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Peak Performer 1 FID User Manual

1. APPOCANCN Peak Laboratories LLC 402 779 4680 fiv 408 776 5184 fax Layout Rack Mounting ront View Page 9 Figure 2 Rack Mount Front View with Dimensions Peak Performer 1 Users Manual RF ISIONS AUX 1 SAMPLES SAMPLE 1 j CARRIER IN QUT IN 4 T i 4 i i Pi ie ees i of FIDAR SAMPLE2 ee ae ae ea N 4 i pogo FIC H2 A i i Ea i Voy s 1 i pA i H y K f i i l oes 2 50 I no pope g yoy 4 f 1 yA z i l I 1 00 TYP A Si i r lt a at tre 05 0 75 1 25 a COM 1 A i 10 i i FID DRAIN 5 J fe a COM 2 _ Q 6 fo fe Q LPT 1 AC POWER b atsa zai Peak Laboratories LLC man Matman Deso 408 779 4630 v 408 776 5184 fax Layout PROPRIETARY AND CONFIDENTIAL Rack Mount Ter NODRMIAT DA DUWA MEJ mee ee Rear View ede ST owe so A ADD DAT O a a eat Tw A m E J SpA RFYISIONS Ball Bearing Slide Accuride Model 2907 26 or equivalent we 26 inches long atsa zai Peak Laboratories LLC wann Hartman aes 408 779 4680 fv 403 776 5184 fax Layout Rack Mounting Top View ca ST owe so A ATE DATOS SONG Ra E eaa a e ENN t Figure 4 Rack Mount Top View with Dimensions Page 10 Peak Performer 1 Users Ma
2. oe l n u Page 88 Peak Performer 1 Users Manual 8 4 1 Restriction of Water Flow Out of the FID Drain Line Cause Any restriction or reduction in size lt inside diameter or sagging portion of the FID Drain line can create the opportunity for water bubbles to form with the FID Drain Line These bubbles can create momentary back pressure within the entire FID as they are forced down the drain line to the exit point The induced pressure variations will create random momentary spikes on the FID chromatogram Corrective Actions a Examine the entire FID Drain Line and verify that no reduction in internal diameter occur along it s entire length b Examine the FID Drain Line over it s entire length and verify that no horizontal or Sagging sections where bubbles can form exists c Verfiy that the exit of the FID Drain Line is not submerged 8 4 2 Moisture Trapped Within the FID Tower Cause The flame within the FID Tower is ignited prematurely at FID Flame lt 90 C or power was lost and the FID Tower temperature dropped below 100 C while the flame was still lit Under these circumstances condensed moisture can become trapped within the FID Tower Trapped moisture can compromise the electrical insulators inside the FID Tower and create false signal readings Corrective Action a Reduce only the FID H2 pressure to zero to eliminate the FID Flame this eliminates the source of moisture within the FID T
3. Figure 54 Peak Shifting as a Result of Improper Vent Needle Valve Flow Comparison of retention times for un vented versus vented chromatograms will reveal improper adjustment of the vent flow control needle valve Careful adjustment of the vent needle valve will enable the operator to minimize peak retention drift and create a consistent chromatogram 7 5 Effects of Temperature and Flow on Analytical Columns The normal chromatogram can be affected by changes in column flow and temperature Be aware that changes of operating parameters from final test conditions can require parametric adjustments i e peak detection parameters response factors valve timing within the analyzer Page 69 Peak Performer 1 Users Manual Name Conc Area R Time R Factor A Type H2 420 3 1341021 48 8 3191 V CO 347 5 4616126 106 8 13283 V 16 5 Uni 1S 81 MS13X A K Column Temperature 105 C Carrier Flow 20 5 mi min N2 orser e arren 428 SPAN nn Rane Pe b gt b Peak Time L Oitset Critect Pask Haight l Fem A H B nal _ Peak Cons Resp Fo amp Volsige 41m t aysa Type pi j Figure 55 Standard chromatogram The normal PP1 chromatogram Figure 55 is affected by changes in column temperature as illustrated in comparison with the chromatogram of Figure 56 In the circumstance of column temperature change an increase of 30C has shifted the late eluting peak carbon monoxide forward Early eluting peaks such as h
4. 37 The analyzer may display a red light after this action 38 If the analyzer displays a red light on the front panel the parameters must be accepted and saved on board the analyzer before proceeding any further a Press PAGE touchpad until MAIN SCREEN appears has SN and temperature zone controls Page 102 Peak Performer 1 Users Manual f Press the DOWN arrow until you reach the Parameter Change Update Needed line g Press the ACCEPT touchpad button then the SAVE touchpad button permanently save the temperature parameters in analyzer memory 39 Repeat steps 33 through 38 for the other 3 event programs by selecting the other radio buttons under the heading File entering the appropriate event program parameters and then forcing the PeakHost to send the event program to the analyzer 40 Close the Event Editor window 41 Close the PeakHost program The analyzer should be fully updated and ready for use at this time Be sure to make record of any new parameters that were installed in the PP1 analyzer Please consult the factory if a power outage occurs during this function Page 103 Peak Performer 1 Users Manual Figure 83 Heater Resistance for 200 240 VAC AC Service Page 104 Peak Performer 1 Users Manual 9 9 Main DC Power Supply Replacement Main DC Power Supply Replacement Purpose Replace upgrade Phihong PSA4531 DC Supply with Power One MAP40 300 DC Power Supp
5. The chromatographic parameters for the FID O2 analyzers are adjusted to minimize this reactivity the 93 HayeSep D columns used for O2 analysis are unique undergoing an extensive set of proprietary processes for stabilizing the material for O2 service Do not use HayeSep D columns intended for Inert gas sampling in an FID O2 PP1 the detection limit of the analyzer will be severely compromised Additionally the analytical cycle time for the FID O2 analysis is longer than normal The column temperature for FID O2 analyzers is set at 45C to retard the carbon reactions and this creates a longer chromatographic cycle Page 81 Peak Performer 1 Users Manual FID PP1 Stabilization to O2 Samples 600000 O2 Upset Unvented CH4 Peak 500000 At the Start of O2 Sampling 400000 After 0 8 Hours of O2 Sampling After 16 5 Hours of O2 Sampling 300000 After 19 Hours of O2 Sampling Detector Signal Vout 200000 CO2 Peak 100000 0 50 100 150 200 250 300 Time seconds Figure 69 A Sequence of O2 Sample Chromatograms Showing Improvements With Additional Injections Figure 69 overlays several O2 chromatograms over a period of 19 hours The overall chromatogram undergoes a significant shift as more O2 samples are taken Decreasing magnitude of the O2 upset Improved baseline resolution at the CH4 peak leading edge Improved baseline stability at the CH4 peak trailing edge Imp
6. gt CHO H O Depending upon operating parameters this reaction releases electrons until the end reaction products are reached These electrons are collected and the resulting current measurement is used for quantification The net result is in simplest terms that electrons are released in direct proportion to the number of carbon atoms present C3Hg O Heat gt 3CHO H20 3e Therefore instrument response is directly proportional to the number of carbon atoms present in the compound being measured Unfortunately the ionization efficiency of the flame is relatively low and roughly 1 in 10 000 hydrocarbon molecules follows the electron liberating reaction path described The vast majority of combustion reactions follow the direct net product reaction 2CH 40 gt 2CQO 4H O Heat This reaction sequence is applicable to any hydrocarbon It can be seen that the FID is a mass flow type of detector the number of ions created is independent of carrier flow therefore detector response is the same regardless of carrier flow rate Mes COLLECTOR PROBE Ct A aS n A FLAME SENSOR Paea L Hj at Ale i a YT ED Z Sii Bide FLAME TI P BIAS IG
7. END Ends the Event Program and prepares the analyzer for the next run HEAT ON Not currently in use HEAT OFF Not currently in use Page 39 Peak Performer 1 Users Manual 4 5 2 Event Editor Screen Button Function ii Moves the cursor upwards iS Moves the cursor downwards Load 1 Allows the user to load the event program 1 Toggle Allows the user to scroll through event program choices Page Advances the user to the next screen 4 6 Stream Selector Program Editor Screen Peak offers a dual sample stream option for most analyzers The selection and timing of sample streams can be pre programmed on this screen NOTE This screen will only appear when the STREAM method of analysis is selected on the RUN screen stream Selector Program Editor Figure 25 Stream Selector Sequence Screen 4 6 1 Stream Selector Commands The selection of sample streams and appropriate Event Program can be run in a pre programmed sequence Stream Establishes which sample stream to be utilized for analysis Event Prog Establishes which Event Program to be utilized for the sample stream Cycles Establishes the number of repeat analysis Page 40 Peak Performer 1 Users Manual 4 6 2 Stream Selector Program Editor Screen Button Function ie Moves the cursor upwards ie Moves the cursor downwards Edit Allows the user to chose event program and of repetitions Page Advances the user to the nex
8. Zone 3 P Value Zone 3 Value Zone 3 Limit Analyzer Serial MCPU Version Detector Version RCP y n FID y n Valve 1 Cycles Valve 2 Cycles Oper Hours Rotary y n Diaphragm y n Stream Select y n FID Flame Temperature checked circle yes checked circle yes checked circle yes checked circle yes checked box yes Force the PeakHost program to obtain fresh analyzer peak database information under the PeakHost program main screen toolbar select Analysis Database the peak database window will pop up Under the Peak Analysis Database main screen toolbar select File then Receive From Analyzer to force an update of the information Page 98 Peak Performer 1 Users Manual 9 Save the peak analysis database parameters by using the print function in the Peak Analysis Database window under the toolbar select File then Print If no printer is available manually write the following all four columns of the peak analysis database parameters Peak Name Peak Center RT Window Peak Height Left Width Right Width Convo Filter Response Factor Beer s Law Factor 10 Close the Peak Analysis Database window 11 Force the PeakHost program to obtain fresh Event program information under the PeakHost program main screen toolbar select Event the event editor window will pop up Under the Event Editor main screen toolbar select File then Receiv
9. Air Generator Gas Type TO No 21 O2 Maximum Flowrate lt 500 cc min THC Concentration lt 10 ppm CO Concentration lt 10 ppm CO Concentration lt 1000 ppm H2 H2O Concentration lt 100 ppm Page 16 Peak Performer 1 Users Manual Synthetic air sources suitable for use as FID Air include Zero and Breathing Quality grades CAUTION Compressed room air is not recommended unless refined by regenerative drying and combustion purification 1 Connect the Zero Air gas supply to the bulkhead and set the source regulator to approximately 20 psig 2 There are no internal regulators in the standard FID PP1 all gas pressures are controlled by external regulators customer supplied 2 5 4 Actuator Gas Supply The actuator supply is attached at the rear panel of the instrument Attach the air or inert gas actuator supply to ACTUATOR IN port on the rear panel Preset the source to 60 80 psig Nominal Clean Dry Air lt 10 ppm 2 5 5 Sample Gas Supply Sample lines are normally attached to the rear panel of the instrument Attach sample or span gas lines to the SAMPLE IN port on the rear panel The SAMPLE OUT port must be unrestricted Sample gas must be supplied to the analyzer at low pressure 0 3 to 1 0 psig and moderate flow 30 to 120 ml min The analyzer does not have any sample gas pressure flow regulation equipment Please contact the factory for sample handling instruct
10. BYPASS OUT port is flowing approximately 25 35 sccm Carrier flow within the analyzer is split with a portion of the flow passing through a gas sampling valve the other portion passes through a restrictor tube terminating at the location of the BYPASS OUT port Under normal operating conditions this port is Capped During column reconditioning the plug may be removed and the SAMPLE IN switched to the bypass flow In this manner column reconditioning may be performed without requiring a shutdown of the sample gas flow avoiding the lengthy re equilibration period Page 14 Peak Performer 1 Users Manual H2 venting H2 shut off valving and H2 supply safety equipment must be supplied by customer The analyzer provides a NORMALLY OPEN switch contact for H2 safety purposes The analyzer will close the switch contact CLOSED position temporarily for 120 seconds any time the IGNITE command in invoked If the FID Flame temperature is greater than the setpoint value the switch contact will remain closed Any time the FID Flame temperature is less than the setpoint value the switch contact will revert to the NORMALLY OPEN position automatically see Section 4 7 3 Combustion fuel must be supplied to the Flame lonization Detector The PP1 FID H2 gas connection utilizes a 1 16 female VICI bulkhead labeled FID H2 on the rear panel 1 Connect the Hydrogen gas supply to the bulkhead and set the source regulator to
11. approximately 25 psig 2 There are no internal regulators in the standard FID PP1 all gas pressures are controlled by external regulators customer supplied FID Hydrogen Gas Specifications High Pressure Cylinder or Hydrogen Generator Gas Type Hydrogen CAUTION High moisture content in the FID H2 gas supply has been shown to irreversibly damage the methanizer s ruthenium catalyst Page 15 Peak Performer 1 Users Manual 2 5 2 1 FID H2 Gas Generators Peak recommends only the use of Palladium Transfer Tube or Regenerative Drying Hydrogen Generators Hydrogen produced by electrolytic decomposition of water is extremely humid at nearly 100 relative humidity H2 generators using only single stage gas H2 dryers molecular sieves will saturate with moisture within a week or two of normal use and therefore require frequent manual exchange and regeneration to maintain acceptable H2 gas quality 2 5 2 2 FID H2 Gas Cylinders Cylinder sources suitable for use as FID H2 include UHP and Zero Quality grades Nominal UHP Grade lt 10 ppb THC Fut Hydrogen lt 10 ppm H20 29 psig 2 5 3 FID Zero Air Gas Supply Oxygen bearing gas must be supplied to the Flame lonization Detector for combustion support The PP1 FID Air gas connection utilizes a 1 16 female VICI bulkhead labeled FID AIR on the rear panel FID Zero Air Gas Specifications High Pressure Cylinder or Zero
12. o B gt Q 60 0 60 a 5 40 0 40 a 20 0 2 0 0 0 0 0 15 0 20 0 25 0 30 0 35 0 40 0 45 0 50 0 55 0 60 0 Total H2 Flow to Flame Tip cc min Figure 73 FID Response to Varying H2 Flow Note that the analyzer is relatively insensitive to H2 flow rate changes between 33 and 43 sccm Detector signal to noise is roughly maximized in the same regime Page 87 Peak Performer 1 Users Manual FID Response With Varying Air Flow H2 40sccm amp Carrier 55 sccm 14 0 12 0 10 0 8 0 6 0 CO2 a Signal to Noise 140 0 120 0 100 0 80 0 60 0 40 0 20 0 0 0 Relative Area Response Signal to Noise Ratio 2 0 0 0 100 125 150 175 200 225 250 275 300 325 350 375 400 Total FID Air Flow cc min Figure 74 FID Response to Varying Air Flow Note that the analyzer is relatively insensitive to Air flow rate above 200 sccm and detector signal to noise reaches a stable value above 200 sccm Peak Labs recommends that the analyzer be operated in the flow regions that yield the most stable response and signal to noise characteristics 8 4 Resolving Random Spikes on the FID Baseline There are two primary causes for random baseline spikes appearing on the chromatogram PE Oy Py oP 7 E C E Figure 75 Chromatograms Showing Random Baseline Spikes Due to Moisture
