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Peak Performer 1 PDHID (930- Series) User Manual

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1. Sicccastencersisnssesens peun a w aeat tes fo tor tt Figure 46 Peak Development Midway on the Analytical Column INES e Figure 47 Peak Development Midway on the Analytical Column Analytes of interest can be allowed to continue on to the detector as long as desired In some cases the resulting chromatogram can become quite long in duration In other circumstances it is not necessary to quantify all possible peaks and the remaining balance of the sample is backflushed to vent or detector Page 72 Peak Performer 1 Users Manual SBUECEEOS AO EN ges ges ges ses se Ket epee F pat F pat ee T P Pr Tp Piit ED a a TE a pp Figure 48 Peak Development on the Analytical Column After Backflush EDARRA nA Santen T E E E tee OA aces PT soas Figure 49 The Completed Chromatogram 7 4 Flow Venting and Balancing Several problems can arise in the development of the chromatogram e Presence of compounds that may be damaging to the detector e Disproportionate peak sizes e Length of analysis Several models of Peak analyzers are equipped with one or two valve plumbing arrangements to handle these situations Often a second valve is used to perform cutting actions at particular times during the chromatogram redirecting the column effluent towards a safe flow controlled vent outlet During the cutting action it is necessar
2. where H gt the signal differential between the instantaneous baseline level and the peak signal value tx the time difference between data points Using a constant value for tx the peak area calculation simplifies to Peak Area tx xX Hgt Hgte Hgts Hgt Peaks quantified using the Variable method is denoted with a V in the last column of the data report Page 86 Peak Performer 1 Users Manual CAUTION Do not begin detector heating without carrier gas flow Damage to the detector may result CAUTION The maximum Column temperature is 200 C CAUTION The normal PDHID operating temperatures is 100 C Maximum temperature is 155 C Detector Temperature range 40 C gt 155 C Temperature accuracy 8 1 Helium lonization Detector Principles The pulsed discharge detector is a non radioactive universal detector configured to function as a helium ionization detector HID As the name implies a stable low power pulsed DC discharge in helium is utilized as the ionization source Effluents from the column flowing counter to the flow of helium from the discharge zone are ionized by photons from the helium discharge above Resulting electrons are focused toward the collector electrode by the two bias electrodes The principal mode of ionization is photoionization by radiation arising from the transition of diatomic helium He2 A1 to the dissociative 2He 1S1 ground state
3. gt 1000 0 to 1000 ppb 0 1 VDC scale Maximum scale is 999 999 Optional converters to provide other current voltage outputs are available Please contact your local Peak representative for additional information Terminal 7 e Analog recorder raw signal 0 1 VDC range Page 35 Peak Performer 1 Users Manual Terminal 8 e Remote Start Input The remote start input is activated by shorting the terminal 8 to COMMON GND for at least 100ms The remote start input must then return to an open state unshorten Terminal 9 e FID Flame Switch Relay The FID Flame and General Alarm switch relays are SPST N O and rated for 0 5 amps 200VDC 10VA Terminal 10 e General Alarm Relay The FID Flame and General Alarm switch relays are SPST N O and rated 0 5 amps 200VDC 10VA j NOTE The Analog recorder signal is only active when the COM1 setting is set to Viewer i eera SEA ANALOG 4 COMMON GHO D 1 0 VDC OUTPUT ANALOG 2 a o E COMMON GND 0 4 0 VOC OUTPUT ANALOG 3 eS H y COMMON GND 10 vD OUTPUT ANALOG4 a T E COMMON GHD 1 0 VEC OUTPUT ANALOG 5 7 YY COMMON GHD Q 1 0 VDC OUTPUT ANALOG 6 fp __ _ _ ie cf COMMON GND O OVRCOUTPUT DETECTOR OUT a ae E COMMON GND REMOTE START REMOTE START FLAMESW of RECO FLAME SW GENERAL ALARM S4 GENERAL ALARM Si GENERAL ALARM AND FLAME SWITCH RATED AT 0 5 4 120 VAC Figure 20 Analog Output Wiring Schem
4. C SCaCE S CNNSSUCNSNYNCCWds Compound 3 Concentration soos compou uiNts2 40068 40069 Spare CS S S S C LSCOC CNC TUCNCSCRL WNNNNSSSCNCS 40070 Compound 4 Name 8CharStrinc 40074 Compound 4 Area Counts UINT32 Compound 4 Concentration 40076 PPB 10 UINT32 Read 40078 40079 Spare d o d o o Page 66 Peak Performer 1 Users Manual 40080 Compound 5 Name 8CharStrin 40084 Compound 5 Area Counts UINT32 Compound 5 Concentration 40088 40089 Spare o oo o o 40090 Compound 6 Name 8CharStrino 40092 Compound 6 Area Counts UINT32 Compound 6 Concentration soos Compou UINT32 D a 40098 40099 _ Spare S d o Table 3 Modbus Holding Registers Supported by the PP1 6 5 Trend Analog Outputs There are seven independent analog outputs on the back of the PP1 The first six are tied to the six impurities as trend outputs and the last channel is a simple recorder output These trend outputs are provided via 0 1 0 VDC screw terminals Each impurity can be independently scaled by entering the desired range e g 0 gt 1000 0 to 1000 ppb 0 1 VDC scale At the end of each run the analog trend signal is updated and holds until the end of the next run is completed As an accessory Peak can provide standard commercial VDC mA converters as needed Page 67 Peak Performer 1 Users Manual 6 6 Setting up a RS485 Network The RS 485 specification supports two wir
5. Figure 1 AC Power Connection Details The PP1 has been CE certified to be immune to AC frequency and voltage variances of 10 of the nominal AC operating voltage Refer to the final test report and or markings on the rear of analyzers to verify the proper operating voltage for each unit For best stability power to the analyzer should originate from an electrical circuit free of large inductive or other current loads Be sure to mount the analyzer in an area of adequate ventilation and make sure the cooling fan inlet is unobstructed There are no battery back ups or reserve power supplies built into the PP1 therefore any disruption of the AC supply will result in restarting of the analyzer Peak Labs recommends the installation of a high quality on line or double conversion type of uninterruptible power supply UPS Be sure to mount the analyzer in an area of adequate ventilation and make sure the cooling fan inlet is unobstructed The operating environment for the PP1 analyzer should be maintained between 15 C and 30 C CAUTION Do not use a wrench to tighten the SMC connectors on the bias and electrometer cables as this may damage the internal connections in the PDHID fingers Connections should be finger tight only 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 th
