HP 5890 II Plus - Manual

Contents Chapter 8 — Preventive Maintenance 155 . . . . . . . . . . . . . . Conditioning columns 156 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . (Re)Packing columns 158 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . ....

Contents Chapter 9 — Chromatographic Troubleshooting 201 . . . . . . Introduction 202 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Baseline symptoms 202 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . ...

10 Columns and Fittings The HP 5890 SERIES II (hereafter referred to as HP 5890) providesflexibility in choices among inlets, columns, and detectors through use ofliners and adapters, allowing any standard column to be used withoutsacrificing performance. Additional flexibility is gained through pos...

Columns and FittingsColumn 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, ispressed upward to open the door. Motor•drivenflaps at the rear of the oven admit room air for cool down ornear•ambientopera...

Columns and FittingsColumn 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. Distance relationships among inlets and de...

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

Columns and FittingsFittings 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 thecolumn in...

Columns and FittingsLiners/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 toprovide correct internal volume for proper operation. ...

Columns and FittingsInlet/detector liners/adapters 20 Inlet/detector liners/adapters Interchangeable stainless steel liners/adapters, installed from inside theoven, are used with the packed column inlet, and with all detectors,depending upon the column to be installed. Packed column inlet liners Lin...

Columns and FittingsInlet/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 packedmetal columns (either 1/8•or 1/4•inch),and with any type of capillarycolumn. Normall...

Columns and FittingsInlet/detector liners/adapters 23 ECD and TCD adapters A makeup gas adapter must be installed in the ECD or TCD base toinstall a capillary column, and to augment carrier flow through thecolumn with additional gas flow needed for optimal detector operation.The adapter must be remo...

Columns and FittingsInlet/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 Series 530 ¿ Capillary Column Use Nut and Ferrule Installed on a Liner/Adapter Figure 1-7 With one ex...

Columns and FittingsInlet 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. 4. Use a wrench to tighten the nut an...

Columns and FittingsInlet inserts 26 Exercise care! the oven, and/or inlet, or detector fittings may be hotenough 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 inter...

Columns and FittingsInlet 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 theliner; the column may prevent it from dropping completely into the liner. If the insert does not drop completely i...

Columns and FittingsInlet inserts 28 The split insert contains packing material (10% OV•1on 80/100 HighPerformance Chromosorb•W),held in place by silanized glass wool plugs,located immediately above a mixing chamber. This ensures propervolatilization and homogeneous mixing of the sample prior to its...

Columns and FittingsInlet 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 in...

Columns and FittingsJet 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 NPDmay be necessary. This must be done prior to column installation, and is particul...

32 Keyboard and Displays Alphanumeric Display InstrumentStatus Run Control TemperatureControl MiscellaneousFunctions Numeric andModifier Keys Signal Definitionand 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 . 4 CLEAR VALVE FLOW TIME FLOW CRYO PARAM PARAM PU...

Keyboard and DisplaysDisplaying setpoints 33 HP 5890 SERIES II (hereafter referred to as HP 5890) operation ismonitored and controlled through its front panel keyboard, andalphanumeric and LED displays. Some instrument functions are monitored continuously: signal levels,temperatures, carrier gas flo...

Keyboard and DisplaysEntering setpoints 34 Examples of possible displays are provided where appropriate throughoutthe manual. If a particular function is not installed in your instrument, an appropriate message is displayed when the key corresponding to thefunction is pressed. For example, if no hea...

Keyboard and DisplaysEntering setpoints 35 To display the function and its setpoint: necessary for a fewinstrument functions (Instrument Function Key) ( or ) A B then, EITHER ( through , , ) 0 9 - . to enter a new setpoint value OR, for a few functions, ( or ) to switch the function on or off ON OFF...

Keyboard and DisplaysEntering setpoints 36 CLEAR can be used anytime during an entry, prior to pressing ENTER , to erase the entry in progress. The * disappears, and the original setpoint display is restored. Rules regarding keyboard usage are summarized below: C An instrument function key, when pre...

Keyboard and DisplaysKeyboard operation, INET control 37 C CLEAR is used anytime during setpoint entry, prior to pressing ENTER , to erase the entry in progress. C CLEAR , if pressed when no setpoint entry is in progress, displays HP 5890 readiness . C Run Control Key START , if pressed while a setp...

Keyboard and DisplaysProtecting 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. Protecting setpoints The HP 5890 provides a keyboard lock fe...