13. options and save the settings in a file on the computer Com Port a 5 3 E Cancel Baud Rate gg00 C 18200 tf 38400 Data Bits Stop Bits 7 eS f 1 2 Figure 31 Viewer Software Communications Setting screen 5 5 COM1 COM2 Port and Cable Wiring The cable connected from the PC to the PP1 should be a straight through wired 9 pin M F cable attached to the PC s COM port and the PP1 s COM port Figure 31 is the minimum cable configuration See Section 6 for details on communications protocols PC MALE PP 1 FEMALE 9 Pin Cable from PC to PP 1 Figure 32 COM Cable Wiring Page 47 Peak Performer 1 Users Manual 5 6 Viewer Software Window The Viewer window shown in Figure 33 shows the main Viewer screen with a RED DOT in the upper right corner This RED DOT signifies that there is a connection problem with the PC and the PP1 Verifying the following can solve this connection problem e Communication Settings e Connection of 9 pin cable between PC and PP1 e RS 232 cable plugged into the PP1 s COM 1 port e PP1 is powered off After the connection problem has found and corrected the RED DOT should be CLICKED to verify if communication between the PC and PP1can be properly established cit Fiewer Yer 3 12 i l Birr X File Start Stop Chrom view Event Info Run Time Stream a Figure 33 Viewer main window showing Communications Error The Viewer window shown in Figure 34
14. this mode the normal detector baseline is calculated very simply Peak start time PkKCen LW Peak end time PkCen RW All other possible aspects of peak start and end time determination are disabled and the normal detector baseline is rigidly established only by the Peak Database parameters PkCen LW RW Figure 63 Baseline as Established in Fixed Mode Peaks quantified using this method are denoted with an F in the last column of the data report 7 6 2 Peak Quantification Forced Baseline Mode The Forced Baseline Mode is enabled when the maximum detector signal value at the calculated peak maximum signal is less than the PkHgt parameter value but is greater than zero Page 76 Peak Performer 1 Users Manual The time associated with the peak maximum signal is always calculated first for Forced Baseline and Variable modes by using the convolution filter to find the maximum detector signal point The time associated with the peak maximum signal must be within the time regime of interest PkCen PkWin for any peak quantification to occur In Forced Baseline Mode the normal detector baseline is calculated based upon the peak maximum signal time value rather than the PkCen value Peak start time Peak end time Peak signal maximum time value LW Peak signal maximum time value RW Peak Maximum LW RW Figure 64 Baseline as Established in Forced Baseline Mode Peaks quantif
15. what the port assignments on your computer are 14 In the Device Manager click on Ports to expand heading so you can see what COM port number your computer gave to the USB to DB9 adapter 15 Note which COM port number is now assigned to the new USB to Serial RS232 Port adapter it s COM4 on most computers 16 Go back to the Viewer window 17 Under File on toolbar select Port Settings 18 Enter COM number assigned to first USB to DB9 adapter probably COM4 check that Baud Rate 38400 Data Bits 8 Stop Bits 1 19 Click OK box to save these settings 20 Communications settings for that USB to DBY adapter will be saved in the folder and will be used automatically every time you launch the Viewer software in that folder 21 Leave the first Viewer window open 22 Insert second USB to DB9 adapter into USB hub your computer should detect the connection and launch the hardware installation program 23 Insert USB to DBY adapter INSTALL CD in CD drive it will launch automatically if autoplay in enabled on your computer 24 Follow installation instructions that come with USB to DB9 adapter I confirm that it is okay to click the Continue anyway box 25 Your computer may prompt to install the USB to DB9 adapter a second time do not cancel it is best to let the computer re install the software again 26 Open the second new folder and select the Viewer exe file in that folder 2 Double click
16. 4 CO NMHC 13 23 67 6 168 4 196 5 342 5 13 32 L 60 8 167 3 196 5 366 1 13 41 68 6 167 6 197 1 368 0 14 06 L 178 6 187 0 207 2 386 2 14 15 L 186 7 188 1 210 5 285 4 14 24 L 191 8 183 1 207 9 339 3 14 41 L 2 0 1 2 10 8 4 4 14 50 L 1 3 0 0 6 8 2 0 14 59 L 1 5 1 6 10 7 0 3 Figure 36 Viewer screen showing concentration data There are ten individual error conditions that can cause the Viewer Line to appear red Detector Communication Error Temperature Zone Out of Range Temperature Zone Disabled Detector Zeroing Target Error Page 50 Peak Performer 1 Users Manual Viamp Low Voltage Out of Range FID Flame Temperature Out of Range Event Program Load Error Stream Selector Program Error System Parameters Corrupted Parameter Change Update Needed 5 6 1 1 Viewer Line Details Window This window is displayed by double clicking on any time stamp on the Viewer window The screen provides detailed analytical information about the run selected Figure 37 shows the data on a Viewer Details window screen Viewer Details 2008 11 13 13 50 Fel ES Print Name co CH4 coz NMHC Peak Time sec 90 9 115 6 713 2 425 8 fo 13 6 29 16 4 3 odode 1511028 423r 4041 Lett Width Sec F B iT mi Right Width sec 12 4 Measured Grea 137910 Response Factor 2246 4740 Wicth Analysis variable Variable Variable Variable au pam a Z p a Cycle Lamp voltage 24 0 mi Beer s Lavy Correct
17. CREEN SCREEN SET UP MAIN O E escxey SCREEN Figure 10 Software Menu Structure 4 1 Set up Screen The Set up screen is multi functional Different command buttons appear at the bottom line of the screen dependent upon the section containing the asterick cursor 1 The upper section 3 lines contains commands related to analyzer set up 2 The middle section 5 lines contains commands related to temperatures zones and detector parameters 3 The lower section is reserved for error messages and non volatile memory updates Page 25 Peak Performer 1 Users Manual 4 1 1 Set up Screen Upper Section wf M t fi a Hizer Column FID Flame FIDO Wet at Figure 11 Main or Setup Screen Upper Section 4 1 1 1 Set up Screen Upper Section Button Functions Ve Moves the cursor upwards ee Moves the cursor downwards Edit Allows the user to change the Date Time or Protocols Page Advances the user to the next screen Page 26 Peak Performer 1 Users Manual 4 1 2 Set up Screen Middle Section Power up The middle section of the Setup screen is concerns temperature zone and detector function HeS HOwW 17 OCOL Uy ewer Methanizer Column FID Flame FID Uont CN i Ja JTT mo iT i aan Ts Figure 12 Screen Commands Upon Power up NOTE The heater zones are not energized automatically upon power up and the detector electronics are not fully initialized unt
18. NITER PROBE iF FID Air a ONY COLUMN EFFLUENT FID H2 Figure 70 Standard FID Section Page 85 Peak Performer 1 Users Manual Normal life of the methanizer is approximately 84 months under continuous use Replace and dispose of properly in accordance with local and federal regulations 8 2 Temperature Effects Within The Methanizer and FID Tower The FID Tower is heated indirectly by the methanizer block to roughly 95 C to minimize moisture condensation It is critical to allow the FID Tower to heat thoroughly before igniting the flame Failure to do so may trap moisture within the FID Tower and compromise the ceramic insulators Between the temperatures of 250 C and 325 C this reaction on the surface of the Ruthenium Oxide catalyst can proceed CO 4H gt CH 2H20 and CO 3H gt CH H O The rate and completion of these reactions is dependent upon temperature and residence time It is critical to note that the catalyst reaction can halted by the presence of moisture in the gas stream particularly if the hydrogen for methanization has high moisture content Above 360 C CO thermally decomposes on the catalyst surface and methanization is not possible The Peak Lab FID methanizer has been optimized for methanization of CO since under normal FID chromatographic applications the CO peak is not chemically distinct Peak Labs recommends the use of the RCP models for the measurement
19. Peak Performer 1 Users Manual Peak Performer 1 FID User Manual LABORATORIES Peak Laboratories LLC www peaklaboratories com 650 691 1267 Version 3 2 11 20 2008 Page 1 Peak Performer 1 Users Manual This manual is a reference guide for the operation of the Peak Performer 1 series of gas analyzers The Peak Performer 1 should only be operated by trained personnel familiar with the safe operating procedures of the analyzer The following cautions should always be considered High voltages are required for proper detector operation and are present when the unit is energized High operating temperatures are required for proper detector and chromatographic operation Hot surfaces may be present when the unit is energized Illustrations and photographs contained herein are for example only Actual configurations may vary depending on specific application and installed options Improper installation operation or service of the analyzer can cause permanent damage to the instrument The analyzer is designed to be operated with all covers installed connected to a properly grounded 3 conductor AC line source gt PPP In event of fire Class A B or C fire extinguishers can be used The Peak Performer 1 must have standard electrical power and applicable gas supply pressures as noted on the test documentation for proper operation Permanent damage and voiding of the warranty may Operators should not attempt t
20. Rate Effects 87 8 4 Resolving Random Spikes on the FID Baaseline 88 8 4 1 Restriction of Water Flow Out of the FID Drain Line 89 8 4 2 Moisture Trapped Within the FID Tower 89 9 0 Analyzer and FID Maintenance and Service Procedures 91 9 1 Peak Performer 1 System Block Diagram 92 9 2 Monitor Regulator Pressures 93 9 3 Verifying Valve Integrity Carrier Blank Zero Gas 94 9 4 Start up Sequence for Replacement Methanizer 95 9 5 Adjusting the Display Contrast 96 9 6 Altering the Analytical Range of the Instrument 97 9 7 Updating the Analyzer Software with Peak Host 98 9 8 Testing the Heater Resistance 104 9 9 Main DC Power Supply Replacement 105 9 10 Adjusting the 5 Volt DC Power Supply 108 9 11 COM 1 Viewer Connections on Multiple Analyzers to a Single Computer Adjusting the 5 Volt DC Power Supply 110 9 12 Discussion About VICI Diaphragm Valves vs Rotary Valves 113 Page 6 Peak Performer 1 Users Manual 1 0 Introduction The Peak Laboratories Peak Performer 1 PP1 gas analyzer is a trace level gas analysis system capable of detecting part per trillion ppt concentrations of reducing gases and hydrocarbon gases in a variety of sample matrices Due to the specific nature of the detection method analysis times are rapid and chromatographic complexity is minimized The result is a simple and reliable system capable of following rapid trends in component concentration in laboratory field and process gas applications The Peak Perfor
21. Therefore it is recommended to use a substantial calibration peak concentration to facilitate easy LW and RW measurements 4 4 2 Analysis Screen Button Function T Moves the cursor upwards fe Moves the cursor downwards Edit Allows the user to enter new peak compound name or analysis parameters Page Advances the user to the next screen Page 38 Peak Performer 1 Users Manual Analysis Averaging When enabled the last four chromatograms are averaged data point by data point to create a composite chromatogram which is then quantified using normal techniques Analysis averaging does not average concentration data values From a cold start it will take approximately 30 minutes to obtain the best averaged results 4 5 Event Program Editor Screen The Event Program Editor screen stores critical information regarding pre programmed instrument actions needed to perform an analysis Event Program Editor Wal al Map ey iI Cr N e ra J CO2 amp NMHC IN 02 C z amp NMHC IN OF 4 Lead Figure 24 Event Editor Screen 4 5 1 Event Program Commands The instrument actions can be pre programmed to create an analysis method or Event Program The analyzer stores up to 4 distinct Event Programs V17 CW Moves V1 to the Inject position V1 CCW Moves V1 to Load position V2 CW Moves V2 to the In line position V2 CCW Moves V2 to the Vent position ZERO Invokes the detector ZERO command
22. Window COM1 COM2 Port and Cable Wiring Viewer Software Window File Menu on the Viewer Taskbar Viewer Line Details Window Start Menu on the Viewer Taskbar Stop Command on the Viewer Taskbar Chrom View Window and Chromatogram Viewer Window Chromatogram Files File Menu on the Chrom Viewer Taskbar Viewer Menu on the Chrom Viewer Taskbar Communication Port Protocols and Data Formats COM1 COM2 Port and Cable Wiring Port 1 Protocol COM 1 Port Settings Viewer Output Format Detector Output Format External Start Command String Detector Signal Data String EZChrom Elite Output Protocol Port 2 Protocol PLC COM 2 Port Settings COM 2 Port Output Format Trend Analog Output Format Setting up a RS485 Network RS232 to RS485 Converters Peak Performer 1 Users Manual 6 5 2 PP1 Port 2 Protocol 61 7 0 Chromatographic Principles 62 7 1 Sample Injection 62 7 2 Carrier Gas Purification 62 7 3 Component Separation 63 7 4 Venting and Flow Balancing 66 7 5 Effects of Temperature and Flow on Analytical Columns 69 7 6 Peak Identification and Quantification 72 7 6 1 Peak Quantification Fixed Mode 76 7 6 2 Peak Quantification Forced Baseline Mode 76 7 6 3 Peak Quantification Variable Mode 77 1 1 Chromatographic Stabilization of the Analyzer When Injecting O2 Samples 81 8 0 Flame lonization Detector FID 84 8 1 Flame lonization Detector Principles 84 8 2 Temperature Effects Within the Methanizer and FID Tower 86 8 3 Detector Flow
23. a direct analog signal from the detector for use with a chart recorder or integrator NOTE The analog outputs are locked if the Port 1 Protocol on the MAIN SCREEN is set to DETECTOR See Section 4 1 1 Analog signals generated from this information appear on the rear panel s green DIN terminal blocks See Figure 19 Manus Set a aS M SS SS SE 5 A mr m m a mpm m LbN a t Hd E E E k Figure 18 Analog Interface Screen 4 2 1 Analog Interface Screen Button Function ie Moves the cursor upwards lig Moves the cursor downwards Page 32 Manset Page Peak Performer 1 Users Manual Allows the user to select the full scale concentration range associated with the maximum 1 25 VDC signal for each compound The ranges are as follows 0 gt 125 ppb 0 gt 1250 ppb 0 gt 5500 ppb 0 gt 12500 ppb 0 gt 125000 ppb e g 0 1250 ppb readings in the analyzer 0 1 25 VDC output scale At the end of each run the analog signal is updated and holds until the next run is completed As an accessory Peak can provide standard commercial VDC gt mA converters as needed If RECORDER appears in the 4 compound location the RANGE button for the recorder function is not tied to any specific concentration range In lieu of a specific concentration range the RANGE button for the recorder function toggles through 4 choices of raw s
