plus.
Little Falls Site Hewlett-Packard Company 2850 Centerville Road Wilmington, DE 19808-1610 Hewlett-Packard Company 1989, 1990, 1991, 1993, 1994 All Rights Reserved. Reproduction, adaptation, or translation without permission is prohibited, except as allowed under the copyright laws.
Contents Chapter 1 — Columns and Fittings 9 ................. Column oven 11 .......................................................... Column placement 12 ................................................. Packed column 12 ..........................
Contents Chapter 4 — Electronic Flow Sensing 57 ............... Displaying gas flow rate 58 ............................................... Designating gas type 59 .................................................. Electronic flow sensor (EFS) calibration 60 .
Contents Chapter 6 — Inlet Systems 99 ......................... Packed column inlet 100 ................................................... Electronic flow sensor 102 .............................................. Septum•purgedpacked column inlet 103 .
Contents Chapter 8 — Preventive Maintenance 155 .............. Conditioning columns 156 .................................................. (Re)Packing columns 158 .................................................. Packed column inlet 159 ...........
Contents Chapter 9 — Chromatographic Troubleshooting 201 ...... Introduction 202 .......................................................... Baseline symptoms 202 .................................................... Position 202 .....................
T his pag e inte ntional l y le f t blank..
1 Columns and Fittings.
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.
Columns and Fittings Column oven 11 Column oven Inlet Ftg Det Ftg Nut Plate Figure 1-1 The Column Oven The oven door latch, located beneath the lower right corner of the door , is pressed upward to open the door .
Columns and Fittings Column oven 12 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 .
Columns and Fittings Column oven 13 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 .
Columns and Fittings Fittings 14 Column Hanger Part No. 1460-1914 Column Installed Installed Bracket for Hewlett-Packard Capillary Columns Figure 1-4. 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.
Columns and Fittings Fittings 15 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.
Columns and Fittings Fittings 16 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 .
Columns and Fittings Liners/adapters and inserts, general 17 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.
Columns and Fittings Liners/adapters and inserts, general 18 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 ty.
Columns and Fittings Liners/adapters and inserts, general 19 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.
Columns and Fittings Inlet/detector liners/adapters 20 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.
Columns and Fittings Inlet/detector liners/adapters 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 capillary column.
Columns and Fittings Inlet/detector liners/adapters 22 Detector liners/adapters Liner/Adapter Typical Installed Detector Liner/Adapter Figure 1-6 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.
Columns and Fittings Inlet/detector liners/adapters 23 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.
Columns and Fittings Inlet/detector liners/adapters 24 Liner/adapter installation 1/4-inch Ferrule Liner Liner Retainer Nut 1-mm Graphite Ferrule Capillary Column Nut Packed Column Inlet Liner for HP .
Columns and Fittings Inlet inserts 25 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.
Columns and Fittings Inlet inserts 26 Exercise care! the oven, and/or inlet, or detector fittings may be hot enough to cause burns. WARNING Flared End Insert Installing a Glass Insert in a Packed Column Inlet Figure 1-9 1. In handling the insert, avoid contaminating its surface (particularly its interior).
Columns and Fittings Inlet inserts 27 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 .
Columns and Fittings Inlet inserts 28 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.
Columns and Fittings Inlet inserts 29 Installation, Split/Splitless Capillary Inlet Insert Figure 1-11 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.
Columns and Fittings Jet replacement, FIDs or NPDs 30 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.
2 Keyboard and Displays.
32 Keyboard and Displays Alphanumeric Display Instrument Status Run Control Temperature Control Miscellaneous Functions Numeric and Modifier Keys Signal Definition and Control Oven Status SIG 2 ZERO TCD SENS DET SIG 1 B A OFF ON ENTER 7 8 9 6 5 1 2 3 - 0 .
Keyboard and Displays Displaying setpoints 33 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.
Keyboard and Displays Entering setpoints 34 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.
Keyboard and Displays Entering setpoints 35 T o display the function and its setpoint: necessary for a few instrument functions (Instrument Function Key) ( or ) A B then, EITHER ( through , , ) 0 9 - .
Keyboard and Displays Entering setpoints 36 CLEAR can be used anytime during an entry , prior to pressing ENTER ,t o erase the entry in progress. The * disappears, and the original setpoint display is restored.
Keyboard and Displays Keyboard operation, INET control 37 CLEAR is used anytime during setpoint entry , prior to pressing ENTER , to erase the entry in progress.
Keyboard and Displays Protecting setpoints 38 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.
Keyboard and Displays Loading default setpoints 39 W ith the keyboard locked, Figure 2•6shows the display occurring if a setpoint entry is attempted: ACTUAL SETPOINT KEYBOARD LOCKED KEYBOARD LOCKED .
Keyboard and Displays Loading default setpoints 40 Upon pressing ENTER , default setpoints are loaded into memory , erasing setpoints already present. T able 2•1 lists resulting HP 5890 default setpoints.
Keyboard and Displays Loading default setpoints 41 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.
