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Chromatographic Troubleshooting
Baseline symptoms

203

C

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.

C

This symptom also can occur if the septum suddenly begins to
leak; Avoid the problem by changing septa regularly.

C

Offset•see troubleshooting procedure for the particular detector
in use.

Wander and drift

Baseline wander or drift may occur when a flow or temperature setting is
changed. If the system is not stabilized at the new conditions before
starting a run, some baseline changes are to be expected. Cases following
assume that sufficient stabilization time has elapsed since the last
change in operating conditions.

Wander and drift are often accompanied by noise, discussed below.

1. Baseline moves steadily upscale or downscale (drift) during the run:

C

This is most frequently seen during temperature programming:
Operation with a single column (no column compensation) at
moderate to low attenuation causes this. If dual columns are used,
check that the signal mode is correct for column compensation.

C

It is also possible the compensation is insufficient (upscale
movement) or too great (downscale movement).

This cause of drift is minimized by thorough column conditioning.
Operating at lower oven temperature also helps but prolongs the
analysis. Use of a chromatographically equivalent column with
higher temperature limit is also possible.

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Summary of Contents for 5890 Series II

Page 1: ...Reference Manual HP 5890 Series II and HP 5890 Series II Plus ...

Page 2: ...ion or possible situation that could damage or destroy the product or the user s work Important User Information for In Vitro Diagnostic Applications This is a multipurpose product that may be used for qualitative or quantitative analyses in many applications If used in conjunction with proven procedures methodology by qualified operator one of these applications may be In Vitro Diagnostic Procedu...

Page 3: ...acked column inlet inserts 25 Split splitless or split onlycapillary inlet inserts 27 Jet replacement FIDs or NPDs 30 Metal capillary columns 30 Chapter 2 Keyboard and Displays 31 Displaying setpoints 33 Entering setpoints 34 Keyboard operation INET control 37 Protecting setpoints 38 Loading default setpoints 39 Chapter 3 Temperature Control 43 Valid setpoint ranges 46 Cryogenic sub ambient oven c...

Page 4: ...tpoints 75 Entering setpoints 76 Switching off the 1 mV output 76 Test signal output 77 Instrument network INET 79 The controller 79 An instrument 81 Active workspace 82 HP 5890 INET states 82 INET operation 83 Automatic INET reconfiguration 85 INET configuration 85 Switching between Global and Local 86 INET HP ILaddresses 87 HP ILloopback test 90 Warn and fault messages 92 File compatibility with...

Page 5: ...ng 121 Chapter 7 Detector Systems 123 Capillary makeup gas flow rate 124 FID and NPD jets 125 Flame ionization detector FID 126 FID flameout problems 128 Nitrogen phosphorusdetector NPD 129 Performance considerations 132 Electron capture detector ECD 135 Requirements for USA owners 135 Temperature 140 Background level 141 Thermal conductivity detector TCD 143 Optimizing performance 146 Analyzing f...

Page 6: ...ition problems 177 Nitrogen phosphorusdetector NPD 178 Cleaning 178 Removing replacing the NPD collector 181 Type B NPD transformer collector assembly 184 Reinstallation 186 Electron capture detector ECD 188 Frequency test 188 Carrier gas evaluation 188 Leaks 189 Thermal cleaning 190 Packed column 191 Capillary column 191 Radioactivity leak test wipe test 192 Thermal conductivity detector TCD 192 ...

Page 7: ...ntion time wander reproducibility 207 Peak symptoms 209 No peaks 209 Inverted peaks 209 Extra peaks 209 Deformed peaks 211 Troubleshooting valve systems 214 Chromatographic symptoms 214 Locating leaks 216 Pressure check 217 Electronic pressure control 218 Safety shutdown 219 Proper configuration 220 Switch setting examples 221 Chapter 10 Test Sample Chromatograms 223 Test sample chromatograms 225 ...

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Page 9: ...1 Columns and Fittings ...

Page 10: ...his section provides information for the following C The column oven C Fittings C Liners and inserts C ECD and TCD capillary makeup gas adapters The first three items must be considered before a column may be installed properly at either an inlet or a detector In addition for an FID or NPD and depending upon the column to be installed packed versus capillary the correct jet must be installed befor...

Page 11: ...down or near ambientoperation so the door is kept closed except for access to columns the oven cools most efficiently with its door closed The oven can maintain temperature down to about 7 C above ambient without auxiliary cooling If lower temperatures are required a cryogenic valve for either liquid CO1 or liquid N1 is needed Liquid CO1 permits reliable temperature control down to 50 C liquid N1 ...

Page 12: ...st inlet can only be installed in the B rear most detector Distance relationships among inlets and detectors are shown in Figure 1 2 Top View showing relationship of inlets to detectors 228 1 mm Front B A B A Figure 1 2 Installation Restrictions Rigid Columns Packed column Packed columns require no physical support other than that provided by proper installation at inlet and detector fittings ...

Page 13: ...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 Figure 1 3 Typical Hewlett Packard Capillary Columns ...

Page 14: ...ich best centers the column in the oven Column ends should come off the bottom of the frame making smooth curves to inlet and detector fittings Avoid allowing any section of the column itself to come in contact with oven interior surfaces Fittings The following is a brief comparison of common types of fittings nuts ferrules O rings used to install columns and to install inlet and detector liners a...

Page 15: ...or with temperature programming C Also commonly used with metal columns and tubing stainless steel fittings minimize possibility of leakage at high temperature but require care in installing columns overtightening may damage the column end or inlet detector fitting C Teflon ferrules may be used to 250 C but are recommended only for isothermal work because they develop leaks when temperature progra...

Page 16: ...etector liners 5080 8774 pkg of 10 1 4 inch glass packed columns Vespel 1 8 inch ferrule metal columns 0100 1107 pkg of 10 graphite 1 0 mm ferrule capillary columns 5080 8773 pkg of 10 graphite 0 5 mm ferrule capillary columns 5080 8853 pkg of 10 graphite 6 35 mm O ring inlet detector liners 0905 0767 1 4 inch glass packed columns split capillary inlet insert graphite 6 52 mm O ring splitless capi...

Page 17: ...e inlet these are discussed specifically later in this section see Inlet inserts In general the analysis to be performed determines the column to be used The column then dictates hardware required for the inlet and detector liner insert adapter jet FID or NPD Note C A correctly designed 1 4 inchpacked glass column requires no liners since the column ends themselves serve this purpose C The appropr...

Page 18: ... glass insert requires glass insert FID NPD2 19231 805211 19231 805301 None Liners Adapters TCD Liners Adapters None 19302 800201 19302 800201 may require altering the column ECD Liner Adapters 19301 805301 None None Packed Columns 1 Use 1 4 inch swage type nut and Vespel or graphite ferrule to install liner adapter 2 See Chapter 8 for details regarding jet exchange if necessary 3 See information ...

Page 19: ...r Insert Splitless silicone O ring Sampling Programmable 19245 205803 19245 20520 19245 20510 19245 On Column 20550 Capillary Inlet Insert FID NPD2 19244 805501 Same Same Same Liners Adapters TCD 18740 20950 19232 805501 Same Same Liners Adapters and 18740 209603 ECD 19244 805501 3 19233 80530 Same Same Liners Adapters Capillary Columns 1 Use 1 4 inch swage type nut if a nut is not supplied as par...

Page 20: ...side the oven are used with the packed column inlet and with all detectors depending upon the column to be installed Packed column inlet liners Liner Installed Liner Packed Column Inlet Figure 1 5 Liners for the packed column inlet are available in three sizes one for 1 8 inchcolumns one for 1 4 inchcolumns and one for HP Series 530 capillary columns ...

Page 21: ...cked glass columns The long leg of the column fits into the inlet body replacing the liner Packing and glass wool plug must be below the tip of the needle for best results C Metal columns are installed with a liner appropriate for the column diameter C If necessary glass columns can be installed using a metal liner preferably those accepting a glass insert but this is not recommended There may be ...

Page 22: ... installed when used with packed metal columns either 1 8 or 1 4 inch and with any type of capillary column Normally no liner is required with 1 4 inchpacked glass columns since the leg of the column itself serves as the liner For the FID or NPD the correct detector jet must be installed prior to installation of the liner If jets must be exchanged see Chapter 8 Preventive Maintenance ...

Page 23: ...mn applications In addition to install an HP Series 530 capillary column in an ECD or TCD having no capillary makeup gas adapter the following adapters are used Part No 19244 80550for the ECD and Part No 18740 20950and 18740 20960for the TCD Finally to use a 1 4 inchcolumn with the TCD having a base designed for 1 8 inchcolumns a 1 8 to 1 4 inchadapter is required Part No 19302 80020 For the ECD h...

Page 24: ...sion for capillary makeup gas Part No 18740 20950and 18740 20960 In this case no ferrule is required to form a seal with the detector base Note A graphite ferrule is strongly recommended since metal ferrules tend to lock permanently onto the liner adapter their use may require replacing the entire liner adapter should a permanent leak develop Exercise care The oven and or inlet or detector fitting...

Page 25: ...n the nut an additional 1 4 turn 5 Install the column then heat the oven inlet and detector to desired operating temperatures and only if necessary to stop leaks tighten fittings further Inlet inserts Inserts are used in inlets and can be installed from the top of the particular inlet Packed column inlet inserts Flared End Glass Insert for Packed Column Inlet Liner Figure 1 8 Assuming the correct ...

Page 26: ...t Figure 1 9 1 In handling the insert avoid contaminating its surface particularly its interior 2 Remove the septum retainer nut and septum 3 Carefully remove the old insert if present by withdrawing it straight up A match stick or similar fibrous item may be used as an aid in lifting the insert from the inlet 4 Install the new insert by dropping it carefully straight into the inlet liner flared e...

Page 27: ...r the liner or the column may shatter instead remove the column seat the insert and then replace the column 5 Replace the septum and septum retainer nut Split splitless or split only capillary inlet inserts Viton O ring Preferred Viton O ring Split Use Splitless Use Split Splitless and Split Only Capillary Inlet and Inserts Figure 1 10 A specific inlet insert is required depending upon the particu...

Page 28: ...e The oven and or inlet or detector fittings may be hot enough to cause burns WARNING Caution If operating in split mode carrier gas pressure must be reduced before opening the inlet If not done pressure may blow insert packing out of the inlet altering its characteristics Pressure is reduced at the backpressure regulator for the inlet 1 In handling the insert avoid contaminating its surface parti...

Page 29: ... and packing is inserted first into the inlet 5 Place a graphite or silicone O ringon the insert about 2 to 3 mm from its top end 6 Install the insert pressing it straight down as far as possible into the inlet Caution Do not add any seal either at the bottom of the inlet or at the bottom of the insert to do so will damage the inlet and or shatter the insert 7 Replace the insert retainer nut tight...