24. ad of the heated getter material for complete removed of methane hydrocarbon CH4 a common contaminant in commercial nitrogen sources Hydrogen Carbon Monoxide Carbon Dioxide Hydrocarbons and Moisture carrier gas impurities are reduced to less than 10 ppt by this type of purifier Page 62 Peak Performer 1 Users Manual Gas Purifier Specifications Heated Reactive Metal Getter Maximum Flowrate gt 300 cc min lt 5 L min Gases Purified N2 Ar He alternative THC Concentration outlet lt 10 ppt CO CO Concentration outlet hee H2 H2O Concentration outlet lt LOPPI Expected Life Consult Manufacturer 7 3 Component Separation Component separation is normally performed by isothermal packed analytical columns Column materials vary by application and are noted in the Test report documentation Contact Peak Laboratories for additional details specific to your application In general applications samples are introduced into the instrument through the SAMPLE IN connection A controlled portion of the sample gas is injected via the pneumatically actuated gas sampling valve into the carrier flow path The injected sample passes onto the head of the analytical column s inside the isothermal column oven and moves through the analytical column where the separation of the components begins The analytes of interest are further refined and methanized on the optional Ruthenium catalyst and continue on to the detector for quan
25. after the chromatogram data is loaded the display can be adjusted by the Offset Attenuation and Span scroll bars P Chrom iewer 2006 11 13 1341 chm i Z iol xi File viewer Analysis DB Open 2 ATTEH 32 SPAH FET Saves 4 gt 4 w Baseline Figure 39 Chromatogram Viewer Window NOTE Viewer window scaling does not match the analyzer s display scaling A higher degree of resolution is available in the Viewer window For instance Viewer ATTN 8 approximately is equivalent to analyzer display ATTN 1 Page 53 Peak Performer 1 Users Manual 5 6 4 1 Chromatogram Files Chromatograms are archived on the host computer as text files suffixed chm The text files can be imported into most common laboratory analysis spreadsheet and word processor programs as needed Data points in the chromatogram file are time sequenced at 0 2 seconds per data point The filename of the chromatogram file is generated by time of day on the host computer and the file is stored in a folder that corresponds to the date of collection A corresponding Viewer data file is created and or updated at the time the chromatogram file is created As an example the fourth chromatogram shown in Figure 36 would be archived on the host computer as follows Main directory C Viewer Sub directory 2003 12 22 YYYY MM DD of archive creation Viewer filename 2003 12 22 cSV Filename 1335 chm 5 6 4 2 File Menu on the Chrom Viewer Tas
26. assing through the detector Since the analyzer is monitoring the detector electronic signal over time the added signal is measured in real units such as volt sec By virtue of a conversion factor called the Response Factor the volt sec signal can be directly related to concentration units Page 72 Peak Performer 1 Users Manual PEAK START PEAK END Figure 59 Illustration of Measurement of Chromatographic Peak Area Note The PP1 analyzer supports only area based concentration determinations Determinations based upon peak height as not currently available The first task in quantifying peaks is establishment of the normal stable detector signal baseline This is accomplished by determining the signal departure and return points for the peak event The parameters used when defining detector baseline signal and peaks are Analysis Databs Figure 60 Typical PP1 Peak Analysis Database Page 73 Peak Performer 1 Users Manual PkWin Figure 61 Illustration of Chromatographic Peak Parameters Name The peak identification tag expressed as 5 alphanumeric characters A Z 0 9 PkCen The normally expected peak retention time in seconds used for assigning the appropriate Name LW The typical time span measured from the start of the peak s baseline rise to the peak apex PkCen in seconds Minimum value is 3 maximum is 35 RW The typical time span measured from the
27. cles Valve 1 Add Valve 2 0 Vake 1 Valve 2 Rotary Operating Hours SEND Pi an Diaphragm 0 365 Pilot Valve Interface FID Flame Interface Pwi so PW3 Pw5 J 0 Pvz Pw4f PW l Flame Out Flame Set Pt 0 Set Point 0 P Value 0 Value i Limit Figure 79 Peak Host Main Window Normal Peak Performer Yer 1 71 E loj x File Event Chrom View Analysis DB Viewer Touch Screen Upload Temperatures Detector Control Zoned Zone Zone3 _ Ain DA Value 265 8 105 5 0 0 zuu Wee VSig mV 0644 0 RCP G Bias Off FD O Ignite On Gas Sampling Interface System ID s Analyzer Serial 14 MEPU version 171 Detector Version 110 Valve Cycles Valve 1 594 Valve 2 0 Vake 1 Valve 2 Rotary Operating Hours SEND fl R Diaphragm Q 365 Pressure Transducer Pilot Valve Interface FID Flame Interface Carrier Pressure 000 Set Point 0 P Value O value 0 Limit Pva Py3 Pys 0 Pv P4 Pep Flame Out Flame Set Pt Figure 80 Peak Host Main Window with Upload Command Visible 17 Double click the Upload button The standard Windows Open window will pop up Page 100 Peak Performer 1 Users Manual Look in i Peak Host 1 77 My Recent Documents Desktop O M
28. d The final value is represented by point 5 when the change in peak area became less than 0 5 Page 78 Peak Performer 1 Users Manual The trial evaluation of peak area continues for the peak ending point again using a fixed percentage of the LW and RW values as intial baseline points again illustrated as the hypothetical baseline between points L and R in Figure 67 The first hypothetical calculation of the peak end time is labeled 1 in Figure 67 After calculating the hypothetical peak area the mathematics package makes another peak area calculation using a slightly later time value The peak areas of the two calculations are compared and if the peak area increases by more than 0 5 the mathematics package repeats the process The net effect is illustrated in Figure 67 where multiple hypothetical peak start points were evaluated The final value is represented by point 6 when the change in peak area became less than 0 5 Peak Maximum ao u o Se N PEAK START PEAK END Figure 67 Progression of Peak End Time Calculation Using the newly established peak start and end times the mathematics package determines the normal detector baseline as illustrated in Figure 68 The signal contribution due to the peak passing through the detector can then be quantified by area calculation using time slices and signal differentials above the newly established baseline Page 79 P
29. ded to navigate to the RUN screen If multiple sample runs are desired press the SINGLE command to toggle to CYCLE repetitive analysis mode Press the RUN key to initiate analysis the P1 event program will be loaded automatically and executed Allow the analyzer to fully execute the event program Current concentration data will be displayed as an overlay on the RUN screen as peaks are identified and quantified 3 6 Calibration The Peak Performer 1 chromatograph determines concentration peak area to quantify the amount of contaminants in the sample gas The direct instrument response in units of uV sec is reported simultaneously as an overlay on the RUN CHROMATOGRAM SCREEN and in the AREA column on the CALIBRATION DATABASE SCREEN As the concentration peak area is determined the analyzer applies the pre programmed response factor as an inverse proportional factor to generate the reported concentration value PEAK CONCENTRATION PEAK AREA RESPONSE RESPONSE FACTOR 3 6 1 Establishing New Instrument Response Factors Connect a known calibration standard gas span gas to the analyzer at the SAMPLE IN port on the front panel If soan gas connection is made at the rear panel SAMPLE IN port ensure that the front jumper is connected between SAMPLE OUT and SAMPLE IN on the front panel Page 22 Peak Performer 1 Users Manual Verify that sample is flowing freely through loop exit flow from the SAMPLE OUT sh
30. e 112 Peak Performer 1 Users Manual 9 12 Discussion About VICI Diaphragm Valves vs Rotary Valves Port 1 Port 2 Port 3 Port 4 D S g lt S a Figure 90 Diaphragm Valve Cross Section CCW Position CCW Position Not Pressurized Gas flows from Port 1 to Port 2 Port 3 to Port 4 etc The diaphragm and pistons are moved into position by the return spring and carrier and sample gas pressure Port 1 Port 2 Port 3 Port 4 Figure 91 Diaphragm Valve Cross Section CCW Position CW position Pressurized Gas flows from Port 2 to Port 3 etc The diaphragm and pistons are moved into position by the actuation pressure Page 113 Peak Performer 1 Users Manual Disadvantages e Higher back pressure through this style of valve because of the requirement of the internal gas stream to force the gas path open e Possible incomplete sweep of the gas flow path due to residual volume between the gas port and piston diaphragm pinch point e Larger circumferential seal length e Low sealing force to atmospheric intrusion single screw generates all sealing force for interior and exterior flat diaphragm seal faces e Increased internal cross port leakage e More expensive Advantages e Fewer moving parts e Smaller size e Single pilot valve required Page 114
31. e EzChrom Elite output protocol is used when the PP1 is interfacing with EzChrom Elite please consult the EZChrom manual for details on setup of the host computer 6 3 Port 2 Protocol PLC The COM2 port is a dedicated RS232 output intended for use with PLCs programmable logic controller There are two modes of operation AUTO and POLL Proper selection of protocol is determined by the application interfaced on the host computer 6 3 1 COM 2 Port Settings The RS 232 settings for COM 2 port are 9600 baud rate 8 bit data 1 stop bit and no parity Page 58 Peak Performer 1 Users Manual Two modes of transmission are available AUTO or POLL e In AUTO mode the current PLC data string is transmitted at the end of analytical cycle e In POLL mode the PP1 will transmit the latest PLC data string only when prompted by the host computer This mode is recommended for use in a RS 485 network Selecting the POLL mode on the MAIN SCREEN configures the PP1 to wait for a request before transmitting The master controller of the RS 485 network must first request data from the PP1 in order for receive the COM2 port output data The protocol to request data from the PP1 consists of 1 A start of transmission character 2 Followed by the unit serial number 3 An end of transmission character or STX character 02 hex SSS ETX character 03 hex The requesting command format follows lt STX gt SSS lt ETX gt where SSS ser
32. e From Analyzer to force retrieval of the P1 event program 12 Save the event program information by using the print function in the Event Editor window under the toolbar select File then Print If no printer is available manually write down the P1 event program 13 Repeat steps 11 and 12 for the other 3 event programs by selecting the other radio buttons under the heading File 14 Close the Event Editor window The analyzer is now documented and ready for software update and or parameter re initialization 15 Place the new motherboard software file typical name file name is MCPU vX XX hex in the same directory on the host computer as the Viewer and Peak host programs 16 Under the PeakHost program main screen toolbar note that the UPLOAD command on the upper toolbar is not fully visible or active Double mouse click on the number box located to the right of the words MCPU Version and the Upload button on the main toolbar will become fully visible and active Page 99 Peak Performer 1 Users Manual Peak Performer Yer 1 71 _ Ioj x File Event Chrom View 4nalyvsis DB Viewer Touch Screen Upload Temperatures Detector Control Zone l Zone Zone3 Ain D A Value 265 6 105 5 0 0 saki Wer VSig mW ia 20666 0 RCP Bias Off FID Ignite On Gas Sampling Interface System ID s Analyzer Serial 14 MEPU version 171 Detector wersion 110 Valve Cy
33. eak Performer 1 Users Manual E J Fd x D a PEAK START PEAK END Figure 68 Peak Area Calculation The formula for peak area calculation can be expressed as Peak Area 1 2 x Hgt Hgt2 x t4 2 x Hgt2 Hgts x t2 12 x Hgt Hgt x tz where Hgt the signal differential between the instantaneous baseline level and the peak signal value t the time difference between data points Using a constant value for tx the peak area calculation simplifies to Peak Area t x Hgt H gt Hgt Hgt Peaks quantified using the Variable method are denoted with a V in the last column of the data report Page 80 Peak Performer 1 Users Manual 7 7 Chromatographic Stabilization of the Analyzer When Injecting O2 Samples O2 samples present particular challenges for the FID PP1 analyzer due to the extreme reactivity of 100 O2 with any possible carbon source even at relatively low temperatures via these basic reactions 2C O gt 2CO C O gt CO Potential carbon sources include residual carbon within stainless steel tubing and valve bodies polymeric valve components and column packing materials CO and CO produced from these sources can be detected in the FID and create a wide variety of symptoms Unstable detector baseline False positive peaks when measuring pure O samples Difficult small peak quantification Transient peaks in the chromatogram
34. eight less than or equal to PkHgt will be quantified using the ForceB mode JJ Fit The convolution filter value expressing the overall peak shape FIt 2 is recommended for sharp narrow peaks such as H2 and FIt 8 is recommended for broad peaks such as CO As a general rule LW and RW values do not change significantly with peak concentration so calibration peak size is not critical in determining proper LW and RW values Page 37 Peak Performer 1 Users Manual H2 Peak Left and Right Widths as a Function of Concentration ALeft Width Right Width Left Width seconds Right Width seconds 1 10 100 1000 10000 Blended Concentration ppb CO Peak Left and Right Widths asa Function of Concentration ALeft Width Right Width 10 0 1 10 100 1000 10000 Blended Concentr ation ppb Figure 23 Left and Right Peak Width as a Function of Concentration Total peak width LW RW is primarily a function of sample loop unloading Larger sample loops require a long time period to fully inject The relative values of LW and RW are dictated by the skew factor of the peak Peaks need about 25 30 data points minimum to be well measured at 5 data points per second this means total peak width should be greater than 6 seconds
