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Peak Performer 1 TCD User Manual

1. Analysis Database Screen Parameters all Event Program Editor Screen Parameters for all active Event Programs Page 83 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 the 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 84 Peak Performer 1 Users Manual Page 85 Peak Performer 1 Users Manual Page 86 Peak Performer 1 Users Manual Page 87 Peak Performer 1 Users Manual 9 9 Adjusting the LCD Contrast Figure 79 View of the MCPU Showing the LCD Contrast Potentiometer Page 88 Peak Performer 1 Users Manual 9 10 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 loo
2. 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 PP1 COM2 Be el Master Controller PP4 COM2 RS232 to RS485 E Converter i a Power tid Power Supply Figure 43 System configuration 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 58 Peak Performer 1 Users Manual 7 0 Chromatographic Principles As an analytical system the PP1 RCP performs five 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 RCP analysis methods use stainless steel 1 cc sample loops An on column injection adapter is available from Peak Labs if smaller sample volumes are required using standard micro volume or Luer type syringes 7 2 Carrier Gas Purification Chromatographic instrument detection limit is directly related to carrier gas pu
3. Starting the Viewer Software Communications Settings 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 Menu 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 PP1 Port 2 Protocol Chromatographic Principles Sample Injection Carrier Gas Purification Page 6 Peak Performer 1 Users Manual Component Separation Flow Balancing Venting Back flushing Effects of Temperature and Flow on Analytical Columns Peak Identification and Quantification Peak Quantification Fixed Mode Peak Quantification Forced Baseline Mode Peak Quantification Variable Mode Chromatographic Stabilization of the Analyzer When injecting O2 Samples Thermal Conductivity Detector Analyzer and Maintenance and Service Procedures Peak Performer 1 System Block Diagram Monitor Regulator Pressures Verifying Valve Inte
4. ake Pa a m Peak Time Sec 43 2 Lett Width sec 5 2 14 8 270534 5320 Right Width sec 3 0 Measured Area 33084 Response Factor 310 BIA Width Analysis Variable Variable Cycle Flame Temperature 135534 0 T J mg I ci J Ho oo iT T a Es T of 5 DJ Ja System Alarm OK Figure 37 Viewer Detail screen showing raw analysis data The information on the screen is linked to run 13 35 displayed in figure 36 Page 48 Peak Performer 1 Users Manual 5 6 2 Start Menu on the Viewer Taskbar ii Viewer Yer 1 8 O x File Stark Stop Chrom view Run Single Run Cycle Run Stream Run Figure 38 Start menu on the taskbar The Start menu contains the following commands Function enero O 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 49 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
5. 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 evaluated The final value is represented by point 5 when the change in peak area became less than 0 5 Page 75 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 ag w Oo 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 a
6. 1 0 Se phe 4 p a fr Ne Mm a On i SV yh E Jf 8 Vi my Xx 6 Nv2 CW Toa ee SAMPLE j f LOOP jag 2 SH SS ee VALVE 1 Figure 44 Standard RCP 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 Page 61 Peak Performer 1 Users Manual Figure 45 Peak Development on the Analytical Column Soon After Injection Figure 46 i eE Ae BE OQ IA 200 Or oe ORLOX ID ou LC sont X wO LOE OE ED ORLOQY KIC O x 4 i VA SOS oe TSE a Peak Development Midway on the Analytical Column y Me ee o OR IA QOD ROD 2052 TO SOS STO EOC pon lge Olge Og ext QRWN x ase ses SR SIST fd Figure 47 Peak Development Midway on the Analytical Column Page 62 Peak Performer 1 Users Manual 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 Figure 48 Peak Development on the Analytical Column After Backflush Figure 49 The Completed Chromatogram 7 4 Flow Venting and Balancing Several problems can arise
7. 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 YG 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 The 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 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 Page 55 Peak Performer 1 Users Manual 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 requ
8. A AB Diaphragm 0 365 Pressure Transducer Pilot Valve Interface FID Flame Interface Carrier Pressure 000 Pv1 Pv3 Pys O Pv Pw4 PVE TT Flame Out Flame Set Pt Set Point 0 P alle 0 Value 0 Limit Figure 81 Peak Host Main Window with Upload Command Visible 17 Double click the Upload button The standard Windows Open window will pop up Page 92 Peak Performer 1 Users Manual open lt i _OC s C S Look ir G Peak Host 1 71 do ft pi Ei My Recent Documents Deskto p gt fi My Documents ar My Computer k File name A Wiener Files of type Hex Files HEX Cancel we Open as read only Figure 82 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 Verificati
9. 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 27 Double click 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 DB9Y adapter it will be displayed directly under the note for the first USB to DB9 adapter 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 Page 103 Peak Performer 1 Users Manual 32 Under File on toolbar select Port Settings 33 Enter COM number as
10. collection of the chromatogram data The software also provides the ability to display and print the data from a 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 5 2 5 3 5 4 System Requirements 1 2 GHz 20 GB 256 Mb RAM 1 USB port Windows XP or Windows Vista USB to DB9 RS232 Adapter SIIG US2308 JU CB1 12 or equivalent DB9 Extension cable DB9M to DB9F wired straight through 10 feet Optional USB 4 port self powered Hub Inland 08302 or equivalent 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 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 Communication Settings Window The Communication Settings window is shown in figure