6. Poly l b bI i gt ETY aul ak J ee Figure 56 Effect of 30 C 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 Conc Area R Time R Factor A Type H2 136 6 436425 32 4 3191 Vv CO 201 5 2675877 71 13283 Y 16 5 Uni 1S 81 MS13X PEAK Column Temperature 105 C Carrier Flow 41 2 ml min N2 OFFSET ATTEN EE A SFAM F Cona Poly aj b i i ma zd al He i gt s ie Aa lI a I Figure 57 Effect of 2X Increase in Column Flow Rate Page 77 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 i Figure 57 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
7. This Modbus numbering corresponds to an address map of 0 to 9998 The PP1 responds with a packet containing the values of the registers in the range defined in the request See PP1 address map table to verify address range and content Read Holding Registers Packet Example The next example the PP1 s Modbus slave address is 92 and the master requests to read two parameters from the PP1 These two parameters are requested from Modbus registers 40013 and 40014 In accordance with the Modbus protocol holding register 40013 is numbered as address 12 when requested Slave Address 92 5C Hex Modbus Function 03 03 Hex Starting Register 12 000C Hex Num of Register 02 0002 Hex LRC Checksum 109 93 Hex 39 33 ASCII Request Packet non shaded background denotes the DATA field of the packet Page 62 Peak Performer 1 Users Manual Starting Register Num of Registers 40013 2 Response Packet Slave Modbus Byte Register 1 Register2 check Address Function Count Address 12 Address 13 The Master device receives the above data packet in response to the request packet Modbus Register 40013 4E38 Hex 20024 Modbus Register 40014 2A60 Hex 10848 Function 06 Preset Single Register Preset a value into a single holding register Place specific values into a single holding registers in the PP1 There is only one holding register that can be written to the PP1 See PP1 register map below Pr
8. This is the well known Hopfield emission The photon energy from the Hez continuum is in the range of 13 5 eV to 17 7 eV lonization is independent of carrier flow therefore detector response is the same regardless of carrier flow rate The PDHID is essentially non destructive 0 01 0 1 ionization occurs yet highly sensitive The response to organic compounds is linear over five orders of magnitude with minimum detectable quantities MDQs in the low to sub picogram range The response to fixed gases is positive the standing current increases with MDQs in the low ppb range The PDHID response is universal except for neon which has an ionization potential of 21 56 eV Since this potential is close to the energy of metastable He 19 8 eV but greater than the photon energy from the He2 continuum neon exhibits a low ionization efficiency and low detector response Page 87 Peak Performer 1 Users Manual GROUND PIN HID PAU AAN HELIUM INLET __ DISCHARGE REGION VENT DOPANT INLET BLAS ELECTRODE T SAPPHIRE INSULATORS COLLECTOR ELECTRODE CAPILLARY COLUMN BIAS ELECTRODE COLUMN INLET Figure 58 PDHID Assembly Safety Notes and Information HIGH VOLTAGE Voltages presenting the risk of electric shock are present in several places in the equipment Avoid contact with hazardous live parts Do not probe into openings or attempt to defeat safety mechanisms A HOT SURFACE The surface of the
9. 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 43 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 Page 70 Peak Performer 1 Users Manual COLUMN 2 COLUMN 1 81 MS13X 16 5 UNI 1S CARRIER IN REAR PANEL TO DETECTOR INTERNAL EXTERNAL DETECTOR BYPASS R3 R2 ACT IN REAR PANEL INTERNAL EXTERNAL NV1 TO PILOT VALVE MANIFOLD NV2 BYPASS OUT FRONT PANEL SAMPLE OUT REAR PANEL R2 VALVE 1 SAMPLE IN FRONT PANEL INTERNAL EXTERNAL e INTERNAL EXTERNAL SAMPLE OUT FRONT PANEL SAMPLE IN REAR PANEL Figure 44 Typical PDHID 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 een ig eign ig nae et sfz etana EET Figure 45 Peak Development on the Analytical Column Soon After Injection Page 71 Peak Performer 1 Users Manual
10. baseline offset of the chromatogram These functions mimic those of a standard chart recorder Figure 30 Run Display screen 4 7 4 1 Display Screen Button Functions VOff VOff Attn Attn Page 47 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 Span Toggles the window view horizontal scaling in seconds Esc Exits from the Display sub screen to the Run screen Peak Performer 1 Users Manual 5 0 Peak View Software The Peak View software has two main capabilities Primary functions concern acquisition and archiving of compound concentration and acquisition and collection of the chromatogram data The software also provides the ability to display and print the data from a remote computer platform Peak View software is written specifically for the Peak Laboratories Peak Performer 1 PP1 gas analyzer covering communications port protocols and data formats and is not intended for use with other manufacturer s analyzers 5 1 System Requirements 1 2 GHz 20 GB 256 Mb RAM 1 USB port Windows XP or Windows Vista Windows 7 Windows 8 USB to DB9 RS232 Adapter Maker Gigaware Model 26 949 or equivalent DB9 Extension cable DB9M to DBYF wired straight through 10 feet Optional USB 4 po
11. 256 Mb RAM CD R drive with at least 1 USB port Dell Inspiron 8500 laptop or equivalent Operating System Windows XP Home Edition v2002 Service Pack 1 1 each USB Hub Inland 4 Port USB Hub Self powered Stock 08302 manufactured by Inland International www inland products com 2 each USB to DBY RS232 Adapter SIIG Inc USB to Serial Adapter Model US2308 Part JU CB1S12 manufactured by SIIG Inc www siig com Comes with installation software 2 each DB9 Extension Cable DB9M to DB9F wired straight through 10 feet long GQ Cables 10 Mouse Keyboard Extension DB9M to DB9YF Part M05 103 E USB Hub USB to DB9 aces A A A a o000 o000 Figure 73 Multiple Analyzer Connection Installation of Multiple Analyzers via USB 1 Connect DB9M to DB9F extension cables to analyzers 2 Power up analyzers do not heat 3 Set Port 1 Protocol on the analyzers to Viewer Page 101 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 Connect the USB to DB9 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 DBY adapter INSTALL CD in CD drive it will launch automatically if autoplay in enabled on yo