35. emotely starts a RUN The PP1 system processes the external start command only if the analyzer is in IDLE mode Not running a sample Upon receipt of the external start command the PP performs the following functions Sets system run mode to SINGLE RUN mode Loads event program P1 Starts a Single Run Sends Detector Signal Data stream i e Vout reading to the COM71 port At the end of the run the PP1 sends an End Of Data string to identify the end of the data stream e Sets analyzer to IDLE mode and waits for the next start command 6 2 3 1 External Start Command String The External Start Command string format transmitted by host computer must consist of three ASCII characters Below are four forms of the same command Form 1 Start Of Text S End Of Text Form 2 STX S EXT Page 57 Peak Performer 1 Users Manual Form 3 ABS 4C Form 4 02 53 03 6 2 3 2 Detector Signal Data String The PP1 Detector Signal Data string format is a decimal number followed by a carriage return CR and line feed LF An example 104345 104763 104832 The End Of Data string format consists of three ASCII characters The following are four forms of the same command Form 1 Start Of Text E End Of Text Form 2 STX E EXT Form 3 AB E eG Form 4 02 45 03 An example 104345 104763 104832 Last sample sent to Host ABEAC End Of Data command to Host from PP 6 2 4 EzChrom Elite Output Protocol Th
36. en Upper Section Set up Screen Upper Section Button Functions Set up Screen Middle Section Power up Set up Screen Middle Section Button Functions Power up Set up Screen Middle Section Normal Set up Screen Middle Section Button Functions Normal Set up Screen Lower Section Display Screen Button Functions Clearing Error Messages on the Set up Screen Set up Screen Lower Section Button Functions Analog Interface Screen Analog Interface Screen Button Function Analog Interface Connections and Wiring Calibration Database Screen 4 3 1 4 3 2 4 3 2 1 4 4 1 4 4 2 4 5 1 4 5 2 4 6 1 4 6 2 4 7 1 4 7 2 4 7 3 4 7 3 1 4 7 4 4 7 4 1 Peak Performer 1 Users Manual Calibration Screen Button Functions Calibration Establishing New instrument Response Factors Analysis Database Screen Analysis Screen Parameters Analysis Screen Button Function Event Program Editor Screen Event Program Commands Event Editor Screen Button Function Stream Selector Sequence Editor Screen Stream Selector Commands Stream Selector Program Editor Screen Button Function Run Chromatogram Screen Run Screen Button Functions Run Screen Continuous Monitoring Analysis Manual Screen Sub Screen of Run Screen Manual Screen Button Functions Display Screen Sub screen of Run Screen Display Screen Button Functions Viewer Software System Requirements Installing the Viewer Software Starting the Viewer Software Communications Settings
37. er 1 Users Manual port ensure that the front jumper is connected between SAMPLE OUT and SAMPLE IN on the front panel Verify that sample is flowing freely through loop exit flow from the SAMPLE OUT should be 30 to 120 cc min Press the ESC or PAGE keys as needed to navigate to the RUN screen Press the SINGLE CYCLE RERUN key to toggle to SINGLE mode Press the RUN key to initiate analysis the P1 event program will be loaded automatically and executed Allow the analyzer to fully execute the event program Current concentration data will be displayed as an overlay on the RUN screen as peaks are identified and quantified Press the PAGE key as needed to toggle to the CALIBRATION DATA BASE screen Place the at the first compound of interest and press the EDIT key use the up down left and right arrow keys to enter the span gas concentration in the CONC field Be certain to use the right arrow key to fully exit the CONC field or all updates will be lost With the before the compound name press the UPDATE key The analyzer will recalculate the appropriate response factor for the compound based upon the span gas concentration and analyzer area response using the following formula RESPONSE FACTOR AREA RESPONSE SPAN GAS CONCENTRATION NOTE The LED on the analyzer s front panel will change from green to red to remind the user that the current calibration information is stored in volatile temporary memory
38. erator to adjust the horizontal scale vertical scale and baseline offset of the chromatogram These functions mimic those of a standard chart recorder Page 44 Peak Performer 1 Users Manual Figure 30 Run Display screen 4 7 4 1 Display Screen Button Functions VOff VOff Attn Attn Span Esc Page 45 Scrolls the screen up maximum Voff 11 without changing the scale Scrolls the screen down minimum Voff 0 without changing the scale Toggles the attenuation vertical scaling max Attn 11 up Toggles the attenuation vertical scaling min Attn 1 down Toggles the window view horizontal scaling in seconds Exits from the Display sub screen to the Run screen Peak Performer 1 Users Manual 5 0 Viewer Software The Viewer software has two main capabilities Primary functions concern acquisition and archiving of compound concentration and acquisition and collection of the chromatogram data The software also provides the ability to display and print the data from any remote computer platform Viewer software is written specifically for the Peak Laboratories Peak Performer 1 PP1 gas analyzer covering communications port protocols and data formats and is not intended for use with other manufacturer s analyzers 5 1 System Requirements 1 2 GHz 20 GB 256 Mb RAM 1 USB port Windows XP or Windows VIsta USB to DBY RS232 Adapter SIIG US2308 JU CB1 12 or equivalent DB9 Exten
39. ext screen 4 7 2 Continuous Monitoring Analysis Continuous monitoring is intended for on line analysis or other applications which ReRun analysis is not required Use the PAGE key to scroll to reach the Run screen Toggle the Single Cycle ReRun key until Cycle appears See Figure 28 Press Run to initiate a repetitive analytical cycle By pressing the RUN key event program 1 P1 is automatically loaded and the system will begin to collect data in repetitive mode see Figure 28 To halt the cycle pressing the IDLE will cause the analysis run to cease immediately Toggle between the Single Cycle Rerun or optional Stream to select the next mode of analysis 4 7 3 Manual Screen Sub Screen of the Run Screen The Manual sub screen allows the operator to invoke all the event program commands on demand Page 43 Peak Performer 1 Users Manual Tgnit Figure 29 Run Manual screen 4 7 3 1 Manual Screen Button Functions Zero Pressing this key will electronically zero the detector Ignite Pressing this button applies power to the ignition probe for 20 seconds Bias Toggles the negative accelerating voltage within the FID to ON BIAS or OFF V1 Toggles Valve 1 between CW and CCW positions V2 Toggles Valve 2 between CW and CCW positions Esc Exits from the Manual sub screen to the Run screen 4 7 4 Display Screen Sub Screen of the Run Screen The Display sub screen allows the op
40. figuration diagram with basic connections 6 5 1 RS232 to RS485 Converters There are numerous manufacturers of RS232 to RS485 converters and the selection of the converter must be determined by the system engineer designer to meet unique requirements 6 5 2 PP1 Port 2 Protocol Please refer to Section 6 3 1 and 6 3 2 for information on the PP1 COM 2 Port Protocols Page 61 Peak Performer 1 Users Manual 7 0 Chromatographic Principles As an analytical system the PP1 FID performs four primary functions Sample injection Component separation Component analysis Integrated microprocessor system control with operator and data interface 7 1 Sample Injection A standard air actuated VICI injection valve is used to inject samples Standard FID analysis methods use stainless steel 5 cc sample loops 7 2 Carrier Gas Purification Chromatographic instrument detection limit is directly related to carrier gas purity Improved carrier gas purity enables improved sensitivity Typical Nitrogen 99 999 Carrier Gas Specifications Pre Purification High Pressure Cylinder or Liquid Dewar Gas Type N Ar He alternative Consequently the analyzer s minimum detectable quantity MDQ would be quite high gt 10 ppm unless the carrier gas is purified Peak recommends use of the best quality heated metal getter purifier available for carrier gas purification This style of purifier typically has a hot catalyst element ahe
41. gure 49 The Completed Chromatogram 7 4 Flow Venting and Balancing Several problems can arise in the development of the chromatogram e Presence of compounds that may be damaging to the detector e Disproportionate peak sizes e Length of analysis Several models of Peak analyzers are equipped with one or two valve plumbing arrangements to handle these situations Often a second valve is used to perform cutting actions at particular times during the chromatogram redirecting the column effluent towards a safe flow controlled vent outlet During the cutting action it is necessary to maintain pure gas flow to the detector This pure gas flow is provided by an additional branch on the internal carrier gas main line feeding other ports on the valve Ultra high purity flow control components can be bulky and expensive To diminish installed cost of flow control components Peak has chosen a different method based upon flow restrictors to create a flow divider A typical flow divider is shown in Figure 50 Page 66 Peak Performer 1 Users Manual CARRIER GAS MAIN LINE FLOW ADJUSTMENT NEEDLE VALVE MAIN FLOW LIMITER 110 sccm 60 PSIG EXCESS FLOW VENT TO DETECTOR DETECTOR BALANCE RESTRICTOR Figure 50 Flow Divider Schematic The gas flow path to the detector is extremely clean and free of moving parts The gas passing from the main flow limiting restrictor can be split to follow both gas paths Study
42. he sample loop 2 Wait 10 minutes to purge the analyzer completely of any residual gas samples 3 Initiate a standard sampling run in CYCLE mode 4 Collect 5 sample runs with Peak Viewer 5 Average the concentration data of the 5 runs for each peak of interest 6 Average readings higher than 1 ppb for any compound indicates a loss of valve seal integrity and possibly suggests valve head replacement Page 94 Peak Performer 1 Users Manual 9 4 Start up Sequence for Replacement Methanizer Turn off FID H2 and FID Air supplies to analyzer Cool FID to below 60C Remove FID Oven Cover Remove 3 insulation blocks and stuffing Take care to not disturb the heater and T C leads Use along handled 2 Phillips screwdriver ot reach ansd remove the heater block cover retaining screw on the left side of the FID Lift out the heater block cover and screw Loosen the methanizer from the heater block Vacuum insulation dust form the FID chassis area Uncouple the FID methanizer inlet and outlet 1 16 VICI fittings Remove the methanizer Bend replacement methainzer tubing to roughly match the old methnizer AUN O1 6 T 8 9 1 1 1 0 1 2 Install the methanizer in the heater block 13 Re install heater block cover 14 Connect 1 16 Inlet And outlet VICI fittings 15 Re install 3 insulation blocks and stuffing Take care to not disturb the heater and T C leads 16 Make sure the FID Carrier is pre
43. ial number of unit is used as the RS 485 ID 6 3 2 COM 2 Port Output Format The COM 2 port output format consists of date and time stamp error alarm stream number and impurity data This data format is transmitted at the end of every run automatically using a general protocol envelope This envelope consists of a start of transmission character followed by data and end of transmission character The record start of transmission indicator is STX character 02 hex and the record end of transmission indicator is ETX character 03 hex The fields within each record are defined as follows lt STX gt YYYY MM DD HH MM SS E X N1 AREA1 CONC1 N2 AREA2 CONC2 N3 AREA3 CONC3 N4 AREA4 CONC4 lt ETX gt YYYY MM DD Date 2003 03 23 HH MM SS Time 12 23 44 12 hours 23 minutes 44 seconds Page 59 Peak Performer 1 Users Manual E General Error Alarm 0 No error 1 Error X Stream Number N1 Name of impurity 1from Calibration Database AREA Area of impurity 1 CONC1 Concentration of impurity 1 in 0 1 ppb N2 Name of impurity 2 from Calibration Database AREA2 Area of impurity 2 CONC2 Concentration of impurity 2 in 0 1 ppb N3 Name of impurity 3 from Calibration Database AREA3 Area of impurity 3 CONC3 Concentration of impurity 3 in 0 1 ppb N4 Name of impurity 4 from Calibration Database AREA4 Area of impurity 4 CONC4 Concentration of impurity 4 in 0 1 ppb IMPORTANT NOTE The least s
44. ied using this method are denoted with a B in the last column of the data report 7 6 3 Peak Quantification Variable Mode If the peak maximum signal value exceeds the PkHgt value the Variable Mode is enabled for determination of peak start and end points The time associated with the peak maximum signal is always calculated first for Forced Baseline and Variable modes by using the convolution filter to find the maximum detector signal point Page 77 Peak Performer 1 Users Manual o z rs 2 N Figure 65 Initial parameters for Baseline Determination Initially the mathematics package makes a trial evaluation of peak area using a fixed percentage of the LW and RW values as initial baseline points illustrated as the hypothetical baseline between points 2 3 of LW and 2 3 of RW in Figure 65 The hypothetical calculation of the peak start time is labeled L in Figure 66 Peak Maximum a u e N PEAK START Figure 66 Progression of Peak Start Time Calculation After calculating the hypothetical peak area based upon the L and R values the mathematics package makes another peak area calculation using a slightly earlier time value The peak areas of the two calculations are compared and if the peak area increases by more than 0 5 the mathematics package repeats the process The net effect is illustrated in Figure 66 where multiple hypothetical peak start points were evaluate
45. ify that the analyzer reports data values within normal calibration tolerances i e 5 3 7 Shutdown and Transport 1 Allow the temperature zones to cool below 50 C approximately 2 hours 2 Allow carrier to flow during cool down time Shut off carrier after cool down time and plug the CARRIER IN FID H2 FID AIR ports on the rear of the analyzer Power off analyzer Cap the SAMPLE IN SAMPLE OUT and ACTUATOR IN ports Plug the BYPASS OUT port on the front panel Ensure that the front jumper tube is connected between SAMPLE IN and SAMPLE OUT OO NOOO Ff Page 23 Peak Performer 1 Users Manual 8 Package the analyzer in a hard cover carrying case or comparable shipping container If cardboard packaging is used Peak recommends double boxing of the analyzer using at least 2 of resilient packing material between the inner and outer box walls Page 24 Peak Performer 1 Users Manual 4 0 Peak Performer Operator Interface SET UP MAIN SCREEN PAGE KEY TREND amp ANALOG OUTPUT PURCHASED OPTION SCREEN cir ieee CALIBRATION DATABASE SCREEN PAGE KEY ANALYSIS DATABASE SCREEN PAGE KEY EVENT PROGRAM EDITOR SCREEN PAGE KEY STREAM SELECTOR PROGRAM EDITOR PURCHASED OPTION SCREEN PAGE KEY ANALYZER POWERS UP ON RUN CHROMATOGRAM SCREEN RUN 7 DISPLAY KEY RUN DATA me RSET Rur CHROMATOGRAM mom r aona i UAL CONTROL DISPLAY CONTROL ree ee S
46. ignal attenuation X1 X2 X4 X8 This function is similar to the RANGE switch on a chart recorder Temporarily over rides the signal output with a known output voltage for test purposes Four MANSET options are available 0 00 VDC 0 312 VDC 0 625 VDC and 1 250 VDC There is not any zero offset or full voltage scale adjustment within the PP1 if this function is a requirement Peak Labs recommends the use of standard commercial voltage converters attached externally to the analyzer Advances the user to the next screen 4 2 2 Analog Interface Connections All analog interface connections are made via the rear panel DIN connector To make a proper connection strip all wires back approx 3 8 unscrew the terminal locking screw fully insert the wire and tighten A common error is insufficient length of bare wire creating the condition where the terminal contacts only the wire insulation Page 33 Peak Performer 1 Users Manual SAMPLE 1 SAMPLE1 ACTUATOR CARRIER IN IN IN OUT AIR He 2 IN OUT COM2 SPAN IN ANALOG 1 ANALOG 2 ANALOG 3 ANALOG 4 REC COMMON GND ZERO START PLAMESW _ FLAME SW E o S Figure 19 Analog Output Connections 90 120 VAC 59 00 HZ ANALOG 1 OOO ANALOG 2 OO gt cil ANALOG 3 ANALOG 4 REC LL COMMON GND ZERO START 7 o PNE 2 POWER mene vay saoo source STON FLAME SWITCH RATED AT 0 5 A 120 VAC Figure 20 Ana
