Agilent Fundementals GC [PDF]

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Agilent GC Fundamentals Jagat Adhiya, Global Software Support ©2007 Waters Corporation



Agenda



0. Open Discussion 1. Review of GC Theory 2. Supported Configurations  Plus: Upcoming New Features 3. Creating Methods & Running GC Systems 4. Common Problems & Error Messages 5. Qualification: GC PQ 6. Conclusion and Final Review 7. Optional: Using GSS Knowledge Tools Company Confidential



© 2007 Waters Corporation



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Open discussion  What are your needs?  How do you currently lookup GC-related information?  What are the suitable ways for sharing info ? —(Webcasts, presentation, physical training)



 How can we be more successful with supporting GC systems at customer sites?



Company Confidential



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3



Part 1 Review of GC Theory



©2007 Waters Corporation



Basics of Gas Chromatography



Company Confidential



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5



Gas “The Mobile Phase” Gas



Helium - #1



Nitrogen #2



Hydrogen - # 3



Argon



Air



Use



Capillary Carrier Gas



Capillary Carrier Gas



Capillary Carrier Gas (non industrial)



GC/MS Carrier Gas



Detector Fuel Gas (FID)



Other



GC Use for all GC Detectors Detectors less –GC/MS/MS efficient



Detector Fuel Gas



Positives



Universal



Best HETP – Fast



Negatives



High Cost



Company Confidential



Need EPC*



Explosive



*Electronic Pressure Control



© 2007 Waters Corporation



6



Injector Port



 Purpose of port is to flash evaporate the sample and introduce it to the column — Good rule of thumbTinj > 50ºC above Tcolumn



Company Confidential



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GC Van Deempter Curve



Increasing the speed (flow rate) of the carrier gas speeds analysis time; but may reduce optimal chromatographic resolution. Company Confidential



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GC Injectors



Company Confidential



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EPC- Electronic Pneumatics Control



 Sets Pressure and Setpoints constant run to run  Retention Time Locking



Company Confidential



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Injecting the sample : Making it a Gas



 Sample is introduced by a injection port with a syringe.  Analytes are vaporized by the high temperature  Analytes kept gaseous by keeping temperatures above the analytes boiling point  Analytes are swept onto the chromatographic column by the mobile phase.



Company Confidential



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Split/Splitless Injector



 Split – Concentrated Samples — Volatile — Different Concentrations — Dirty — Usual GC Capillary Columns



 Spitless – Trace Analysis — More Difficult — Wide Range



 Sample Injected >50 degrees above boiling point  Packed Columns - .1-20ul  Capillary Columns - .001 ul



Company Confidential



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Split/Splitless Inlet



Company Confidential



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13



COC Injection  Inert Compounds  Underivatized drugs  Quantitation – no molecular weight discrimination  No Split uncertainty  Polymer additives



Company Confidential



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PTV Injection



 Large Volume Injections  Environmental  Semi-volatiles in water  Clean samples  Trace Detection  High Temperature Applications



Company Confidential



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15



Other: Headspace Sampling



 For Volatiles  The air space of a 2ml vial is called the headspace  Sample is at Room Temperature  Example: Driving Under the Influence of Alcohol Blood test



Company Confidential



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GC Columns



 Standard (N < 10,000) -- also called Packed — Gas-Solid Chromatography (GSC) o similar to adsorption liquid chromatography — Gas-Liquid Chromatography (GLC) o liquid stationary phase coated on support material o usually reversed phase



 Capillary (N < 200,000) — Have internal diameters that are less than 1 mm — 90% of GC is Capillary



Company Confidential



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GC Columns



 Narrower df = better resolution, longer retention time, lower β value  In general, more volatile compounds (smaller molar mass) spend less time on column than less volatile compounds  Low-β columns (large df) needed to separate low-molecularweight compounds  High-β columns (small df) needed to separate highmolecular-weight compounds



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Temperature Programming



 Isothermal (Isocratic)- the temperature is held constant during the entire analysis



Typical Temperature Ramp



 Temperature Program — Vary the temperature during the analysis



Temp



— Equivalent to a gradient run



 With homologues, the retention time increases exponentially with the number of carbons



Time



 As Tretention increases — Width of peak increases — Height of peak decreases — Detection becomes extremely difficult



Company Confidential



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Empower 6890 Control Choices Detector



Type



Support gases



Selectivity



Sensitivity



Flame ionization (FID)



Mass flow



Hydrogen and air



Most organic cpds.