11. 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 third run of concentration data at 13 32 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 next run at 13 35 Port Port Settings i Viewer 2003 12 22 E 5 xj File Start Stop chrom view Run Time Stream H2 CO 13 26 0 43 0 54 4 13 29 0 37 3 52 1 13 32 1 46 2 49 5 13 35 1 36 4 50 9 13 38 1 38 9 52 1 Figure 36 Viewer screen showing concentration data There are ten individual error conditions that can cause the Viewer Line to appear red e Detector Communication Error e Temperature Zone Out of Range e Temperature Zone Disabled Page 47 Peak Performer 1 Users Manual 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 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 Q Viewer Details 2003 12 22 13 35 x Print Hame
12. 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 orser a aren a span 70 Cone Poly i eg i SE i 3j e bitte R Ottse dd h Figure 51 Properly Flow Balanced Baseline Page 64 Peak Performer 1 Users Manual oreser a arren a span 70 aoe al F yi 4 a X epee 3 IF pee co coe Oe e AF osa TRS ziki _ al lvl OFFSET atten ca i zis Cons Paty b daft 4 8 X y i H ze AE g W c Figure 53 Low FID flow from NV1 note drop after the V1 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 65 Peak Performer 1 Users Manual NV2 Flow 59 sccm CH4 RT 93 sec fi 4 NV2 Flow 39 sccm E a CH RT 97sec mh CH4 RT 102 sec
13. 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 87 Figure 87 Main DC Power Supply Fully Removed Page 98 Peak Performer 1 Users Manual 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 88 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 Install the new DC Power Supply by reversing the disassembly sequence 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 99 Peak Performer 1 Users Manual 9 14 Adjusting the 5 Volt DC Supply Adjust this potenkbomeler so that the vallage between the RED and ee BLACK wires is 5 1 10 5 2 VOC Figure 89 Adjusting the 5 Volt DC Supply Page 100 Peak Performer 1 Users Manual Page 101 Peak Performer 1 Users Manual 9 16 COM 1 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
14. 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 Suggested parameters for frequent logging are Analyzer S N Date and Time Carrier Gas Type Carrier Gas Supply Pressure Carrier Gas Flow at Hg Scrubber Outlet V1 CW Carrier Gas Flow at Hg Scrubber Outlet V1 CCW 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 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 RCP Vout Signal after zeroing RCP Vlamp 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
15. 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 91 Peak Performer 1 Users Manual 2 Peak Performer Yer 1 71 d Ioj x File Event Chrom view Analysis DB Viewer Touch Screen Upload Temperatures Detector Control Zonei Zone Zone3 Ain D A Value 265 6 105 5 0 0 woes 1727 VSig mV ag E 20666 0 RCP Bias OM FID OO Ignite On Gas Sampling Interface System ID s Analyzer Serial 14 MEPU version 171 Detector version 110 Valve Cycles Valve 1 p94 Valve 2 0 i valve 1 Valve 2 Rotary Operating Hours SEND A N Diaphragm OC 365 Pilot Valve Interface FID Flame Interface Pwi PV TT PVS J O Pvz oPV4 TT PVE TT Flame Out Flame Set Pt 0 Set Point 0 P Value 0 Value 0 I Limit Figure 80 Peak Host Main Window Normal Peak Performer Yer 1 71 E lol x Fie Event Chrom View Analysis DB Viewer Touch Screen Upload Temperatures Detector Control Zoned Zone Zone3 Ain DA Value 265 8 1055 0 0 Svd Wer VSig mV 8 20644 0 Repro Besom FD Ignite On Gas Sampling Interface System ID s Analyzer Serial 14 MEPU version 171 Detector Version 110 Valve Cycles Valve 1 5594 valve 2 0 m valve 1 Valve 2 Rotary Operating Hours SEND
16. ppb 0 gt 1250 ppb Page 29 Page 30 Manset Page 4 2 2 Peak Performer 1 Users Manual 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 signal 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 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 w
17. s NV2 Flow 79 sccm 0 20 40 60 80 100 120 140 160 180 200 220 240 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 66 Peak Performer 1 Users Manual Name Conc Area R Time R Factor A Type H2 o 420 3 1341021 48 8 3191 V co 347 5 4616126 106 8 13283 V 16 5 Uni 1S 81 MS13X PEAK Column Temperature 105 C Carrier Flow 20 5 ml min N2 ory atten f 123 span rie Cons Poly eee 4 FE Ee Tm ze H2 A gai z Lamp Volatge 744 1 mV AL oe po _ Analysis Type Figure 54 Standard chromatogram The normal PP1 chromatogram Figure 54 is affected by changes in column temperature as illustrated in comparison with the chromatogram of Figure 55 In the circumstance of column temperature change an increase of 30C has
18. selected on the RUN screen 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 37 Peak Performer 1 Users Manual 4 6 2 Stream Selector Program Editor Screen Button Function 1 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 next 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 38 Peak Performer 1 Users Manual Manual Manual Disk Cycle Pade Figure 28 Run screen in Idle mode at end of run 4 7 1 Run Screen Button Functions Page 39 Run Idle Manual Disp Single Loads a standard event program and r
19. 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 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 its 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 DB9 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
20. 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 95 Peak Performer 1 Users Manual 9 12 Testing the Heater Resistance Figure 84 Heater Resistance for 200 240 VAC AC Service Page 96 Peak Performer 1 Users Manual 9 13 Main DC Power Supply Replacement Purpose Replace upgrade Phihong PSA4531 DC Supply with Power One MAP40 300 DC Power Supply 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 85 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 97 Peak Performer 1 Users Manual oom _ B le P Figure 86 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