Keyboard and DisplaysLoading default setpoints 39 With the keyboard locked, Figure 2•6shows the display occurring if asetpoint entry is attempted: ACTUAL SETPOINT KEYBOARD LOCKED KEYBOARD LOCKED Message Display Figure 2-6 If the HP 5890 keyboard is locked while the instrument is under INET control, ...

Keyboard and DisplaysLoading default setpoints 40 Upon pressing ENTER , default setpoints are loaded into memory, erasing setpoints already present. Table 2•1lists resulting HP 5890 defaultsetpoints. Function Default Setpoint Inj Temp (A & B): 50 ^ C, OFF Det Temp (A & B): 50 ^ C, OFF Oven T...

44 Temperature Control Oven temperature, and temperatures of up to five separate heated zones(detectors, inlets, and/or heated valves), are controlled through keysshown in Figure 3•1. Oven Control Heated Zone Control INITVALUE FINALVALUE FINALTIME INJ ATEMP INJ BTEMP DET ATEMP OVENMAX EQUIBTIME OVEN...

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. Given sufficient time for...

Temperature ControlValid setpoint ranges 46 Valid setpoint ranges Table 3•1lists valid setpoint ranges for the 13 keys controlling oven andheated zone temperatures. NOTE: TOTAL run time will not exceed 650.00 minutes regardless of values entere , , and . INIT TIME RATE FINAL TIME -80 to 450 1 ^ C Ov...

Temperature ControlCryogenic (sub-ambient) oven control 47 Cryogenic (sub-ambient) oven control Liquid N 1 or liquid CO 1 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...

Temperature ControlCryogenic (sub-ambient) oven control 48 Oven profile using CRYO, for operationduring runs at subambient temperatures 25 50 75 (CRYO ON) CRYO OFF at ambient +15 ^ CRYO ONat ambient + 25 ^ 9 9 Figure 3-4 Oven profile using CRYO BLAST, for very fast cool down between runs 40 80 120 C...

Temperature ControlProgramming oven temperature 49 Programming oven temperature HP 5890 oven temperature programming allows up to three ramps, inany combination of heating or cooling. Keys defining an oven temperatureprogram include: INIT TEMP A setpoint temperature value at which the oven ismaintai...

Temperature ControlOven 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, 650minutes. A is included in key sequences defining parameters for a second ramp; B is included in key sequences defining parameters for...

Temperature ControlOven safety 51 In complex two•or three•rampoven temperature programs, informationas 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 speci...

Temperature ControlFault: 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, ...

Temperature ControlOven temperature calibration 54 INITIALTIME RATE OVEN FINALTIME 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 theoven returns to its setpoint value. ...

Temperature ControlOven temperature calibration 55 The HP 5890 provides the means to (if necessary) reset oven temperaturemonitoring so the displayed ACTUAL value accurately represents the correct temperature. Oven temperature calibration requires entering the difference ( delta ) value (in ^ C) bet...

Temperature ControlOven temperature calibration 56 3. CALIB DELTA is displayed until ENTER is pressed; then oven temperature recalibration occurs. Note that, after calibration, thedisplayed oven temperature value should match closely the measuredvalue. Any delta value within the range -10.00 through...

58 Electronic Flow Sensing Two channels of electronic flow rate sensing continuously monitor gasflow rates (usually carrier) in the HP 5890 SERIES II. Proper scaling ofdisplayed values for different commonly used gases is defined throughkeyboard entries. The two flow channels are distinguished throu...

Electronic Flow SensingDesignating gas type 59 Designating gas type To scale the displayed flow rate value properly, one of four commonly usedgases must be designated. The appropriate gas type is selected accordingto Table 4•1: 1 He (Helium) TCD 2 N 2 (Nitrogen) General 3 H 2 (Hydrogen) Capillary 4 ...

Electronic Flow SensingElectronic 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 theinstrument, and then lift. 2. Through the keyboard, select CALIB AND TEST mode, function 2: ...

Electronic Flow SensingElectronic 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. Outlet Line, Chann...

Electronic Flow SensingElectronic 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. Setting the GAIN calibration va...

Electronic Flow SensingElectronic 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). C Press TIME to access the timer function. C After obtaining the desired flow rate, press: CLEAR . 2 ENTE...

Electronic Flow SensingElectronic 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 thekeyboard if necessary, without repeating the entire calibra...

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. Output sources include dete...

Signal OutputZeroing signal output 70 Self- ZERO setpoint Referencing Figure 5•2for the +1 V output, note that using ZERO can increase dynamic range available for signal output by shifting an existingconstant offset signal to a lower level (usually electrical zero). There arelimits to this, however,...