100 pg



1.07E+02



Thermal conductivity (TCD)



Concentration



Reference



Universal



1 ng



1.07E+02



50 fg



1.05E+02



Dynamic range



Electron capture (ECD)



Concentration



Make-up



Halides, nitrates, nitriles, peroxides, anhydrides, organometallics



Nitrogenphosphorus



Mass flow



Hydrogen and air



Nitrogen, phosphorus



10 pg



1.06E+02



Mass flow



Hydrogen and air possibly oxygen



Sulphur, phosphorus, tin, boron, arsenic, germanium, selenium, chromium



100 pg



1.03E+02



Flame photometric (FPD)



Company Confidential



Other: µECD, Unknown, None,



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GC Detectors Sensitvity



pg – ng GC-Micro – GC-TOF



Company Confidential



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21



FID – Flame Ionization Detector



 Sensitivity from flame chemistry of component  He plus H2 and air as carrier gases  Sample enter at detector base mixes with hydrogen and enters the flame.  Ions are produce and measured  Response = number of carbons.  For hydrocarbons and other combustibles  Second-most common GC detector in use



Company Confidential



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22



Electron Capture Detector (ECD)



 For organics containing electronegative atoms  Beta particle source (63Ni or 3H) emits electrons that mix with carrier gas (Ar or N2 plus 10% CH4) to form plasma  Analyte electrons (from electronegative atoms) are “captured” upon interacting with plasma



Company Confidential



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Electron Capture Detector uECD - ECD



 Sample needs a gas phase electrophore  Compounds are ionized in a furnace, and the ion current is collected  Non-Destructive  Limit of Detection = ~0.1 pg Cl/second  Linear range = ~104  Mode of Detection: Absorption of beta (β) particles for sulfur-, nitrogen-, and halogencontaining compounds



Company Confidential



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ECD vs. FID



 ECD and FID analyses often compliment each other  Organics with electronegative atoms are usually not combustible and cannot be detected by FID  ECD shows little response toward hydrocarbons



Company Confidential



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Thermal Conductivity Detector



 Most common detector for GC  Uses He carrier gas  Non Destructive  Limit of Detection = ~400 pg/mL  Linear Range = ~ 106  Mode of Detection: resistance change from variations in the thermal conductivity of the gas from the column.



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Nitrogen-Phosphorus Detector (NPD)  Similar in principle to FID, but with no flame  Analyte is ionized by reaction with a heated Rb+ salt  Either positive or negative ions can be collected  Most sensitive to phosphorus- or halogen-containing compounds  Specific: sample must contain nitrogen or phosphorus  Destructive  Limit of Detection = ~ 0.4 pg N/second ~ 0.2 pg P/second  Linear range = 104  Mode of Operation: modified FID. Active element acts to block undesired species.



Company Confidential



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GC Detectors -- Summary



Company Confidential



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Part 2 Supported Configurations



©2007 Waters Corporation



Agenda  Supported hardware combinations  Supported new(er) Agilent hardware  Third-party instrument control and software  New GC Features in Empower 2 FR4 and FR5  Upcoming Releases of GC Related Software Features



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Supported Hardware Combinations Instrument



ALS Controller



ALS



Interface Device



6850 series II (G2630A)



Internal



7683 or 7683B



Ethernet



6850 series I (G2630A)