12. A O N CO N O1 Page 25 Peak Performer 1 Users Manual SET UP MAIN SCREEN a RUN DATA SCREEN 4 1 UPPER RIGHT CORNER RUN PAGE KEY TREND amp ANALOG OUTPUT SCREEN PAGE KEY CALIBRATION DATABASE SCREEN PAGE KEY ANALYSIS DATABASE oo SCREEN PAGE KEY EVENT PROGRAM EDITOR Nii SCREEN j PAGE KEY e EA STREAM SELECTOR PROGRAM EDITOR SCREEN PURCHASED OPTION va PAGE KEY CHROMATOGRAM L SCREEN PAGE KEY SET UP MAIN SCREEN Figure 10 Software Menu Structure Set up Screen MAMUAL KE Y MANUAL CONTROL SCREEN ESC KEY DISPLAY KEY F DISPLAY CONTROL SCREEN SE ee The Set up screen is multi functional Different command buttons appear at the bottom line of the screen dependent upon the section containing the asterick cursor 1 The upper section 3 lines contains commands related to analyzer set up 2 The middle section 5 lines contains commands related to temperatures zones and detector parameters 3 The lower section is reserved for error messages and non volatile memory updates Page 26 Peak Performer 1 Users Manual 4 1 1 Set up Screen Upper Section Figure 11 Main or Setup Screen Upper Section 4 1 1 1 Set up Screen Upper Section Button Functions ie Moves the cursor upwards i Moves the cursor downwards Edit Allows the user to chang
13. 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 Page 39 Peak Performer 1 Users Manual 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 ageneral 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 a eon HHEH eH HH HH eRiohtwidh J f le tiie ieo a ia A A A S Bea LU Tt A ta TNA a S ee Pe sa A A A at A OP TTT A ot TTT oT ETT TT ot TTT TT PT U E A ee b S r fi a 5 Fight E E Bight Width ice reba a ic Figure 23 Left and Right Peak Width as a Function of Concentration e Total peak width LW RW is primarily a function of sample loop unloading e Larger sample loops require a long time period to fully inject e The relative values of LW and RW are dictated by the skew factor of the peak e 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 secon
14. 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 7 Shutdown and Transport Power off analyzer Allow the temperature zones to cool below 35 C approximately 2 hours Allow carrier to flow during cool down time Shut off carrier after cool down time and plug the CARRIER IN SAMPLE IN and SAMPLE OUT ports on the rear of the analyzer to prevent atmospheric contamination Cap the ACTUATOR IN port Plug the BYPASS OUT port on the front panel Cap the detector vent line Ensure that the front jumper tube is connected between SAMPLE IN and SAMPLE OUT 9 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
15. detector baseline stability cn be affected as well as the retention times Stable 1 psig carrier supplies are suggested Page 89 Peak Performer 1 Users Manual 8 4 Troubleshooting High Background Current The background current is indicated by the quality number located to the right of the Vout signal on the Systems Setting screen A value of 50 255 indicates a high background current A value of 7 12 is typical If the quality number does not drop below 200 after a 12 hour bakeout on clean gas there is either a leak in the system or the column effluent is not clean To see if the high background current is due to the column 1 Manually zero the detector 2 Completely disconnect the column from the detector inlet tube leaving the inlet open 3 Watch the detector Vout signal It should read zero 0 If the current remains high then either the system has a leak in the discharge gas supply line or the discharge gas has impurities in it If the current decreases dramatically then either the carrier gas supply has leaks and or contaminants or the column is the source of contamination and needs a bakeout conditioning 8 5 Checking for Leaks in the Discharge Gas Plumbing 1 Disconnect the column from the detector inlet and cap plug the detector inlet 2 Verify all connections are tight from the carrier source up to the detector including valve connections If the current remains the same proceed to the next fitting If t
16. 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 Page 93 Peak Performer 1 Users Manual 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 94 Peak Performer 1 Users Manual 9 5 Testing the Heater Resistance ROIO _MINMAX RANGE Figure 63 Heater Resistance for 90 120 VAC AC Service 177 AUS AAG MA TTR Page 95 Peak Performer 1 Users Manual a iiti th A i a 5 a 5 a f 5 1 5 h a 5 a 5 7 5 a a m 5 w L ee ot oe oe oe oe a a F i 2 ee se a SSP PP Peer i s fy riera eta J Caman ioe reh e e G cme e eiea J i ee es ee Pi Adjust this potentiometer to change display instensity and contrast Figure 65a View of the MCPU Showing the LCD Contrast Potentiometer MCPU adjustments for software versions 1 3 Adjust this potentiometer to change display instensity and contrast Figure 65b View of the MCPU Showing the LCD Contrast Potentiometer MCPU adjustme
17. performs the same calculation without the error check field on the entire packet it receives The resulting value is compared to the error check field Transmission errors Page 61 Peak Performer 1 Users Manual are indicated when the calculated checksum does not equal the checksum stored in the incoming packet The receiving device ignores a bad packet To calculate the LRC 1 Add up all the data bytes in the message before converting to ASCII and without the initial colon and final CR LF 2 Throw away any bits that carry over 8 bits 3 Make the result negative by twos complement to get the LRC byte 4 Convert from the 8 bit hex value to two ASCII characters 6 4 3 Packet Communications The PP1 analyzer only supports two Modbus functions Read Holding Registers and Preset Single Register Function codes 03 06 respectively Modbus Function ModBus Description Function Description 03 Read Holding Fetch the current value in one or more holding registers Registers from the PP1 06 Preset Single Register oe a specific values into a single holding register to the Table 1 Modbus Functions Supported by the PP1 as a Slave Function 03 Read Holding Registers To read PP1 parameter values a Master must send the PP1 a Read Holding Registers request packet The Read Holding Registers request packet specifies a starting address and the number of 16 bit registers to read The Modbus registers are numbered from 40001 to 49999