Signal OutputSignal 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. User-defi...

Signal OutputSignal 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 outp...

Signal OutputSignal 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. Entering RANGE 2 ! ( ) / ATTN 2 !...

Signal OutputTest signal output 77 Test signal output A test chromatogram, consisting of three peaks, is permanently stored inthe HP 5890. Each peak is approximately 1/10 the height of the previouspeak, with the first (tallest) peak having a height value of about 125 mVat RANGE 2 ! ( ) = 0 ( + 1 V a...

Signal OutputTest signal output 78 To access this function, the following key sequence is entered: SIG 1 ( or SIG 2 ) 9 ENTER Test plot mode is confirmed by the display SIGNAL 1 (or 2 ) TEST PLOT . Pressing SIG 1 (or SIG 2 ) a second time displays the current signal level value (which is 0.0 initial...

Signal OutputInstrument 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 agroup of devices (consisting of a controller , and some number of data Producers and data Consumers ) t...

Signal OutputInstrument 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 . The controller is responsible for network configura...

Signal OutputInstrument 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. It has a single pair...

Signal OutputInstrument network (INET) 82 Except for the controller, each instrument handles setpoints forinstrument(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 setpointsand parameters. ...

Signal OutputInstrument network (INET) 83 INET operation In using the INET function, chromatographic parameters are enterednormally through the HP 5890 keyboard. Integration parameters areentered at the controller. Parameters for other devices on the INET loopmay be entered at the controller, or at ...

Signal OutputInstrument network (INET) 84 If a setpoint entry at the HP 5890 keyboard is in progress when aworkfile or method is stored or listed at the controller, the entry isaborted. After the operation finishes, the HP 5890 returns to the samesetpoint display. C When a stored workfile or method ...

Signal OutputINET configuration 85 Automatic INET reconfiguration In the following circumstances, INET automatically reconfigures underdirection of the controller: C Recovery from a power failure. C Recovery from any particular device on the loop being switched off,then on again. C Recovery from a d...

Signal OutputINET configuration 86 Figure 5•8shows displays resulting from the key sequence: CLEAR . 3 ENTER Switching between Global and Local With regard to the INET function at the HP 5890, there are twooperating modes: global or local . In global mode (default mode), HP 5890 START and STOP keys,...

Signal OutputINET 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 theINET system, GLOBAL is displayed continuously. This featur...

Signal OutputINET configuration 88 The specific number shown depends upon how INET cables are connected among devices included in the loop. The value shown in theexample ( 8 ) implies the HP 5890 is the first instrument on the loop, starting from the OUT receptacle on the controller device (the cont...

Signal OutputINET configuration 89 Figure 5•11 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 RANGE ACTUAL SETPOINT SIG 1 ON RANGED INET Signal Definition Displays Figure 5-11 From the displays, the f...

Signal OutputHP-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. If FAILED ...

Signal OutputWarn: and fault: messages 93 C WARN: SIGNAL CHANGED and/or WARN: NO DETECTORS is displayed if a detector previously assigned to a particular signalchannel is found to be absent; for example, if the signal board for agiven detector should fail or be removed for service. C FAULT: INET CPU...

Signal OutputFile compatibility with data handling devices 94 File compatibility with data handling devices You must have the HP 5890 SERIES II in the proper mode for filecompatibility with your data handling device. What are the modes? There are 2 file transfer modes: HP 5890A and HP 5890 SERIES II...

Signal OutputFile 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. Turn power off . 2. Remove the GC side panel, and locate the...

Signal OutputFile 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. Set the jumper (Part No. 1258•0141) for the proper mode. To avoid electrostatic damage to the main board, ground yourself to the GCchassis wi...

Signal OutputFile compatibility with data handling devices 97 How to convert HP 339X Integrator workfiles from 5890A toSERIES II mode: 1. Turn the GC off . 2. Follow the previous instructions to set the GC for 5890A mode (use proper grounding). 3. Download the workfile from the integrator. 4. Turn G...

100 Inlet Systems This chapter provides information for the following HP 5890 SERIES II(hereafter referred to as HP 5890) inlet systems: C Packed column inlet C Septum•purgedpacked column inlet C Split/splitless capillary inlet For cool on•columninformation, see the manual Programmable CoolOn•Column...

Inlet SystemsPacked 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 SystemsPacked column inlet 102 Trap(s) ExternalPlumbing InternalPlumbing Pressure Gauge Packed ColumnInlet Electronic Flow Sensor (optional) MassFlowController Column To Detector Carrier Gas Flow Diagram, Packed Column Inlet (with electronic flow sensor) Figure 6-2 Liquid sample is rapidly vol...