Internal



7683 or 7683B



Equinox card



6890 N (G1530N)



Internal



7683 or 7683B



Equinox card



6890 Plus (G1530A)



Internal



7683 or 7683B



Equinox card



6890 A (G1530A)



G1512A or G2912A



7683 or 7683B



Equinox card



5890 series I or series II



G1512A or 7673 or G2912A



7673 or 7683B



Equinox card or busLAC/E card



HS7694 (G1290B or G1289B Only)



N/A



N/A



Equinox card



G1888A Headspace



N/A



N/A



Ethernet



Company Confidential



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Supported New(er) Agilent Hardware



Company Confidential



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Supported New(er) Agilent Hardware Agilent 6850 Series I and II Gas Chromatographs (via Waters ICS)



Agilent 7683B Autosampler



Agilent G1888 Headspace Analyzer (via Waters ICS) Agilent G2912A ALS Controller



Company Confidential



Agilent 7694 Headspace Analyzer (via Waters ICS)



© 2007 Waters Corporation



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Headspace Control Option v2.00  Headspace Control Option v2.00 — Released Dec. 2007, Part number 667003493 (not free) — Supported with models G1888A, G1289B and G1290B — Supported with Empower 1154 and Empower 2 software o For Millennium32 V4.0, use Control Option v1.00 for model G1290B only



 Supported in Empower Personal and Enterprise — LAC/E32 may be used to control headspace modules — G1888A is an Ethernet controlled headspace analyzer — G1289B and G1290B are Serial controlled analyzers



 Compatible with 6890, 6850 and 5890 series GCs — Future support:7890 GC Company Confidential



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Agilent 6850 GC ICS v1.20



 Agilent 6850 Instrument Control Software v1.20 — Released Dec. 2007, Part number 667003518 — Supported with Empower 1154 and Empower 2 — Older GC model is supported via RS-232 only — Newer GC model is supported via Ethernet only



 Adds control of Cool-On-Column (COC) inlet



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35



Agilent 7683B Autosampler  Supported with 6890 series GCs for full Waters CDS control — Interface with 5890SII is required for control



 Older style GCs require upgrade to ALS Controller (G2912A)  You cannot mix and match 7673 modules with 7683 modules



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36



Agilent G2912A Autosampler Controller  Supported with 6890 series GCs for full Waters CDS control — IMPORTANT Interface with 5890SII is required for control



 Replacement for G1512A and G2612A ALS controllers — Controls the 7683 and 7683B ALS when installed on a GC



 The controller has no interface for entering settings



Company Confidential



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37



Third-Party Drivers



Company Confidential



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Equinox Drivers and Hardware



 Versions 5.41.0.0 and 5.30.0.5 supported by Empower 2 and Empower Build 1154  New batch file released by vendor to correct driver installation on systems with Windows XP Service Pack 2 —Batch file, installation procedure document and drivers can be ordered on a FREE CD using p/n 667003119 —Can be used on Windows 2000 SP 4 also  New style Equinox card and cables in stock —Waters Equinox control kit and spare parts part numbers remain unchanged Company Confidential



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Other 3rd Party Hardware (via OIP)



CTC Autosampler family



Teledyne Tekmar Headspace



Varian 39XL Gas Chromatograph



Company Confidential



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Open Interface Portal (OIP) Program  Waters Open Interface Portal, or O.I.P., program — Waters have an agreement with Agilent for instrument control — Allows development of instrument drivers outside Waters development by a 3rd party for end users (e.g., Varian, and Teledyne Tekmar drivers)



 Waters policies for 3rd party instrument control — Waters FSEs do not support 3rd party instrument drivers — Customers should approach the respective vendors for support their own software, including minimum Waters software requirements, firmware, etc.