21. 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 after the chromatogram data is loaded the display can be adjusted by the Offset Attenuation and Span scroll bars PE Chrom Viewer 2003 12 225 1335 chm eS j File viewer ATTEH 16 SPAH 450 gt 4 H Open Saves Ww Baseline Print Exit co 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 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 Page 50 Peak Performer 1 Users Manual 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 four
22. 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 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 33 Peak Performer 1 Users Manual i 4 Disable WwW Correction Disable 3 T 4 Edit Figure 22 Analysis Database Screen 4 4 1 Analysis Database Parameters Name The peak identification tag expressed as 5 a
23. 31 This screen displays the serial communication settings used by the PC to communicate to the PP1 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 Page 43 Peak Performer 1 Users Manual 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 options and save the settings in a file on the computer Communication Settings EA Com Port a i H E Cancel Baud Rate C 9600 C 19200 f 38400 Data Bits Stop Bits 7 f amp if 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 32 is the minimum cable configuration See Section 6 for details on communications protocols PC MALE PP1 FEMALE 9 Pin Cable from PC to PF1 Figure 32 COM Cable Wiring Page 44 5 6 Peak Performer 1 Users Manual 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 th
24. AMPLE 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 4 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 Itis 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 ka 7 VVV IN KO FLOW LIMITER 20 30 sccm 60 PSIG Figure 8 Span Gas Supply Flow Schematic Page 16 3 0 Peak Performer 1 Users Manual Standard Start up Procedure Peak Labs recommends that the user read the entire operating manual prior to using the Quick Start sequence 3 1 o 0 a ee i 13 14 15 16 17 18 19 20 21 A CAUTION Do not begin detector heating without carrier gas flow Damage to the detector may result Quick Start Sequence Confirm that all gas connections and supplies are properly made Remove the top cover of the instrument Pressurize the carrier gas supply line to 60 to 100 psig Verify that sample is flowing freely through loop exit flow from the rear SAMPLE OUT port should be 20 to 120 cc min Verify BYPASS OUT flow gt 20 cc minute Verify the analyzer is connected to the correct line vol
25. CAUTION Never energize heaters of the instrument unless carrier gas flowing The TCD detector does not normally require conditioning treatment however it does require 20 to 24 hours at normal operating temperature to achieve optimum stable performance Normal detector operating temperature for the RCP is 60 C although operating temperatures may vary with the specific application The table below illustrates some typical compounds and detection capabilities of the TCD on Helium carrier 8 1 Thermal Conductiivty Detection Section under development Page 79 Peak Performer 1 Users Manual Page 80 Peak Performer 1 Users Manual 9 0 Analyzer and Maintenance and Service Procedures gaat ever Figure 75 Chassis Overview PEAK PERFORMER 1 TCD COMPONENT LAYOUT MCPU PCB ASSEMBLY P N 604 002 TCD TCD TCD ASSEMBLY VALVE 1 10 port n a COLUMN OVEN and COVER FLOW CONTROL NEEDLE VALVE ASSEMBLY OONAAARWNA 10 n a 11 LCD TOUCHSCREEN ASSEMBLY P N 604 013 12 REAR PANEL PCB ASSEMBLY INCLUDES MAIN DC POWER SUPPLY P N 604 001 Page 81 Peak Performer 1 Users Manual 9 1 Peak Performer 1 System Block Diagram Detector Module IOCO4H4 S c R E N Chassi Ground Figure 76 PP1 Functional Block and Interconnect Diagram Page 82 Peak Performer 1 Users Manual 9 2 Monitor Regulator Pressures Carrier supply settings should not vary Carrier and Actuator Air settings
26. 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 PP 1 Figure 42 COM Cable Wiring 6 2 Port 1 Protocol On analyzers with Software versions 3 00 and 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 6 2 2 Viewer Output Format Columns Format in CSV files 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 Page 53 Peak Performer 1 Users Manual 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 Ti
27. CTUATOR 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 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 N CONDO OO Ff Page 20 Peak Performer 1 Users Manual Page 21 Peak Performer 1 Users Manual 4 0 Peak Performer Operator Interface SET UP MAIN SCREEN PAGE KEY TREND amp ANALOG OUTPUT PURCHASED OPTION _ SCREEN PAGE KEY 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 tg RUN RUN I DATA SoSH BeTa CHROMATOGRAM anes SCREEN PAGE KEY SET UP MAIN SCREEN Figure 10 Software Menu Structure ANALYZER POWERS UP ON RUN CHROMATOGRAM SCREEN MANUAL CONTROL DISPLAY CONTROL SCREEN SCREEN ESC KEY 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 temperat
28. Peak Performer 1 Users Manual Peak Performer 1 TCD User Manual LABORATORIES Peak Laboratories LLC www peaklaboratories com 650 691 1267 Version 3 0 7 13 09 Page 1 Peak Performer 1 Users Manual Forward 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 Page 2 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 RCP equipped instruments utilize an intense ultraviolet light source Proper eye protection to block 254 nm radiation is required whenever the UV lamp cover is removed 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 RCP equipped instruments utilize small amounts of mercury Hg based compounds and small amounts of mercury may
29. Screen The Manual sub screen allows the operator to invoke all the event program commands on demand Page 40 Peak Performer 1 Users Manual Figure 29 Run Manual screen 4 7 3 1 Manual Screen Button Functions Zero Pressing this key will electronically zero the detector 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 operator to adjust the horizontal scale vertical scale and baseline offset of the chromatogram These functions mimic those of a standard chart recorder Page 41 4 7 4 1 Page 42 Peak Performer 1 Users Manual Figure 30 Run Display screen Display Screen Button Functions V Off VOff Attn Attn Span Esc 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