18. proportional factor to generate the reported concentration value PEAK CONCENTRATION PEAK AREA RESPONSE RESPONSE FACTOR 3 6 1 Establishing New Instrument Response Factors Connect a known calibration standard gas span gas to the analyzer at the SAMPLE IN port on the front panel If soan gas connection is made at the rear panel SAMPLE IN port ensure that the front jumper is connected between SAMPLE OUT and SAMPLE IN on the front panel Verify that sample is flowing freely through loop exit flow from the SAMPLE OUT should be 30 to 120 cc min Press the ESC or PAGE keys as needed to navigate to the RUN screen Press the SINGLE CYCLE RERUN key to toggle to SINGLE mode Press the RUN key to initiate analysis the P1 event program will be loaded automatically and executed Allow the analyzer to fully execute the event program Current concentration data will be displayed as an overlay on the RUN screen as peaks are identified and quantified Press the PAGE key as needed to toggle to the CALIBRATION DATA BASE screen Page 24 Peak Performer 1 Users Manual 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
19. sample inlet stream for most analyzers Connection to the SAMPLE 1 IN and SAMPLE 2 IN ports should replicate Figure 7 Sample lines are normally attached to the rear panel of the instrument Attach sample or span gas lines to the SAMPLE IN port on the rear panel The SAMPLE OUT port must be unrestricted 2 5 5 Calibration Gas Connection for Analyzers Equipped with the Optional Internal Span Gas Blender Peak Labs offers an optional internal span gas blender for most analyzers Connection to the SPAN GAS IN port should replicate Figure 8 Nominal inlet soan gas pressure is 50 psig and flow through the internal blender is preset within the analyzer External restrictors are not required It is important to measure the pressure applied to the SPAN GAS IN port as closely to the analyzer rear panel as possible 2 5 5 1 Span Gas Supply Optional For internal span gas blender units only Peak Labs offers an optional internal soan gas blender for most analyzers Connection to the SPAN GAS IN port should replicate Figure 8 It is important to measure the pressure applied to the SPAN GAS IN port as closely to the analyzer rear panel as possible Nominal inlet span gas pressure is 50 psig and flow is restricted inside the analyzer External restrictors are not required for these units SPAN GAS FEED SUPPLY SPAN GAS FEED SUPPLY ROC fea TO PP1 SPAN GAS INLET Poke Figure 8 Span Gas Supply Flow Schematic Page 20 Peak Performer 1 Users M
20. 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 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 Cancel Baud Rate C 9600 f 19700 amp 38400 Data Bits Stop Bits i Teg f f 2 Figure 34 Viewer Software Communications Setting screen Page 51 Peak Performer 1 Users Manual Once the CSV file is opened the Viewer window automatically updates and shows concentration data Figure 35 is an example with consecutive runs The third run of concentration data at 15 29 is displayed in RED to denote that there was a general error in the PP1 during this run The error was cleared at 15 49 014 02 16 File Starkt Stop Chrom view Event Info Upload ro Ppewer Fun Time Stream AR NH 14 28 1 8765 6 9712 0 15 29 1 10403 2 10204 2 15 37 1 100345 8 10528 T 15 49 1 10417 1 10442 5 15 57 L 1476 2 104433 5 16 06 L 10556 3 10355 9 Figure 35 Viewer screen showing concentration data There are eleven individual error conditions that can cause the Viewer Line to appear red e Detector Communication Error e Temperatur
21. supply pressures match those listed in the final test report Press the PAGE command 4 times to reach the RUN SCREEN Press the MANUAL command once Press the POWER command once Press the BIAS command once The screen will display BIAS to indicate that the bias voltage 140 VDC has been turned on gre Oy Page 23 Peak Performer 1 Users Manual 3 5 Sample Analysis Verify that sample is flowing freely through loop exit flow from the rear SAMPLE OUT port should be 30 to 120 cc min Press the ESC or PAGE commands as 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 peaks are identified and quantified 3 6 Calibration The Peak Performer 1 chromatograph determines concentration peak area to quantify the amount of contaminants in the sample gas The direct instrument response in units of uV sec is reported simultaneously as an overlay on the RUN CHROMATOGRAM SCREEN and in the AREA column on the CALIBRATION DATABASE SCREEN As the concentration peak area is determined the analyzer applies the pre programmed response factor as an inverse
22. that retain the DC power supply to the rear panel circuit board Disconnect only the two cable assemblies that attach the DC power supply to the rear panel circuit board it is recommended to disconnect the cables at the circuit board connector end Remove the DC power supply by sliding it under the overlayed cable assemblies do not remove the other cable assemblies see Figure Ti ew ac Soa DET HEAT AC DET AC aP OVEN ACN c AC SSP p AC SSR moe eae vs 7 rh perna a SOSbaEO PEAK LABORATORIES REAR PANEL INTERCONNECT _ 484 001 Rev ia Figure 69 Main Dc Power Supply Fully Removed Lay the old DC power supply on the workbench aside the new Power one DC power supply Orient such that the 6 pin and 2 pin connectors are aligned see Figure 70 Page 99 Peak Performer 1 Users Manual Old Versions of DC Power Supplies Figure 70 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 Please refer to Figures 65a and 65b Page 100 Peak Performer 1 Users Manual 9 9 COM 1 Connections on Multiple Analyzers to a Single Computer Equipment 1 each Computer 1 2 GHz 20 Gb Hard drive
23. used automatically every time you launch the Viewer software in that folder 21 Leave the first Viewer window open 22 Insert second USB to DB9 adapter into USB hub your computer should detect the connection and launch the hardware installation program 23 Insert USB to DBY adapter INSTALL CD in CD drive it will launch automatically if autoplay in enabled on your computer 24 Follow installation instructions that come with USB to DB9 adapter confirm that it is okay to click the Continue anyway box 25 Your computer may prompt to install the USB to DBY 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 DB9 adapter it will be displayed directly under the note for the first USB to DB9 adapter Page 102 Peak Performer 1 Users Manual 30 Note which COM port number is now assigned to the second USB to Serial RS232 Port adapter its COM5 on most computer