Inlet SystemsPacked 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 systemshould be noted via the EFS. The original column flow rate is reestablished simply by adjusting themass flow contro...

Inlet SystemsPacked column inlet 104 Problems at high inlet temperatures A common problem with conventional packed column inlets operated athigh temperatures is septum bleed and the associated ghost peaks. Tominimize this effect, some inlet systems are designed with steeptemperature gradients throug...

Inlet SystemsPacked 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 ^ COven 150 ^ C Oven 300 ^ COven Injection Port SetpointTemperature 350 ^ C Thermal Profiles Figure 6-4 This optimiz...

Inlet SystemsSplit/splitless capillary inlet 107 Split/splitless capillary inlet 1 2 3 Insert1, 2, or3 Sealing O-Ring Split Direct Injection Splitless 1/4” Packed Glass Column Packed Metal Column SealingO-Ring 4 A. CAPILLARY COLUMN B. PACKED COLUMN Item Part No. Description Number 1 Split Insert (pa...

Inlet SystemsSplit/splitless capillary inlet 108 The multiple•modesplit/splitless capillary inlet system may be used withany of the common types of capillary columns (fused silica, quartz, glass,metal). Specific sampling modes include: C Split, for major•componentanalyses. C Purged splitless, for tr...

Inlet SystemsSplit/splitless capillary inlet 110 Van Deemter curves demonstrate advantages of using either He or H 1 as carrier gas. From the curves, several observations may be made: C Minima for He and H 2 occur at much higher average linear velocities than N 2 . Thus, He, or even better, H 2 , ca...

Inlet SystemsSplit/splitless capillary inlet 111 NominalID (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 recommendedas starting points only!Values listed are independent of carrier gas used. Table 6-1. Suggested Ini...

Inlet SystemsSplit/splitless capillary inlet 112 IN OUT IN OUT GA ExternalPlumbing InternalPlumbing Trap(s) Carrier Gas MassFlowController ElectronicFlowSensor(optional) To Detector Solenoid Valve Back-pressureRegulator SplitVent Septum Purge Vent PressureGauge SeptumPurgeControl CapillaryInlet Colu...

Inlet SystemsSplit/splitless capillary inlet 113 The split ratio is an indicator of the fraction of total sample entering thecolumn: the higher the value, the less sample enters the column. For setting flow for split sampling, see Chapter 4 of the HP 5890Operating Manual. Verifying inlet purge statu...

Inlet SystemsSplit/splitless capillary inlet 114 Splitless sampling For splitless operation, the dilute sample is vaporized inside the inletinsert. 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 p...

Inlet SystemsSplit/splitless capillary inlet 115 C Low Volatility Solute C 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. andGrob, K., Jr., Journal of Chromatography, 94, page 53 (...

Inlet SystemsSplit/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 30 Carbon Disulfide 46 10 to 35 Chloroform* 61 25 to 50 Methanol* 65 35 to 55 n-Hexane 69 40 to 60...

Inlet SystemsSplit/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 headof the column. Components with lower boiling points are reconcentratedvia the solvent effect. Temperature p...

Inlet SystemsSplit/splitless capillary inlet 118 A recommended procedure is to perform a series of analyses atincreasingly higher inlet temperatures using components representativeof those of interest, and analyzed using the conditions for later sampleanalyses. The optimum temperature is where maxim...

Inlet SystemsSplit/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: IsooctaneColumn: 16.5 m x 0.25 mm SE-5480 ^ C (0.5 min) – 170 ^ C @ 15 ^ /min Sample Si...

Inlet SystemsSplit/splitless capillary inlet 121 Noting Figures 6•11 and 6•12,the splitless sampling process is as follows: C Before Injection: Carrier gas flow enters through the mass flow controller, into the top of the inlet. A small fraction is split off to purgethe septum and insert seal, then ...

Inlet SystemsSplit/splitless capillary inlet 122 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 entire...

124 Detector Systems This chapter provides information for the five HP 5890 SERIES II(hereafter referred to as HP 5890) detector systems: C Flame Ionization Detector (FID) C Nitrogen•PhosphorusDetector (NPD) C Electron Capture Detector (ECD) C Thermal Conductivity Detector (TCD) C Flame Photometric ...

Detector SystemsFID 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 beperformed, exchanging the jet in an FID or NPD may be necessary. Table7•1lists available jets. Note: ...