T h is page intentio nall y le ft bl ank..
3 Temperature Control.
44 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.
Temperature Control 45 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.
Temperature Control Valid setpoint ranges 46 Valid setpoint ranges T able 3•1 lists valid setpoint ranges for the 13 keys controlling oven and heated zone temperatures. NOTE: TOTAL run time will not exceed 650.00 minutes regardless of values enter e , , and .
Temperature Control Cryogenic (sub-ambient) oven control 47 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.
Temperature Control Cryogenic (sub-ambient) oven control 48 Oven profile using CRYO, for operation during runs at subambient temperatures 25 50 75 (CRYO ON) CRYO OFF at ambient +15 CRYO ON at ambient + 25 Figure 3-4 Oven profile using CRYO BLAST, for very fast cool down between runs 40 80 120 CRYO BLAST OFF (30 sec.
Temperature Control Programming oven temperature 49 Programming oven temperature HP 5890 oven temperature programming allows up to three ramps, in any combination of heating or cooling.
Temperature Control Oven status 50 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.
Temperature Control Oven safety 51 In complex two• or three•rampoven temperature programs, information as to the part of the program in progress is monitored by pressing OVEN TEMP .
Temperature Control Fault: messages 52 The message displayed when this occurs is shown in Figure 3•6. ACTUAL SETPOINT WARN: OVEN SHUT OFF Message, Oven SHUT DOWN Figure 3-6 The oven remains off until switched on again via the keyboard ( OVEN TEMP ON ), unless a FAULT: message is displayed (see below , Fault: messages ).
Temperature Control After a power failure . . . 53 ACTUAL SETPOINT FAULT: OVEN > MAX+20 ACTUAL SETPOINT FAULT: OVEN TEMP RDG ACTUAL SETPOINT FAULT: DETA TEMP RDG ACTUAL SETPOINT FAULT: INJA TEMP RD.
Temperature Control Oven temperature calibration 54 INITIAL TIME RATE OVEN FINAL TIME STATUS RUN NOT READY ACTUAL SETPOINT PASSED SELF TEST Message Display, Power Failure and Recovery Figure 3-8 Heated zones return to their respective setpoint values, after which the oven returns to its setpoint value.
Temperature Control Oven temperature calibration 55 The HP 5890 provides the means to (if necessary) reset oven temperature monitoring so the displayed ACTUAL value accurately represents the correct temperature.
Temperature Control Oven temperature calibration 56 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.
4 Electronic Flow Sensing.
58 Electronic Flow Sensing T wo 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.
Electronic Flow Sensing Designating gas type 59 Designating gas type T o scale the displayed flow rate value properly , one of four commonly used gases must be designated.
Electronic Flow Sensing Electronic flow sensor (EFS) calibration 60 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 .
Electronic Flow Sensing Electronic flow sensor (EFS) calibration 61 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 .
Electronic Flow Sensing Electronic flow sensor (EFS) calibration 62 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.
Electronic Flow Sensing Electronic flow sensor (EFS) calibration 63 EFS Flow-Measuring Adapter (Part No. 05890-80620) Figure 4-3 5. Assuming there is no gas flow through the channel being calibrated, press ENTER at the keyboard. This updates the zero calibration value.
Electronic Flow Sensing Electronic flow sensor (EFS) calibration 64 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 TIME to access the timer function. After obtaining the desired flow rate, press: CLEAR .
Electronic Flow Sensing Electronic flow sensor (EFS) calibration 65 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.
T h is page intentio nall y le ft bl ank..
5 Signal Output.
68 Signal Output A standard signal channel, controlled via SIG 1 , always is provided. A second signal channel, controlled via SIG 2 , is provided if Option 550/ Accessory 19242A ( Communications Interface Board ), or Option 560/ Accessory 19254A ( RS•232 ), is installed.
Signal Output Zeroing signal output 69 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).
Signal Output Zeroing signal output 70 Self- ZERO setpoint Referencing Figure 5•2 for the +1 V output, note that using ZERO can increase dynamic range available for signal output by shifting an existing constant offset signal to a lower level (usually electrical zero).
Signal Output Zeroing signal output 71 Figure 5-3 1.0 mV maximum output level + 1.000 mV + 0.100 mV + 0.006 mV 0m V Constant 0.1 mV detector background HP 5890 SERIES II electrical zero signal 0.
Signal Output Signal attenuation 72 Note: If a self• ZERO determination is performed on an active signal exceeding the maximum permitted setpoint value for ZERO (see User•defined ZERO setpoint ), the maximum setpoint value is assigned and the message SIG 1 (or 2 ) ZERO TOO HIGH is displayed.
Signal Output Signal attenuation 73 Thus, signal output level at the +1 mV analog output may be set separately from that at the +1 V output. T able 5•2 gives values permitted for either function, and the output affected.
Signal Output Signal attenuation 74 For analytical information from a detector , proper settings for RANGE 2 () and ATTN 2 () 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.