Page 30: ... to 1 0 mm od can be connected directly Some metal capillaries have a large diametersleeve soldered on each end this must be removed Use a small triangular file to score the tubing behind the sleeve then bend the sleeve back and forth until it breaks It is important to have fresh ends of the column free of burrs jagged edges and or loose particles of column stationary phase and or material from a ...

Page 31: ...2 Keyboard and Displays ...

Page 32: ...RAM PURGE FINAL VALUE INJ A TEMP INJ B TEMP DET A TEMP INIT VALUE IINIT TIME RATE FINAL TIME DET B TEMP OVEN TEMP OVEN MAX AUX TEMP EQUIB TIME STOP START STATUS RUN NOT READY FINAL TIME OVEN RATE INITIAL TIME STORE LOAD INJ B INJ A PRES PRES OVEN TRACK TABLE ADD DELETE PREVIOUS NEXT TIME Timetable Control Programmable Cool on Column Control Setpoint Storage Control ACTUAL SETPOINT HP 5890 SYSTEM R...

Page 33: ...ly monitored instrument functions and warning error information and diagnostic messages C LED Display Consists of two parts the left half OVEN displays oven status during a run the right half STATUS gives overall instrument status at any given time Displaying setpoints Any particular instrument current value and or setpoint is displayed at the alphanumeric display simply by pressing the appropriat...

Page 34: ...sing DET B TEMP gives the display ACTUAL SETPOINT DET B NOT INSTALLED Typical Display a Function NOT Installed in the Instrument Figure 2 3 Entering setpoints To enter a setpoint value for a particular instrument function the function is first displayed by pressing the appropriate key s Once the chosen HP 5890 function is displayed a new setpoint value can be entered at any time by pressing approp...

Page 35: ...MP 2 5 0 ENTER function key numeric key s Once detector A temperature is displayed by pressing DET A TEMP the new setpoint value may be entered at any time thereafter Note that the display shows a flashing asterisk while the new setpoint is entered disappearing when ENTER is pressed When ENTER is pressed the setpoint value is verified and if satisfactory becomes the new setpoint for the function I...

Page 36: ...required in terminating a sequence to assign a particular detector to a given output signal channel In general any display showing the flashing must be terminated using ENTER Upon pressing ENTER the value is verified to ensure it is within the range permitted for the particular function and or that the value is internally consistent with previously defined setpoint values for other related functio...

Page 37: ...eneral terms HP 5890 operation is the same whether the instrument is under local control or INET control controlled by a separate device If the HP 5890 is to be controlled through INET the following should be noted C In the event communication is lost e g by power lost at one or more devices on the loop a disconnected INET cable etc HP 5890 START and STOP keys will be disabled C Should the HP 5890...

Page 38: ...being altered unintentionally When the HP 5890 keyboard is locked setpoint values numeric values A B OFF and ON may only be displayed they cannot be altered START and STOP remain functional so runs may be started or stopped To lock instrument setpoints first enter the key sequence CLEAR ENTER Then press ON to lock the keyboard or OFF to unlock the keyboard Figure 2 5shows displays occurring during...

Page 39: ...d After locking or unlocking the keyboard return to operation by pressing any function key e g OVEN TEMP Loading default setpoints This function permits resetting HP 5890 operating setpoints to a standard set of values Only the following information is retained C Calibration constants for oven temperature control C All gas flow rate monitoring information gas types and calibration constants C Colu...

Page 40: ...ng OFF Cryo Blast OFF Equib Time 3 min Init Temp 50 C Init Time 650 min Oven Prog Rates 0 C min Final Temp 0 C Final Time 0 min Inlet Purge ON Purge Time 0 min Detector A B OFF Signal 1 Det Detector A Signal 2 Det Detector B if BOTH detectors A and B are installed otherwise detector A Range 1 2 0 Attn 1 2 0 ON Zero 1 2 0 ON HP IL INET Address 31 INET Global unconfigured Keyboard Lock OFF Timetable...

Page 41: ...e battery protecting memory should fail when main power is turned off the default setpoints are loaded into memory when the battery is replaced In addition calibration constants for oven temperature control and gas flow rate monitoring are also reset to default values ...

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Page 43: ...3 Temperature Control ...

Page 44: ...L TIME INJ A TEMP INJ B TEMP DET A TEMP OVEN MAX EQUIB TIME OVEN TEMP INIT TIME RATE DET B TEMP AUX TEMP Temperature Control Keys Figure 3 1 In these cases both current setpoint value and current monitored value are displayed by pressing the appropriate temperature control key For example Figure 3 2shows typical displays obtained by pressing OVEN TEMP ACTUAL SETPOINT OVEN TEMP 279 350 Typical Disp...

Page 45: ...SETPOINT values become equal In addition to keys 0 through 9 CLEAR and ENTER used in defining setpoint values ON OFF A and B are used in certain specific key sequences C ON and OFF add convenience in being able to switch on or off the oven and or heated zones without losing their current setpoint values C A and B are used in key sequences defining a multiple rampoven temperature program A as part ...

Page 46: ...e Oven Control 80 to 450 1 C Oven Control 0 to 650 00 0 01 minute Oven Control 70 to 450 1 C Oven Control 0 to 200 00 0 01 minute Oven Control 0 to 400 1 C Zone Control 0 to 400 1 C Zone Control 0 to 400 1 C Zone Control 0 to 400 1 C Zone Control 0 to 400 1 C Zone Control Valid Setpoint Range In Increments Of Function Key OVEN TEMP INIT TIME INIT TEMP FINAL TEMP INJ A TEMP INJ B TEMP FINAL TIME RA...

Page 47: ...ions These options include CRYO for operation during the entire run CRYO BLAST for very fast cool down between runs and AMBIENT to regulate on and off times to optimize coolant use For operation during runs at subambient temperatures ACTUAL SETPOINT CRYO ON ACTUAL SETPOINT CRYO BLAST ON For very fast cool down between runs ACTUAL SETPOINT AMBIENT 25 Lets you regulate Cryo and Cryo Blast on and off...

Page 48: ...O for operation during runs at subambient temperatures 25 50 75 CRYO ON CRYO OFF at ambient 15 CRYO ON at ambient 25 9 9 Figure 3 4 Oven profile using CRYO BLAST for very fast cool down between runs 40 80 120 CRYO BLAST OFF 30 sec modulation CRYO BLAST ON ambient 50 9 9 Figure 3 5 ...

Page 49: ...me for which oven temperature is held at INIT TEMP RATE Rate at which the oven is to be heated or cooled FINAL TEMP Temperature the oven attains at the end of a heating or cooling ramp In a multiple ramptemperature program final temperature for one ramp is also the initial temperature for the next ramp FINAL TIME Time period over which oven temperature is held at FINAL TEMP In a multiple ramptempe...

Page 50: ...ively through the entire group including A and B displays for second and third ramps This is an efficient way in which to review and if necessary change oven temperature program setpoints Oven status During a temperature programmedrun the LED OVEN display provides indication of oven status at any given time C Isothermal Run Assuming INIT TIME is assigned a value greater than 0 and that RATE 0 only...

Page 51: ...ched off OVEN TEMP OFF prior to accessing the oven interior e g to change columns check for leaks etc For safety this turns off power to the oven heater fan and cryogenic valve if installed but maintains the setpoint value in memory The oven is equipped with a shut offfeature to protect against unintentional opening of the oven door and or the possibility of mechanical and or electronic failure af...

Page 52: ...ated with heated zones or the oven In general the following problems are indicated when a FAULT message appears C ADC OFFSET indicates a problem with one or more electronic components in circuitry associated with temperature control C LINE SENSE indicates a problem with AC power to the instrument an excessively high source voltage C Any of the TEMP RDG messages indicate an inoperative temperature ...

Page 53: ...to the message the red NOT READY LED blinks All zones and the oven are turned off and made inoperative until power is switched off and then on again setpoints are maintained After a power failure Setpoint values are protected during a power failure even if intentional by disconnecting the power cord or by switching off the HP 5890 at its main power switch by a lithium battery 10 yearnominal life w...

Page 54: ...spective setpoint temperatures C The oven can be switched ON through the keyboard at any time without waiting for heated zones to first come to correct temperature C An analytical or column compensation run in progress at the time of a power failure is aborted similarly a keyboard entry in progress is aborted Oven temperature calibration To maximize precision with respect to retention time informa...

Page 55: ...Setting the oven calibration value An oven temperature calibration measurement should be made at a temperature in the middle of the range of interest Allow ample time up to 1 2 hour for thermal equilibration at the selected temperature no drift should be observed The temperature sensingprobe should be placed in the region of the oven occupied by the column s 1 Through the keyboard select CALIB AND...

Page 56: ... value should match closely the measured value Any delta value within the range 10 00 through 10 00 C may be entered If a value outside this range is entered the message CORRECTION TOO HIGH is displayed Assuming the battery protecting HP 5890 memory is operational a new calibration constant remains in effect even if the instrument is switched off or disconnected from its power source or if power f...

Page 57: ...4 Electronic Flow Sensing ...

Page 58: ...distinguished through A and B If carrier gas flows are monitored A implies flow through column A nearest the instrument front B implies flow through column B nearest the instrument rear Displayed flow rate values are in ml minute Displaying gas flow rate Current flow rate is displayed by pressing FLOW A or B Typical gas flow rate displays are shown in Figure 4 1 ACTUAL SETPOINT FLOW A 25 4 N2 ACTU...

Page 59: ...el press FLOW B to display FLOW A or FLOW B 1 2 3 or 4 is then pressed followed by ENTER Upon pressing ENTER the current flow rate is displayed scaled appropriately for the chosen gas type If a gas other than one of the above standard four is used select He N1 H1 or Ar CH3 according to which one is closest in thermal conductivity to the gas being used Under no circumstances should any corrosive ga...

Page 60: ...e zero value defined with no flow through the given flow channel and then the gain value calculated based upon a measured flow rate value If calibration is being performed for H2 observe proper safety precautions to prevent fire or explosion hazard WARNING Prior to performing the calibration procedure the following must be done C The instrument must be on for at least one hour for thermal equilibr...

Page 61: ...ion value The zero calibration value must be set with no gas flow through the channel being calibrated 1 Press ZERO FLOW A ZERO is displayed followed by a value the current zero calibration value for EFS Channel A Note that Channel A is assumed by default if channel B is to be calibrated instead press B 2 Disconnect the gas source to the particular flow channel being calibrated Do not trust an on ...