24. 0 ppbv impurities in the carrier gas will limit detection of 100 ppbv impurities in sample gas We suggest using a purified lt 1 0 ppb total contaminants helium source through a dual stage UHP regulator for optimum performance The user must provide Helium carrier gas purification see below regarding purification Typical 99 9999 Helium Gas Specifications Pre Purification High Pressure Cylinder or Liquid Dewar Argon Concentration lt 10 ppb Page 15 Peak Performer 1 Users Manual Consequently the analyzer s minimum detectable quantity MDQ would be quite high gt 3 ppm for certain compounds unless the carrier gas is purified The performance of the detector is adversely affected by the presence of any impurities in the gas streams carrier discharge or dopant Peak Labs recommends that a quality grade of helium 6 0 99 9999 pure or better be used at all times Major gas suppliers offer research grade helium 99 9999 pure which is particularly low in fixed gas impurities and should give good results in a clean system but even the highest quality carrier gas may contain some water vapor and fixed gas impurities hence a helium ourifier should be included as part of the detector system Whenever a new batch of discharge gas is received Peak Labs recommends performing a blank GC analysis of the new cylinder gas to detect and identify the presence of any impurities Peak recommends use of the best quality heat
25. 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 Figure 26 Run Chromatogram screen in the Idle state and the mode displayed upon initial power up Page 43 Peak Performer 1 Users Manual a Figure 28 Run screen in Idle mode at end of run Page 44 Peak Performer 1 Users Manual 4 7 1 Run Screen Button Functions Run Loads a standard event program and runs an analysis in the mode selected Idle Stops the analysis immediately Manual Opens the Manual Run Screen Disp Opens the Display Screen Single Toggle Starting a run in the Single mode will command the PP1 to run one time and return to the idle mode Cycle Toggle Starting a run in the Cycle mode shall configure the PP1 to run continuously until the Idle key is pressed ReRun Toggle Starting a run in the ReRun mode shall recompute the area and concentration based on the parameters in the analysis data base Stream Toggle Starting a run in the Stream mode will configure the PP1 to initiate the Stream Selector Sequence until the Idle key is pressed Page Advances the user to the next screen 4 7 2 Run Screen Continuous Monitoring Analysis Con
26. ID to BIAS ON 17 Press the ESC command once 18 Press the PAGE command once 19 Allow the 8 16 hours for the analyzer to thoroughly stabilize the heated zones After temperature stabilization 20 If automatic sample cycles are desired press the SINGLE command once to change the setting to CYCLE 21 To initiate sampling press the RUN command once The P1 event program will be automatically loaded and run NOTE To display concentration data only press the upper right corner of the AY 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 Conditions warranting column reconditioning are a Start up after storage shipment b Reduced detector response c Unstable baseline d Merging of peaks Normal column operating temperatures are 45 to 110 C The maximum PP1 PDHID column operating temperature is 200 C To prevent detector contamination Peak Labs recommends disconnecting the column from the detector during column bakeout procedures When the column in reinstalled after bakeout conditioning the PDHID Vout standing current should be at an acceptable level Page 22 Peak Performer 1 Users Manual CAUTION Never energize heaters of the instrument unless carrier
27. MPLIANT MADE IN THE USA Figure 5 Rear View of PP1 PDHID Oxygen Nitrogen Argon Helium Hydrogen Samples 120 VAC Oxygen Nitrogen Argon Helium TZ Hydrogen or Samples p D H D SAMPLE TZ PHe ZS CARRIER 4 ACTUATOR GHe V NY Column In Column Out Jr OXYT RAP HTS Vent Figure 6 PDHID PP1 Gas Supply Schematic Page 14 Peak Performer 1 Users Manual 2 5 1 Carrier Gas Supply The instrument will accept only Ultra high purity helium as carrier gas The helium used for carrier must be certified to be free of residual argon the presence of argon in the carrier gas stream will create an elevated and unstable detector baseline Attach a 60 0 2 PSIG source of carrier gas or specific pressure setting as indicated in the application section of the final test data to the carrier inlet fitting CAUTION Oxygen is never a suitable carrier or actuator supply gas Oxygen is highly reactive and many pneumatic components contain greases and oils that combust spontaneously when exposed to oxygen Consult the test data shipped with the analyzer in CD format for carrier gas details specific for your analyzer 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 e g 10
28. P1 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 PPican be properly established H PeakView Ver 5 0 a File Start Stop ChromView Event Info Upload Run Time Stream Figure 31 Viewer main window showing Communications Error The Viewer window shown in Figure 32 shows the viewer screen without the RED DOT This signifies the communication connection between the PC and the PP1 is function correctly Page 49 Peak Performer 1 Users Manual File Start Stop Chrom View Event Info Upload Run Time Stream Figure 32 Viewer main window showing no Communications Error 5 5 1 File Menu on the Viewer Taskbar Start Stop Chrom View Event Info Upload Open Port Settings Print Exit Figure 33 File Menu on the taskbar Page 50 Peak Performer 1 Users Manual The File menu contains the following commands Opens a CSV file that was created by the Viewer software Use this command to open a CSV file to view the concentration data Port Settinas Opens serial communication settings window for setting RS 232 g configurations between the Host PC and the PP1 As shown in figure 34 O Prit Prints all concentration data of selected CSV file Exit Exit Viewer application 5 5 1 1 Communication Setting Window The Communication Settings window Is shown in figure 34 This screen displays the serial communication