Signal Output Signal attenuation 75 From T able 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 5 cover the entire useful output range for an ECD.
Signal Output Signal attenuation 76 Note that if RANGE 2 () or ATTN 2 () is pressed without first pressing SIG 1 or SIG 2 , SIGNAL 1 channel is assumed (and displayed). If desired, SIG 2 can then be pressed to display the same function for the SIGNAL 2 channel.
Signal Output Test signal output 77 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 .
Signal Output Test signal output 78 T o access this function, the following key sequence is entered: SIG 1 ( or SIG 2 ) 9 ENTER T est 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.
Signal Output Instrument network (INET) 79 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.
Signal Output Instrument network (INET) 80 Figure 5-6 OUT IN IN OUT OUT IN Sampler S/ECM Controller & Integrator 5890 HP 5890 SERIES II Gas Chromatograph Typical INET Loop Each INET must have one (and only one) device defined as the controller .
Signal Output Instrument network (INET) 81 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 .
Signal Output Instrument network (INET) 82 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.
Signal Output Instrument network (INET) 83 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.
Signal Output Instrument network (INET) 84 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 .
Signal Output INET configuration 85 Automatic INET reconfiguration In the following circumstances, INET automatically reconfigures under direction of the controller: Recovery from a power failure. Recovery from any particular device on the loop being switched off, then on again.
Signal Output INET configuration 86 Figure 5•8 shows displays resulting from the key sequence: CLEAR . 3 ENTER Switching between Global and Local W ith regard to the INET function at the HP 5890, there are two operating modes: global or local .
Signal Output INET configuration 87 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 .
Signal Output INET configuration 88 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 ).
Signal Output INET configuration 89 Figure 5•1 1 shows resulting displays. INET-HP 5890 Signal Definition ACTUAL SETPOINT GLOBAL ADDR: 8,31 ACTUAL SETPOINT SIG 2 OFF ACTUAL SETPOINT SIG 1 ON FULL RA.
Signal Output HP-IL loopback test 90 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 () . Dynamic range for FULL RANGE data is limited only by the detector itself.
Signal Output HP-IL loopback test 91 ACTUAL SETPOINT PASSED SELF TEST ACTUAL SETPOINT FAILED SELF TEST ACTUAL SETPOINT HPIL LOOPBACK TEST HPIL LOOPBACK TEST Displays Figure 5-12 The message PASSED SELF TEST indicates INET , at least with respect to the HP 5890, is performing satisfactorily .
Signal Output Warn: and fault: messages 92 Warn: and fault: messages ACTUAL SETPOINT FAULT: INET CPU RAM ACTUAL SETPOINT FAULT: INET CPU ACTUAL SETPOINT FAULT: INET RAM TEST ACTUAL SETPOINT FAULT: INE.
Signal Output Warn: and fault: messages 93 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.
Signal Output File compatibility with data handling devices 94 File compatibility with data handling devices Y ou 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.
Signal Output File compatibility with data handling devices 95 ACTUAL SETPOINT HP 5890A mode ACTUAL SETPOINT HP 5890 SERIES II mode EMULATION MODE OK PASSED SELF TEST GC Displays for File Transfer Modes Figure 5-14 How do I change modes? 1. T urn power off .
Signal Output File compatibility with data handling devices 96 P15 Main PC Board P13 P12 P5 P6 P2 P3 Finding component P15 on the Main PC Board. Figure 5-16 4.
Signal Output File compatibility with data handling devices 97 How to convert HP 339X Integrator workfiles from 5890A to SERIES II mode: 1. T urn 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 .
T h is page intentio nall y le ft bl ank..
6 Inlet Systems.
100 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•purged packed column inlet Split/splitless capillary inlet For cool on•columninformation, see the manual Programmable Cool On•ColumnInlet.
Inlet Systems Packed column inlet 101 Septum Liner Glass Insert Carrier Gas Column Septum Retainer Nut Graphite Ferrule Swage-type Nut and Ferrules Packed Column Inlet Figure 6-1.
Inlet Systems Packed column inlet 102 Trap(s) External Plumbing Internal Plumbing Pressure Gauge Packed Column Inlet Electronic Flow Sensor (optional) Mass Flow Controller Column To Detector Carrier Gas Flow Diagram, Packed Column Inlet (with electronic flow sensor) Figure 6-2 Liquid sample is rapidly volatilized inside the inlet.
Inlet Systems Packed column inlet 103 Assuming the system to be leak•free(and if total flow is < 200 ml/min), after setting the desired column flow rate, total flow through the system should be noted via the EFS.
Inlet Systems Packed column inlet 104 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.
Inlet Systems Packed column inlet 105 10 20 30 40 60 70 80 90 50 50 100 150 200 250 300 350 400 Bottom of Sep- tum Syringe Tip Base of Injection Port Temperature in Gas Stream — C 35 C Ove n 150 C O.
Inlet Systems Packed column inlet 106 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 T eflon•coatedO•ring sealing the purge cavity should be replaced.