30. 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 passing 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 69 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 Database Figure 60 Typical PP1 Peak Analysis Database Page 70 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 fo
31. Update Needed Figure 16 Parameter Change Error Message Accept Allows the user to initiate permanent updates to non volatile memory 1 Moves the cursor upwards Moves the cursor downwards Page Advances the user to the next screen Pressing the ACCEPT button alters the screen appearance z005 NOU 17 ocol WUlewer Locals Auto eeraneter Change a Update Needed Figure 17 Parameter Change Prompt Page 28 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 a direct analog signal from the detector for use with a chart recorder or integrator Analog signals generated from this information appear on the rear panel s green DIN terminal blocks See Figure 19 Figure 18 Analog Interface Screen 4 2 1 Analog Interface Screen Button Function i Moves the cursor upwards Moves the cursor downwards Range 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
32. ack to the column outlet after normal operating temperature is achieved After a 5 10 minute detector re equilibration period samples may be run 6 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 Page 18 Peak Performer 1 Users Manual 3 3 Detector Conditioning CAUTION The detector filament operating temperature is preset at the factory The TCD detector does not normally require conditioning treatment however it does require 20 to 24 hours at normal operating temperature to achieve optimum stable performance Normal detector operating temperature for the TCD is 60 C although operating temperatures vary with the specific application 3 4 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 needed 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 peak
33. alytical columns Column materials vary by application and are noted in the Test report documentation Contact Peak Laboratories for additional details specific to your application Page 60 Peak Performer 1 Users Manual 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 analytical column s inside the isothermal column oven see figure 44 and moves over first Stripper column where the separation of the components begins Analytes of interest are allowed to continue onto the second Analytical column and the remaining balance of the sample is backflushed to vent The analytes of interest are further separated on the second column and continue to the detector inlet COLUMN 2 coun HE lt 4 B I TO DETECTOR ST SH E M UN ji J I f a COMBUSTOR FPR1 DETECTOR BYPASS e S z N ANA _ 7 VV ST ap i Ti oi CARRIER INLET K y a pi a Ri i i 5 r FPR2 n CARRIER SAMPLE 1 2 4 a AKA J e Filer
34. ameters 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 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 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 Page 94 Peak Performer 1 Users Manual 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
35. be present in the detector bed and scrubber after use Proper safety protection to block mercury ingestion is required when handling these components 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 result from improper use Peak Performer 1 Users Manual Operators should not attempt to 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 dispose of properly in accordance with local and federal regulations Normal life of the mercury scrubber is 24 months under continuous use Replace and Glossary and Terms TCD RCP HgO Hg Scrubber Molecular Sieve Unibeads HSD Molecular Sieve Unibeads Gas Purity Span Gas Response Factor Name PkCen LW RW PkWin PkHgt Flt Page 3 Thermal Conductivity Detector Reducing Compound Photometer Mercuric Oxide Mercury vapor trap Zeolite column packing material Silica column packing material 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 uni
36. cally 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 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 Save the peak analysis database parameters by using the print function in the Peak Analysis Database window under the toolbar select File then Prin
37. d 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 The PP1 RCP has an internal carrier gas pressure regulator for final gas carrier flow control 1 Connect carrier gas supply gas N2 Ar He or Air to the carrier bulkhead and set the source regulator to 70 100 psig Page 14 Peak Performer 1 Users Manual 2 The internal carrier regulator of the RCP PP1 are pre set at the factory using this external pressure 3 Verify detector flow with a flow meter attached to the mercury scrubber outlet at the rear panel is approximately 20 sccm 4 Verify the BYPASS OUT is flowing approximately 25 sccm Carrier flow exiting the internal combustor is split with a portion of the flow passing through a gas sampling valve another portion of the carrier flow passing through a restrictor tube terminating at the location of the detector inlet and a third portion passing through a restrictor tube terminating at the location of the BYPASS OUT port Under normal operating conditions these ports are 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
38. e rather than the PkCen value Peak signal maximum time value LW Peak signal maximum time value RW Peak start time Peak end time Peak Maximum LW RW Figure 64 Baseline as Established in Forced Baseline Mode Peaks quantified 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 74 Peak Performer 1 Users Manual oc rs S 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 w 2 Q 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