Page 62: ...revent twisting the tubes Outlet Line Channel B EFS Module Outlet Line Channel A Detail Electronic Flow Sensor EFS Module Figure 4 2 4 Install the EFS flow measuringadapter Part No 05890 80620 into the female OUT fitting to the EFS module Connect a bubble flow meter to the adapter Allow ample time up to 1 2 hour for residual gas within connected plumbing to bleed off Verify that absolutely no flow...

Page 63: ... keyboard press FLOW GAIN A or GAIN B is displayed followed by two values the observed flow rate through the channel and the current gain calibration value for the channel 2 Reconnect the gas supply to the channel being calibrated Do not reconnect the OUT fitting for the particular channel 3 Using a suitable flow measuringdevice accurate to better than 1 ml min connected at the OUT fitting for the...

Page 64: ...note the flow rate value at the connected flow measuringdevice Enter this measured value through the keyboard Measured Value ENTER Upon pressing ENTER CALIBRATING is displayed 6 After a short time GAIN A or GAIN B is again displayed followed by the observed flow rate and a new gain calibration value based upon the measured flow rate Note that the displayed flow rate value now should be quite close...

Page 65: ... the current gain calibration value for the channel Note that Channel A is assumed by default If Channel B is to be calibrated instead press B 2 Enter the desired gain calibration value preceded by Numeric Value ENTER is necessary to signify entry of a gain calibration value rather than a measured flow rate 3 Press ZERO FLOW A ZERO is displayed followed by a value the current zero calibration valu...

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Page 67: ...5 Signal Output ...

Page 68: ...separate levels of ANALOG output are provided depending upon the analog signal cable used 1 V or 1 mV 0 to 1 mV for strip chart recorders 0 01 to 1 V for electronic integrators with analog inputs The two output levels are independent and may be connected simultaneously to separate data receivingdevices Note A tick mark electrical pulse is produced at the 1 mV analog output when either START or STO...

Page 69: ...l channel key SIG 1 or SIG 2 followed by ZERO or simply press ZERO alone if the desired signal channel is already displayed Typical displays are shown in Figure 5 1 ACTUAL SETPOINT SIG 1 ZERO 104 5 ACTUAL SETPOINT SIG 2 NOT INSTALLED ACTUAL SETPOINT ZERO 1 104 5 OFF ACTUAL SETPOINT ZERO LIMIT 83000 Typical Displays ZERO Figure 5 1 Table 5 1lists conversions between detector units and the scale use...

Page 70: ...is good practice to have background reduced as much as possible by minimizing column bleed using clean supply gases and by performing proper detector maintenance 1 0 V maximum output level 1 000 V 0 100 V 0 010 V 0 V HP 5890 SERIES II electrical zero Constant 0 100 V detector background signal pressed 0 9 V usable dynamic range 1 0 V usable dynamic range ENTER ZERO O U T P U V O L T A G E T 1 V Ou...

Page 71: ...gure 5 3 identical treatment is made for the 1 mV output except that the signal is shifted to an offset somewhat above electrical zero This ensures a small positive offset about 6 of full scale in pen position at a connected chart recorder and permits uninterrupted plotting even if a small negative baseline drift occurs Once current ZERO setpoint value is displayed for the desired signal channel p...

Page 72: ...he expense of available output range for example to capture negative peaks or to compensate for negative baseline drift Signal attenuation Analog signal output levels 1 mV or 1 V outputs for either signal channel controlled by SIG 1 and by SIG 2 if Option 550 Accessory 19242A or Option 560 Accessory 19254A is installed are attenuated via RANGE 2 and ATTN 2 For RANGE 2 each step to a higher setpoin...

Page 73: ... be set properly first for the integrator or computer then ATTN 2 set appropriately for the chart recorder To minimize integration error for an integrator or A D converter RANGE 2 normally should be set to the lowest value possible provided the largest peaks of interest do not exceed 1 volt Attenuation functions at the integrating device or computer are then used to ensure that plotted peaks remai...

Page 74: ... to be measured Table 5 3lists maximum detector output producing 1 volt at the 1V output for each RANGE 2 setpoint value FID NPD pA TCD mV High Gain TCD mV Low Gain ECD kHz Maximum Detector Signal Producing 1 V Output 0 1 0 103 25 800 10 1 2 0 103 50 C 20 2 4 0 103 C C 40 3 8 0 103 C C 80 4 1 6 104 C C 160 5 3 2 104 C C 320 6 6 4 104 C C C 7 1 3 105 C C C 8 2 6 105 C C C 9 5 1 105 C C C 10 1 0 106...

Page 75: ...nt setpoint value for RANGE 2 or ATTN 2 is displayed by pressing the appropriate signal channel key SIG 1 or SIG 2 followed by either RANGE 2 or ATTN 2 or simply press RANGE 2 or ATTN 2 alone if the desired signal channel is already displayed For example the following key sequence displays current setpoint for RANGE 2 for the SIG 2 output channel SIG 2 RANGE 2 Typical displays that occur are shown...

Page 76: ...nction are displayed appropriate keys for the new value are pressed followed by ENTER to terminate the entry Switching off the 1 mV output The 1 mV signal output can be switched off providing no signal to the data receivingdevice This is often useful in setting the zero position at a connected strip chart recorder This is done through the following key sequence SIG 1 or SIG 2 ATTN 2 OFF The third ...

Page 77: ...ANGE 2 0 1 V analog output half heightwidth of this peak is about 0 13 minutes LIST LIST PEAK CAPACITY 1159 ZERO 3 1 5 ATT 2 7 CHT SP 1 3 PK WD 3 13 THRSH 3 AR REJ 3 HP 5890 RANGE 2 ATTN 2 0 0 1 V Analog Output START 25 75 1 25 STOP RUN 8 AREA RT AREA TYPE AR HT AREA 3 25 7939433 BB 3 135 93 397 3 75 793533 PB 3 135 9 335 1 25 79394 BB 3 134 3 898 TOTAL AREA 8812133 MUL FACTOR 1 3333E 33 Typical H...

Page 78: ... equivalent functions on the receiving device C An oven temperature program e g a setpoint value for RATE other than 0 must be set up at the HP 5890 for the test plot to function The test chromatogram is useful as a troubleshooting aid in deciding whether a lost or noisy signal observed at a connected integrating or chart recording device is due to a chromatographic problem lost sample due to leak...

Page 79: ...of setpoint and parameter information among INET instruments C Automation of data collection sample tracking and report generation Note In default operation the HP 5890 supplies only Signal 1 data to the INET loop That is HP 5890 data supplied to the INET loop is defined according to the assignment made via SIG 1 To use Signal 2 data instead signal reassignment is done at the HP 5890 The controlle...

Page 80: ...ntroller then retains this status for subsequent loop operations maintaining its responsibility as network traffic manager Note that the device defined as controller usually has other capabilities The controller assigns addresses to each device on the loop and configures them to operate in orderly fashion In addition the controller provides user access to the network configuration so desired chang...

Page 81: ...example integration Data or a command message destined for a particular instrument is labelled with the corresponding address for the instrument Setpoints The controller passes setpoints among INET instruments including itself and to and from local storage Setpoints are grouped according to the instrument to which they belong and labelled with the corresponding INET address Setpoint traffic is aut...

Page 82: ... its idle state waiting for initiation of some action e g starting a run listing information etc In this state the HP 5890 NOT READY LED is turned on if the HP 5890 is not ready and or if the INET system itself is not ready e g if a device on the loop is busy A message SYSTEM NOT READY will appear on the HP 5890 if some other device on the INET loop reports not ready and the HP 5890 is itself read...

Page 83: ...or specific information regarding INET loop control configuration workfile storage and recall etc consult the appropriate operation manuals for the INET controller device Also consult appropriate manual s for other devices sampler event control module etc configured in the loop Typical displays occurring when the HP 5890 is under INET control are shown in Figure 5 7 INET Displays ACTUAL SETPOINT U...

Page 84: ...e entry is aborted C If problems occur in transferring chromatographic setpoints to the HP 5890 the HP 5890 retains its present setpoints so there is no indication at the HP 5890 that transfer was attempted Appropriate error messages are printed at the controller device C SYSTEM NOT READY if displayed indicates one or more devices on the INET loop report not ready C UNDER REMOTE CONTROL is display...

Page 85: ...f these circumstances INET configuration The CONFIGURE NETWORK function provides four features verifying the INET address for the HP 5890 as determined through automatic loop configuration setting the default HP ILaddress to be used when the HP 5890 is connected to some device where addresses must be set manually i e no automatic loop configuration switching the INET function at the HP 5890 betwee...

Page 86: ...er devices on the INET loop In local mode note that the HP 5890 remains part of the INET system it reports its readiness to the system and pressing START and STOP keys on other devices on the INET loop e g the controller will affect HP 5890 operation Once in CONFIGURE NETWORK pressing ON or OFF switches respectively between global or local mode shows resulting displays as in Figure 5 9 ACTUAL SETP...

Page 87: ...urring either in verifying an INET address set through automatic loop configuration or in entering a specific HP IL default address used when the HP 5890 is included in an HP ILloop without automatic configuration The address is maintained in battery protectedmemory along with other instrument setpoints ACTUAL SETPOINT GLOBAL ADDR 8 31 ACTUAL SETPOINT GLOBAL ADDR 8 25 ACTUAL SETPOINT DEFAULT ADDRE...

Page 88: ...f cabling is altered or if one or more devices are powered off and then on again automatic loop configuration initiated by the controller updates the displayed value accordingly Setting the default HP IL address Remaining displays in Figure 5 10show the process of defining a specific HP ILaddress for the HP 5890 Entry of any value from 8 through 31 is permitted An attempt to enter an invalid value...

Page 89: ...ed SIG 1 or SIG 2 C ON indicates the given signal channel is considered active by the controller data from this signal channel is transmitted to other devices on the INET loop Similarly OFF indicates the channel is considered inactive no data from this signal channel is transmitted to other devices on the loop It is important to note that ON or OFF in this context are strictly INET definitions def...

Page 90: ... the HP 5890 to send an INET message directly to itself by connecting its INET output to its INET input The following procedure is used 1 Disconnect INET cables at their respective INSTRUMENT NETWORK IN and OUT receptacles on the HP 5890 located beneath the top right cover panel 2 Choose either one of the cables and disconnect it at the next device on the INET loop 3 Connect this free cable to bot...

Page 91: ... INET cable and repeat the test If FAILED SELF TEST is displayed again for a second cable electronic problems within the HP 5890 are indicated Note The loopback test may be used to check for continuity in an INET cable an open cable causes test failure Verify that the cable is at fault rather than the HP 5890 by testing a second cable If an intermittent cable problem is suspected the test may be r...