Inlet Systems Split/splitless capillary inlet 107 Split/splitless capillary inlet 1 23 Insert 1, 2, or 3 Sealing O-Ring Split Direct Injection Splitless 1/4” Packed Glass Column Packed Metal Column Sealing O-Ring 4 A. CAPILLARY COLUMN B. PACKED COLUMN Item Part No.
Inlet Systems Split/splitless capillary inlet 108 The multiple•mode split/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•component analyses.
Inlet Systems Split/splitless capillary inlet 109 In general, the carrier gas is chosen to maximize component resolution and detector performance while minimizing overall analysis time.
Inlet Systems Split/splitless capillary inlet 110 V an 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 2 occur at much higher average linear velocities than N 2 .
Inlet Systems Split/splitless capillary inlet 111 Nominal ID (mm) 12 25 50 0.20 135 223 347 0.32 45 82 137 0.53 11 23 42 Nominal Length (m) It must be emphasized that values in this table are recommended as starting points only ! Values listed are independent of carrier gas used.
Inlet Systems Split/splitless capillary inlet 112 IN OUT IN OUT GA External Plumbing Internal Plumbing Trap(s) Carrier Gas Mass Flow Controller Electronic Flow Sensor (optional) To Detector Solenoid Valve Back- pressure Regulator Split Vent Septum Purge Vent Pressure Gauge Septum Purge Control Capillary Inlet Column (C) (P) (S) COM N.
Inlet Systems Split/splitless capillary inlet 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.
Inlet Systems Split/splitless capillary inlet 114 Splitless sampling For splitless operation, the dilute sample is vaporized inside the inlet insert. Most of the sample is then swept onto the column.
Inlet Systems Split/splitless capillary inlet 115 Low Volatility Solute High Volatility Solute Column Carrier Gas Needle (a) (b) (c) (d) The Solvent Effect Figure 6-9 The solvent effect is described in great detail elsewhere: see Grob, K. and Grob, K.
Inlet Systems Split/splitless capillary inlet 116 Solvent Boiling Point ( C) Suggested Initial Oven Temperature Range ( C) Diethyl Ether 36 10 to 25 n-Pentane 36 10 to 25 Methylene Chloride 40 10 to 3.
Inlet Systems Split/splitless capillary inlet 117 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.
Inlet Systems Split/splitless capillary inlet 118 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.
Inlet Systems Split/splitless capillary inlet 119 10 20 30 40 50 60 Area Counts + 1.2% Deviation + 1.2% Deviation ~ 20 ppm n-C 14 (Cold Trapped) ~ 10 ppm n-C 11 (Solvent Effect) Purge Activation Time, Sec Solvent: Isooctane Column: 16.5 m x 0.25 mm SE-54 80 C (0.
Inlet Systems Split/splitless capillary inlet 120 IN OUT IN OUT GA External Plumbing Internal Plumbing Trap(s) Carrier Gas Mass Flow Controller Electronic Flow Sensor (optional) To Detector Solenoid Valve Back- pressure Regulator Split Vent Septum Purge Vent Pressure Gauge Septum Purge Control Capil- lary Inlet Column (C) (P) (S) N.
Inlet Systems Split/splitless capillary inlet 121 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.
Inlet Systems Split/splitless capillary inlet 122 2. W ipe excess solvent from the syringe needle. 3. W ithout introducing air , draw in excess sample. 4. Position the syringe plunger for the required injection volume. W ipe excess sample from the needle.
7 Detector Systems.
124 Detector Systems This chapter provides information for the five HP 5890 SERIES II (hereafter referred to as HP 5890) detector systems: Flame Ionization Detector (FID) Nitrogen•Phosphorus Detecto.
Detector Systems FID and NPD jets 125 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 .
Detector Systems Flame ionization detector (FID) 126 Flame ionization detector (FID) Inlet H 2 Inlet FID Collector Assembly Jet Flame Ionization Detector (FID) Figure 7-1 The flame ionization detector (FID) responds to compounds that produce ions when burned in a H •airflame.
Detector Systems Flame ionization detector (FID) 127 Compounds producing little or no response include: Rare gases N N Nitrogen Oxides CO *CCl Silicon Halides CO H OC S NH O * Measured at the jet tip. This selectivity can be advantageous: for example, H Oo rC S , used as solvent, do not produce large solvent peaks.
Detector Systems Flame ionization detector (FID) 128 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).
Detector Systems Nitrogen-phosphorus detector (NPD) 129 Nitrogen-phosphorus detector (NPD) NPD Collector Assembly Air Inlet H 2 Inlet NPD Collector Active Element Jet Nitrogen-Phosphorus Detector (NPD.
Detector Systems Nitrogen-phosphorus detector (NPD) 130 H and air are required, but at flows significantly less than those for an FID. Normal FID•type ionizations are therefore minimal, so response to compounds not containing nitrogen or phosphorus is reduced.
Detector Systems Nitrogen-phosphorus detector (NPD) 131 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.