47. ignificant decimal of the concentration resolution represents 0 1 ppb I E a CONC1 reading of 1 represents a 0 1 ppb concentration level 6 4 Trend Analog Output Format Three independent impurity trend outputs are provided via 0 1 25 VDC screw terminals Each impurity can be scaled from the front screen to match desired range The ranges are as follows Q gt 125 ppb Q gt 1250 ppb 0 gt 5500 ppb Q gt 12500 ppb Q gt 125000 ppb e g O 1000 ppb 0 1 VDC scale At the end of each run the analog signal is updated and holds until the next run is completed As an accessory Peak can provide standard commercial VDC gt gt mA converters as needed Page 60 Peak Performer 1 Users Manual 6 5 Setting up a RS 485 Network The RS 485 specification supports two wire half duplex communications only one unit may transmit at a time but allows up to 32 users on a party line network NOTE The RS 422 specification supports four wire full duplex communications two units may transmit at a time and also allows up to 32 users on a party line network The following information is provided to enable the users to install the Peak Performer 1 into a RS 485 network This system diagram consists of the PP1 RS 232 to RS 485 converter and master host controller COM2 RS232 to RS485 PP1 Converter Master Controller PP COM2 RS232 to R5485 Converter Figure 43 System con
48. il the ZERO command is invoked 4 1 2 1 Set up Screen Middle Section Button Functions Power up If both heater zones are de energized the following command buttons are available Zero Allows the initialize the detector electronics and establish a consistent baseline signal Moves the cursor upwards J Moves the cursor downwards Edit Allows the user to energize each heater zone or change heater setpoint temperatures Heat Energizes all the heater zones Page Advances the user to the next screen Page 27 Peak Performer 1 Users Manual 4 1 3 Set up Screen Middle Section Normal The middle section of the Setup screen concerns temperature zone and detector function MetLhanizer Colunmr FIDI Flame ia iat nd oe ok Li iT Af cae Figure 13 Screen Commands After Warm up 4 1 3 1 Set up Screen Middle Section Button Functions Normal Zero Allows the initialize the detector electronics and establish a consistent baseline signal i Moves the cursor upwards LG Moves the cursor downwards Edit Allows the user to energize de energize each heater zone or change heater setpoint temperatures Page Advances the user to the next screen Page 28 Peak Performer 1 Users Manual 4 1 4 Set up Screen Lower Section The lower portion of the Setup screen is reserved for error messages and non volatile memory updates 4 1 4 1 Error Messages on the Set up Screen Lowe
49. inches x 16 38 4 re arranging L in inches 0 777 x V in cc s ID 2 in inches an example for a 1 cc loop L inches 0 777 x 1cc 0 040 2 49 inches tube length 4 Measure to length cut and install VICI fittings 5 Blow the tube out with compressed air to remove any particles Page 97 Peak Performer 1 Users Manual 9 7 UPDATING THE ANALYZER SOFTWARE WITH PEAK HOST Procedure 1 Power down analyzer chassis 2 Connect DB9 serial cable and host computer to COM1 port on the rear of the 3 PP1 analyzer Power up analyzer chassis Do not re energize the heaters at this time Open the PeakHost exe program on the host computer Adjust the PeakHost serial communications settings as required to establish communications with the PP1 analyzer Normal settings are COM3 38400 8 1 The PeakHost program will automatically start acquiring information from the analyzer Force the PeakHost program to obtain fresh analyzer information under the PeakHost program main screen toolbar select File then Receive From Analyzer Save the analyzer operating parameters by using the print function in PeakHost under the PeakHost program main screen toolbar select File then Print If not printer is available manually write the following parameter values Zone 1 Set Point Zone 1 P Value Zone 1 Value Zone 1 Limit Zone 2 Set Point Zone 2 P Value Zone 2 Value Zone 2 Limit Zone 3 Set Point
50. ing temperature is 105 C when exposed to oxygen bearing gases CAUTION Never energize heaters of the instrument unless carrier gas flowing Page 20 Peak Performer 1 Users Manual CAUTION The maximum PP1 FID column operating temperature is 105 C when exposed to oxygen bearing gases Do not exceed 210 C of column oven temperature at any time Temperatures in excess of 210 C can destroy column material 1 Connect the front jumper tube between SAMPLE IN and BYPASS OUT 2 Use the t and keys to navigate and alter the SET value for the Column heater zone to 180 to 200 C 3 After 8 to 12 hours of stable conditioning temperature the column temperature may be restored to the original factory setting See the Final Test Data shipped with the analyzer 4 After normal operating temperature is achieved the front jumper tube may be reconnected between SAMPLE IN and SAMPLE OUT 5 After a 5 10 minute detector re equilibration period samples may be run Normal operating temperatures vary with specific application Consult the Final Test Data for special settings special reconditioning requirements etc for your application 3 3 Detector Conditioning CAUTION The maximum detector operating temperatures for the FID is 350 C The FID does not normally require conditioning treatment however it does require 8 to 12 hours at normal operating temperature to achieve optimum stable perfor
51. ing the schematic it can be seen that the detector flow can be adjusted by changing the amount of gas that is allowed to exit via the excess flow vent as more gas exits the excess flow vent less gas is available to flow towards the detector The controlling needle valves for detector flow rate and column venting are co mounted in the chassis for convenience see Figure 61 The detector flow control needle valve is color coded red Differences in DETECTOR flow during normal and venting valve positions can be expressed as shifts in detector baseline Careful adjustment of the detector flow control needle valve will enable the operator to minimize baseline drift and create a smooth chromatogram OFFSET 3000 ATT 3 SPAN 14 Cons Poty EO N ni a paca Peak Tima Le oa a bo rew HICE Hh Us a we ami T EERS A Figure 51 Properly Flow Balanced Detector Baseline Page 67 Peak Performer 1 Users Manual Pesi Time pire pita p a 2 Ms 8 we Figure 53 Low FID flow from NV1 note drop after the V2 CCW command Differences in COLUMN flow during normal and venting valve positions will be expressed as shifts in peak retention time compared to a chromatogram without any venting action Page 68 Peak Performer 1 Users Manual NV2 Flow 59sccm a NV2 Flow 39 sccm a NV2 Flow 79 sccm
52. ion he System Alarm GR Analysis Index AECGEGEG Figure 37 Viewer Detail screen showing raw analysis data The information on the screen is linked to run 13 50 displayed in figure 36 Page 51 Peak Performer 1 Users Manual 5 6 2 Start Menu on the Viewer Taskbar i Viewer Yer 3 12 i O x File Start Stop Chrom View Event Info Pun Single Rur Cycle Run Stream Run Figure 38 Start menu on the taskbar The Start menu contains the following commands Se Single Run Single Run selection commands the PP1 to start a Single Run Cycle Run Cycle Run option commands the PP1 to start a continuous Cycle Run Stream Run selection commands the PP1 to start a Stream Selection Run This operation only function if the Stream Selection option is installed 5 6 3 Stop Command on the Viewer Taskbar The Stop Command selection instantly sends a command the PP1 to terminate the current run immediately Page 52 Peak Performer 1 Users Manual 5 6 4 Chrom View Menu and Chromatograph Viewer Window The Chrom View menu selection opens the Chromatograph Viewer window Two methods can open the Chrom Viewer window 1 The first method is to select the Chrom View menu selection from the Viewer taskbar and then select a chm file to display 2 The second method of opening the Chrom Viewer is double clicking one of the concentration values displayed in the Viewer window Using either method
53. ions if these input conditions are not available SAMPLE GAS SUPPLY TO PP1 va gt lt aa Vi Vi Y p FLOW RESTRICTOR 30 60 sccm ATMOSPHERIC PRESSURE Figure 7 Sample Supply Flow Schematic Page 17 Peak Performer 1 Users Manual Sample gas must be supplied to the analyzer at low pressure 0 3 to 1 0 psig and moderate flow 30 to 120 ml min The analyzer does not have any sample gas pressure flow regulation 2 5 5 1 Second Sample Gas Supply Peak Labs offers an optional second sample inlet stream for most analyzers Connection to the SAMPLE 1 IN and SAMPLE 2 IN ports should replicate Figure 7 Sample lines are normally attached to the rear panel of the instrument Attach sample or span gas lines to the SAMPLE IN port on the rear panel The SAMPLE OUT port must be unrestricted 2 5 6 Span Gas Supply Peak Labs offers an optional internal span gas blender for most analyzers Connection to the SPAN GAS IN port should replicate Figure 8 It is important to measure the pressure applied to the SPAN GAS IN port as closely to the analyzer rear panel as possible SPAN GAS FEED SUPPLY AA KA Z 7 CA 4 NS o N ed gt N s N FLOW LIMITER 20 30 sccm 60 PSIG Figure 8 Span Gas Supply Flow Schematic Page 18 Peak Performer 1 Users Manual 3 0 Start up Procedure Peak Labs recommends that the user read the entire operating
54. is considered the best multi purpose carrier gas However the best carrier to use approximates the sample matrix i e nitrogen carrier for analysis of impurities in nitrogen Matching the carrier gas to the sample will prevent upsets caused by the elution of high concentration sample balance peaks For optimum performance the carrier gas must match the balance gas of your analytical sample although other carrier gases can be used for specific applications with factory assistance A PLEASE CONSULT THE TEST DATA ATTACHED TO YOUR ANALYZER IF UNCERTAINTY OF CARRIER GAS SELECTION EXISTS Page 12 Peak Performer 1 Users Manual 2 5 1 1 Carrier Gas Purity Chromatographic instrument detection limit is directly related to carrier gas purity Improved carrier gas purity enables improved sensitivity Typical Nitrogen 5N Gas Specifications Pre Purification High Pressure Cylinder or Liquid Dewar Gas Type No Ar He alternative Consequently the analyzer s minimum detectable quantity MDQ would be quite high gt 10 ppm unless the carrier gas is purified Peak recommends use of the best quality heated metal getter purifier available for carrier gas purification This style of purifier typically has a hot catalyst element ahead of the heated getter material for complete removal of methane hydrocarbon CH4 a common contaminant in commercial nitrogen sources Hydrogen Carbon Monoxide Carbon Dioxide Hydrocarbons and Moistu
55. kbar PA Chrom iewer 2008 11 13 1341 chm ID x File Viewer Analysis DE Open Javes NMHC CO Page 54 Peak Performer 1 Users Manual 15 x Open Saves Figure 41 Baseline Deselected The File menu offers the following commands ee ae Opens a chromatogram file Use this command to open and load the chromatogram data for display Save the chromatogram data that is currently displayed BaseLine Enables Enables display of compound name and integration baseline information Enables display of compound name and integration baseline information compound name and integration baseline information es a 5 6 4 3 Viewer Menu on the Chrom Viewer Taskbar The Viewer menu selection returns the user to the original Viewer window See Figure 36 Page 55 Peak Performer 1 Users Manual 6 0 Communication Port Protocol and Formats There are two serial communications ports on the rear of the PP1 COM1 isa multifunctional serial port COM2 port is a dedicated PLC output port 6 1 COM1 COM2 Port and Cable Wiring The cable connected from the PC to the PP1 should be a straight through wired 9 pin M F cable attached to the PC s COM port and the PP1 s COM port PC MALE PP 1 FEMALE 9 Pin Cable from PC to PF1 Figure 42 COM Cable Wiring Peak Labs recommends limiting cable lengths to 25 feet maximum 6 2 Port 1 Protocol On analyzers with Software versions 3 00 a
56. log Output Wiring Schematic 4 3 Calibration Database Screen The Calibration Database screen stores critical information regarding calibration Span gas concentrations and instrument response and provides tools to easily update the response factors Page 34 Peak Performer 1 Users Manual Figure 21 Calibration Database Screen 4 3 1 Calibration Screen Button Function Update Allows the analyzer to calculate new RFactor ie Moves the cursor upwards Moves the cursor downwards Edit Allows the user to change concentration data or response factor Page Advances the user to the next screen 4 3 2 Calibration The Peak Performer 1 chromatograph determines concentration peak area to quantify the amount of contaminants in the sample gas The direct instrument response in units of uV sec is reported simultaneously as an overlay on the RUN CHROMATOGRAM SCREEN and in the AREA column on the CALIBRATION DATABASE SCREEN As the concentration peak area is determined the analyzer applies the pre programmed response factor as an inverse proportional factor to generate the reported concentration value PEAK CONCENTRATION PEAK AREA RESPONSE RESPONSE FACTOR 4 3 2 1 Establishing New Instrument Response Factors Connect a known calibration standard gas span gas to the analyzer at the SAMPLE IN port on the front panel If span gas connection is made at the rear panel SAMPLE IN Page 35 Peak Perform
57. ly Procedure Power off analyzer if gas umbilical tubing is used it is not necessary to cool down the analyzer Maintain normal gas supplies Disconnect AC power cord Remove top cover Locate the main DC power supply in the right rear portion of the chassis see Figure 1 Figure 84 Main DC Power Supply Location Remove the 4 each 6 32 screws that hold down the plastic protective shield to expose the DC power supply see Figure 84 Page 105 Peak Performer 1 Users Manual TE p p p s mN mug _ ail i Figure 85 Main DC Power Supply with Shield Removed Unscrew the 4 each standoffs that retain the DC power supply to the rear panel circuit board Disconnect only the two cable assemblies that attach the DC power supply to the rear panel circuit board it is recommended to disconnect the cables at the circuit board connector end Remove the DC power supply by sliding it under the overlayed cable assemblies do not remove the other cable assemblies see Figure 85 Page 106 Peak Performer 1 Users Manual Figure 86 Main DC Power Supply Fully Removed Lay the old DC power supply on the workbench aside the new Power one DC power supply Orient such that the 6 pin and 2 pin connectors are aligned see Figure 86 Figure 87 Correct Alignment and Cable Transfer from Old to New DC Power Supply Transfer the two cable assemblies from the old power supply to the new supply I