Page 92: ...TUAL SETPOINT WARN SIGNAL CHANGED ACTUAL SETPOINT WARN NO DETECTORS ACTUAL SETPOINT WARN INET TIMEOUT Signal Control WARN and FAULT Messages Figure 5 13 Figure 5 13shows possible WARN and FAULT messages associated with signal functions In general the following problems are indicated if the following messages appear C WARN INET TIMEOUT is displayed if information transmission on the INET loop is in...

Page 93: ... a particular signal channel channel 1 in the example displays In general if signal problems are suspected power to the HP 5890 may be turned off and then on again to perform internal self testing Appropriate message displays occur if problems are found to exist Note In case multiple problems exist simultaneously press CLEAR to roll through NOT READY and or FAULT displays Note that with exception ...

Page 94: ...e Transfer Mode HP 5890 SERIES II File Transfer Mode Transmits HP 5890 setpoints Transmits HP 5890 setpoints plus Timetable events Inlet pressure and temperature pro grams Up to 450 oven and FID temperature Cryo Blast and Ambient setpoints TCD sensitivity Aux temperature setpoint What is the proper mode for my data handling device Selection of the proper mode depends on the product and version of ...

Page 95: ...890 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 main PC board Main PC Board Top Hinge for Grounding Finding the Main PC Board Figure 5 15 3 Find component P15 on the main PC board ...

Page 96: ...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 GC chassis with an ESD strap or touch an unpainted area of the oven such as the door hinge HP 5890A mode HP 5890 SERIES II mode Setting the jumper Figure 5 17 ...

Page 97: ... to set the GC for 5890A mode use proper grounding 3 Download the workfile from the integrator 4 Turn GC power off 5 Remove the P15 jumper Now the GC is in SERIES II mode 6 Turn GC power on 7 Add SERIES II setpoints time table etc 8 Store the workfile at the integrator Note Using STORE on the HP 5890 SERIES II up to 4 integrator workfiles can be converted with each jumper change sequence ...

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Page 99: ...6 Inlet Systems ...

Page 100: ...l on columninformation see the manual Programmable Cool On ColumnInlet Maintenance information is provided in Chapter 8 Preventive Maintenance Packed column inlet The packed column inlet may be used with HP Series 530 capillary columns metal packed or glass packed columns Additionally on column injection is possible with 1 4 inchglass packed columns The packed column inlet is optimized for low to ...

Page 101: ...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 ...

Page 102: ...perature to be used Assuming column and liner plus insert if used are properly installed and the system is leak free the following is information necessary for proper operation Electronic flow sensor If Electronic Flow Sensing EFS is installed in the carrier gas system to the inlet total supply flow rate through the system may be displayed see Chapter 4 Electronic Flow Sensing for details This is ...

Page 103: ...rgedpacked column inlet may be used with HP Series 530 capillary columns metal packed or glass packed columns Additionally on columninjection is possible with 1 4 inchglass packed columns The septum purgedinlet provides superior reproducibility and quantitative accuracy at high inlet temperatures 250 to 400 C Trap s Carrier Gas External Plumbing Internal Plumbing Pressure Gauge Septum Purge Packed...

Page 104: ...int compounds resulting in nonreproducibility and discrimination against these compounds This effect has sometimes been mistakenly called needle fractionation A thermally optimized high temperature inlet The septum purgedpacked column inlet has been thermally optimized to provide an extremely uniform thermal profile throughout the flash vaporization region This thermal profile remains very close t...

Page 105: ...virtually eliminates injection port discrimination against high boiling point components When combined with fast automated injection excellent quantitative accuracy is possible Septum purge Best results are obtained by running a very low septum purge flow 1 to 2 ml min of purge flow is recommended never more than 10 of column flow rate Once the purge flow has been set it will remain constant regar...

Page 106: ... the system may be displayed see Chapter 7 Electronic Flow Sensing for details This is particularly convenient in situations when carrier flow must be turned off as when changing gas supplies or if supplies must be turned off nightly weekends etc Note The EFS requires at least one hour for thermal equilibration for reliable readings Assuming the system to be leak free and if total flow is 200 ml m...

Page 107: ... Metal Column Sealing O Ring 4 A CAPILLARY COLUMN B PACKED COLUMN Item Part No Description Number 1 Split Insert packed 18740 60840 1 Split Insert unpacked 18740 80190 2 Direct Injection Insert18740 80200 3 Splitless Insert 18740 80220 4 1 8 in Column Insert18709 80030 5 1 4 in Column Insert18745 80010 Available for Purchase NOTE Not shown Split Splitless Capillary Inlet Figure 6 5 ...

Page 108: ...ailable Inlet Inserts Figure 6 6 Note that performance in capillary analyses is closely related to the insert used and sampling mode Inserts supplied are average suitable for good performance over a variety of general applications For specialized applications however to optimize inlet performance custom madeinserts may be used any custom madeinsert must not exceed 6 52 mm od and must be 78 5 0 1 m...

Page 109: ... 2 1 0 8 6 4 2 10 20 30 40 50 60 70 80 90 H2 He N2 H E T P mm C17 at 175 C k 4 95 Glass W C O T OV 101 25 m x 0 25 mm Average Linear Velocity cm sec H E T P versus Linear Velocity Figure 6 7 Where temperature programming is to be performed a linear velocity value should be chosen in the region 1 1 2to 2 1 2times the linear velocity at the minimum point on the HETP curve for the particular carrier ...

Page 110: ...H1 and He to a lesser extent exhibit relatively flat minima Both are better suited as carrier gases when temperature programmed analyses are performed An unrelated problem with N2 is that it is available in many grades and is often contaminated with water and or light hydrocarbons He and H2 are typically available in higher purities Overall H1 is the best carrier gas choice with He nearly as good ...

Page 111: ...for Various Capillary Column Bores and Lengths It is important to note that flow settings made for one particular column are not necessarily correct for any other column or for every application Column flow rate should be verified and adjustments made as necessary whenever the column or other parts of the flow system are changed Split sampling In performing split sampling when using hazardous chem...

Page 112: ...ires rapid volatilization thus inlet temperature must be high enough to ensure this The backpressure regulator in the split vent path maintains constant pressure at the head of the column Total inlet flow controlled by a mass flow controller divides between a septum purge path and flow down the inlet insert Flow through the insert is divided again between flow into the column and flow around the b...

Page 113: ... to be made in split sampling mode C To display current inlet purge status PURGE VALVE A or B If OFF is displayed press ON to restore inlet purging C To display elapsed time during a run when inlet purging will be halted PURGE VALVE A or B TIME OFF C To display elapsed time during a run when inlet purging will be restored PURGE VALVE A or B TIME ON or ON alone if PURGE TIME is already displayed Fo...

Page 114: ...ntration This can create a long substantial solvent tail obscuring peaks of interest Thus after a short time interval the inlet insert is purged of solvent vapor After the inlet insert is purged oven temperature is increased causing solvent trapped at the head of the column to volatilize and move through the column Sample components are thus released to be separated Since sample residence time ins...

Page 115: ...phy 94 page 53 1974 Grob K and Grob G Chromatographia 5 page 3 1972 To reconcentrate sample components via the solvent effect oven temperature must be low enough so solvent remains at the head of the column for a sufficiently long time period A good guideline is to have the column 10 to 30 C below the solvent boiling point Table 6 2gives boiling points for some common solvents along with suggested...

Page 116: ... Table 6 2 Some Common Solvents Suggested Initial Oven Temperatures to Use the Solvent Effect The best solvent for a given application is found by trial and error depending upon sample solubility and volatility column polarity and type of stationary phase and detector selectivity sensitivity Note that because of the solvent effect retention times for the same components but dissolved in different ...

Page 117: ...mple requirements Injection volume is generally in the range 0 5 to 2 l Individual component concentrations must not be so great as to overload the column Retention indices for components of interest should be greater than 600 The maximum amount of sample injected without column overload depends upon column bore loading efficiency and component polarity Inlet temperature Because gas flow through t...

Page 118: ...he head of the column which may interfere with peaks of interest A solvent blank run to check solvent purity is strongly recommended before the solvent is used to dilute samples for analysis Inlet insert purge After injection sufficient time is allowed for solvent and sample components to reconcentrate at the head of the column then solvent vapor within the inlet insert is vented purged The specif...

Page 119: ...eas but does increase interference by the solvent tail Purging too early risks venting light components not allowing sufficient time for heavier components to enter the column and or not having sufficient solvent enter the column to ensure good reconcentration A recommended procedure is to analyze a known standard using conditions identical to those to be used for later sample analyses Ideally the...

Page 120: ...uge Septum Purge Control Capil lary Inlet Column C P S N O N C COM Flow Diagram Splitless Operation inlet purge Figure 6 11 IN OUT IN OUT GA 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 N O N C COM External Plumbing Internal Plumbing ...

Page 121: ...er flows through the top of the inlet to the split vent via the solenoid valve and backpressure regulator C After Injection At a predefined time after injection the solenoid valve returns to its original state restoring purge flow through the inlet insert In going from column flow septum purge flow at injection typically less than 5 ml min to total flow column split vent septum purge through the i...

Page 122: ...ample about 0 7 l helps to wash sample components from the syringe and needle bore For split sampling with high gas velocity through the inlet injection must be made in a continuous rapid manner Any lack of smooth motion may cause multiple injections For splitless sampling with low gas velocity through the inlet injection may be at a slower pace but must also be done smoothly Also note that retent...

Page 123: ...7 Detector Systems ...

Page 124: ...y makeup gas to ensure a total flow rate carrier makeup of at least 20 ml min The TCD is an exception requiring a total flow rate of only 5 ml min For the FID NPD and TCD HP Series 530 capillary columns may be used without capillary makeup gas as long as carrier flow rate is between 10 and 20 ml min Some loss of detector sensitivity may occur at lower flow rates For the ECD capillary makeup gas sh...

Page 125: ...ard FID and NPD 19244 80560 0 011 Capillary Column FID and NPD FID high sensitivity packed column Measured at the jet tip Use Jet Tip ID inch Part No Table 7 1 Available FID NPD Jets For an FID the 0 011 inchjet maximizes detector sensitivity and must be used with capillary columns if used with packed columns flame out and clogging problems may occur For an NPD exchanging jets is less critical to ...

Page 126: ...t H2 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 H1 airflame These include all organic compounds although a few e g formic acid acetaldehyde exhibit poor sensitivity ...

Page 127: ...mum detectable limit Linear range depends on each specific compound it is directly proportional to sensitivity of the FID toward the given compound In general where sample components of interest are in high concentration increased air flow may be necessary up to 650 ml min Where components of interest are in low concentration reduced air flow rates are acceptable 375 to 425 ml min For maximum sens...