39. e PP1 Verifying the following can solve this connection problem Communication Settings Connection of 9 pin cable between PC and PP1 RS 232 cable plugged into the PP1 s COM 1 port 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 LA 1 8 Mia x File Stark Stop Chrom view Run Time Stream amp Figure 33 Viewer main window showing Communications Error The Viewer window shown in Figure 34 shows the viewer screen without the RED DOT This signifies the communication connection between the PC and the PP1 is function correctly Page 45 Peak Performer 1 Users Manual it Viewer Yer 1 8 T Me X File Starkt Stop Chrom view Run Time Stream 2 Figure 34 Viewer main window showing no Communications Error 5 6 1 File Menu on the Viewer Taskbar Fie Start Stop Chrom view Open Pork Settings Print Exit Figure 35 File Menu on the taskbar Page 46 Peak Performer 1 Users Manual The File menu contains the following commands Hele eae 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
40. 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 ee USB to DB9 e LN OLA Aa gt oooo oooo Figure 91 Multiple Analyzers Connected to a Single Computer For Using Viewer Software Installation of Multiple Analyzers via USB 1 Connect DB9M to DBYF extension cables to analyzers 2 Power up analyzers do not heat 3 Set Port 1 Protocol on the analyzers to Viewer Page 102 Peak Performer 1 Users Manual 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
41. eak Performer 1 Users Manual 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 22 To halt sampling press the IDLE command once 3 2 Column Conditioning conditioning columns AN CAUTION Be sure to put the RCP detector on standby flow before 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 90 to 130 C The maximum PP1 TCD column operating temperatures 195 C A CAUTION Never energize heaters of the instrument unless carrier gas flowing excess of 210 C can destroy column material CAUTION Do not exceed 210 C of column oven temperature Temperatures in 1 Connect the front jumper tube between SAMPLE IN and BYPASS OUT 2 Use the 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 4 After normal operating temperature is achieved the front jumper tube may be reconnected between SAMPLE IN and SAMPLE OUT 5 The detector inlet may be switched b
42. eaned and baked T300 stainless steel tubing Restek P N 21508 G gt IN OUT IN AIR H2 A IN OUT S S 9 9 3 J LEI SAMPLEt ACTUATOR CARRIER IN g E A COM E SPAN IN ANALOG I ANALOG ANALOG 3 ANALOG 4 REC COMMON GND Figure 5 Rear View of PP1 Some Fittings May Not Be Present on Certain Models ACTUATOR IN CARRIER IN FLOW LIMIT RESTRICTOR o SAMPLE IN ACTUATOR SUPPLY 5N NITROGEN GAS SUPPLY SAMPLE GAS SUPPLY Figure 6 TCD PP1 Gas Supply Schematic Page 11 Peak Performer 1 Users Manual 2 5 1 Carrier Gas Supply The instrument will accept a variety of carrier gases including No Ar He or Air Oxygen is highly reactive and many pneumatic components contain greases and CAUTION Oxygen is never a suitable carrier or actuator supply gas A 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 a purified carrier gas supply and helium is considered the best multi purpose TCD 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
43. entified 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 verify that the analyzer reports data values within normal calibration tolerances i e 5 3 6 Shutdown and Transport 1 Allow the temperature zones to cool below 50 C approximately 2 hours Allow carrier to flow during cool down time Shut off carrier after cool down time and plug the CARRIER IN port on the rear of the analyzer Power off analyzer Cap the SAMPLE IN SAMPLE OUT and A
44. erature 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 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 par
45. ers 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 concentration 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 Chromatographic peak width can vary significantly depending upon column selection detector characteristics sample loop size etc Consequenlty there are several different convolving Page 72 Peak Performer 1 Users Manual 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
46. est 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 serial 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 General Error Alarm 0 No error 1 Error X Stream Number N1 Name of impurity 1from Calibration Database AREA1 Area of impurity 1 CONC1 Concentration of impurity 1 in 0 1 ppb N2 Name of impurity 2 from Calibration Database AREA2 Area of impuri
47. former 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 Page 32 Peak Performer 1 Users Manual 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 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
48. g Sample Analysis Calibration Establishing New Instrument Response Factors Shutdown and Transport Peak Performer 1 Operator Interface Set up Screen Set up Screen 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 Calibration Screen Button Functions Calibration Establishing New instrument Response Factors Analysis Database Screen Analysis Screen Parameters Analysis Screen Button Function Page 5 Peak Performer 1 Users Manual 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 Sytem Requirements Installing the Viewer Software
49. grity Adjusting the Display Contrast Altering the Analytical Range of the Instrument Updating the Analyzer Software with Peak Host Testing the Heater Resistance Main DC Power Supply Replacement Adjusting the 5 Volt DC Supply Replacing the Lamp Driver Printer Circuit Board COM1 Connections on Multiple Analyzers to a Single Computer Discussion About VICI Diaphragm Valves vs Rotary Valves 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 Performer 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 2 2 2 3 Unpacking Instructions Remove the Peak Performer 1 from the packing material or traveling case taking care to