29. PONSE FACTOR Page 37 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 soan gas connection is made at the rear panel SAMPLE IN port ensure that the front jumper is connected between SAMPLE OUT and SAMPLE IN on the front panel Verify that sample is flowing freely through loop exit flow from the SAMPLE OUT should be 30 to 120 cc min Press the ESC or PAGE keys as needed to navigate to the RUN screen Press the SINGLE CYCLE RERUN key to toggle to SINGLE mode Press the RUN key to initiate analysis the P1 event program will be loaded automatically and executed Allow the analyzer to fully execute the event program Current concentration data will be displayed as an overlay on the RUN screen as peaks are identified and quantified Press the PAGE key as needed to toggle to the CALIBRATION DATA BASE screen Place the at the first compound of interest and press the EDIT key use the up down left and right arrow keys to enter the span gas concentration in the CONC field Be certain to use the right arrow key to fully exit the CONC field or all updates will be lost With the before the compound name press the UPDATE key The analyzer will recalculate the appropriate response factor for the compound based upon the span gas concentration and analyzer area response using
30. Peak Performer 1 Users Manual Peak Performer 1 PDHID 930 Series User Manual SPEAK Peak Laboratories LLC www peaklaboratories com 650 691 1267 Version 5 0 1 30 14 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 High voltages are required for proper detector operation and are present when the unit is energized chromatographic operation Hot surfaces may be present when the unit is energized Illustrations and photographs contained herein are for example only Actual configurations may vary depending on specific application and installed options AN High operating temperatures are required for proper detector and 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 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 Operators sho
31. Save the chromatogram data that is currently displayed BaseLine Enables display of compound name and integration baseline information Exit window cr Pre O 5 5 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 56 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 and COM2 are multifunctional serial ports 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 Figure 42 is the minimum cable configuration PC MALE PP 1 FEMALE 9 Pin Cable from PC to PP 1 Figure 41 COM Cable Wiring 6 2 Port 1 Protocol There are two COM1 output formats Peak View and Detector Proper selection of protocol is determined by the application in use on the host computer 6 2 1 COM 1 Port Settings The RS 282 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 Peak View Output Columns Format in CSV files The Peak View 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 ar
32. Text Form 2 STX S EXT Form 3 aBS C Form 4 02 53 03 6 2 3 2 Detector Signal Data String The PP1 Detector Signal Data string format is an integer number followed by a carriage return CR and line feed LF An example 104345 104763 104832 The End Of Data string format consists of three ASCII characters The following are four forms of the same command Form 1 Start Of Text E End Of Text Form 2 STX E EXT Page 58 Peak Performer 1 Users Manual Form 3 SBE C Form 4 02 45 03 An example 104345 104763 104832 Last sample sent to Host ABE C End Of Data command to Host from PP1 6 3 Port 2 Protocol There are two COM2 protocol formats PLC programmable logic controller and MODBUS protocols There are three modes of operation AUTO POLL and MODBUS PLC protocol can operate in 2 modes AUTO or POLL The MODBUS Protocol mode is predefined and not user changeable Proper selection of protocol is determined by the application in use on the host computer 6 3 1 COM 2 Settings The RS 232 settings for COM 2 port are 9600 baud rate 8 bit data 1 stop bit and no parity for AUTO and POLL modes The RS 232 settings for COM 2 port in MODBUS mode are 9600 baud rate 7 bit data 1 stop bit and even parity for Three modes of transmission are available AUTO or POLL or MODBUS e In AUTO mode the current PLC data string is transmitted at the end of analytical cycle without any request from the host
33. W and RW values as initial baseline points This is illustrated as the hypothetical baseline between points L and R in Figure 66 The first hypothetical calculation of the peak end time is labeled 1 in Figure 66 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 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 6 when the change in peak area became less than 0 5 Peak Maximum 5 S5 o N N PEAK START PEAK END Figure 66 Progression of Peak End Time Calculation Using the newly established peak start and end times the mathematics package determines the normal detector baseline as illustrated in Figure 67 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 85 Peak Performer 1 Users Manual PEAK START PEAK END Figure 67 Peak Area Calculation The formula for peak area calculation can be expressed as Peak Area 12 x Hgt Hgte x t1 2 x Hgte Hgts x t2 2 x Hgts Hgta x ts
34. air circulation Position the controller unit where the mains switch on the rear panel can be reached easily Page 9 Peak Performer 1 Users Manual 2 2 1 Carrier Discharge Gas Considerations The performance of the detector is adversely affected by the presence of any impurities in the gas streams carrier discharge or dopant We recommend that a quality grade of helium 6 0 99 9999 pure or better be used at all times Residual Argon content is the primary concern with lesser grade Helium gases residual Argon cannot be removed from cylinder Helium gas it must be removed prior to the cylinder filling process Major gas suppliers offer research grade helium 99 9999 pure which is particularly low in fixed Argon gas impurities and should give good results in a clean system but even the highest quality carrier gas may contain some water vapor and fixed gas impurities hence a helium purifier should be included as part of the detector system The discharge gas must always be run through the helium purifier Whenever a new batch of discharge gas is received we recommend performing a blank GC analysis of the gas in the PDHID mode to detect and identify the presence of any impurities prior to connecting the cylinder as carrier gas supply 2 2 2 Installing and Purging of Gas Regulators 1 Make sure the on off valve on the helium cylinder is completely closed 2 Screw the CGA fitting nut of the regulator into the helium cylind