Company Confidential



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New Features in Empower 2 Feature Release 4



Company Confidential



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42



New GC Features in Empower 2 FR 4 Three new tabs added to the Instrument Method Editor:  Auxiliary – control an auxiliary device (e.g., G1888 HS Analyzer**), by selecting thermal or pressure channels  Events – add events to instrument method, triggered by signal, valve, or pressure channels  Valves – control a maximum of 8 valves individually rather than as an event  In the Column 1 and Column 2 tab of the Instrument Method editor, a new outlet pressure selection box was added that lets you select from ambient, pressure correct, or vacuum correct outlet pressure.  See also: Empower 2 Help (In Instrument Method Editor, press F1 in the Auxiliary, Events, or Valves tab.) Company Confidential



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Empower and 6890 New Features in FR 4: Auxiliary Channels and Valve Control



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44



New in Empower 2 Feature Release 5



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Selected GC New Features in Empower 2 FR 5  PCS 21060 – 6890 - Add FID and FPD Lit Offset  PCS 40326 – 6890 - Add Gas Type selection for Makeup Gas  6890 - Add ECD parameter for Adjust Offset  PCS 35145 – 6890 - Add more digits of precision to inlet flow parameters to avoid round-off errors in flow  See also: Updated Empower 2 Help (In Instrument Method Editor, press F1 in the Instrument Method editor.)



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Selected GC Defect Fixes in Empower 2 FR 5  PCS 38495 – Allow any GC with 2 inlets/2 detectors to run in dualtower mode (CTC)  PCS 41493 – 6890 PTV inlet does not configure in the Back Position  PCS 41541 – 6890 Method parameters are not downloaded to instrument if components are not enabled  PCS 41659 – 6890 Inlet purge valve won’t hold pressure in Constant Pressure mode  PCS 37887 – 6890 Inst Fail with G1512 without 'next inject delay'  PCS 37151 – 5890 purge valve goes Off during instrument setup  PCS 37272 – 5890 can't do multiple injections on same line  PCS 38297 – cannot monitor baseline with 5890 or 6890 with G1512  PCS 38047, 41889 – 6890A and 6890Plus GC injection volume is incorrect if nanoliter adapter is not installed Company Confidential



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47



Upcoming Releases of GC Related Software Features



Company Confidential



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48



Upcoming ICS Release  Agilent 7890A GC Control ICS v1.1 — Will provide control of the 7890A GC — Phase 1 anticipated release is in 2008



Company Confidential



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49



Agilent 7890A GC ICS  Phase 1 for Empower Software control — Inlets: Split/Splitless (S/SL), Programmable Temperature Vaporization (PTV) and Cool On-Column (COC) — Detectors: Flame Ionization (FID), Thermal Conductivity (TCD) and Electron Capture Detectors (ECD) — Additional: Autosampler, Tray, Valves, Programmed Events and Aux Channels — Capabilities cover 95% of typical user requirements — Target Release – November 2008



 Phase 2 – Targeted for Early 2009 — Additional inlets and detectors — Dual-tower injector capabilities



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50



Part 3 Creating Methods & Running the GC



©2007 Waters Corporation



GC 5890 Series II



•Control with either 7673 or G1512 Controller • Dual Tower capability (With serial card only) • Detector Supported FID,NPD,TCD,ECD • Sampling Rates of 1.25, 2.5, 5, 10, 20 points per second. •Fully Programmable temperatures: limits, ramps, and hold times. • Injector inlet zone temperature setting. Company Confidential



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Agilent 6890 / 6890N GC •6890 supported in both Single and Dual Tower mode. •Sampling Rates of 0.1, 0.2, 0.5, 1, 2, 5, 10, 20, 50, 100, and 200 points per second. •Fully Programmable temperatures: • limits, ramps, and hold times •Detector options: • Unknown (Other detectors) • FID (Flame Ionization) • TCD (Thermal Conductivity) • NPD (Nitrogen Phosphorous) • ECD (Electron Capture) • uECD (Micro Electron Capture) • FPD ( Flame Photometric) Company Confidential



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Agilent 6890 / 6890N GC



•Inlet options: • CIS4 (Gerstel PTV with aux temp) • COC (Cool on column) • COC EPC • PP (Purged packed) • PP EPC • PTV ( Program temp vaporization) • S/SL ( Split/Splitless) • S/SL EPC • Volatiles Interface • Unknown (used for other inlets)



Company Confidential



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Agilent 6890 / 6890N GC



• Enter column Dimensions. • Select gas type: •Nitrogen •Hydrogen •Helium •Argon/Methane •Oxygen •Air •Argon •Unknown • Select Column mode: •Constant Pressure •Constant Flow •Ramped Pressure •Ramped Flow Company Confidential



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General



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Oven



1



2



Activate/deactivate oven



2.