50. i 068 3 50 I i id ha i I Roay v i i i l 1 00 TYP i eh fof oa TU j jooh 058 075 125 p COM 1 K 7 1 0 i i k ee FID DRAIN 6 i fe gt COM 2 __ 5 D e Q PT o Fal AC POWER bl Peak Laboratories LLC emah oon 408 779 4680 v 403 776 5184 fax Layout PROPRIETARY AND CONFIDENTIAL 3 gt Rack Mount rs i ors cera Rear View Z TATON DONG da Ew Br n A Figure 3 Rack Mount Rear View with Dimensions i 7 REVISIONS S Ball Bearing Slide Accuride Model 2907 26 or equivalent a we 26 inches long Peak Laboratories LLC sAm ai 408 779 4680 v 408 776 5184 fax Hartman arogi Layout PROPRIETARY AND CONFIDENTIAL n F Rack Mounting eer ose oa Top View i CO MUN KUA ENO GWG vO are A ATR CATON DIO OWO ETAC TEM NO w hal Figure 4 Rack Mount Top View with Dimensions Page 10 Peak Performer 1 Users Manual 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 cl
51. 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 Page 63 Peak Performer 1 Users Manual 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 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 Gas passing from the main flow limiting restrictor can be split to follow both gas paths Studying the schematic it can be seen that the detector flow can be adjusted by changing the amount of gas that
52. ire and tighten A common error is insufficient length of bare wire creating the condition where the terminal contacts only the wire insulation 4 3 Peak Performer 1 Users Manual COM 1 K I y I uv s IN OUT IN IN AIR He M 2 SA IN LE IN OUT COM 2 ANALOG 1 ANALOG 2 ANALOGD ANALOG 4 REC COMMON GND ZERO START PLAME SW FLAME SW I A Figure 19 Analog Output Connections 90 120 VAC 50 80 HZ 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 1 ANALOG 2 EN gt E ANALOG 3 fo ANALOG 4 REC ZERO START 3 o POMER POWER ODEN ane SRC aa FLAME SWITCH RATED AT 0 5 A 120 VAC Figure 20 Analog Output Wiring Schematic 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 31 Peak Performer 1 Users Manual Cored RF actor Figure 21 Calibration Database Screen 4 3 1 Calibration Screen Button Function Update Allows the analyzer to calculate new RFactor i 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 Per
53. lphanumeric 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 height less than or equal to PKHgt will be quantified using the ForceB mode Fit The convolution filter value expressing the overall peak shape FIt 2 is recommended for sharp narrow peaks such as H2 and Flt 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 34 Peak Performer 1 Users Manual H2 Peak Left and Right Widths as a Function of Concentration A Left Width Right Width Left Wid
54. me 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 remotely 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 PP1 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 Form 3 AB SAG 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 Page 54 Peak Performer 1 Users Manual An example 104345 104763
55. 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 General Considerations e Analyzer size is 20 L x 17 W x 7 H e Maximum operating environment for the PP1 analyzer is 30 C e Power consumption is 160 watts maximum e Fuse size is 2 5 ampere 250 VAC 5 x 20 mm SLO BLO e Free air flow for adequate ventilation to the rear of the unit is required e Communication between the PP1 and your PC is via 9 pin straight through cable connection to COM 1 and COM 2 Analog outputs are available from the DIN screw terminal strip on the rear panel e The PP1 RCP contains an extremely light sensitive detector do not place the analyzer in a location where bright light sunlight can enter the rear air vent slots 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 Power Cord End PP1 Power Entr
56. 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 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 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 73 Peak Performer 1 Users Manual The time associated with the peak maximum signal must be within the time regime of interest PkCen 74 PkWin for any peak quantification to occur In Forced Baseline Mode the normal detector baseline is calculated based upon the peak maximum signal time valu
57. on 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 analyzer 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 93 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 temp
58. p 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 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 89 9 11 Peak Performer 1 Users Manual UPDATING THE ANALYZER SOFTWARE WITH PEAK HOST Procedure 1 2 3 4 5 6 7 Power down analyzer chassis Connect DB9 serial cable and host computer to COM1 port on the rear of the 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 automati
59. perature 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 26 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 2008 NOU 1 7 vey Figure 15 Typical RCP Vlamp 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 a Moves the cursor upwards ee Moves the cursor downwards Page Advances the user 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 27 Peak Performer 1 Users Manual Jer Tate Time 2008 NOU 17 11 56 46 Fort 1 Protocol Viewer Port 2 Protocol Auto Parameter Change
60. r 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 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 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 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 71 Peak Performer 1 Us
61. ration 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 INERTS O2 Load Togdle Pade 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 V1 7 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 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 36 Peak Performer 1 Users Manual 4 5 2 Event Editor Screen Button Function ti Moves the cursor upwards 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