Detector SystemsFlame ionization detector (FID) 126 Flame ionization detector (FID) Inlet H 2 Inlet FID CollectorAssembly Jet Flame Ionization Detector (FID) Figure 7-1 The flame ionization detector (FID) responds to compounds that produceions when burned in a H 1 •airflame. These include all organi...

Detector SystemsFlame 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 switchto a more restrict...

Detector SystemsNitrogen-phosphorus detector (NPD) 129 Nitrogen-phosphorus detector (NPD) NPD CollectorAssembly Air Inlet H 2 Inlet NPD Collector Active Element Jet Nitrogen-Phosphorus Detector (NPD) Figure 7-3 The nitrogen•phosphorusdetector uses a jet and collector similar to theFID; however, the ...

Detector SystemsNitrogen-phosphorus detector (NPD) 131 Other gas flow effects of too high flow rates of the hydrogen may allow atrue flame to exist around the active element. This would overheat theactive element severely and destroy the specific response. Too low flowrates of air tend to quench the...

Detector SystemsNitrogen-phosphorus detector (NPD) 132 Performance considerations Contamination Very little contamination can create serious NPD problems. Commonsources include: C Columns and/or glass wool treated with H 2 PO 3 (phosphoric acid) C Phosphate•containingdetergents C Cyano•substitutedsi...

Detector SystemsNitrogen-phosphorus detector (NPD) 133 Residual silanizing reagents from derivatization, and/or bleed fromsilicone columns, may coat the active element with silicon dioxide. Thisdecreases ionization efficiency, reducing sensitivity. If silanizing is necessary, remove excess reagent b...

Detector SystemsNitrogen-phosphorus detector (NPD) 134 Both detector baseline and sensitivity change with carrier flow rate dueto change in temperature of the active element. This is the reason for thebaseline drift in pressure•controlledinlet systems (capillary inlets) whentemperature•programmingth...

Detector SystemsElectron capture detector (ECD) 135 Electron capture detector (ECD) The effluent gas stream from the detector must be vented to a fumehood to prevent possible contamination of the laboratory withradioactive material. Specific cleaning procedures are provided in Chapter 8, PreventiveM...

Detector SystemsElectron 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 1000 Anhydrides and tri-Cl compounds 10 4 Mono-I, di-Br and nitro compounds 10 5 Di-I, tri-Br, poly-...

Detector SystemsElectron capture detector (ECD) 141 Background level If the ECD system becomes contaminated, whether from impurities inthe carrier (or makeup) gas, or from column or septum bleed, a significantfraction of detector dynamic range may be lost. In addition, the outputsignal becomes noisy...

Detector SystemsElectron capture detector (ECD) 142 A very clean system may produce a value below the low end of 10 (100Hz). To correct this condition, an adjustment is made to the presentpotentiometer located on the ECD electronics board. ECD Potentiometer Switch and Adjustment ECD Potentiometer Sw...

Detector SystemsThermal conductivity detector (TCD) 145 Because of its exceptionally high thermal conductivity and chemicalinertness, He is the recommended carrier gas: it gives large thermalconductivity differences with all compounds except H 1 (considerations necessary in H 1 analyses are discusse...

Detector SystemsThermal conductivity detector (TCD) 146 Optimizing performance The following sections aid in choosing operating parameters to obtainoptimal TCD performance. Temperature TCD sensitivity increases as the temperature difference between thedetector filament (automatically set) and the su...

Detector SystemsThermal conductivity detector (TCD) 147 As Figure 7•9shows, however, the lower the detector zone temperature,the greater is the temperature difference between the filament versus thesurrounding detector body temperature. Thus, for maximum sensitivity,the detector zone should be opera...

Detector SystemsThermal conductivity detector (TCD) 148 Note that TCD response becomes relatively flat (insensitive) to referencegas flow rates equal to, or somewhat greater than, flow rate through thecolumn. Analyzing for hydrogen, special considerations Only H 1 has thermal conductivity greater th...

Detector SystemsThermal conductivity detector (TCD) 149 TCD-to-FID series connection The following describes, for a TCD whose exhaust vent returns to theinside of the oven, connecting the TCD to an FID. C If necessary (see NOTE below), exchange the standard FID jet for the0.030•inchjet (Part No. 187...

Detector SystemsThermal conductivity detector (TCD) 150 filament. The immediate symptom is a permanent change in detectorsensitivity due to change in filament resistance. If possible, such offending materials should be avoided. If this is notpossible, the filament may have to be replaced frequently....