Page 128: ... pressure ramp or switch to a more restrictive column longer and or smaller id Compressed Air Hydrogen Gas Capillary Makeup Gas Traps Final Pressure Regulators and Gauges Flow Manifold Block Vent to Ignitor Power Ignitor Button On Off On Off On Off MAKEUP GAS HYDROGEN AIR PRESS TO IGNITE Power to Ignitor Air Hydrogen Plus Makeup Gas Detector From Inlet Column External Plumbing Internal Plumbing Fl...

Page 129: ... Figure 7 3 The nitrogen phosphorusdetector uses a jet and collector similar to the FID however the collector contains a small alumina cylinder coated with a rubidium salt the active element which is heated electrically In the presence of this thermionic source nitrogen and phosphorus containing organic molecules are efficiently ionized Ions are collected and the resulting current is measured ...

Page 130: ...d of the active zone around the active element itself Because of this temperature dependence the output of the detector is very sensitive to anything that affects the temperature of this active zone Some of the important variables and their effects are listed below 1 Increasing detector temperature This increases the active element temperature and the response 2 Increasing electrical power to the ...

Page 131: ...of the active element and this results in a re equilibrationtime that is too long to establish proper background response negative solvent peaks killing the active element Compressed Air Hydrogen Gas Capillary Makeup Gas Flow Manifold Block On Off On Off On Off MAKEUP GAS HYDROGEN AIR Air Hydrogen Plus Makeup Gas Detector From Inlet Column External Plumbing Internal Plumbing Power to Active Elemen...

Page 132: ...e that gives a more positive offset than would normally result with a clean system When this happens there is a tendency to try to operate the detector with too little power to the active element with the final result that the detector does not appear as sensitive as desirable because the temperature of the active element is actually less than normal If the contamination is a negative type of cont...

Page 133: ...be turned off or element power reduced to zero when changing columns replacing septa and or replacing gas cylinders Power to the element with gas flow off can destroy an element within a few minutes Humidity also affects element lifetime adversely keep the detector warm 100 to 150 C when not in use A collector removed from an NPD for an extended period of time or spare collectors should be stored ...

Page 134: ... before changing septa When the detector is first turned on its sensitivity and signal level change slowly over several hours Therefore for applications requiring very stable operation leave the detector on overnight lowering oven temperature to prevent contaminating the active element with column bleed To preserve the active element lifetime it is good practice to reduce the power to the active e...

Page 135: ... USA owners Detector venting must be in conformance with the latest revision of Title 10 Code Of Federal Regulations Part 20 including Appendix B This detector is sold under General License owners may not open the detector cell or use solvents to clean it Additional information is available in the Publication Information For General Licensees Pub No 43 5953 1798 D Owners of this detector must perf...

Page 136: ...C After turning off main power and allowing the instrument to cool cap ECD inlet and exhaust vent openings Wear disposable plastic gloves and observe normal safety precautions C Return the cell for exchange following directions included with the form General License Certification HP Pub No 43 5954 7621 It is unlikely even in this very unusual situation that radioactive material will escape the cel...

Page 137: ...e detector ECD cell contains Ni a radioactive isotope emitting high energyelectrons µ particles These undergo repeated collisions with carrier gas molecules producing about 100 secondary electrons for each initial µ particle Further collisions reduce energy of these electrons into the thermal range These low energy electrons are then captured by suitable sample molecules thus reducing total electr...

Page 138: ...erted to a voltage linearly related to amount of electron capturingmaterial in the cell Flow Diagram Electron Capture Detector ECD Figure 7 6 Flow Manifold Block Capillary Makeup Gas Traps Final Pressure Regulators and Gauges On Off On Off PURGE FLOW MAKEUP GAS Detector Vent Anode Purge Flow Column Makeup Gas Adapters Capillary Columns Only Internal Plumbing External Plumbing Thus the ECD responds...

Page 139: ...oms molecule can be measured in the 1 to 10 picogram range The ECD is designed for use either with N1 or with 5 CH3 in Ar as carrier gas A switch selects operation with either carrier gas the ECD does not operate properly if the switch is incorrectly set See Chapter 5 of the Operating Manual Because of its high sensitivity the ECD should never be used without traps moisture chemical should be in g...

Page 140: ...rmance Ar CH3 as makeup gas may also be used For most purposes 60 ml min of makeup gas is satisfactory For very fast runs this can be increased to 100 ml min to sharpen peaks but some sensitivity will be lost since the ECD is a concentration dependentdetector H1 or He carrier gas affords the best column performance with reduced retention times Ar CH3 or N1 makeup gas is used in the range of 30 60 ...

Page 141: ...lyses to be flushed from the system and then make a blank run one with no sample injected Prior to the run enter the following DET A or B ON SIG 1 or SIG 2 A or B Pressing SIG 1 or SIG 2 again displays the signal source assigned to the particular output channel Ideally the value displayed should be within the range 10 to 40 100 to 400 Hz indicating a clean system For trace levelanalysis a reading ...

Page 142: ...on the ECD electronics board ECD Potentiometer Switch and Adjustment ECD Potentiometer Switch Up Adj Down Fixed ECD Potentiometer Adjustment 1 Remove the right side of the panel 2 Flip the switch up to the Adj position 3 Using a small screwdriver turn the potentiometer clockwise until the background level is at or slightly above 20 200 Hz low reading for trace analysis 4 Replace the right side of ...

Page 143: ...ng Flow 1 off 30 ml min Column Flow 30 ml min Switching Flow 2 on 30 ml min Switching Flow 1 on 30 ml min Column Flow 0 ml min Switching Flow 2 off VENT 60 ml min VENT 60 ml min 24 6 6 36 24 36 24 6 36 HP 5890 SERIES II TCD Cell Thermal Conductivity Detector TCD Figure 7 7 Filament Channel Filament Channel ...

Page 144: ...manently damaged if gas flow through the detector is interrupted while the filament is operating Make sure the detector is off whenever changes adjustments are made affecting gas flows through the detector Likewise exposure to O2 can permanently damage the filament Make sure the entire flow system associated with the TCD is leak freeand that carrier reference gas sources are uncontaminated before ...

Page 145: ...out 400 picograms ml of He carrier gas The TCD exists in two configurations either its exhaust vent tube exits at the top of the detector or the exhaust vent tube returns to the inside of the oven for connection to an FID or other device Reference Gas Capillary Makeup Gas Traps Final Pressure Regulators and Gauges External Plumbing Internal Plumbing Flow Manifold Block On Off MAKEUP GAS On Off REF...

Page 146: ...ure increases To minimize changes in detector sensitivity with different operating temperatures filament temperature is maintained at a relatively constant difference above detector operating temperature Filament resistance proportional to temperature is monitored and power is adjusted as needed to maintain the filament at constant temperature 500 400 300 200 100 0 100 200 30 0 400 Detector Temper...

Page 147: ... one of increased filament lifetime Gas flow rates After the detector and instrument are allowed time for thermal stabilization about 1 2 hourafter the oven and zones achieve desired setpoint values two gas flow rates column and reference gas must be set independently After setting optimal carrier gas flow rate through the column Figure 7 10may be used to determine the corresponding optimal refere...

Page 148: ...ay be used as carrier when analyzing for H1 this eliminates problems inherent in using He as carrier but detector sensitivity is substantially reduced toward components other than H1 To ensure normal peak shape in H1 analyses with He as carrier it is advisable to operate the detector at relatively high temperature between 200 and 300 C A specific detector operating temperature is found by analyzin...

Page 149: ...y it is recommended that operation with the standard 0 018 inchjet be tried first before deciding to switch to the 0 030 inchjet C Inside the oven connect the TCD oven returnexhaust vent tube to the base of the FID using the TCD to FID jumper tube Part No 19302 80600 and standard 1 8 inchstainless steel swage typenuts and ferrules Ferrules should be preset and two wrenches should be used in opposi...

Page 150: ...mn bleed C After setting column flow rate makeup gas should be set so total flow rate column makeup is 5 ml min Reference gas should be turned off while making this measurement Measure the column flow rate Open counterclockwise the On Off valve for TCD makeup gas flow Use a small screwdriver to adjust the variable restrictor at the center of the On Off valve as necessary to obtain the desired tota...

Page 151: ... air or hydrogen oxygen ratio Less critical are the auxiliary nitrogen carrier combined flows A suggested way to set near optimalflows is to begin with recommended flow rates located in the HP 5890 Operating Manual Then vary each gas until a local maximum is reached Optimize hydrogen first then air or oxygen and lastly the auxiliary nitrogen flows This may require a couple of iterations tries Adju...

Page 152: ...erature may give the best results If analyzing compounds with high boiling points the detector temperature should be set at least 25 C but not 300 C above the final oven temperature but not greater than 300 C C Quenching Quenching can result to some degree if sulfur or phosphorus peaks coelute with large hydrocarbon peaks For many applications this effect can be reduced by better chromatographic s...

Page 153: ...e after pressing the ignitor If the FPD flame won t light or stay lit check do the following 1 Be sure there is a problem Under some conditions the flame lights so quietly that the pop is nearly inaudible Also especially in oxygen mode the increase in signal offset on the LED display is usually only a few counts Flame ignition is best verified by holding a mirror or shiny surface near the aluminum...

Page 154: ...ector temperature raised to 200 C or higher but do not exceed the detector s maximum temperature of 300 C and ignite the flame After the flame is lit set the detector to the required temperature 6 If none of the above are sufficient to light the flame try increasing the hydrogen supply pressure by 20 40 After igniting the flame reduce the hydrogen supply pressure to the initial value 7 If the flam...

Page 155: ...8 Preventive Maintenance ...

Page 156: ...ith capillary columns since there is little stationary phase For the same reason however conditioning must be gentle not to drive stationary phase from the column The following are general guidelines for conditioning 1 Switch off detectors Shut off support gases if any to detectors particularly H1 2 a If the column to be conditioned is already installed disconnect its detector end b If the column ...

Page 157: ...m id establish a head pressure in psi equal to about half the column length in meters For example a 50 m column should have a head pressure of about 25 psi 172 kPa c For a fused silica capillary column establish a column head pressure in psi equal to column length in meters 4 Set oven temperature to 100 C for about an hour Then slowly raise oven temperature to the conditioning temperature for the ...

Page 158: ... of the column make sure neither packing nor a glass wool plug retaining the packing comes in contact with the bottom of the detector jet 2 For 1 8 inchcolumns where flash volatilization is used packing should be as close to the inlet end of the column as feasible leaving room for a glass wool plug to retain packing material Glass Wool 75 mm 3 in 45 mm 1 3 4 in Inlet End Flash Vaporization Detecto...

Page 159: ...eaking septum is evidenced by longer retention times loss of response and or loss of column head pressure as well as degradation in detector signal quality the signal becoming increasingly noisy Where the instrument is used on a regular basis daily septum replacement is recommended Septum Retainer Nut Septum Packed Column Inlet Replacing the Septum Figure 8 2 Caution Turn off the detector particul...