Detector Systems Nitrogen-phosphorus detector (NPD) 132 Performance considerations Contamination V ery 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.
Detector Systems Nitrogen-phosphorus detector (NPD) 133 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 .
Detector Systems Nitrogen-phosphorus detector (NPD) 134 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•controlled inlet systems (capillary inlets) when temperature•programming the column.
Detector Systems Electron capture detector (ECD) 135 Electron capture detector (ECD) The effluent gas stream from the detector must be vented to a fume hood to prevent possible contamination of the laboratory with radioactive material. Specific cleaning procedures are provided in Chapter 8, Preventive Maintenance .
Detector Systems Electron capture detector (ECD) 136 In the extremely unlikely event that both the oven and the ECD heated zone should go into thermal runaway (maximum, uncontrolled heating in excess .
Detector Systems Electron capture detector (ECD) 137 Anode Purge Vent Makeup Gas Adapter Electron Capture Detector (ECD) Figure 7-5 Nickel Plating Fused Silica Liner Makeup Gas Column Plated 63 Ni Surface Anode The electron capture detector (ECD) cell contains Ni, a radioactive isotope emitting high•energyelectrons ( •particles).
Detector Systems Electron capture detector (ECD) 138 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.
Detector Systems Electron capture detector (ECD) 139 Chemical Type Hydrocarbons 1 Ethers, esters 10 Aliphatic alcohols, ketones, amines; 100 mono-Cl, mono-F compounds Mono-Br, di-Cl and di-F compounds.
Detector Systems Electron capture detector (ECD) 140 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.
Detector Systems Electron capture detector (ECD) 141 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.
Detector Systems Electron capture detector (ECD) 142 A very clean system may produce a value below the low end of 10 (100 Hz). T o correct this condition, an adjustment is made to the present potentiometer located on the ECD electronics board.
Detector Systems Thermal conductivity detector (TCD) 143 Thermal conductivity detector (TCD) 0 ml/min Switching Flow 1 (off) 30 ml/min Column Flow 30 ml/min Switching Flow 2 (on) 30 ml/min Switching F.
Detector Systems Thermal conductivity detector (TCD) 144 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.
Detector Systems Thermal conductivity detector (TCD) 145 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).
Detector Systems Thermal conductivity detector (TCD) 146 Optimizing performance The following sections aid in choosing operating parameters to obtain optimal TCD performance.
Detector Systems Thermal conductivity detector (TCD) 147 As Figure 7•9 shows, however , the lower the detector zone temperature, the greater is the temperature difference between the filament versus the surrounding detector body temperature.
Detector Systems Thermal conductivity detector (TCD) 148 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.
Detector Systems Thermal conductivity detector (TCD) 149 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.
Detector Systems Thermal conductivity detector (TCD) 150 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 .
Detector Systems Flame photometric detector (FPD) 151 Flame photometric detector (FPD) Optimizing FPD sensitivity and selectivity FPD sensitivity and selectivity are affected by several important parameters. These are listed below , with suggested ways to optimize for each application.
Detector Systems Flame photometric detector (FPD) 152 140 120 100 80 60 40 20 0 0 50 100 150 200 250 300 350 400 450 500 10 20 30 40 50 60 70 = Hydrogen = Nitrogen = Oxygen + = Air Pressure-psig Pressure-kPa Flow ml/min + + + + + FPD Flows versus Supply Pressures Figure 7-11 B.
Detector Systems Flame photometric detector (FPD) 153 Flame ignition problems T wo 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.
Detector Systems Flame photometric detector (FPD) 154 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.
8 Preventive Maintenance.
156 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.
Preventive Maintenance Conditioning columns 157 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.
Preventive Maintenance (Re)Packing columns 158 (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.
Preventive Maintenance Packed column inlet 159 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.
Preventive Maintenance Packed column inlet 160 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 enough to cause burns.
Preventive Maintenance Packed column inlet 161 4. Fully open the mass flow controller counterclockwise and wait 1 to 2 minutes to ensure equilibrium. 5. T urn off gas to the inlet at its source. 6. W ait 10 minutes while observing carrier source pressure.
Preventive Maintenance Packed column inlet 162 Packed Column Inlet, Leak-Checking the Septum Figure 8-3 Cleaning T urn 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 .
Preventive Maintenance Split/splitless capillary inlets 163 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.
Preventive Maintenance Split/splitless capillary inlets 164 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. Capillary Inlet Septum Replacement, Split/Splitless and Split-Only Capillary Inlet Figure 8-4 2.
Preventive Maintenance Split/splitless capillary inlets 165 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.
Preventive Maintenance Split/splitless capillary inlets 166 6. T urn 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).
Preventive Maintenance Split/splitless capillary inlets 167 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.
Preventive Maintenance Split/splitless capillary inlets 168 Solenoid Valve Assembly Solenoid Valve, Split/Splitless Capillary Inlet Figure 8-7 Cleaning T urn 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.
Preventive Maintenance Liner and/or insert care 169 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.