Detector SystemsFlame photometric detector (FPD) 151 Flame photometric detector (FPD) Optimizing FPD sensitivity and selectivity FPD sensitivity and selectivity are affected by several importantparameters. These are listed below, with suggested ways to optimize foreach application. A. FPD Flow Rates...

Detector SystemsFlame 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 X = Nitrogen E = Oxygen + = Air Pressure-psig Pressure-kPa Flowml/min } } } } } } X X X X X X + + + + E E E E E + FPD Flows versus Supply Pressure...

Detector SystemsFlame photometric detector (FPD) 153 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. The correct ignition...

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

Preventive Maintenance(Re)Packing columns 158 (Re)Packing columns In packing columns (particularly 1/4•inchglass columns), one mustconsider the type of packing, column bore, and type (metal or glass), themethod of sample introduction (flash vaporization or on•column),inlet ordetector base requiremen...

Preventive MaintenancePacked column inlet 159 Packed column inlet Changing septa Septum lifetime is dependent upon frequency of use and upon needlequality; burrs, sharp edges, rough surfaces, or a blunt end on the needledecreases septum lifetime. A leaking septum is evidenced by longer retention tim...

Preventive MaintenancePacked column inlet 160 Caution Column flow is interrupted while changing septa; since some columnsmay be damaged at elevated temperature without carrier flow, cool theoven to ambient before proceeding. Exercise care! The oven and/or inlet or detector fittings may be hotenough ...

Preventive MaintenancePacked column inlet 161 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),...

Preventive MaintenancePacked column inlet 162 Packed Column Inlet, Leak-Checking the Septum Figure 8-3 Cleaning Turn off the heated zone for the inlet and allow it to cool. Remove the septum retainer nut and septum; remove also the columnand inlet liner. Using a suitable light source, illuminate the...

Preventive MaintenanceSplit/splitless capillary inlets 163 Split/splitless capillary inlets Changing septa For a conventional disk•typeseptum, lifetime is dependent upon needlequality; needles should be sharply pointed and free of burrs or roughsurfaces. Choice of septum material is less critical th...

Preventive MaintenanceSplit/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 septumretainer nut. Capillary Inlet Septum Replacement, Split/Splitless and Split-Only Capillary Inlet Figure...

Preventive MaintenanceSplit/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 anytime a leak is suspected. 1. Switch off detector! 2. Install an inlet plug (a paper clip...

Preventive MaintenanceSplit/splitless capillary inlets 167 C Use leak detection fluid to check for leakage at the column nut. Ifleakage 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 falseindic...

Preventive MaintenanceSplit/splitless capillary inlets 168 Solenoid Valve Assembly Solenoid Valve, Split/Splitless Capillary Inlet Figure 8-7 Cleaning Turn off the heated zone for the inlet and allow it to cool. Remove septum retainer nut, septum, insert retainer nut, and inletinsert; also remove th...

Preventive MaintenanceLiner and/or insert care 169 Liner and/or insert care Regardless of the inlet system, inlet inserts and/or liners must be keptclean for optimum performance, particularly their interiors from whichcontamination may enter the column and/or interact with samplecomponents. Note: Ex...

Preventive MaintenanceLiner and/or insert care 170 Repacking a split insert Since, for a split insert, its packing material is discarded in cleaning, theinsert must be repacked. Note: Repacking with small•diameterglass beads is not recommended: they are usually contaminated with metal filings due to...

Preventive MaintenanceFlame ionization detector (FID) 171 Metal inserts and/or liners C Do not use concentrated acid(s) on metal inserts or liners! C The insert is washed with noncorrosive solvents (H 1 O, CH 2 OH (methanol), (CH 2 ) 1 CO (acetone), CH 1 Cl 1 (methylene chloride), etc), and then dri...

Preventive MaintenanceFlame ionization detector (FID) 172 Jet exchange/replacement Depending upon the column type to be used, and/or analyses to beperformed, 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 ins...

Preventive MaintenanceFlame ionization detector (FID) 174 Collector Assembly Cover Removed, Flame Ionization Detector (FID) Figure 8-10 Turn off the detector and its heated zone; also turn off gases to thedetector (particularly H 1 !). Allow time for the detector zone to cool. Open the top cover at ...

Preventive MaintenanceFlame ionization detector (FID) 175 Wash the collector in distilled water, hexane, and/or CH 2 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...

Preventive MaintenanceFlame 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) toloosen/remove internal deposits. Be careful in using the wire with the0.011•inc...

Preventive MaintenanceFlame 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, thesystem is leak•free,flow rates are set correctly, and externa...