Page 160: ... is spring loadedto provide sufficient pressure for sealing Restore carrier flow Insert liner care Cleaning inlet inserts and or liners is discussed under Liner and or insert care later in this chapter Leaks Leaks in the gas plumbing system can affect chromatographic results dramatically The following procedure checks the flow system up to but not including the column connection If this portion of...

Page 161: ...and C Use a suitable leak detectionfluid to check for leakage fittings Correct or replace leaking fittings as needed Caution Leak detectionfluids often leave contaminating residues after each application the area checked should be rinsed with CH3OH methanol and allowed to dry C After verifying fittings are leak free there are two locations at the inlet itself where leakage may occur at the septum ...

Page 162: ...uminate the inside of the inlet from inside the oven while looking through the inlet from the top If there is evidence of contamination or deposits the inlet should be cleaned Use a swab and an appropriate solvent to scrub interior walls until deposits are removed A suitable wire may be used to dislodge solid particles carefully Dry thoroughly with compressed filtered dry air or N1 before reassemb...

Page 163: ...y Septa 11 mm Part No 5181 1263 package of 25 are recommended Note that regardless of the material septa must be clean and free of particulate matter Exercise care The oven and or inlet or detector fittings may be hot enough to cause burns WARNING Caution If operating in split mode carrier gas pressure must be reduced before opening the inlet If not done pressure may blow insert packing out of the...

Page 164: ...8 4 2 The new septum is placed in the top of the inlet base Make sure that sealing surfaces at the top of the inlet and inside the retainer nut are clean no particulate matter 3 Replace the septum retainer nut tightening it to finger tightness as tight as possible by hand without using any kind of tool Do not overtighten the retainer nut is spring loadedto provide sufficient pressure for sealing I...

Page 165: ...g a paper clip or similar gaugewire in the same manner as a capillary column Capillary Inlet Plug Installed for Leak Test Figure 8 5 3 Adjust the split flowflow controller to about 60 ml min 4 Adjust or set the column head pressure to obtain a column pressure of 138 kPa 20 psi gold 2 0 ENTER Set inlet B pressure to 20 psi INJ B PRES 5 Shut off septum purge or cap the septum purge vent with a suita...

Page 166: ...panel and onto the supply itself Repair or replace fittings and components as necessary Caution Leak detectionfluids often leave contaminating residues After each application the area checked should be rinsed with CH3OH methanol and allowed to dry C Check the inlet itself at three possible locations The septum The column connection The seal O ring around the insert retainer nut Note The following ...

Page 167: ...s replace the ferrule Note that if the inlet is hot leak detection fluid may boil giving false indication of a leak C If the septum and column nut prove to be leak free replace the seal O ring on the inlet insert Repressurize the system and check again for overall system leak down Flow Module Split Splitless Capillary Inlet Location of the Split Splitless Capillary Inlet Solenoid Valve Figure 8 6 ...

Page 168: ...e of the inlet If there is evidence of contamination or deposits the inlet should be cleaned Use a swab and an appropriate solvent to scrub interior walls until deposits are removed A suitable wire may be used to dislodge solid particles carefully Dry thoroughly with compressed filtered dry air or N1 before reassembling Vent lines can be removed for cleaning or replaced as necessary Compressed dry...

Page 169: ...ert for a split splitless or split only capillary inlet system is to be cleaned remove its packing C Because contamination is often in the form of carbonaceous materials insoluble in organic solvents immersion in concentrated chromic acid for up to 24 hours is recommended as the first cleaning step Concentrated chromic acid is highly toxic and corrosive Observe proper safety precautions WARNING C ...

Page 170: ... procedures used If they must be used thorough cleaning chemical and physical is required C Use a fresh small amount of a conventional coated packing such as 2 OV 1on 100 120 mesh Chromosorb W HP C Packing is held in place between plugs of silanized glass wool Part No 8500 1572 Glass Wool Packing 35 mm Packing Requirements Split Insert Figure 8 8 C To ensure compatibility with standard 2 inchsyrin...

Page 171: ... loose material out of the insert or liner C For any of the inserts used with the dedicated on columncapillary inlet use a stainless steel cleaning wire Part No 19245 20570 0 007 inch 0 2 mm od 1 5 inch 3 8 cm long package of 4 to dislodge solid material Flame ionization detector FID In addition to the detector itself other systems associated with the detector may also require routine maintenance ...

Page 172: ... be necessary Flame Ionization Detector Figure 8 9 Note The proper jet must be installed prior to column installation If switching from packed column operation to capillary operation the jet for capillary use must be installed prior to column installation Depending upon the column type to be installed packed versus capillary the proper jet must be installed Table 8 1lists available jets ...

Page 173: ...ur with solvent peaks Measured at the jet tip Table 8 1 Available FID NPD Jets Because jet exchange requires disassembling the collector assembly from the detector base it is also a convenient opportunity to inspect the detector collector and base for contaminating deposits Proceed to the next section to disassemble the detector to exchange the jet and to perform any necessary cleaning Cleaning Bo...

Page 174: ...ol Open the top cover at its front edge to access the detector 1 Using a Pozidriv typescrewdriver remove three screws around the detector cover and remove the cover 2 Remove the FID collector assembly by pulling it straight up 3 Use a cleaning brush Part No 8710 1346 to scrub the interior of the collector Using compressed air or N1 blow out loose material from inside the collector Wear proper eye ...

Page 175: ...D 175 Wash the collector in distilled water hexane and or CH2OH 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 ...

Page 176: ...nternal bore and exterior of the jet with a 1 1 V V solution of CH2OH methanol and CH2 1CO acetone 6 Clean the detector base cavity using solvents a swab and compressed air or N1 7 Reinstall the jet tightening it to finger tightness and then an additional 1 8 turn Caution Do not overtighten the jet Overtightening may permanently deform and damage the jet the detector base or both 8 Replace the col...

Page 177: ...that flame lighting problems may occur at very high flow rates 50 ml min If problems arise with He carrier makeup gas try using the lowest flow rate possible consistent with obtaining good chromatography Assuming these things are correct that the detector is contaminant free and that the ignitor is operational if ignition problems persist a damaged jet may be the cause Remove and inspect the jet l...

Page 178: ...se H2 gas as fuel If H2 flow is on and no column is connected to the detector inlet fitting H2 gas can flow into the oven and create an explosion hazard Inlet fittings must have either a column or a cap connected at all times WARNING Cleaning Both the jet and the detector base require occasional cleaning to remove deposits usually consisting of white silica from column bleed Such deposits reduce s...

Page 179: ...detector cover and carefully remove the cover see Caution below Caution Note that the transformer supplying power to the active element is secured to the inside of the cover It may be left in place but be careful not to stress its leads either those to the collector or those to the detector signal board NPD Collector Assembly Active Element Active Element Transformer NPD Collector and Active Eleme...

Page 180: ...erprints and or other contamination may cause baseline drift and noise 3 If worn or cracked replace the collector sealing gasket Part No 0905 0915 see Figure 8 1 1 4 Using a 1 4 inchhex nut driver unscrew counterclockwise and remove the jet from the detector base see Figure 8 12 5 The jet exists in two sizes 0 018 or 0 011 inch Use a cleaning wire 0 016 inchod 12 inchlength Part No 18765 20070 to ...

Page 181: ...certain the spring contact to the signal board is in good contact with the groove on the collector see Figure 8 13 During reassembly do not touch the lower portion of the collector assembly because fingerprints and or other contamination may will cause baseline drift and or noise Removing replacing the NPD collector Collector Body Note Position of Collector NPD Active Element NPD Collar Cross Sect...

Page 182: ...ector assembly Use clean lint freegloves to prevent contamination of the assembly Suitable gloves HP Part No 8650 0030 are available 1 Following the procedure under Cleaning remove the collector assembly from the detector base A 1 5 mmhex wrench is required for disassembly 2 Loosen the setscrew in the brass collar at the top of the collector assembly Remove the transformer lead from the collar the...

Page 183: ... the collector body against the stainless steel spring spacer 7 Inspect the brass collar note that the hole through it is slightly larger on one side than the other Install the brass collar onto the end of the collector so the side with the larger hole is toward the collector body 8 Press the assembly together firmly by pressing down on the brass collar while holding the collector body Make sure t...

Page 184: ...aution During disassembly do not touch the lower portion of the collector assembly Use clean lint freegloves to prevent contamination of the assembly Suitable gloves HP Part No 8650 0030 are available 1 Remove the two screws holding the transformer inside the cover 2 Remove the two screws holding the collector insulator to the cover These are removed from the top side 3 Slide the transformer wires...

Page 185: ...y dirty it should be replaced with the 1 4 in nutdriver supplied with the instrument Using the nutdriver unscrew turn jet counterclockwise and remove the jet from the detector base C The jet exists in two sizes 0 018 in and 0 011 in id A cleaning wire may be used to help remove deposits from the bore of the jet jet cleaning wire Part No 18765 20070is 12 inches of 0 016 od wire that can be used for...

Page 186: ...overtighten the jet Overtightening may permanently damage the jet the detector base or both 2 Cleaning and reassembly of the collector collector assembly is as follows C Powdery deposits may be removed from the interior of the collector by gently blowing out the loose material with low pressurecompressed air or nitrogen Caution Do not attempt to clean out the inside of the collector by inserting o...

Page 187: ...tor body 2 examine the collector sealing gasket for wear or cracks and replace if necessary 3 place the stainless steel spacer spring onto the collector body assembly 4 place the Teflon spacer on top of the spring the side with the groove faces up 5 if necessary replace the bottom transformer secondary wire into the hole in the collector body and tighten the setscrew onto the wire connector C Atta...

Page 188: ... 2 A or B If the displayed value exceeds 100 1000 Hz indicating a high background signal investigate the following possibilities C Contaminated carrier gas trap s and or supply C Insufficient column conditioning C Contaminated detector C Column inlet and or septum bleed C Leaks C Anode insulation leakage Carrier gas evaluation Because of its very high sensitivity the ECD is particularly prone to c...

Page 189: ...ayed signal values should be within the range 40 to 100 400 to 1000 Hz there may be downward drift 8 If displayed values are greater than this range trap s may be at fault Connect the carrier gas supply line directly to the detector base and repeat the test If values are now within range trap s are likely at fault if still out of range the carrier gas supply itself may be contaminated Leaks Note T...

Page 190: ...assembly and or cleaning procedures other than thermal should be performed only by personnel trained and licensed appropriately to handle radioactive materials Trace amounts of radioactive 63Ni may be removed during other procedures causing possible hazardous exposure to µ and X radiation bremsstrahlung Cleaning by bake out of the detector is performed only after verification that carrier supply g...