58. lyzer may display a red light after this action 25 If the analyzer displays a red light on the front panel the parameters must be accepted and saved on board the analyzer before proceeding any further Page 101 Peak Performer 1 Users Manual a Press PAGE touchpad until the SETUP SCREEN appears this screen has SN and temperature zone controls b Press the DOWN arrow until you reach the Parameter Change Update Needed line c Press the ACCEPT touchpad button then the SAVE touchpad button to permanently save the temperature parameters in analyzer memory 26 Force the PeakHost program to obtain fresh analyzer information under the PeakHost program main screen toolbar select File then Receive From Analyzer 27 Verify the correctness of the temperature control parameters again Verify Install the Peak Analysis Database 28 Force the PeakHost program to obtain fresh analyzer information under the PeakHost program main screen toolbar select Analysis DB then under File select Receive From Analyzer 29 Verify the correctness of the peak analysis parameters compared to the original values If errors are noted overwrite each parameter including any zero values recorded for all fields Be sure to include all the zero values in the entire database table Note while you cannot enter a blank value e g spacebar for the unused peak names it is best to enter a number 3 or 4
59. mance Normal detector operating temperature for the FID is 295 C although operating temperatures may vary with the specific application CAUTION Do not ignite the flame unless the FID FLAME reading is greater than 90C See Section 8 for details concerning the effects of operating parameters temperature and flow on FID detector performance 3 4 Igniting the FID Flame 1 Verify that Carrier FID H2 and FID Air supply pressures match those listed in the final test report Verify that the FID FLAME temperature is greater than 90C Press the PAGE command 4 times to reach the RUN SCREEN Press the MANUAL command once aN Page 21 Peak Performer 1 Users Manual 5 Press the IGNITE command once wait 30 seconds and press the IGNITE command again Press the ESC command once Press the PAGE command once Verify that the FID FLAME MEAS reading is greater than the FID FLAME SET reading if not repeat steps 3 through 8 9 Press the PAGE command 4 times to reach the RUN SCREEN 10 Press the MANUAL command once 11 Press the BIAS command once The screen will display BIAS to indicate that the bias voltage 140 VDC has been turned on OTAD 3 5 Sample Analysis Verify that sample is flowing freely through loop exit flow from the rear SAMPLE OUT port should be 30 to 120 cc min Press the ESC or PAGE commands as nee
60. manual prior to using the Quick Start sequence CAUTION Do not begin detector heating without carrier gas flow Damage to the detector may result 3 1 Quick Start Sequence 1 Confirm that all gas connections and supplies are properly made 2 Remove the top cover of the instrument Figure 9 FID Detector 3 Pressurize the carrier gas supply line to 60 psig 4 Pressurize the FID H2 gas supply to 25 psig 5 Pressurize the FID Air gas supply to 20 psig 6 Pressurize the Actuator gas supply to 65 psig Verify that sample is flowing freely through loop exit flow from the rear SAMPLE OUT port should be 20 to 120 cc min 8 Verify BYPASS OUT flow gt 20 cc minute 9 Verify the analyzer is connected to the correct line voltage supply 10 Energize the main power switch located to the right of the power cable see Figure 1 11 After energizing the instrument will display the RUN screen in the IDLE state Page 19 Peak Performer 1 Users Manual 12 Press the PAGE command once 13 Press command three times to position the cursor in the middle 1 3 of the screen 14 Press the HEAT command once to activate heater zones 15 Allow the 4 6 hours for the analyzer to thoroughly stabilize the heated zones After temperature stabilization 16 Verify that the FID FLAME reading is greater than 90 C 17 If the analyzer has been stored or idle without carrier gas flow f
61. mer 1 has a fully integrated stand alone microprocessor operating system Key functions of the operating systems include detector and temperature control data collection and analysis and operator data interface Temperature range 50 C gt 295 C 160 watts maximum Page 7 Peak Performer 1 Users Manual 2 0 Installation Considerations 2 1 Unpacking Instructions Remove the Peak Performer 1 from the packing material or traveling case taking care to not scar the exterior surfaces of the analyzer Set the analyzer on a firm even surface and remove the protective plastic wrap Each analyzer ships with adequate supplies for installation Be certain to remove the installation accessories tubing power cord compression fittings etc from the packing materials Remove the sleeve containing the Certificate of Conformity and Installation CD from the analyzer top panel All shipping materials are reusable please recycle these materials appropriately 2 2 General Considerations Analyzer size is 26 Lx 17 W x 7 H Maximum operating environment for the PP1 analyzer is 30 C Power consumption is 160 watts maximum Fuse size is 2 5 ampere 250 VAC 5 x 20 mm SLO BLO Free air flow for adequate ventilation to the rear of the unit is required Communication between the PP1 and your PC is via 9 pin straight through cable connection to COM 1 and COM 2 e Analog outputs are available from the DIN screw terminal strip o
62. n regime of interest is the opposite case where it is desirable to detect and extract the smallest possible peak signal Under these circumstances it is advantageous to utilize signal processing techniques that magnify signal differences Mathematical convolution is one such method Convolution rolls two waveforms together as the product of data matrices with the resulting new waveform having exaggerated characterisitcs Detector Baseline Cross Multiplied by the Convolution Fllter Yields the Resultant Baseline Figure 62 Convolution to Enhance Signal Characteristics As seen in Figure 62 it is much simpler to identify the peak maximum on the convolved baseline Convolution functions work best when the convolving peak filter width closely matches the expected chromatographic peak width Page 75 Peak Performer 1 Users Manual Chromatographic peak width can vary significantly depending upon column selection detector characteristics sample loop size etc Consequenlty there are several different convolving peak widths available in the PP1 s mathematics package Fit 1 is the narrowest filter width FIt 8 is the widest filter width NOTE Final determination of the optimum filter width is best performed by re processing chromatograms representing typical peaks 7 6 1 Peak Quantification Fixed Mode When the PkHgt variable is set to zero the Fixed Mode of detector baseline is enabled In
63. n the rear panel e The FID drain line must be inside diameter minimum and without restrictions its entire length H2 venting H2 shut off valving and H2 supply safety equipment must be supplied by customer 2 3 Electrical Connections Verify the correct operating voltage as marked on the rear of the analyzer at the main power switch Attach a standard power cable to the rear of the instrument see Figure 1 and connect to an appropriately grounded outlet Page 8 Peak Performer 1 Users Manual Power Cord PP1 Power Entrv Figure 1 AC Power Connection Details For best sensitivity power to the analyzer should originate from an electrical circuit free of large inductive or other current loads Be sure to mount the analyzer in an area of adequate ventilation and make sure the cooling fan inlet is unobstructed 2 4 Rack Mount Specifications The PP1 is designed for mounting in a standard 19 instrument rack The analyzer occupies 4U 6 9 of panel height 26 in depth Rack retaining flanges provided with the Peak rack mount kit attach via the analyzer top cover to provide secure connection to the instrument rack rails Peak recommends use of high quality 26 full extension ball bearing slides for instrument mounting such as Jonathan QD375 26 or equivalent 18 88 REVISIONS gue omena 281 1 25 TYP 16 88 18 25
64. nd greater there are two COM1 output formats Viewer and Detector Proper selection of protocol is determined by the application interfaced on the host computer Note On older analyzers with Software versions 2 06 and lower there are three COM1 output formats in the PP1 Viewer Detector and EzChrom Elite EZChrom Elite output is available for Software versions 2 06 and lower only 6 2 1 COM 1 Port Settings The RS 232 settings for COM 1 port are 38400 baud rate 8 bit data 1 stop bit and no parity These settings are fixed and are not user selectable Page 56 Peak Performer 1 Users Manual 6 2 2 Viewer Output Format Format of columns in CSV file The Viewer software stores information in a common text format Comma Separated Variable CSV CSV files can be opened in common spreadsheet applications for further analysis The column format in the CSV files are A Data Time B Run Mode C Analysis Buffer Number and Stream Number D General Error Alarm E RCP Lamp Voltage or FID Flame Temperature F Compound Name G Retention Time H Left Point Offset Right Point Offset J Area K Response Factor L Processing Flag Columns F to L are repeated for M to S T to Z and AA to AG for the next three compounds listed in the Calibration Data Base 6 2 3 Detector Output Format The detector output format of the COM1 interface currently supports one command from a host computer system This command r
65. nstall the new DC Power Supply by reversing the disassembly sequence Page 107 Peak Performer 1 Users Manual After installation and power up it may be necessary to re adjust the contrast on the front panel display it may be too light or too dark Page 108 Peak Performer 1 Users Manual Adjust polentiometer so that voltage g between the RED and BLACK wines at the motherboard is 6 1 to 5 2 VOC Figure 88 Adjusting the 5 Volt DC Supply Page 109 Peak Performer 1 Users Manual 9 11 COM 1 Viewer Connections on Multiple Analyzers to a Single Computer Equipment 1 each Computer 1 2 GHz 20 Gb Hard drive 256 Mb RAM CD R drive with at least 1 USB port Dell Inspiron 8500 laptop or equivalent Operating System Windows XP Home Edition v2002 Service Pack 1 1 each USB Hub Inland 4 Port USB Hub Self powered Stock 08302 manufactured by Inland International www inland products com 2 each USB to DBY RS232 Adapter SIIG Inc USB to Serial Adapter Model US2308 Part JU CB1S12 manufactured by SIIG Inc www siig com Comes with installation software 2 each DB9 Extension Cable DB9M to DBYF wired straight through 10 feet long GQ Cables 10 Mouse Keyboard Extension DB9M to DB9F Part M05 103 USB Hub USB to DB9 apes A A p S 0000 o000 Figure 89 Multiple Analyzers Connected to a Single Computer For Using Viewer Software Installation of Multiple Analyzer
66. nual 2 5 Gas Supplies and Connections All plumbing connections are 1 16 female VICI bulkhead fittings The Peak Performer 1 is shipped with tubing and fittings required to connect the analyzer to gas sources Replacement materials are available from Peak Laboratories or may purchased directly a Standard gas fittings are 1 16 VICI compression fittings VICI P N ZN1 amp ZF 1 b Supply tubing is 1 16 O D x 0 03 I D cleaned and baked T300 stainless steel tubing Restek P N 21508 AIR H2 aR Re e Et ACTUATOR CARRIER E i i Figure 5 Rear View of PP1 FID Page 11 Peak Performer 1 Users Manual O D GETTER PURIFIER ACTUATOR IN FID AIR FLOW LIMIT RESTRICTOR SAMPLE IN FID H2 FLAME SWITCH m m m FLAME SWITCH m mmu mo PNEUMATIC CONTROL SOLENOID SAMPLE GAS SUPPLY HYDROGEN GAS SUPPLY Figure 6 FID PP1 Gas Supply Schematic 2 5 1 Carrier Gas Supply The instrument will accept a variety of carrier gases No Ar or He See Section 2 5 1 1 CAUTION Oxygen is never a suitable carrier or actuator supply gas Oxygen is highly reactive and many pneumatic components contain greases and oils that combust spontaneously when exposed to oxygen Consult the test data shipped with the analyzer in CD format for carrier gas details specific for your analyzer Commonly the PP1 will utilize highly purified nitrogen as the carrier gas supply and nitrogen
67. o repair the instrument except under directed to do so by factory trained service technicians Permanent damage and voiding of the warranty may result of improper operation The FID utilizes low flows of pure hydrogen and clean air to generate a small continuously burning flame within the FID Tower Use standard gas handling practices for combustible gases when working with the FID equipped PP 1 1 Page 2 Peak Performer 1 Users Manual H2 venting H2 shut off valving and H2 supply safety equipment must be supplied by customer Glossary and Terms FID Methanizer HSD Molecular Sieve Unibeads Gas Purity Span Gas Response Factor Name PkCen LW RW PkWin PkHgt Fit Page 3 Flame lonization Detector Ruthenium Oxide Catalyst HayeSep D column packing material Zeolite column packing material Silica column packing material Amount of undesired elements in a gas supply Gas supply with known certified amounts of specific compounds Proportionality factor between area count units and concentration units Peak identification tag Expected peak retention time in seconds Typical time span measured from the start of the peak s baseline rise to the peak apex PkCen in seconds Typical time span measured from the peak s apex PkCen to the end of the peak s baseline decline in seconds Total tolerance window in seconds for assignment of a Name to a quantified chromatographic
68. of CO as the RCP applications provide chemical specificity for CO measurement Low Level Linearity Measured Concentration as a Function of Blended Concentration Single Mode 100 90 80 Flame lonization 70 60 50 40 30 20 10 Measured Concentration ppb 0 10 20 30 40 50 60 70 80 90 100 Blended Concentration ppb Page 86 Peak Performer 1 Users Manual Figure 71 FID Linearity lt 100 ppb CO CH4 CO2 and NMHC Dynamic Range Measured Concentration as a Function of Blended Concentration Single Mode 20000 18000 Flame lonization Detector 16000 14000 A 12000 10000 5 CO 8000 6000 E CH4 4000 A CO2 B NMHC Measured Concentration ppb O 2000 4000 6000 8000 1000 1200 1400 1600 1800 2000 0 0 0 0 0 0 Blended Concentration ppb Figure 72 FID Response Curve Showing Linear Range 8 3 Detector Flow Rate Effects Carrier gas flow rate through the FID does not influence the rate of CH ionization However the detector response can be influenced by the relative amounts fuel combustion oxygen and inert carrier gas present FID Response With Varying H2 Flow FID Air 200 sccm amp Carrier 55 sccm 140 0 14 0 120 0 ahs 12 0 ee CO2 T 100 0 a Signal to Noise 10 0 2 a ae O X E 80 0 80 Z o o Q
69. only and will need to be saved to permanent memory at a later time Repeat the sequence for each of the compounds shown on the CALIBRATION DATA BASE screen Repeat analysis of the span gas sample and verify that the analyzer reports data values within normal calibration tolerances i e 5 4 4 Analysis Database Screen The Analysis Database screen stores critical information regarding peak identification and quantification parameters Page 36 Peak Performer 1 Users Manual Figure 22 Analysis Database Screen 4 4 1 Analysis Database Parameters Name The peak identification tag expressed as 5 alphanumeric characters A Z 0 9 PkCen The normally expected peak retention time in seconds used for assigning the appropriate Name LW The typical time span measured from the start of the peak s baseline rise to the peak apex PkCen in seconds Minimum value is 3 maximum is 35 RW The typical time span measured from the peak s apex PkCen to the end of the peak s baseline decline in seconds Minimum value is 3 maximum is 35 PkWin Total tolerance window in seconds for assignment of a Name to a quantified chromatographic peak The tolerance window is centered upon the PkCen value PkHgt A variable for establishing the cross over point in peak detection modes Chromatographic peaks higher than this parameter will be quantified using the Variable mode heights peaks with h