Preventive MaintenanceNitrogen-phosphorus detector (NPD) 178 is best to have a new jet on hand to exchange if a damaged jet issuspected. Nitrogen-phosphorus detector (NPD) In addition to the detector itself, other systems associated with thedetector may also require routine maintenance. Nitrogen•pho...

Preventive MaintenanceNitrogen-phosphorus detector (NPD) 179 Turn off the detector and its heated zone; also turn off gases to thedetector (particularly H 1 ! ). Allow time for the detector zone to cool. Open the top cover at its front edge to access the detector. 1. Using a Pozidriv•typescrewdriver...

Preventive MaintenanceNitrogen-phosphorus detector (NPD) 181 Caution Do not overtighten the jet! Overtightening may permanently deformand 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...

Preventive MaintenanceNitrogen-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 Transformer Strap Collector Collector Body O-ring Whenever the collector must be removed from the det...

Preventive MaintenanceNitrogen-phosphorus detector (NPD) 183 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 dete...

Preventive MaintenanceNitrogen-phosphorus detector (NPD) 184 lead on the collector body. Tighten the setscrew to secure the wire andcollar. Type B NPD transformer/collector assembly Type B NPD Detector Assembly Figure 8-18. Remove the transformer/collector assembly from the Type B NPD coveras follow...

Preventive MaintenanceNitrogen-phosphorus detector (NPD) 185 4. Remove the collector from the collector assembly as follows: C Loosen the 1.5•mmscrew holding the transformer secondary wire to thetop of the collector and disconnect the wire. The hex key wrench requiredis a 1.5•mmsize and was provided...

Preventive MaintenanceNitrogen-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 couldcause damage. If there is any binding, the cause should bedetermined and corrected befo...

Preventive MaintenanceElectron 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. Uselow•bleedsepta and condition a new septum prior to us...

Preventive MaintenanceElectron capture detector (ECD) 190 flow through the system is available. Allow time for the system tobecome 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 ...

Preventive MaintenanceElectron 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. 4. Open th...

Preventive MaintenanceThermal 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 bythe Nuclear Regulatory Commission and/or responsible state...

Preventive MaintenanceFlame photometric detector 193 Caution Failure to turn off the TCD and to cap the detector column fitting maycause 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 t...

Preventive MaintenanceFlame photometric detector 195 A B C D E 8 5 2 1 11 4 6 7 9 10 16 6 7 15 141213 1920 21 22 3 27 4 Places O-ring(8) 3 to 6 mm a x Subassembly Parts Identification Figure 8-20.

Preventive MaintenanceFlame photometric detector 197 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), theFPD jet should be inspected fo...

Preventive MaintenanceFlame 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. If the jet is damaged in any way, it should berepl...

Preventive MaintenanceFlame photometric detector 199 this indicates a leak in the system. Begin checking possible leak sourcesand 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. supply line swage•type...

Preventive MaintenanceConditioning chemical traps 200 Conditioning chemical traps Remove the trap from its installed location and attach it to a clean, drygas source (helium or nitrogen). Attach the 1/8•inchend (male) of thechemical trap assembly to the reconditioning gas source using a graphiteor a...

202 Chromatographic Troubleshooting Introduction This chapter is concerned with diagnosis: the process of going fromunexpected behavior of the HP 5890 SERIES II (hereafter referred to asHP 5890) (symptoms) to the probable location of the difficulty (causes). Problems arise from many causes. Some of ...

Chromatographic TroubleshootingBaseline symptoms 203 C It can also result from valve operations: If valves are beingswitched during a run, examine the valve time program to see ifthe change coincides with a valve operation. C This symptom also can occur if the septum suddenly begins toleak; Avoid th...

Chromatographic TroubleshootingBaseline symptoms 204 2. Baseline is erratic, moves up and down (wander): C Suspect a leak in the system: Check septum condition and replaceif necessary. Check column connections. If the leak is at the detector end of the column, retention times arestable from run to r...

Chromatographic TroubleshootingBaseline symptoms 206 Spiking Spikes are isolated baseline disturbances, usually as sudden (and large)upscale movements. If accompanied by noise, the noise problem should besolved first, since spiking may disappear at the same time. 1. Spikes appear whenever the chart ...

Chromatographic TroubleshootingRetention time symptoms 207 Retention time symptoms Retention time drift Retention time drift is a steady increase or decrease of retention times insuccessive runs. Erratic times (both directions) are discussed below asretention time wander. 1. In a series of runs, ret...