62. requiring a shutdown of the sample gas flow avoiding the lengthy re equilibration period 2 5 2 Actuator Supply The actuator supply is normally independent of the carrier gas inlet Actuator supply is normally attached to 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 Clean Dry Air lt 10 ppm If a combined carrier actuator inlet is requested connect a source of 60 80 psig of air or inlet gas to the CARRIER IN port 2 5 3 Sample 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 instructions if these input conditions are not available Page 15 Peak Performer 1 Users Manual SAMPLE GAS SUPPLY AA NA C J jJj NETA A A A pS wee TO PP1 n e FR FLOW RESTRICTOR 30 60 sccm ATMOSPHERIC PRESSURE Figure 7 Sample Supply Flow Schematic 2 5 3 1 Second Sample Gas Supply Peak Labs offers an optional second sample inlet stream for most analyzers Connection to the SAMPLE 1 IN and S
63. rity Improved carrier gas purity enables improved sensitivity Typical 99 999 Carrier Gas Specifications Pre Purification High Pressure Cylinder or Liquid Dewar Gas Type N Ar He alternative Air Carrier Gas Specifications Pre Purification High Pressure Cylinder or Zero Air Generator Gas Type TO N gt 21 O gt d Page 59 Peak Performer 1 Users Manual THC Concentration lt 10 ppm CO Concentration lt 10 ppm CO Concentration lt 1000 ppm H2 H2O Concentration lt 100 ppm 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 Consequently the analyzers minimum detectable quantity MDQ would be quite high gt 10 ppm unless the carrier gas is purified A catalytic combustor is included as an integral component of the carrier gas flow path of the RCP equipped PP1 Hydrogen and Carbon Monoxide carrier gas impurities are reduced to less than 10 ppt by this combustor Internal Metallic Catalytic Combustor Specifications Maximum Flowrate gt 300 cc min lt 5 L min Gases Purified N Ar He or Air alternative CO Concentration outlet lt 10 ppt H2 Concentration outlet lt 10ppt Expected Life Infinite Regenerable 7 3 Component Separation Component separation is normally performed by isothermal packed an
64. s are identified and quantified 3 5 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 5 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 port ensure that the front jumper is connected between SAMPLE OUT and SAMPLE IN on the front panel Page 19 Peak Performer 1 Users Manual 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 id
65. s 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 76 Peak Performer 1 Users Manual E x 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 Hgt x t 2 x Hgt2 Hgts x t2 1 2 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 Hgt Hgt Hgt Peaks quantified using the Variable method are denoted with a V in the last column of the data report Page 77 Peak Performer 1 Users Manual To achieve maximum analyzer performance when measuring O2 samples Peak Labs recommends continuous O2 sample cycling to minimize surface carbon reactions Page 78 Peak Performer 1 Users Manual 8 0 Thermal Conductiivty Detector TCD CAUTION Do not begin detector heating without carrier gas flow Damage to the detector may result Be sure de energize the filament before conditioning columns CAUTION The maximum detector operating temperatures for the TCD is 100 C A
66. shifted the late eluting peak carbon monoxide forward Early eluting peaks such as hydrogen are not significantly affected by changes in column temperature as interaction with column packing is minimal Page 67 Peak Performer 1 Users Manual eee E E E EE E E E Name Conc Area R Time R Factor A Type H2 413 5 1319343 49 2 3191 V co 343 2 4558519 90 2 13283 Vv 16 5 Uni 15 81 MS13X SAK Column Temperature 135 C Carrier Flow 20 5 mi min N2 oe co H2 I x f a r al ET Em P Figure 55 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 56 with Figure 54 shows the decreased peak retention times Name Cone Area R Time R Factor A Type H2 136 8 436425 32 4 3191 V co 201 5 2675877 T4 13283 W 16 5 Uni 15 81 MS13X AAK Column Temperature 105 C Carrier Flow 41 2 mlimin N2 a Ea l UD co H N ec u INS on 3 al a i s J S F i Figure 56 Effect of 2X Increase in Column Flow Rate Page 68 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
67. signed 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 Page 104 Peak Performer 1 Users Manual 9 17 Discussion About VICI Diaphragm Valves vs Rotary Valves Port 1 Port 2 Port 3 Port 4 gt S g lt N a Figure 92 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 93 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 105 Peak Performer 1 Users Manual Disadvantages Higher back pressure through this st
68. t If no printer is Page 90 Peak Performer 1 Users Manual 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 Receive 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
69. tage supply Energize the main power switch located to the right of the power cable see Figure 1 After energizing the instrument will display the RUN screen in the IDLE state Press the PAGE command once Press command three times to position the cursor in the middle 1 3 of the screen 11 12 Press the HEAT command once to activate heater zones Allow the 20 24 hours for the analyzer to thoroughly stabilize the heated zones After temperature stabilization Energize the filament by toggling the front panle switch upward the green LED will energize when power is applied to the filament Verify that the TCD Vout reading is greater than 50000 mV and less than 20000 The TCD Quality number to the far right of the TCD Vout reading should be between 15 and 40 If necessary adjust the COARSE ZERO knob on the front panel press the ZERO button wait 10 seconds and check TCD Vout and the TCD quality number Repeat as needed to reach the conditions listed in step 15 If the analyzer has been stored or idle without carrier gas flow for more than a few days consider column conditioning as described in Section 3 2 Press the PAGE command 4 times to reach the RUN SCREEN If automatic sample cycles are desired press the SINGLE command once to change the setting to CYCLE To initiate sampling press the RUN command once The P1 event program will be automatically loaded and run Page 17 P