Page 191: ...recommended that the detector be returned to Hewlett Packard for cleaning Capillary column 1 Close the makeup gas and anode purge on off valve 2 Remove the column from the makeup gas detector 3 Install a paper clip or similar gauge wire in the same manner as a capillary column 4 Open the makeup gas on off valve and establish a makeup gas flow rate of 50 to 60 ml min 5 Open the anode purge on off v...

Page 192: ...s supplied with each new ECD Its contents are listed in Table 8 2 Part No 1 Envelope 05750 80036 4 2 Envelope 05890 90920 4 3 Information Card 18713 90040 12 4 Filter Paper Circular 3150 0429 12 5 Service Note 5950 3586 1 6 Plastic Bag 9222 0308 12 Item Description Qty Table 8 2 HP 5890 Radioactivity Leak Test Wipe Test Kit Thermal conductivity detector TCD Cleaning Cleaning by bake out of the det...

Page 193: ... tube PMT window Contamination anywhere along the light path between flame and PMT can reduce detector sensitivity Turn the detector off Turn off hydrogen air or oxygen and auxiliary nitrogen supplies to the detector manifold on offvalves for convenience carrier flow and other temperature zones may be left on and at their respective setpoints Allow time for the detector module to cool Remove the P...

Page 194: ...window in a manner similar to the filter Note placement and types of seals found on disassembled parts Seals should be replaced on reassembly See Figure 8 21for seal part numbers Inspect the windows chips missing scratches and or cracks in the light path scatter light reducing detector sensitivity Replace window s if necessary first window Part No 19256 80030 second window Part No 19256 80060 Reas...

Page 195: ...Preventive Maintenance Flame photometric detector 195 A B C D E 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 3 to 6 mm a x Subassembly Parts Identification Figure 8 20 ...

Page 196: ...cer Ignitor 19256 20590 1 13 Glow Plug 0854 0141 1 14 O ring Kalrez Ignitor 0905 1102 1 15 Weldment Block 19256 80560 1 16 Exit Tube Assembly 19256 20700 1 17 O ring Orange 1 05 inch id Silicone 0905 1104 1 18 Drip Tube Silicone Rubber 19256 20730 1 19 Gasket Head Shield 19256 80040 1 20 Window First Heat Shield 19256 80030 1 21 Disk Heat Shield 19256 20580 1 22 Coupling Stainless Steel 19256 2055...

Page 197: ...plier tube PMT assembly from the detector module also remove the filter Set both in a safe place Also remove exhaust tubing 1 4 inchswage fitting and the chimney assembly two M4 screws on sides Then loosen the U clamp that locks the burner to support bracket Part No 19256 00080 and disconnect the jet assembly from the transfer line tube Carefully lift the detector module vertically from the transf...

Page 198: ...nsfer line Caution Be careful not to crush or side load the fused silica liner when reinstalling the detector Whenever working with exposed fused silica tubing wear eye protection fragments of fused silica could be released if the fused silica is fractured or crushed WARNING 10 Reinstall the PMT assembly on the detector module restore instrument gases and power FPD leak testing GC with electronic ...

Page 199: ...ted in an instrument without an electronic flow sensor possible leak sources can be checked in the order listed 1 through 5 above This can be done by capping off the detector exhaust and pressurizing the system to 140 kPa 20 psig Then close off the supply flow and monitor the rate of pressure drop Pressure should drop no more than 7 kPa 1 psig per minute If using liquid solution to locate leaks to...

Page 200: ...e chemical trap assembly to the reconditioning gas source using a graphite or a graphitized Vespel ferrule Part No 0100 1 107 and swage nut Part No 0100 0058 as metal type ferrules will damage the sealing surface of the 1 8 inchadapter Remove the O ring Part No 5180 4181 as the conditioning temperature will destroy it Set oven temperature to 300 C Establish a purge gas flow of 60 to 100 ml min ove...

Page 201: ...9 Chromatographic Troubleshooting ...

Page 202: ...inappropriate setpoints C Leaks column or septum bleed or other chromatographic difficulties These may interact to a bewildering degree For example baseline problems may arise from any of the above areas Accordingly this chapter is organized by symptoms with reference to most probable causes Baseline symptoms Position 1 Baseline not at left lower part of chart C Check the zero of your recording de...

Page 203: ...Cases following assume that sufficient stabilization time has elapsed since the last change in operating conditions Wander and drift are often accompanied by noise discussed below 1 Baseline moves steadily upscale or downscale drift during the run C This is most frequently seen during temperature programming Operation with a single column no column compensation at moderate to low attenuation cause...

Page 204: ... as attenuation is decreased Noise limits useful detector sensitivity thus it should be minimized 1 Noise appears suddenly on a previously clean baseline C Consider all changes made recently in the system Reduced attenuation for example makes noise more apparent though the absolute noise level is unchanged C New septa may contribute noise from bleed of low molecular weight material If noise decrea...

Page 205: ...re susceptible to gradual buildup of deposits in the collector In extreme cases spiking occurs along with increased noise level Silicon dioxide deposits are formed when bleed from a silicone column is burned in the flame This material is removed mechanically Preventive measures include use of low column loadings stationary phases with high temperaturelimit thorough column conditioning before use a...

Page 206: ...tions regarding servicing boards and connectors for the HP 5890 2 Spikes appear on chromatograms but not when the recorder is isolated no input signal C This indicates a detector problem In extremely dirty FID collectors particles may break away causing disturbances in the most sensitive area of the detector This appears on the chart as a spike C A less common cause is column packing particles bei...

Page 207: ... probably at the beginning of a run C The carrier gas tank may be nearly empty 2 In a series of runs retention times suddenly decrease C This is likely to be due to a setpoint change either in oven temperature or in carrier gas flow rate verify both Retention time wander reproducibility 1 Retention time reproducibility is erratic throughout the run C If the runs are made with manual injection the ...

Page 208: ...is range results can be very erratic 3 Reproducibility is good later in the run but not for the first few peaks C When earliest peaks elute very rapidly they may not have had time to achieve chromatographic equilibrium with the stationary phase they act like solvent peaks and are blown straight through the column A useful rule is that peaks of interest should require at least four times as long to...

Page 209: ... addition to those expected from the sample Ghost peaks appear even when no sample is injected and also appear among the genuine peaks during a sample run 1 Peaks appear during a blank run These are ghost peaks usually found during temperature programmedruns the cause is contaminants trapped at the head of the column at the relatively cool starting temperature These are released and chromatographe...

Page 210: ...a blank run if the peaks persist they are not sample related C A common cause of extra peaks assuming the sample is pure is degradation of one or more components by an overheated inlet Test this by reducing inlet temperature Operate the inlet at as low a temperature as possible without causing peak broadening due to slow vaporization Also perhaps a more volatile solvent can be used In extreme case...

Page 211: ...ormally then drops sharply to baseline Overloaded Peak Figure 9 1 C The most likely cause is column overload dilute the sample ten foldand run it again C This may also be two or more closely merged unresolved peaks lower oven temperature 30 C and repeat the analysis If partial separation is seen merged peaks are present 2 The peak rises sharply and then falls normally to baseline Abnormal Interact...

Page 212: ...peaks C Low inlet temperature may cause this as can poor injection technique 3 Top apex of the peak is deformed Detector Overload Figure 9 3 C Detector overload is the probable cause The distortion is not easily seen on the chart but reveals itself in an integrator report In extreme cases doubling amount injected causes little or no increase in peak size Inject less sample or dilute it whichever i...

Page 213: ...ss overload of an FID may cause the top of the peak to invert giving appearance of a split peak Check gas flows overload is more likely when flows are too low Dilute the sample by a factor of at least 10 and repeat the run If the split disappears overload is the problem It is advisable to dilute samples even more by 100 or 1000 to ensure the detector is not close to its overload condition Such dil...

Page 214: ...al for effective troubleshooting The following symptom causelist gives the most commonly encountered problems and solutions found with valves Loss of sensitivity or excessive drift Several possible causes exist for overall deterioration of the chromatogram C Contamination in the valve requires a thorough cleaning C Internal leakage necessitates a complete disassembly and inspection of the mating s...

Page 215: ...njections of large volume samples or by changing the amount of restriction in the flow path These upsets will become more of a problem when high sensitivity is required Addition of a fixed restriction downstream from the valve may help minimize the upset When possible changes in column length may also help reduce the upsets Fixed restrictors are used immediately before flame detectors to prevent f...

Page 216: ...Extraneous peaks can occur sometimes due to improper conditioning of the valve or contamination If leaks are not apparent clean or condition the valve Obviously other causes totally unrelated to the valve may exhibit similar symptoms Impure i e containing water carrier gas can cause extraneous peaks Locating leaks Leak checkingthe plumbing involved in a valve configured system must be done careful...

Page 217: ...ro flow 3 Turn the knob on the regulator counterclockwise until it turns freely The regulator is now turned off and the gauge is indicating pressure within the valve system 4 Commonly the pressure will drop quickly for approximately 30 60 seconds then stabilize After this initial drop the gauge should not show more than a 6 89 to 13 78 kPa 1 to 2 psi drop during a 10 minuteperiod 5 If no leak is i...

Page 218: ...pass flow maintains a small positive column pressure in the event of power failure protecting the analytical column Symptom Possible Cause Not enough pressure 1 Septum leaks or is missing Safety shutdown activated 2 Column is broken 3 Column ferrule seal leaks 4 Gas supply is off 5 Supply pressure is inadequate 6 Desired pressure may not be achieveable with the column in use Pressure goes to O or ...

Page 219: ...oard A safety shutdown can occur when 1 There is a leak in the system see Pressure control problems This includes missing septa or columns 2 The column is not restrictive enough to reach desired pressure i e 530 columns will not go to 100 psi with available flow Note When using pressure programming this may occur during a pressure ramp to too high a pressure 3 There is insufficient supply pressure...

Page 220: ...l 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 configuration 3 Turn the GC on ...

Page 221: ...LEFT Programmable Cool On Column PID RIGHT Purged Packed Inlet Split Splitless Capillary Inlet PID EPC A MODE A IN A0 IN A1 EPC B MODE B IN B0 IN B1 INLET B Split Splitless Inlet with Electronic Pressure Control INLET A Any Non Electronic Pressure Controlled Inlet RIGHT LEFT LEFT OPEN RIGHT CLOSED RIGHT RIGHT RIGHT RIGHT This group of switches controls the A position inlet If another electronic pr...

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Page 223: ...10 Test Sample Chromatograms ...

Page 224: ... that injection volumes listed with operating conditions in the following chromatograms do not necessarily indicate total absolute volume injected Volume given is simply the graduation plunger position read from a standard 10 l syringe For a heated inlet actual sample volume injected will also include an additional 0 4 0 7 l the volume of sample volatilized from inside the syringe needle For the d...