Activate/deactivate Cryo system



3.



When not check you are in Isotherm else you can define a Ramp. Maximum Temperature supported by the column. (Indicated on the column)



4.



Startup temperature



5.



Time to wait when initial temperature is reach before start the run



6.



Intitial Temperature



7.



Runtime in isothem or first ramp time



3



4



5



6



7



Company Confidential



1.



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Oven  When the temperature reach 120°C(6) and is stable for 1 min(5) the GC is ready.  At the injection the GC temp is 120°C(6) for 2min(7),then temp increase by 5°C up to 250°C and stay 1min to 250°C then increase by 10°C to 310°C and stay 10min



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Injector



1



9



2



10



3 4 5 6 7 8



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Injector  Solvent washes (1,2 & 6,7) The injector fills the syringe to eight-tenths of its volume (4 μl with the 5-μl syringe and 8 μl with the 10-μl syringe) from either the solvent A or solvent B position. Then it dispenses the syringe contents into one of the waste bottles. Solvent washes can be set to occur before taking a sample (preinjection solvent wash) or immediately after the injection (postinjection solvent wash). Pumps (4) The injector fills the syringe to eight-tenths of its volume with the next sample and dispenses it back into the sample vial. Pumps occur after the sample washes and immediately before the injection. Pumps serve to eliminate bubbles. If the needle contains solvent from a previous wash, the pumps may add a small amount of solvent that mixes with the sample and can dilute a small volume. Sample washes (3) The injector fills the syringe to eight-tenths of its volume with the next sample and dispenses the contents into one of the waste bottles. Sample washes occur before the injection. When sample is limited, you can use a solvent prewash to wet the syringe before drawing sample.



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Injector Skim Depht available with skim Enable (8 & 10) Use for small quantity of sample . You can define the position of the needle in the vial before you pump the sample This setpoint allows you to move the position of the needle tip up or down to approximate locations from the nominal position of zero (default). Default is the standard position



(9) Available for On column only when this option is checked the needle will inject slowly in the inlet.



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Inlet



Flow



Purge Valve



Split Flow



Purge valve Column



SPLIT Split RATIO = Company Confidential



FLOW



COLUMN



FLOW



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Inlet Split Mode



(1) Gas



Saver is use to reduce the flow using purge valve at the time set up in On time. Flow indicate the purge flow. Note: In this example the purge start at 2 min.



(1) (2)



At 2 min you can consider that all the sample is in the column.



(2) When



EPC Flow,Split Ratio Split flow are linked. The value change in one inteact with Company Confidential



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Inlet SplitLess Mode



(1)



Company Confidential



 When the sample is on the column the purge valve can be open.



© 2007 Waters Corporation



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Column



(1)



(2) When you have EPC the regulation is made base on the mode selected: If Constant Flow, the pressure will be adjust to maintain the flow.



(2)



(1) Column dimensions, the gas selected is important because it regulate the EPC. Company Confidential



If Constant pressure, the Flow will be adjust to maintain the pressure.



Note: do not forget that a gas that is warm/cool expand/compress means the volume/pressure are impacted. © 2007 Waters Corporation



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Detector



(1)



(2)



(1) Ration 10:1 between Oxidizer and Fuel (2) The Make up is used to protect the FID against pollution. A constant makeup reinforces FID stability against pressure or flow change.