70. th seconds Right Width seconds 1 10 100 1000 10000 Blended Concentration ppb CO Peak Left and Right Widths asa Function of Concentration ALeft Width e Right Width 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 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 i Moves the cursor upwards ee 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 35 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 concent
71. th 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 Taskbar fa Chrom Viewer 2003 12 27 1335 chm En aj File viewer ATTEH 16 SPAH 450 gt 4 k Open Saves Ww Baseline Print Exit co Figure 40 Baseline Selected Page 51 Peak Performer 1 Users Manual BE Chrom Viewer 2003 12 22 1335 chm E x File viewer ATTEH 16 SPAH 450 gt 4 a Open Saves Baseline Prink Exit k Figure 41 Baseline Deselected The File menu offers the following commands CC 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 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 52 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 is a multifunctional serial port
72. tpoint temperatures Energizes all the heater zones Advances the user to the next screen Peak Performer 1 Users Manual 4 1 3 Set up Screen Middle Section Normal The middle section of the Setup screen is concerns temperature zone and detector function 4 1 3 1 Page 25 HEE SNC 1 1 f Wien Ie Column Alame P Uout CNAE LE Figure 13 Screen Commands After Warm up Set up Screen Middle Section Button Functions Normal Zero Allows the initialize the detector electronics and establish a consistent baseline signal ie Moves the cursor upwards 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 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 Lower 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 Tem
73. ts 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 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 Peak Performer 1 Users Manual Table of Contents m_ RR RWWNND Nea 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 Actuator Gas Supply Sample Supply Second Sample Gas Supply Span Gas Supply Standard Start up Procedure Quick Start Sequence Column Conditioning Detector Conditionin
74. ty 2 CONC2 Concentration of impurity 2 in 0 1 ppb N3 Name of impurity 3 from Calibration Database AREA3 Area of impurity 3 Page 56 Peak Performer 1 Users Manual 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 significant 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 Q 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 57 Peak Performer 1 Users Manual 6 5 Setting up a RS485 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
75. uns an analysis in the mode selected Stops the analysis immediately Opens the Manual Run Screen Opens the Display Screen Toggle Starting a run in the Single mode will command the PP1 to run one time and return to the idle mode Peak Performer 1 Users Manual 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 next 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
76. ures zones and detector parameters 3 The lower section is reserved for error messages and non volatile memory updates Page 22 Peak Performer 1 Users Manual 4 1 1 Set up Screen Upper Section Wy ewer Huta iri RCP Bed Column KLF Vlame RCP Let oil wt il Aha CALA ED I COCA Figure 11 Set up or Main Screen Upper Section 4 1 1 1 Set up Screen Upper Section Button Functions ja Moves the cursor upwards J Moves the cursor downwards Edit Allows the user to change the Date Time or Protocols Page Advances the user to the next screen Page 23 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 NOW 17 12 09 35 Uj ewer 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 until 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 Edit Heat Page Page 24 Allows the initialize the detector electronics and establish a consistent baseline signal Moves the cursor upwards Moves the cursor downwards Allows the user to energize each heater zone or change heater se
77. y Module Figure 1 AC Power Connection Details Page 8 Peak Performer 1 Users Manual For best sensitivity power to the analyzer should originate from on an electrical circuit free from 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 REVISIONS ne pcem gn 18 88 281 1 25 TYP I 5 16 88 0 83 Q 18 25 Peak Laboratories LLC 408 779 4680 fv 408 776 5184 fax Layout Rack Mounting Front View Figure 2 Rack Mount Front View with Dimensions Page 9 Peak Performer 1 Users Manual REVISIONS I i AUX 1 hal ma SAMPLE 1 i CARRIER IN OUT IN i i i i ie ta i i of FIDAR SAMPLE ee ae a IN 4 i oda FIC H2 k i i l l Ay i 1 i ee a i i I X k l i
78. yle of valve because of the requirement of the internal gas stream to force the gas path open Possible incomplete sweep of the gas flow path due to residual volume between the gas port and piston diaphragm pinch point Larger circumferential seal length Low sealing force to atmospheric intrusion single screw generates all sealing force for interior and exterior flat diaphragm seal faces Increased internal cross port leakage More expensive Advantages Fewer moving parts Smaller size Single pilot valve required Page 106
79. 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 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 Page 12 Peak Performer 1 Users Manual Typical 99 999 Carrier Gas Specifications Pre Purification High Pressure Cylinder or Liquid Dewar Gas Type N gt Ar He alternative Zero Air Gas Specifications Pre Purification High Pressure Cylinder or Zero Air Generator Gas Type TO No 21900 THC Concentration lt 10 ppm CO Concentration lt 10 ppm CO Concentration lt 1000 ppm H2 H2O Concentration lt 100 ppm Synthetic air sources suitable for use as Zero Air include Zero and Breathing Quality grades CAUTION Compressed room air is not recommended unless refined by regenerative drying and combustion purification Consequently the analyzer s minimum detectable quantity MDQ would be quite high gt 10 ppm unless the carrier gas is purified Page 13 Peak Performer 1 Users Manual 2 5 1 2 Gas Purity Requirements Nominal Nitrogen Carrier Argon Helium e ppt K ra 60 psig 100 sccm orir contaminants Clean Dry Air lt 10 ppm Heated reactive metal getters can also be use

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