Preventive Maintenance Liner and/or insert care 170 Repacking a split insert Since, for a split insert, its packing material is discarded in cleaning, the insert must be repacked. Note: Repacking with small•diameterglass beads is not recommended: they are usually contaminated with metal filings due to sieving procedures used.
Preventive Maintenance Flame ionization detector (FID) 171 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.
Preventive Maintenance Flame ionization detector (FID) 172 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 . Flame Ionization Detector Figure 8-9 Note: The proper jet must be installed prior to column installation.
Preventive Maintenance Flame ionization detector (FID) 173 18789-80070 0.030 Packed Column Only (FID only: Simulated Distillation, TCD-to-FID series operation) 18710-20119 0.018 Packed Column (Standard, FID and NPD) 19244-80560 0.011 Capillary Column (FID and NPD) (FID: high sensitivity, packed column) Part No.
Preventive Maintenance Flame ionization detector (FID) 174 Collector Assembly Cover Removed, Flame Ionization Detector (FID) Figure 8-10 T urn off the detector and its heated zone; also turn off gases to the detector (particularly H !). Allow time for the detector zone to cool.
Preventive Maintenance Flame ionization detector (FID) 175 W ash the collector in distilled water , hexane, and/or CH OH (methanol). Dry in an oven at 70 C for at least 1/2•hour . FID Collector Assembly Figure 8-11 4. Using a 1/4•inchhex nut driver , unscrew (counterclockwise) and remove the jet from the detector base.
Preventive Maintenance Flame ionization detector (FID) 176 Je t FID Jet Figure 8-12 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.
Preventive Maintenance Flame ionization detector (FID) 177 Interconnect Sprin g FID Signal Board Interconnect Figure 8-13 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.
Preventive Maintenance Nitrogen-phosphorus detector (NPD) 178 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.
Preventive Maintenance Nitrogen-phosphorus detector (NPD) 179 T urn 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 .
Preventive Maintenance Nitrogen-phosphorus detector (NPD) 180 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.
Preventive Maintenance Nitrogen-phosphorus detector (NPD) 181 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 .
Preventive Maintenance Nitrogen-phosphorus detector (NPD) 182 Type A Type B NPD Collector and Collector Assembly Figure 8-17 Detector Cover Trans- former Brass Collar Steel Spring Spacer Teflon Spacer.
Preventive Maintenance Nitrogen-phosphorus detector (NPD) 183 3. Remove the T eflon spacer and stainless steel spring spacer from the top of the collector body .
Preventive Maintenance Nitrogen-phosphorus detector (NPD) 184 lead on the collector body . Tighten the setscrew to secure the wire and collar . Type B NPD transformer/collector assembly Type B NPD Detector Assembly Figure 8-18.
Preventive Maintenance Nitrogen-phosphorus detector (NPD) 185 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.
Preventive Maintenance Nitrogen-phosphorus detector (NPD) 186 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.
Preventive Maintenance Nitrogen-phosphorus detector (NPD) 187 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).
Preventive Maintenance Electron capture detector (ECD) 188 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.
Preventive Maintenance Electron capture detector (ECD) 189 remove the column to the 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.
Preventive Maintenance Electron capture detector (ECD) 190 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•free if no pressure drop is observed over a 10•minuteperiod.
Preventive Maintenance Electron capture detector (ECD) 191 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.
Preventive Maintenance Thermal conductivity detector (TCD) 192 Radioactivity leak test (wipe test) ECDs must be tested for radioactive leakage at least every six months. Records of tests and results must be maintained for possible inspection by the Nuclear Regulatory Commission and/or responsible state agency .
Preventive Maintenance Flame photometric detector 193 Caution Failure to turn off the TCD and to cap the detector column fitting may cause irreparable damage to the filament due to O 2 entering the detector . 3. Establish normal reference gas flow rate (20 to 30 ml/min) through the detector (set oven temperature to 250 C).
Preventive Maintenance Flame photometric detector 194 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.
Preventive Maintenance Flame photometric detector 195 AB C DE 8 5 2 1 11 4 6 7 9 10 16 6 7 15 14 12 13 19 20 21 22 3 27 4 Places O-ring (8) 3t o 6m m Subassembly Parts Identification Figure 8-20.
Preventive Maintenance Flame photometric detector 196 F G H 11 29 24 25 23 17 26 28 30 (4 Places) Item Description Part No. Qty 1 Weldment, Base 19256-80540 1 2 Gigabore Liner/Ferrule Assembly (see no.
Preventive Maintenance Flame photometric detector 197 NOTE: Once installed, the ferrule cannot be removed from the liner for reuse unless both parts are still warm.
Preventive Maintenance Flame photometric detector 198 6. Use compressed gas, air , or N 2 to blow out loose particles from the jet and/or detector module body . 7. Inspect and clean deposits from the jet bore and from the threads using a suitable wire.
Preventive Maintenance Flame photometric detector 199 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.
Preventive Maintenance Conditioning chemical traps 200 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 V espel ferrule (Part No.