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66



Channel (1) Define source for acquisition



(1)



(3) (2)



(2) Remember that a peak is consider resolved with 15pts means adapt the sampling rate base and the minimum peak width. Minimum recommended=20



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Injection Volume



Company Confidential



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68



GC Syringe Size Parameters



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69



GC6850



Currently supported: Inlets: Split/Splitless (S/SL), Purged Packed (PP), Cool On-Column (COC) Detectors: Flame Ionization (FID), Thermal Conductivity (TCD)



Currently not supported: Inlets: Programmed Temperature Vaporization (PTV), Detectors: Flame Photometric (FPD), micro-Electron Capture (u-ECD)



Instrument Description



Serial Number Range



Communication



GC Firmware



6850 Series GC System



=US10243001



LAN



6850 Network GC System 6850 Series II Network GC System



Company Confidential



A.05.04 A.05.03



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Headspace 7694



• Three tabs to define the parameters.



Company Confidential



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Headspace 7694



System configuration



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Instrument Parameters



•Think about the headspace:



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73



Time for each operation



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GC6850



Company Confidential



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75



Part 4 Common Problems & Errors



©2007 Waters Corporation



Agenda: Common Problems  Instrument communication issues — Cannot see instrument in Acquisition Node properties — Cannot get instrument status “OK? = Yes”



 Instrument control problems — GC will not inject (“Waiting to Inject”) or stops running — Wrong injection volume



 Common errors and messages — Instrument failures errors — Other errors and messages



 Interpreting GC signal — Peak height — Signal units Company Confidential



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Instrument Communication



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Instrument Status is not “OK? =Yes”  Incorrect or improperly installed Equinox driver version — COM 3 = Port 1 — Supported drivers: 5.41.00 or 5.30.0.5



 Loose, incorrect or faulty cabling  Hardware incompatibility or failure — Supported model and firmware — GC or headspace works in standalone mode?



 Serial port selection in Acquisition Node properties — Dropdown selection for the correct port; COM 3 = Port 1



 Ethernet instrument configuration (for 6850 II GC only) — Startup sequence — Dropdown selection for A6850 in IP address window — MAC address may need to be updated



 GC option or ICS installation (for 6850 GC or headspace) — Installed options are shown in Verify Files output, Windows Add / Remove Programs applet, etc.



 Too many systems online — Check system licenses against number of online systems Company Confidential



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Instrument Control



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GC Will Not Inject  GC is not ready — Is the red “Not Ready” light on GC front panel on? — Use “Status” button to identify not ready modules



 Auto Prep Run is not enabled — Is the orange Prep Run light flashing?



 Loose, incorrect or faulty cabling — Is GC ALS cable plugged into the correct port (front or back)? — Remote cable from the external injector connected?



 Hardware incompatibility or failure — Unsupported system configuration (e.g., GC-HS control via LAC/E) — Unsupported ALS model or firmware — Does the system work in standalone mode?



 Software incompatibility — Known GC control issues fixed or documented in CDS service pack — For 3rd party instrument control software (OIP), contact vendor Company Confidential



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GC Injects Wrong Volume  Wrong GC Syringe Size setting — Is the correct syringe size selected? — Select ‘Use parameters to check injection volumes’ checkbox — If nanoliter option is physically installed, then it must be selected — Nanoliter option setting grayed out in Empower 2 GC Syringe Info



 Hardware incompatibility — Presence of S/SL inlets in 6890plus GC back position may limit splitless injection volumes to 10 – 20 % of syringe volume



 Software incompatibility — For 3rd party instrument control software (OIP), contact vendor



 Sample Set Method injection volume is outside the allowed range



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Common Errors and Messages



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Benign “Run Log” Messages Examples of “Not Ready” Run Log messages in the Empower message center that can be ignored  HP6890 address 3, Run Log, .... — Code = 542, Not ready: B inlet temp 250 at runtime 5.51 — Code = 544, Not ready: Back det temp 250 at runtime 5.51 — Code = 549, Not ready: B inl pres 0.3 psi at runtime 0.20 — Code = 550, Not ready: B inlet flow 15.0 at runtime 5.51 — Code = 551, Not ready: F det H2 flow 30.0 at runtime 7.10 — Code = 553, Not ready: F det makeup 0.3 at runtime 26.96 — Code = 568, Not ready: Front det ignite at runtime 6.75 — Code = 598, Not ready: Oven temp 173 at runtime 0.00 — Code = 599, Not ready: Oven temp 120 at runtime 2.89