35. an output format If the first three are valued False and the remaining three are valued True the output register value is Register 0001110000000000 Bin 1C00 Hex If the first input register became True the output register value changes to Register 1001110000000000 Bin 9C00 Hex 8CharString Format The 8CharString or eight character string register format is four 16 bit Modbus Holding Registers that hold a total of eight ASCII characters 6 4 5 Broadcast Packets The purpose of a broadcast request packet is to allow all slave devices to receive the same request command from the master A broadcast request packet is the same as a normal request packet except the slave address field is set to zero 0 All Modbus slave devices receive and execute a broadcast request command but no device will respond The PP1 does not support broadcast request packets Exception Responses lf a Modbus master device sends an invalid command to a PP1 or attempts to read an invalid holding register an exception response is generated The exception response follows the standard packet format The high order bit of the function code in an exception response is set to 1 The data field of an exception response contains the exception error code The table below describes the exception codes supported by the PP1 and the possible causes Return Function Function Description 01 An invalid command is contained in the function field of t
36. anual 3 0 Standard Start up Procedure Peak Labs recommends that the user read the entire operating manual prior to using the Quick Start sequence CAUTION Do not begin detector heating without carrier gas flow Damage to the detector may result 3 1 Quick Start Sequence 1 Confirm that all gas connections and supplies are properly made 2 Remove the top cover of the instrument Figure 9 PDHID Detector 3 Pressurize the carrier gas supply line to 60 psig Pressurize the Actuator gas supply to 60 psig 5 Verify that sample is flowing freely through loop exit flow from the rear SAMPLE OUT port should be 20 to 120 cc min gt Page 21 Peak Performer 1 Users Manual 6 Verify BYPASS OUT flow gt 20 cc minute 7 Verify the analyzer is connected to the correct line voltage supply 8 Energize the main power switch located to the right of the power cable see Figure 1 9 After energizing the instrument will display the RUN screen in the IDLE state 10 Press the PAGE command once 11 Press command three times to position the cursor in the middle 1 3 of the screen 12 Press the HEAT command once to activate heater zones 13 Press the PAGE command 4 times to reach the RUN SCREEN 14 Press the MANUAL command once 15 Press the POWER ON command once 16 Press the BIAS command once to toggle the negative accelerating voltage within the PDH
37. atic Channels 1 7 output voltage can be tested manually by pressing the MANSET key to send a temporary signal for diagnostics Page 36 Peak Performer 1 Users Manual 4 3 Calibration Database Screen The Calibration Database screen stores critical information regarding calibration Span gas concentrations and instrument response and provides tools to easily update the response factors 14 42 34 Calibration Database lt lt Name Area Cori RFactor FT x AR 18918149 1 S32 19 N2 25113663 1 TEZ JEA Uedate t Edit Page Figure 21 Calibration Database Screen 4 3 1 Calibration Screen Button Function Update Allows the analyzer to calculate new RFactor KIJ T Moves the cursor upwards 649 o Moves the cursor downwards Edit Allows the user to change concentration data or response factor Page Advances the user to the next screen 4 3 2 Calibration The Peak Performer 1 chromatograph determines concentration peak area to quantify the amount of contaminants in the sample gas The direct instrument response in units of uV sec is reported simultaneously as an overlay on the RUN CHROMATOGRAM SCREEN and in the AREA column on the CALIBRATION DATABASE SCREEN As the concentration peak area is determined the analyzer applies the pre programmed response factor as an inverse proportional factor to generate the reported concentration value PEAK CONCENTRATION PEAK AREA RESPONSE RES
38. atogram 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 Name Conc Area R Time R Factor A Type H2 413 5 1319343 49 2 3191 V co 343 2 4558519 90 2 13283 V 16 5 Uni 1S 81 MS13X SPEAK Column Temperature 135 C Carrier Flow Smi minN orrser ATTEN ya SPAN T Fio j i Cors Pot pS am E co Pook Time 3 k Tima L Otfset E tise Rosel _ O09 itea ak Heian i cok Ares H2 Paa a Pok Cons Rosp Fod amp Volatge i Analysi Type ioe a y vaibie a cy pP al ee pp jji J Figure 55 Standard chromatogram Page 76 Peak Performer 1 Users Manual 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 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 Name Conc Area R Time R Factor A Type H2 136 8 436425 32 4 3191 V CO 201 5 2675877 71 13283 V 16 5 Uni 1S 81 MS13X VAs K Column Temperature 105 C Carrier Flow 41 2 m min N2 OFFSET ATTEN 123 SPAN gt i r Cons
39. can be directly related to concentration units Page 78 Peak Performer 1 Users Manual PEAK START PEAK END Figure 58 Illustration of Measurement of Chromatographic Peak Area Note The PP1 analyzer supports only area based concentration determinations Determinations based upon peak height are 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 Figure 59 Typical PP1 Peak Analysis Database Page 79 Peak Performer 1 Users Manual PkWin Figure 60 Illustration of Chromatographic Peak Parameters Name The peak identification tag expressed as 5 alohanumeric 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
40. 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 Flt 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 80 Peak Performer 1 Users Manual All modes of peak are calculation require locating the peak top usually the point of maximum peak signal In cases where the detector signal is strong locating the peak maximum value is Straightforward Often the 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 co