9 Chromatographic Troubleshooting.
202 Chromatographic Troubleshooting 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).
Chromatographic Troubleshooting Baseline symptoms 203 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; A void the problem by changing septa regularly .
Chromatographic Troubleshooting Baseline symptoms 204 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.
Chromatographic Troubleshooting Baseline symptoms 205 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.
Chromatographic Troubleshooting Baseline symptoms 206 Spiking Spikes are isolated baseline disturbances, usually as sudden (and large) upscale movements. If accompanied by noise, the noise problem should be solved first, since spiking may disappear at the same time.
Chromatographic Troubleshooting Retention time symptoms 207 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 .
Chromatographic Troubleshooting Retention time symptoms 208 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 .
Chromatographic Troubleshooting Peak symptoms 209 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.
Chromatographic Troubleshooting Peak symptoms 210 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.
Chromatographic Troubleshooting Peak symptoms 211 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: Overloaded Peak Figure 9-1.
Chromatographic Troubleshooting Peak symptoms 212 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.
Chromatographic Troubleshooting Peak symptoms 213 4. T op (apex) of the peak is split: FID/NPD Flameout, or TCD with H (in He Carrier) Figure 9-4. V erify 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 .
Chromatographic Troubleshooting Troubleshooting valve systems 214 Troubleshooting valve systems Chromatographic symptoms T roubleshooting valves and their related plumbing is primarily a matter of systematic checking and verification of unimpaired mechanical operation of any moving part.
Chromatographic Troubleshooting Troubleshooting valve systems 215 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.
Chromatographic Troubleshooting Locating leaks 216 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.
Chromatographic Troubleshooting Pressure check 217 Pressure check The pressure•check method 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•check methods may be needed to locate the leak specifically .
Chromatographic Troubleshooting Electronic pressure control 218 Electronic pressure control The electronic pressure control option provides very accurate and precise control of column head pressure, resulting in retention time reproducibility of better than 0.
Chromatographic Troubleshooting Electronic pressure control 219 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.
Chromatographic Troubleshooting Electronic pressure control 220 Proper configuration If the inlet is not working at all, there may be a configuration problem. 1. T urn 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.
Chromatographic Troubleshooting Electronic pressure control 221 Switch setting examples EPC A or EPC B MODE A or MODE B IN A0 or IN B0 IN A1 or IN B1 LEFT, Electronic Pressure Control present / RIGHT,.
T h is page intentio nall y le ft bl ank..
10 Test Sample Chromatograms.
224 Test Sample Chromatograms This chapter contains typical examples of test sample chromatograms. They may be used as a general guide to instrument performance. It is assumed that both the instrument and proper test column are installed, that general keyboard control is understood (temperature control, defining signal output, etc.
Test Sample Chromatograms Test sample chromatograms 225 Test sample chromatograms Detector Type FID (or FIDw/MUG) Temp 250 DEGREES C Inlet Type PACKED (OR PURGED PACKED).
Test Sample Chromatograms Test sample chromatograms 226 IF Detector Type NPD (or NPDw/MUG) Temp 220 DEGREES C Inlet Type PACKED (OR PURGED PACKED). Temp 170 DEGREES C Operating Mode N/A Purge Time On N/A min Purge Time Off N/A min Oven Isothermal Init Temp 170 DEGREES C Init Time 3.
Test Sample Chromatograms Test sample chromatograms 227 Detector Type ECD(or ECDw/MUG) Temp 300 DEGREES C Inlet Type PACKED (OR PURGED PACKED). Temp 200 DEGREES C Operating Mode N/A Purge Time On N/A min Purge Time Off N/A min Oven Temp Isothermal Init Temp 160 DEGREES C Init Time N/A min Ramp Rate 0 Fin Temp Fin Time Range 2 COLUMN: Part No.
Test Sample Chromatograms Test sample chromatograms 228 Detector Type TCD(or TCDw/MUG) Temp 300 DEGREES C Inlet Type PACKED (OR PURGED PACKED). Temp 250 DEGREES C Operating Mode N/A Purge Time On N/A .
Test Sample Chromatograms Test sample chromatograms 229 Detector Type FIDw/MUG Temp 250 DEGREES C Inlet Type Ded On-Col Cap Oven Track On Temp N/A C Operating Mode N/A Purge Time On N/A min Purge Time Off N/A min Oven Temp Temp Programmed (1 ramp) Init Temp 60 DEGREES C Init Time 0.
Test Sample Chromatograms Test sample chromatograms 230 Detector Type FIDw/MUG Temp 250 DEGREES C Inlet Type SPLIT ONLY OR SPLIT/SPLITLESS Temp 200 DEG C Operating Mode SPLIT(PURGE ON) Purge Time On 0.
Test Sample Chromatograms Test sample chromatograms 231 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 0 min Purge Time Off 0 min Oven Isothermal Init Temp 180 DEGREES C Init Time 5.