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Instrument Failure errors – 1 of 3  6890@X Setup Failed — Ensure instrument method parameters match physical modules — Check that instrument status is “OK?=yes” — Ensure that instrument hardware working properly



 HP6890 at address:X, Inject Error – 0  HP6890 at address:X, Inject Error – 54  HP6890 at address:X, Inject Error – 122  HP6890 at address:X, Inject Error – 123  HP6890 at address:X, Inject Error – 145 — Check the instrument method General tab — Ensure that GC firmware is compatible with ALS model — Ensure that ALS hardware is working properly Company Confidential



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85



Instrument Failure errors – 2 of 3  HP6890 at address:X, Setup Error – Oven — Ensure that column dimensions and gas type are correct — Check the column configuration in the GC front panel settings



 HP6890 at address:X, Setup Error - Front inlet not enabled — Check the instrument method General tab and Inlet tab



 HP6890 at address:X, Setup Error - Column 2 — Check the mode setting in the Column tabs in Empower Instrument Method Editor



 HP6890 at address:X, Setup Error - Back Detector — Check the column configuration in the GC front panel settings — Check the instrument method General tab and Detector tab Company Confidential



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Instrument Failure errors – 3 of 3  HP6890 at address:X, Setup Error - Configuration Mismatch — Check the column configuration in the GC front panel settings — Ensure instrument method parameters match physical modules — Try recreating the instrument method for the chrom system



 HP6890 at address:X, Setup Error - Communication Failure — Reboot the acquisition node — Re-scan the Instrument after deleting the chrom system



 HP7673 at address:X, Inject error - RKEN NO ERRORS — (PCS # 37272) Cannot make multiple injections on a given sample set line with 5890 under Empower 2 control



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87



Other Errors and Messages  HTML Script errors — PCS 39599 for Headspace under Empower 2 control o Workaround - install ZQ ICS and IIS — PCS 33573 for 6850 under Empower control o Related to Headspace Control Option 1.10; fixed in HCO v2.0 o Only occurs first time an instrument method is opened or closed



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88



Interpreting GC Signal



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Instrument Status is not “OK? =Yes”  Digital (pA) vs. Analog (mV) GC signal acquisition — See TN0000522 — Empower does not convert GC data from µV to pA, or vice versa.  (PCS 37867) Peaks table Empower always displays units: "µV" for Height and "µV*sec" for Area. — Display issue only; does not affect the Height and Area values  Data Sensitivity setting affects signal display — Use default setting (medium) for most methods



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Data Sensitivity :LOW



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Data Sensitivity: MEDIUM



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Data Sensitivity: High



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Part 5 Qualification: GC PQ



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GC PQ



 Goal: Perform a successful performance qualification on a GC system. The metric used to measure success is %RSD of retention times.  Requirements for PQ —Qualified Empower 2 or Empower system —Agilent 6890A/plus/N or 6850 series GC with FID —PN 700001892 PQ Solution (Caffeine in Methylene Chloride) —PN 700000167 - PQ Column (Supelco SPB-1, 15m x 0.53µm x 0.05 µm) —PN 71550025001 – 6890 & 6850w/Emp GCPQ Disk and Document Set



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Movie of Basic Gas Chromatography Separation



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Restrictions of GC PQ



 PQ can only be used qualify an Agilent 6890 or 6850 GC with the following configurations —Split/Splitless/FID —Purged packed/FID



 No qualification is available for Empower headspace control  If the PQ needs to be done for two inlets and two detectors, it will require a second document set  PQ has to be performed using traditional integration only (no ApexTrack)  PQ was tested with helium as the carrier gas; it can be done with nitrogen  The retention time of Caffiene peak will vary depending upon the exact system configuration and performance – this is expected



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Part 6 Conclusion & Final Review (Discussion)



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Part 7 Optional: How to find key information using GSS tools (Discussion)



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