70. or more than a few days consider column conditioning as described in Section 3 2 18 Press the PAGE command 4 times to reach the RUN SCREEN 19 Press the MANUAL command once 20 Press the IGNITE command once wait 30 seconds and press the IGNITE command again 21 Press the ESC command once 22 Press the PAGE command once 23 Verify that the FID FLAME MEAS reading is greater than the FID FLAME SET reading if not repeat steps 18 through 22 24 Press the PAGE command 4 times to reach the RUN SCREEN 25 If automatic sample cycles are desired press the SINGLE command once to change the setting to CYCLE 26 To initiate sampling press the RUN command once The FID bias voltage will be energized automatically and the P1 event program will be automatically loaded and run NOTE To display concentration data only press the upper right corner of the RUN screen once this will hide the chromatogram and display data in large text format To reveal the chromatogram again press the upper right corner of the RUN screen again 2 To halt sampling press the IDLE command once 3 2 Column Conditioning Conditions warranting column reconditioning are a Start up after storage shipment b Reduced detector response c Unstable baseline d Merging of peaks Normal column operating temperatures are 45 to 90 C The maximum PP1 FID column operat
71. ould be 30 to 120 cc min Press the ESC or PAGE keys as needed to navigate to the RUN screen Press the SINGLE CYCLE RERUN key to toggle to SINGLE mode Press the RUN key to initiate analysis the P1 event program will be loaded automatically and executed Allow the analyzer to fully execute the event program Current concentration data will be displayed as an overlay on the RUN screen as peaks are identified and quantified Press the PAGE key as needed to toggle to the CALIBRATION DATA BASE screen Place the at the first compound of interest and press the EDIT key use the up down left and right arrow keys to enter the span gas concentration in the CONC field Be certain to use the right arrow key to fully exit the CONC field or all updates will be lost With the before the compound name press the UPDATE key The analyzer will recalculate the appropriate response factor for the compound based upon the span gas concentration and analyzer area response using the following formula RESPONSE FACTOR AREA RESPONSE SPAN GAS CONCENTRATION NOTE The LED on the analyzer s front panel will change from green to red to remind the user that the current calibration information is stored in volatile temporary memory only and will need to be saved to permanent memory at a later time Repeat the sequence for each of the compounds shown on the CALIBRATION DATA BASE screen Repeat analysis of the span gas sample and ver
72. ower Keep all other flows as normally specified b Increase the Methanizer temperature to 350 C for 8 to 16 hours to thoroughly heat the FID Tower and drive out trapped moisture c After 8 to 16 hours restore the Methanizer temperature to 295 C restore FID H2 flow and re ignite the flame On occasion moisture can also become trapped under the FID Tower Cap at the O ring seal This moisture can be eliminated by simply removing and restoring the FID Tower Cap the act of removal shifts the O ring enough that the moisture is ejected To perform this action d Reduce only the FID H2 pressure to zero to eliminate the FID Flame this eliminates the source of moisture within the FID Tower Keep all other flows as normally specified e Remove the analyzer top cover f Remove the single retaining screw on the top of the FID Oven Cover g Gently pull back any insulation that covers the top of the FID Tower h Remove the hexagonal standoff that retains the FID Tower Cap i Using a pair of pliers the cap is roughly 100 C gently rock and lift the FID Tower Cap approximately 72 until it is completely clear to the FID Tower top surface Page 89 Peak Performer 1 Users Manual j Replace the FID Tower Cap on the FID Tower and rock gently the cap down into position k Reinstall the hexagonal standoff I Replace any insulation m Reinstall the FID Oven Cover Vacuum any loose insulation shreds from the instrumen
73. peak s apex PkCen to the end of the peak s baseline decline in seconds Minimum value is 3 maximum is 35 PkWin Total tolerance window in seconds for assignment of a Name to a quantified chromatographic peak The tolerance window is centered upon the PkCen value NOTE The peak top detection algorithm processes only the data within this window PkHgt A variable for establishing the cross over point in peak detection modes Chromatographic peaks higher than this parameter will be quantified using the Variable mode heights peaks with height less than or equal to PkHgt will be quantified using the ForceB mode JJ Fit The convolution filter value expressing the overall peak shape Flt 2 is recommended for sharp narrow peaks such as H2 and Fit 8 is recommended for broad peaks such as CO For good peak quantification it is important to consistently determine when the peak begins the positive increase in detector signal when the signal maximum occurs and when the peak ends the return to stable detector signal PkCen LW and RW are used to establish starting and ending points for mathematical analysis of the baseline Page 74 Peak Performer 1 Users Manual All modes of peak are calculation require locating the peak top usually the point of maximum peak signal In cases where the detector signal is strong locating the peak maximum value is straightforward Often the concentratio
74. peak The tolerance window is centered upon the PkCen value Variable for establishing the cross over point in peak detection modes Chromatographic peaks higher than this parameter will be quantified using the Variable mode heights peaks with height less than or equal to PkHgt will be quantified using the ForceB mode Convolution filter value expressing the overall peak shape Fit 2 is recommended for sharp narrow peaks such as H2 and Fit 8 is recommended for broad peaks such as CO Peak Performer 1 Users Manual Table of Contents 2 5 9 1 2 5 6 IN _ RROWNND _ _ _ AARAAAA ee ee ee MA o_o AAR Nean A D NO N AAR NN NR Page 4 Introduction Installation Considerations Unpacking Instructions General Considerations Electrical Connections Rack Mount Specifications Gas Supplies and Connections Carrier Gas Supply Carrier Gas Purity Carrier Gas Purity Requirements Carrier Gas Connection FID Hydrogen Gas Supply FID Hydrogen Gas Generators FID Hydrogen Gas Cylinders FID Zero Air Gas Supply Actuator Gas Supply Sample Supply Second Sample Supply Span Gas Supply Standard Start up Procedure Quick Start Sequence Column Conditioning Detector Conditioning Igniting the FID Flame Sample Analysis Calibration Establishing New Instrument Response Factors Shutdown and Transport Peak Performer 1 Operator Interface Set up Screen Set up Scre
75. r Section All error conditions are enunciated by a RED color on front panel LED and a shift in the ERROR FLAG parameter transmitted through the COM1 and COM2 output ports see Section 6 1 for additional details Figure 14 Set up Screen Displaying an Error Message There are ten individual error conditions that can cause the status LED on the front panel to glow red Detector Communication Error Temperature Zone Out of Range Temperature Zone Disabled Detector Zeroing Target Error Viamp Low Voltage Out of Range RCP Analyzers Only FID Flame Temperature Out of Range FID Analyzers Only Event Program Load Error Stream Selector Program Error Page 29 Peak Performer 1 Users Manual e System Parameters Corrupted e Parameter Change Update Needed 4 1 4 2 Clearing Error Messages and on the Set up Screen Lower Section N bo z LHi hes 2 DateTime Fort Pretocol For t Fa Pr ii to ji r T l l SS See ee ee Lil lum Hoe Methanizer Column FID Flame Sut ti ELLJELEE am Ti de Figure 15 Typical FID Flame Out Error Message All error messages except PARAMETER UPDATE can be cleared at any time by pressing the ACCEPT button However if the error condition continues to exist the error message may re appear Accept Allows the user to acknowledge and clear error messages Te Moves the cursor upwards La Moves the cursor downwards Page Advances the user
76. re carrier gas impurities are reduced to less than 10 ppt by this type of purifier Typical Heated Metallic Getter Purifier Specifications Heated Reactive Metal Getter Maximum Flowrate gt 300 cc min lt 5 L min Gases Purified No Ar He alternative THC Concentration outlet lt 10 ppt CO CO Concentration outlet sr Pet H2 H2O Concentration outlet ANPP Expected Life Consult Manufacturer Page 13 Peak Performer 1 Users Manual 2 5 1 2 Carrier Gas Purity Requirements Nitrogen Carrier Argon or ales ppt or 60 psig 150 sccm eiom contaminants UHP Grade lt 10 ppb THC oome yoon 1em 2Ps Combustion Medical Grade Air lt 10 ppm CH4 20 psig 200 sccm Clean Dry Air lt 10 ppm Actuator orbe icr 70 psig 80 sccm Heated reactive metal getters are the only proven reliable technique for generating the specified carrier gas purification Cold metallic getters and absorption getters do not reliably remove all common critical bulk gas contaminants 2 5 1 3 Carrier Gas Connection The PP1 carrier gas connection utilizes a 1 16 female VICI bulkhead labeled CARRIER IN on the front or rear panel 1 Connect purified N2 carrier gas supply gas Ar He alternative to the carrier bulkhead and set the source regulator to approximately 60 psig 2 There are no internal regulators in the standard FID PP1 all gas pressures are controlled by external regulators customer supplied 3 Verify the
77. re zone and 325C for the Methanizer temperature zone To achieve maximum analyzer performance when measuring O2 samples Peak Labs recommends continuous O2 sample cycling to minimize surface carbon reactions Page 83 Peak Performer 1 Users Manual CAUTION Do not begin detector heating without carrier gas flow Damage to the detector may result CAUTION The maximum Column temperature is 200 C CAUTION The normal FID operating temperatures is 295 C Maximum temperature is 350 C The FID detector does not normally require conditioning treatment however it does require 8 to 12 hours at normal operating temperature before flame ignition to achieve optimum stable performance Normal detector operating temperature for the FID is 295 C although operating temperatures vary with the specific application The table below illustrates some typical compounds and detection capabilities of the FID 8 1 Flame lonization Detector Principles Carrier gas containing the compounds from the column passes directly into mixing tee where H2 for combustion and methanization is added At the heated flame tip with the FID tower this gas stream is bathed in a cylindrical flow of combustion air and the H2 O2 flame is ignited Within this flame the following general reactions occur reactions are left unbalanced for simplicity Page 84 Peak Performer 1 Users Manual H O gt H2O Heat and CH O Heat
78. roved baseline stability at the CO2 peak retention time Each of these chromatographic changes will directly enhance the lower detection limit of the analyzer by making it easier to clearly define peak start end points and peak magnitiude These chromatographic improvements occur as the free carbon on the internal surfaces of the analyzer system is consumed Many of the sources i e polymeric valve seals do not become carbon free over time however the available surface carbon can become greatly diminished with continuous exposure to O2 Free carbon may reside within the main body of materials in the system and diffusion forces may bring this carbon load to the surface again during idle analyzer times Consequently it is not unusual to see these instabilities reappear in a previously clean system after extended periods of inactivity The new free carbon can again be diminished by continuous exposure to O2 CAUTION Under certain circumstances the reduction of the analyzer surface carbon may be accelerated with above normal operating temperatures Page 82 Peak Performer 1 Users Manual and continuous exposure to O2 As a general rule O2 conditioning temperatures are much lower than standard conditioning temperatures the high reactivity of pure O2 with polymers at elevated temperatures can easily destroy the valve seals and column packing materials If O2 is being sampled do not exceed 100C for the FID s Column temperatu
79. s via USB 1 Connect DB9M to DB9F extension cables to analyzers 2 Power up analyzers do not heat Page 110 Peak Performer 1 Users Manual 3 Set Port 1 Protocol on the analyzers to Viewer 4 Insert 4 port USB hub into computer USB port your computer should detect the connection and automatically install any required Windows drivers for USB hubs 5 Connect the USB to DBY adapters to the DBY extension cables 6 Insert first USB to DB9 adapter into 4 port USB hub your computer should detect the connection and launch the hardware installation program 7 Insert USB to DB9 adapter INSTALL CD in CD drive it will launch automatically if autoplay in enabled on your computer 8 Follow installation instructions that come with USB to DB9 adapter I confirm that it is okay to click the Continue anyway box 9 Your computer may prompt to install the USB to DB9 adapter a second time do not cancel it is best to let the computer re install the software again 10 Create a new Desktop folder for each analyzer that you will connect with a USB to DB9 adapter Be sure to give the folders a name that relates to the analyzer that you will connect to that adapter 11 Copy the Viewer exe files into each new folder Open one of the new folders and select the Viewer exe file 12 Double click to launch a Viewer window 13 Go to Windows Device Manager Settings gt Control Panel gt System gt Hardware gt Device Manager to see
80. shows the viewer screen without the RED DOT This signifies the communication connection between the PC and the PP1 is function correctly Page 48 Peak Performer 1 Users Manual i Viewer Yer 3 12 f el Fed File Start Stop Chrom View Event Info Pun Time Streams Figure 34 Viewer main window showing no Communications Error 5 6 1 File Menu on the Viewer Taskbar rt Viewer Yer 3 12 7 loj File Start Stop Chrom View Event Info Port Settings Print Exit Figure 35 File Menu on the taskbar Page 49 Peak Performer 1 Users Manual The File menu contains the following commands eT se Opens a CSV file that was created by the Viewer software Use this command to open a CSV file to view the concentration data Opens serial communication settings window for setting RS 232 configurations between the Host PC and the PP1 As shown in figure 31 Print Prints all concentration data of selected CSV file Exit Exit Viewer application Once the CSV file is opened the Viewer window automatically updates and shows concentration data Figure 36 is an example with five consecutive runs The run of concentration data at 14 06 is displayed in RED to denote that there was a general error in the PP1 during this run The error was cleared before the end of the run at 14 24 Port Settings i Viewer 2008 11 13 0 x File Start Stop Chrom View Event Info Run Time Stream CO CH