Page 225: ...in Ramp Rate 15 Fin Temp 150 Fin Time 1 Range 8 COLUMN Part No 19095 100 Dimensions 530 MID 5 M Sta Phase Methyl Silicone FLOW RATES Carrier He 20 1 ml min Hydrogen 33 1 ml min Air 400 20 ml min Makeup N2 10 1 ml min Split Vent N A ml min Septum Purge 1 2 ml min SAMPLE Type FID Sample Inj Volume 1 l Part No 18710 60170 Composition 0 03 V V each C14 C15 C16 normal paraffin hydrocarbons in hexane ST...

Page 226: ...me Range 0 COLUMN Part No 19095S 100 Dimensions 530 MID 5 M Sta Phase Methyl Silicone IF ST 659 START IF 2 138 FLOW RATES Carrier He 20 1 ml min Hydrogen 3 5 0 1 ml min Air 100 120 10 ml min Makeup He 10 1 ml min Split Vent N A ml min Septum Purge 1 2 ml min SAMPLE Type NP FID Sample Inj Volume 3 l Part No 18789 60060 Composition 0 65 ppm azobenzene 100 ppm octadecane 1 0 ppm malathion in isooctan...

Page 227: ...amp Rate 0 Fin Temp Fin Time Range 2 COLUMN Part No 19095S 100 Dimensions 530 MID 5 m Sta Phase Methyl Silicone START 88 12 2 35 STOP FLOW RATES Carrier N2 30 1 ml min Hydrogen N A ml min Air N A ml min Makeup N2 30 1 ml min Split Vent N A ml min Septum Purge 1 2 ml min SAMPLE Type ECD Sample Inj Volume 1 l Part No 18713 60040 Composition 33 pg l 0 033 ppm W V each and aldrin in isooctane LINDANE ...

Page 228: ...0 Fin Time 1 Range 0 COLUMN Part No 19095S 100 Dimensions 530 MID 5 M Sta Phase Methyl Silicone START 2 42 3 38 3 76 25 ST FLOW RATES Carrier He 20 1 ml min Hydrogen N A ml min Air N A ml min Makeup He 1 2 ml min Split Vent N A ml min Septum Purge 1 2 ml min Reference He 30 1 ml min SAMPLE Type FID Sample Inj Volume 3 l Part No 18710 60170 Composition 0 03 V V each C14 C15 C16 normal paraffin hydr...

Page 229: ...Flow Param EPP Constant Flow Off Range 4 COLUMN Part No 19095 100 Dimensions 530 MID 5 M Sta Phase Methyl Silicone START 331 112 4 743 5 398 6 322 267 FLOW RATES Carrier He 15 1 ml min Hydrogen 30 1 ml min Air 400 20 ml min Makeup N2 20 1 ml min Split Vent N A ml min Septum Purge 5 1 ml min SAMPLE Type FID Sample Inj Volume 1 l Part No 18710 60170 Composition 0 03 V V each C14 C15 and C16 normal p...

Page 230: ... 121 Dimensions 530 10 M Sta Phase Methyl Silicone FLOW RATES Carrier He 15 1 ml min Hydrogen 30 1 ml min Air 400 20 ml min Makeup N2 20 1 ml min Split Vent 200 20 ml min Septum Purge 5 1 ml min SAMPLE Type Capillary Sample Inj Volume 1 l Part No 18740 60900 Composition Soln of 0 1 w w n nonane n hexadecane and 0 1 w w each of 1 octanol nonanol n undecane naphthalene 2 deca none n dadecane n tride...

Page 231: ...Temp Fin Time Range 0 COLUMN Part No 19095Z 121 Dimensions 530 MID 10 M Sta Phase START 1 35 2 37 3 22 ST FLOW RATES Carrier He 15 1 ml min Hydrogen 3 5 0 1 ml min Air 100 120 10 ml min Makeup He 10 1 ml min Split Vent 80 5 ml min Septum Purge 5 1 ml min SAMPLE Type NP FID Sample Inj Volume 2 l Part No 18789 60060 Composition 0 65 ppm azobenzene 100 ppm octadecane 1 0 ppm malathion in isooctane AZ...

Page 232: ...Rate 0 Fin Temp Fin Time Range 0 COLUMN Part No 19095S 100 Dimensions 530 MID 5 m Sta Phase Methyl Silicone 43 37 1 13 2 64 ST FLOW RATES Carrier He 15 1 ml min Hydrogen N A ml min Air N A ml min Makeup N2 60 2 ml min Split Vent 60 2 ml min Septum Purge 5 1 ml min SAMPLE Type ECD Sample Inj Volume 1 l Part No 18713 60040 Composition 33 pg l 0 033 ppm W V each lindane and aldrin in isooctane LINDAN...

Page 233: ... 10 Fin Temp 150 Fin Time 2 Range 0 COLUMN Part No 19095Z 121 Dimensions 530 MID 5 M Sta Phase Methyl Silicone FLOW RATES Carrier He 15 1 ml min Hydrogen N A ml min Air N A4 ml min Makeup He 10 1 ml min Split Vent 200 10 ml min Septum Purge 5 1 ml min Reference He 37 1 ml min SAMPLE Type Capillary Inj Volume 1 l Part No 18740 60900 Composition See Split FID 4 45 4 78 6 48 ST 11 15 42 25 3 64 3 85 ...

Page 234: ...w Off Range 0 COLUMN Part No 19095S 100 Dimensions 530 MID 5 M Sta Phase Methyl Silicone START IF IF IF 896 1 966 3 356 ST P FLOW RATES Carrier He 15 1 ml min Hydrogen 4 1 ml min Air 90 10 ml min Makeup He 10 1 ml min Split Vent N A ml min Septum Purge 5 1 ml min SAMPLE Type NP FID Sample Inj Volume 3 l Part No 18789 60060 Composition 0 65 ppm azobenzene 100 ppm octadecane 1 0 ppm malathion in iso...

Page 235: ...w Param EPP Constant Flow Off Range 0 COLUMN Part No 19095S 100 Dimensions 530 MID 5 M Sta Phase Methyl Silicone 4 23 4 82 5 38 FLOW RATES Carrier He 20 1 ml min Hydrogen N A ml min Air N A ml min Makeup He 5 1 ml min Split Vent N A ml min Septum Purge 5 1 ml min Reference He 37 1 ml min SAMPLE Type FID Sample Inj Volume 3 l Part No 18710 60170 Composition 0 03 V V each C14 C15 C16 normal paraffin...

Page 236: ... Flow Param EPP Constant Flow Off Range 2 COLUMN Part No 19095S 100 Dimensions 530 MID 5 m Sta Phase Methyl Silicone 43 1 29 35 3 35 FLOW RATES Carrier He 15 1 ml min Hydrogen N A ml min Air N A ml min Makeup N2 60 2 ml min Split Vent N A ml min Septum Purge 60 1 ml min SAMPLE Type ECD Sample Inj Volume 1 l Part No 18713 60040 Composition 33 pg l 0 033 ppm W V each lindane and aldrin in isooctane ...

Page 237: ...med 1 ramp Init Temp 110 DEGREES C Init Time 0 min Ramp Rate ___10 Fin Temp __170 Fin Time ____3 Range 5 COLUMN Part No 19095S 100 Dimensions 5 M Length 530 ID Sta Phase Methyl Silicone 1 73 07 2 11 3 16 ZE IF Sulfer Filter START START IF 07 44 2 10 2 46 3 16 ZE Phospho rus Filter DODECANETHIOL TRIBUTYLPHOSPHATE DODECANETHIOL TRIBUTYLPHOS PHATE FLOW RATES FPD AIR MODE FLOWS Carrier N2 20 1 ml min ...

Page 238: ...rogrammed 1 ramp Init Temp 110 DEGREES C Init Time 0 min Ramp Rate ___10 Fin Temp _ 170 Fin Time ____3 Range 5 COLUMN Part No 19095Z 121 Dimensions 5 M Length 530 ID Sta Phase Methyl Silicone START IF 11 84 2 88 3 70 ZE START 11 71 2 88 3 70 ZE Phosphorus Filter Sulfer Filter DODECANETHIOL TRIBUTYLPHOS PHATE DODECANETHIOL TRIBUTYLPHOS PHATE FLOW RATES FPD AIR MODE FLOWS Carrier N2 20 1 ml min Hydr...

Page 239: ...ammed 1 ramp Init Temp 90 DEGREES C Init Time 1 0 min Ramp 1 2 Rate 20 10 Fin Temp 110 170 Fin Time 0 3 Flow Param EPP Constant Flow Off Range 5 COLUMN Part No 19095S 100 Dimensions 5 M Length 530 ID Sta Phase Methyl Silicone 1 45 4 08 4 57 5 37 START IF 13 49 Phosphorus Filter Sulfer Filter IF START 13 1 91 4 06 3 35 HP 5890 Test Sample Operating Conditions DODECANETHIOL TRIBUTYLPHOS PHATE FLOW R...

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Page 241: ...mn adapters 17 bracket 14 capillary 13 conditioning 156 ferrules 14 fittings 14 inserts 17 liners 17 nuts 14 o rings 14 packed 12 packing 158 placement 12 conditioning column 156 configuration 220 cryogenic oven control 47 D default setpoints loading 39 displaying gas flow rate 58 setpoints 33 displays 32 E ECD 188 carrier gas evaluation 188 cleaning 190 frequency test 188 leaks 189 on columntest ...

Page 242: ...37 split inlet test chromatogram 238 G gas carrier considerations split splitless capillary inlet 108 designating type 59 flow rate display 58 I ignition problems FID 177 INET keyboard control 37 inlet initial column head pressure 110 insert purge 118 packed problems at high temperatures 104 septum purge 105 packed column 100 159 purge status 113 septum purged packed column 103 split splitless cap...

Page 243: ...togram 234 replacing collector 181 split inlet test chromatogram 231 test chromatogram 226 nuts 14 O o rings 14 oven 11 isothermal 49 programming temperature 49 117 safety 51 status 50 temperature calibration 54 P packed column inlet 100 159 changing septum 159 cleaning 162 leaks 160 packing columns 158 peak problems deformed peaks 211 extra peaks 209 inverted peaks 209 no peaks 209 power fail 53 ...

Page 244: ...7 163 cleaning 168 insert care 164 leaks 165 split splitless inlet inserts 27 split splitless sampling injection technique 121 splitless sampling 114 inlet insert purge 118 inlet temperature 117 sample requirements 117 solvent purity 118 sub ambientoven control 47 T TCD 192 cleaning 192 on columntest chromatogram 235 split inlet test chromatogram 233 test chromatogram 228 temperature control 44 te...

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