Test Sample Chromatograms Test sample chromatograms 232 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 0 min Purge Time Off 0 min Oven Temp Isothermal Init Temp 170 DEGREES C Init Time N/A min Ramp Rate 0 Fin Temp Fin Time Range 0 COLUMN: Part No.
Test Sample Chromatograms Test sample chromatograms 233 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 0 min Purge Time Off 0 min Oven Temp Programmed Init Temp 100 DEGREES C Init Time 1 min Ramp Rate 10 Fin Temp 150 Fin Time 2 Range 0 COLUMN: Part No.
Test Sample Chromatograms Test sample chromatograms 234 Detector Type NPD w/MUG) Temp 220 DEGREES C Inlet Type Ded On-Col Cap Oven Track On Temp N/A C Operating Mode N/A Purge Time On min Purge Time Off min Oven Isothermal Init Temp 170 DEGREES C Init Time 5.
Test Sample Chromatograms Test sample chromatograms 235 Detector Type TCDw/MUG Temp 300 DEGREES C Inlet Type Ded On-Col Oven Track On Temp N/A C Operating Mode N/A Purge Time On N/A min Purge Time Off N/A min Oven Temp Programmed (1 ramp) Init Temp 60 DEGREES C Init Time 0.
Test Sample Chromatograms Test sample chromatograms 236 Detector Type ECDw/MUG Temp 300 DEGREES C Inlet Type Ded On-Column Oven Track On Temp N/A Operating Mode N/A Purge Time On N/A min Purge Time Of.
Test Sample Chromatograms Test sample chromatograms 237 SAMPLE: Type FPD Sample Inj Volume 1 l Part No. 19395•60580 COMPOSITION: 20 ng/ l (20.0 ppm W/V) each of 1-dodecanethiol and tributylphosphate.
Test Sample Chromatograms Test sample chromatograms 238 SAMPLE: Type FPD Sample Inj Volume 2 l Part No. 19305•60580 COMPOSITION: 20 ng/ l (20.0 ppm W/V) each of 1-dodecanethiol and tributylphosphate.
Test Sample Chromatograms Test sample chromatograms 239 SAMPLE: Type FPD Sample Inj Volume 1 l Part No. 19395•60580 COMPOSITION: 20 ng/ L (20.0 ppm W/V) each of 1-dodecanethiol and tributylphosphate.
T h is page intentio nall y le ft bl ank..
241 Index A adapters, 17 detector , 22 ECD, 23 installation, 24 TCD, 23 alphanumeric display , 33 B baseline problems noise, 204 position, 202 spiking, 206 wander and drift, 203 C calibration electron.
Index 242 electronic flow sensor (EFS) calibration, 60 packed inlet, 102, 106 electronic pressure control troubleshooting, 218 entering setpoints, 34 F fault: messages, 52 ferrules, 14 FID, 171 igniti.
Index 243 L 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, F.
Index 244 S 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 disp.
Ein wichtiger Punkt beim Kauf des Geräts HP 5890 II Plus (oder sogar vor seinem Kauf) ist das durchlesen seiner Bedienungsanleitung. Dies sollten wir wegen ein paar einfacher Gründe machen:
Wenn Sie HP 5890 II Plus noch nicht gekauft haben, ist jetzt ein guter Moment, um sich mit den grundliegenden Daten des Produkts bekannt zu machen. Schauen Sie zuerst die ersten Seiten der Anleitung durch, die Sie oben finden. Dort finden Sie die wichtigsten technischen Daten für HP 5890 II Plus - auf diese Weise prüfen Sie, ob das Gerät Ihren Wünschen entspricht. Wenn Sie tiefer in die Benutzeranleitung von HP 5890 II Plus reinschauen, lernen Sie alle zugänglichen Produktfunktionen kennen, sowie erhalten Informationen über die Nutzung. Die Informationen, die Sie über HP 5890 II Plus erhalten, werden Ihnen bestimmt bei der Kaufentscheidung helfen.
Wenn Sie aber schon HP 5890 II Plus besitzen, und noch keine Gelegenheit dazu hatten, die Bedienungsanleitung zu lesen, sollten Sie es aufgrund der oben beschriebenen Gründe machen. Sie erfahren dann, ob Sie die zugänglichen Funktionen richtig genutzt haben, aber auch, ob Sie keine Fehler begangen haben, die den Nutzungszeitraum von HP 5890 II Plus verkürzen könnten.
Jedoch ist die eine der wichtigsten Rollen, die eine Bedienungsanleitung für den Nutzer spielt, die Hilfe bei der Lösung von Problemen mit HP 5890 II Plus. Sie finden dort fast immer Troubleshooting, also die am häufigsten auftauchenden Störungen und Mängel bei HP 5890 II Plus gemeinsam mit Hinweisen bezüglich der Arten ihrer Lösung. Sogar wenn es Ihnen nicht gelingen sollte das Problem alleine zu bewältigen, die Anleitung zeigt Ihnen die weitere Vorgehensweise – den Kontakt zur Kundenberatung oder dem naheliegenden Service.