81. sion cable DB9M to DB9F wired straight through 10 feet Optional USB 4 port self powered Hub Inland 08302 or equivalent 5 2 Installing the Viewer Software 1 Place Viewer software CD ROM disk into CD ROM drive 2 If Autorun is enabled follow the installation screen prompts 3 If the CD ROM does not automatically launch select SETUP from CD ROM disk 4 The installation software will auto install the Viewer in a folder under the PC s main drive as the default The user has options from the installation process to create a new folder and install in a new location 5 3 Starting the Viewer Software 1 Double click the Viewer icon on the Desktop or 1 Select START button on the bottom Taskbar 2 Select PROGRAMS select VIEWER and double click to launch move to Viewer 5 4 Communication Settings Window The Communication Settings window is shown in figure 21 This screen displays the serial communication settings used by the PC to communicate to the PP1 Page 46 Peak Performer 1 Users Manual The baud rate data bits and stop bits settings should match all of the settings in figure 16 baud rate 38400 data bit 8 stop bit 1 The COM port number must match the COM port designated by the PC s terminal The COM Port number is determined by which COM port the serial cable is plugged into on the PC not the PP1 Clicking the OK button will configure the COM port to the correct
82. so there is some value stored in memory It will not be displayed on the analyzer database if the Peak Center value is zero 30 Force the PeakHost program to upload the peak analysis database into the analyzer under the Analysis DB window select File then Send to Analyzer 31 The analyzer may display a red light after this action 32 If the analyzer displays a red light on the front panel the parameters must be accepted and saved on board the analyzer before proceeding any further a Press PAGE touchpad until MAIN SCREEN appears has SN and temperature zone controls d Press the DOWN arrow until you reach the Parameter Change Update Needed line e Press the ACCEPT touchpad button then the SAVE touchpad button permanently save the temperature parameters in analyzer memory Install the Event Programs 33 Force the PeakHost program to obtain fresh analyzer information under the PeakHost program main screen toolbar select Event then under File select Receive From Analyzer 34 Verify the correctness of the P1 event program parameters compared to the original values If errors are noted input the previously saved P1 event program into the editor window 35 Make sure the P1 radio button under File is selected 36 Force the PeakHost program to upload the event program into the analyzer under the Event Editor window select File then Send to Analyzer
83. ssurized and flowing through the FID 17 Do not pressurize the FID H2 and FID Air at this time 18 Turn on analyzer heaters 19 Adjust Methanizer heater zone to 395C 20 Allow the analyzer to heat to 395C for 4 to 12 hours 21 Pressurize the FID H2 to 25 psig and FID Air to 20 psig 22 Allow the analyzer to stabilize for 2 to 4 hours 23 Lower the Methanizer temperature setpoint to 295C 24 Allow the analyzer to stabilize for 30 minutes 25 Ignite the flame 26 Recalibration is recommended after Methanizer replacement Page 95 Peak Performer 1 Users Manual Figure 78 View of the MCPU Showing the LCD Contrast Potentiometer Page 96 Peak Performer 1 Users Manual 9 6 ALTERING THE ANALYTICAL RANGE OF THE INSTRUMENT Sample loops are very easy to customize 1 Determine the desired loop volume Analytical range is directly proportional to sample loop size 2 Select tubing tube internal diameter to use In general use the largest ID tube possible to avoid flow restrictions Guidelines 0 040 ID for 3 8 cc to 2 cc loops 0 030 ID for 3 16 cc to 1 2 cc loops 0 020 ID for 50 uL to 1 4 cc loops Note the shortest practical length of tubing for a sample loop is about 8 inches Note Do not use tubing less than 0 016 ID as it acts like a flow restrictor instead of a sample loop 3 The correct length for the loop tubing is calculated as follows Internal volume V in cc s 3 142 x ID 2 in inches x L in
84. t n Reinstall the analyzer s top cover Page 90 Peak Performer 1 Users Manual 9 0 Analyzer and FID Maintenance and Service Procedures Figure 76 Chassis Overview PEAK PERFORMER 1 FID COMPONENT LAYOUT MCPU PCB ASSEMBLY P N 604 002 FID CONTROLLER PCB ASSEMBLY and COVER n a FID ASSEMBLY P N 614 101 VALVE 1 10 port VALVE 2 4 port COLUMN OVEN and COVER FLOW CONTROL NEEDLE VALVE ASSEMBLY FID H2 INLET 10 FID AIR INLET 11 LCD TOUCHSCREEN ASSEMBLY P N 604 013 12 REAR PANEL PCB ASSEMBLY INCLUDES MAIN DC POWER SUPPLY P N 604 001 OONAORWN Page 91 Peak Performer 1 Users Manual 9 1 Peak Performer 1 System Block Diagram Detector Module TOCO nov cVGOEeE C R E N Figure 77 PP1 Functional Block and Interconnect Diagram Page 92 Peak Performer 1 Users Manual 9 2 Monitor Regulator Pressures Carrier supply settings should not vary Carrier and Actuator Air settings may shift when supply cylinders run low due to regulator creep and should be checked periodically to maintain consistent gas flows and peak retention times Varying carrier pressures can cause peaks to shift out of set retention times and not be flagged properly Critical operating parameters are listed on the top page of the Final Test Data shipped with the analyzer Peak Labs recommends the user create a logbook of critical parameters on a routine basis as an aid to troubleshooting S
85. t screen 4 7 Run Chromatogram Screen The Run Chromatogram screen is provides the real time display and data processing of sample analysis The screen displays the running chromatogram peak markers and concentration data The information displayed on this screen is useful for evaluating instrument health event program validity and analytical stability Manual Sindle Pade Figure 26 Run Chromatogram screen in the Idle state and the mode displayed upon initial power up Page 41 Peak Performer 1 Users Manual Single Wort LE 127 H Figure 28 Run screen in Idle mode at end of run 4 7 1 Run Screen Button Functions Run Loads a standard event program and runs an analysis in the mode selected Idle Stops the analysis immediately Manual Opens the Manual Run Screen Disp Opens the Display Screen Single Toggle Starting a run in the Single mode Page 42 Peak Performer 1 Users Manual will command the PP1 to run one time and return to the idle mode Cycle Toggle Starting a run in the Cycle mode shall configure the PP1 to run continuously until the Idle key is pressed ReRun Toggle Starting a run in the ReRun mode shall recompute the area and concentration based on the parameters in the analysis data base Stream Toggle Starting a run in the Stream mode will configure the PP1 to initiate the Stream Selector Sequence until the Idle key is pressed Page Advances the user to the n
86. tification Page 63 Peak Performer 1 Users Manual 93 HAYESEP D 02 BYPASS OUT FRONT PANEL VVV CARRIER IN REAR PANEL R2 FPR1 INTERNAL EXTERNAL GETTER PURIFIER T1 q4 X1 AUX1 REAR PANEL ND I FPR2 INTERNAL EXTERNAL Le of TO PILOT VALVE MANIFOLD VALVE 2 1 TO FID DETECTOR R3 NV2 SAMPLE OUT REAR PANEL INTERNAL EXTERNAL __ _ INTERNAL EXTERNAL SAMPLE LOOP SAMPLE OUT FRONT PANEL VALVE 1 SAMPLE IN REAR PANEL SAMPLE IN FRONT PANEL Figure 44 Typical FID plumbing diagram Immediately after injection the entire contents of the sample loop are moved to the head of the column s and component separation begins ae Figure 45 Peak Development on the Analytical Column Soon After Injection Page 64 Peak Performer 1 Users Manual Figure 46 Peak Development Midway on the Analytical Column Figure 47 Peak Development Midway on the Analytical Column Analytes of interest can be allowed to continue on to the detector as long as desired In some cases the resulting chromatogram can become quite long in duration In other circumstances it is not necessary to quantify all possible peaks and the remaining balance of the sample is backflushed to vent or detector Page 65 Peak Performer 1 Users Manual Figure 48 Peak Development on the Analytical Column After Backflush Fi
87. to launch Viewer exe you might get a COM port error message window simply click OK and proceed 28 Go to Windows Device Manager gt Settings gt Control Panel gt System gt Hardware gt Device Manager to see what the additional port assignment on your computer is 29 In the Device Manager click on Ports to expand heading so you can see what COM port number your computer gave to the second USB to DB9 adapter it will be displayed directly under the note for the first USB to DB9 adapter Page 111 Peak Performer 1 Users Manual 30 Note which COM port number is now assigned to the second USB to Serial RS232 Port adapter it s COM5 on most computers 31 Go back to the Viewer window 32 Under File on toolbar select Port Settings 33 Enter COM number assigned to second USB to DB9 adapter probably COM5 check that Baud Rate 38400 Data Bits 8 Stop Bits 1 34 Click OK box to save these settings 35 Communications settings for that USB to DB9 adapter will be saved in the folder and will be used automatically every time you launch the Viewer software in that folder 36 Viewer should automatically connect to the other analyzer At this point you should have two PeakHost windows open connected to the different analyzers If you run the analyzers the chromatographic data for each analyzer will be automatically stored in the folder that matches where the Viewer exe file is stored Pag
88. to the next screen 4 1 4 2 1 Set up Screen Lower Section Button Functions The PARAMETER CHANGE UPDATE NEEDED error message can only be cleared when the analyzer is not performing an analysis i e is in IDLE mode The parameter update action forces a complete re write of permanent memory and is irreversible Peak Labs recommends reviewing all parameter screens before performing a parameter update Once in Idle mode the Main Set up screen appears as Figure 13 Page 30 Peak Performer 1 Users Manual Methanizer Column FID Flame FID Wout Parameter Change Update Needed Figure 16 Parameter Change Error Message Accept Allows the user to initiate permanent updates to non volatile memory a Moves the cursor upwards iz Moves the cursor downwards Page Advances the user to the next screen Port f ei Port 2 Protoca Methanizer Column FID Flame FIIN Wo at e Po PIL pit Figure 17 Parameter Change Prompt Page 31 Peak Performer 1 Users Manual Save Allows the user to make changes to permanent non volatile memory Esc Aborts updates to non volatile memory 4 2 Analog Interface Trend and Recorder Output Screen The compound or Channel information for the ANALOG INTERFACE screen is automatically populated using the information from the ANALYSIS DATABASE screen If no compound name is present in the ANALYSIS DATABASE for the 4th compound Channel 4 is dedicated for
89. uggested parameters for frequent logging are Analyzer S N Date and Time Carrier Gas Type Carrier Gas Supply Pressure Carrier Gas Flow at Front Panel Bypass Out Port Carrier Gas Flow at NV1 Outlet V1 CCW Carrier Gas Flow at NV2 Outlet V1 CCW FID H2 Gas Supply Pressure FID Air Gas Supply Pressure Actuator Gas Supply Pressure Sample Gas Type Sample Gas Flow at Rear Panel Sample Out Port Column Setpoint and Measured Temperature Detector Setpoint and Measured Temperature FID Vout Signal after Zeroing FID Flame Reading Rfactor for compounds 1 2 3 amp 4 from Calibration Database screen PkCen for compounds 1 2 3 amp 4 from Analysis Database screen Other critical parameters that should be verified occasionally Actuator Gas Type Port 1 Protocol Setting Port 2 Protocol Setting Calibration Database Screen Parameters all Analog Interface Screen Parameters all Analysis Database Screen Parameters all Event Program Editor Screen Parameters for all active Event Programs Page 93 Peak Performer 1 Users Manual 9 3 Verifying Valve Integrity Carrier Blank Zero Gas In addition to periodic calibration checks the integrity of the rotary valve seal must be tested Determination of valve seal quality is performed by analyzing known purified gas as a sample 1 Connect the front panel SAMPLE IN port to the front panel BYPASS OUT port This will begin flow of purified gas through t
90. y Documents pE ar My Computer File name Open C Seite Files of type Hex Files HE Cancel Places Open as read only Figure 81 Selecting the Analyzer Software file 18 Mouse click select the latest HEX file e g MCPU1 99 HEX then mouse click on the Open tab on the right side of the window Uploading will begin immediately do not interrupt or cut power to the host computer or analyzer as all operating parameters could become corrupt if this operation is not completed 19 When software updating is complete the Programming Complete message will appear in the lower left corner window of the PeakHost main screen and the analyzer will perform a full re boot 20 Power down analyzer but leave the PeakHost wondow open on the computer Verification of Successful MCPU Software Upload 21 Power up analyzer chassis Do not re energize the heaters at this time 22 Force the PeakHost program to obtain fresh analyzer information under the PeakHost program main screen toolbar select File then Receive From Analyzer 23 Verify the correctness of the temperature control parameters compared to the original values If errors are noted overwrite each Setpoint Pvalue Value and Limit parameter including any zero values recorded for all zones 24 Force an analyzer update of the temperature control parameters by mouse clicking on the large SEND box directly below the Limit label The ana
91. ydrogen are not significantly affected by changes in column temperature as interaction with column packing is minimal Page 70 Peak Performer 1 Users Manual Name Conc Area R Time R Factor A Type H2 413 5 1319343 49 2 3191 V co 343 2 4558519 90 2 13283 V 16 5 Uni 15 81 MS13X PEAK Column Temperature 135 C Carrier Flow 20 5 mi min N2 OFFSET ATT 435 SPAN ET pil Den f Sena i D zh Figure 56 Effect of 30C Increase in Column Temperature Column flow rate changes can directly affect peak retention times as peaks are pushed down the column faster or slower Comparison of Figure 57 with Figure 55 shows the decreased peak retention times ee Name Conc Area R Time R Factor A Type H2 136 6 436425 32 4 3191 W CO 201 5 2675877 ry 13283 W 16 5 Uni 15 81 M513X PEK Column Temperature 105 C Carrier Flow 41 2 mifmin N2 He 4 Figure 57 Effect of 2X Increase in Column Flow Rate Page 71 Peak Performer 1 Users Manual 7 6 Peak Identification and Quantification A typical chromatographic peak is generated by the detector s electronic signal as a function of time Vout 2000000 Vout 45000 Time Figure 58 Typical Chromatographic Detector Signal Showing a Peak Chromatographic peaks in the PP1 are measured by establishment of the normal stable detector signal then determining the added electronic signal that was created by the peak p

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