Chromatographic TroubleshootingPeak symptoms 209 Peak symptoms No peaks This is usually due to operator error; possibilities include injection on thewrong column, incorrect signal assignment, attenuation too high (peaksare present but not visible), a bent syringe needle in an automaticsampler, etc. ...

Chromatographic TroubleshootingPeak symptoms 211 Deformed peaks The ideal peak, rarely occurring in chromatography, is a pure Gaussianshape. In practice, some asymmetry is always present, particularly nearthe baseline. 1. The peak rises normally, then drops sharply to baseline: Overloaded Peak Figur...

Chromatographic TroubleshootingPeak symptoms 212 C Interaction with column material is a frequent cause. Silanizedsupport may help. An all•glasssystem may be required if metalcolumn tubing is the source. C Column overload with a gas sample often shows this effect; tryinjecting less. C This may be a ...

Chromatographic TroubleshootingPeak symptoms 213 4. Top (apex) of the peak is split: FID/NPD Flameout, or TCD with H 1 (in He Carrier) Figure 9-4. C Verify that this is not a merged peak situation: Reduce oventemperature 30 ^ C and repeat the run. If the split peak becomes better resolved, it is pro...

Chromatographic TroubleshootingTroubleshooting valve systems 214 Troubleshooting valve systems Chromatographic symptoms Troubleshooting valves and their related plumbing is primarily a matterof systematic checking and verification of unimpaired mechanicaloperation of any moving part. This requires a...

Chromatographic TroubleshootingTroubleshooting valve systems 215 Loss of peaks in specific areas of the chromatogram Entire sections of chromatographic data can be lost due to a valve thatdoes not rotate or one that rotates improperly. Other than obviouscomponent failures (i.e., solenoid, actuator, ...

Chromatographic TroubleshootingLocating leaks 216 Extraneous peaks Air peaks are sometimes seen in a chromatogram when leakage occursbecause the valve rotor does not seal properly. These leaks may not bedetectable by using the soap•bubblemethod. The leak test procedure isdescribed in the Site Prep a...

Chromatographic TroubleshootingPressure check 217 Pressure check The pressure•checkmethod will indicate, but sometimes not isolate, aleak in the flow path. Since this method does not necessarily isolate theleak, one of the leak•checkmethods may be needed to locate the leakspecifically. Note that eac...

Chromatographic TroubleshootingElectronic pressure control 218 Electronic pressure control The electronic pressure control option provides very accurate and precisecontrol of column head pressure, resulting in retention timereproducibility of better than 0.02% RSD when there are no columneffects. Th...

Chromatographic TroubleshootingElectronic pressure control 219 Safety shutdown Systems equipped with electronic pressure programming have a safetyshutdown feature to prevent gas leaks from creating a safety hazard. Ifthe system cannot reach a pressure setpoint it beeps. After about 45seconds the bee...

Chromatographic TroubleshootingElectronic pressure control 220 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 config...

Chromatographic TroubleshootingElectronic 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,Electronic Pressure Control not present LEFT, (FPR) Programmable Cool On-Column Inlet &Purged Pac...

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 areinstalled, that general keyboard control is understood (temperaturecontrol...

Test Sample ChromatogramsTest sample chromatograms 225 Test sample chromatograms Detector Type FID (or FIDw/MUG) Temp 250 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 Programmed (1 ramp) Init Temp 110 DEG...

Test Sample ChromatogramsTest sample chromatograms 230 Detector Type FIDw/MUG Temp 250 DEGREES C Inlet Type SPLIT ONLY ORSPLIT/SPLITLESS Temp 200 DEG C Operating Mode SPLIT(PURGE ON)Purge Time On 0 min Purge Time Off 0 min Oven Temp Programmed (1 ramp) Init Temp 100 DEGREES C Init Time 0 min RampRat...

Test Sample ChromatogramsTest 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 RampRate 10 Fin...

Test Sample ChromatogramsTest 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 in isooctane Detector Type FPD Temp 200 DEGREES C Inlet Type PACKED OR PURGED PACKED Temp 200 DEGR...

Test Sample ChromatogramsTest 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 in isooctane Detector Type FPD Temp 200 DEGREES C Inlet Type SPLIT ONLY OR SPLIT/SPLITLESS Temp 20...

241 Index A adapters, 17 detector, 22ECD, 23installation, 24TCD, 23 alphanumeric display, 33 B baseline problems noise, 204position, 202spiking, 206wander and drift, 203 C calibration electronic flow sensor, 60oven temperature, 54 capillary columns, metal, 30 clear dot function, 39 cold trapping, 11...