41. computer 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 but can also be used for RS 232 connections e In MODBUS mode the PP1 will transmit the latest PLC data string only when prompted by the host computer See MODBUS uses manual for operational details Selecting the POLL mode on the MAIN SCREEN configures the PP1 to wait for a request before transmitting The master controller of the RS 485 network must first request data from the PP1 in order for receive the COM2 port output data The protocol to request data from the PP1 consists of 1 A start of transmission character 2 Followed by the unit serial number 3 An end of transmission character or STX character 02 hex SSSS ETX character 03 hex Page 59 Peak Performer 1 Users Manual The requesting command format follows lt STX gt SSSS lt ETX gt where SSSS serial number of unit is used as the RS 485 ID 6 3 2 COM 2 Port PLC Output Format The COM 2 port output format consists of unit serial number date and time stamp error alarm stream number followed by impurity data This data format is transmitted at the end of every run automatically if the COM 2 mode is set to Auto This format uses a general protocol envelope This envelope consists of a start of transmission character followed by data and end of transmission character The start of transmi
42. d it can be regenerated by connecting pure H2 and increasing the operating temperature of the trap using the procedure below Stop analyzer and return valves to load CCW position Turn helium plasma to Poweroff and Bias off Edit column Set point from 50 gt gt 150 C Disconnect Oxy trap outlet from Det ector In Cap Det in fitting Connect Oxy trap outlet to 20 sccm ml min H2 supply Disconnect V2 out from Oxy trap Inlet OF pa Or ae Ue IN a Let V2 fitting continue to vent Connect H2 vent to Oxy trap In union s Let purge for 8 hours or overnight h o_o Turn Set point on the column back to 50 C from 150 C s Disconnect H2 supply and shut off s Disconnect H2 vent from Oxy trap In union h gt Connect V2 out to Oxy trap Inlet o_o A Allow to purge for 2 hours or when column temperature is back to 50 C whichever is longer 16 Uncap Detector Inlet 17 Connect Oxy trap outlet to Det ector Inlet 18 Turn helium plasma PowerOn and Bias on 19 Start normal run cycle but allow baseline to stabilize until all H2 has been purged 2 4 hours Page 104
43. d by a SLAVE device are RESPONSES At most one SLAVE can respond to a single request from a MASTER The PP1 does not support broadcast request packets The PP1 shall only support the ASCII mode Modbus protocol The PP1 is only a SLAVE device The PP1 does not conform to all stated requirements according to the MODBUS Application Protocol Specification v1 1b3 and MODBUS over Serial Line Specification and Implementation Guide V1 02 Page 60 Peak Performer 1 Users Manual 6 4 1 Mode of Transmission The PP1 only supports the ASCII mode Modbus protocol The PP1 analyzer requires the serial communications channel to be configured to 9600 bps 7 data bits even parity and one stop bit 6 4 2 Modbus Packet Structure Every Modbus packet consists of four fields e Slave Address Field e Function Field e Data Field e Error Check Field LRC Checksum Slave Address Field The slave address field of a Modbus packet Is one byte two ASCII characters in length and uniquely identifies the slave device involved in the transaction Valid addresses will be in a range between 1 and 247 A slave device performs the command specified in the packet when it receives a request packet with the slave address field matching its own address A response packet generated by the slave has the same value in the slave address field Function Field The function field of a Modbus request packet is one byte in length and tells the addressed slave which funct
44. detector body may be hot while in operation possibly in excess of 150 C Caution should be observed Page 88 Peak Performer 1 Users Manual A CAUTION During normal operation the detector produces j ultraviolet energy UVA UVB some of which may be emitted Do not watch the arc without eye protection The PDHID detector does not normally require conditioning treatment however it does require 8 to 12 hours at normal operating temperature to achieve optimum stable performance Normal detector operating temperature for the PDHID is 100 C although operating temperatures vary with the specific application The table below illustrates some typical compounds and detection capabilities of the PDHID Detected Compound Typical Detection Limit Hydrogen lt 10 ppb Carbon Monoxide lt 10 ppb Carbon Dioxide lt 5 ppb Methane lt 3 ppb Other Hydrocarbons lt 3 ppb Helium No Significant Response Argon lt 10 ppb Nitrogen lt 10 ppb Oxygen lt 10 ppb 8 2 Temperature Effects Within The PDHID Tower The PDHID Tower is heated directly to roughly 100C to minimize moisture condensation It is critical to allow the PDHID Tower to heat thoroughly before energizing the discharge arc igniting the flame Failure to do so may trap moisture within the PDHID Tower and compromise the insulators 8 3 Detector Flow Rate Effects Carrier gas flow rate through the PDHID does not influence the rate of ionization However the
45. ds Therefore it is recommended to use a Substantial calibration peak concentration to facilitate easy LW and RW measurements Page 40 Peak Performer 1 Users Manual 4 4 2 Analysis Screen Button Function tK ie Moves the cursor upwards KI i 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 Analysis Averaging When enabled the last four chromatograms are averaged data point by data point to create a composite chromatogram which is then quantified using normal techniques Analysis averaging does not average concentration data values From acold 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 Figure 24 Event Editor Screen Page 41 Peak Performer 1 Users Manual 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
46. e 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 NOTE No values to be measured for TCD or PDD and will show up as 0 F Compound Name G Retention Time H Left Point Offset Right Point Offset J Area Page 57 Peak Performer 1 Users Manual K Response Factor L Processing Flag V F or B Columns F to L are repeated for M to S T to Z and AA to AG for the next five compounds listed in the Calibration Data Base 6 2 3 Detector Output The detector output 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 COM1 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
47. e 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 Flit 2 is recommended for sharp narrow peaks such as H2 and FIt 8 is recommended for broad peaks such as CO Valco Instruments Company Inc www vici com Peak Performer 1 Users Manual Table of Contents 2 9 4 1 2 0 4 2 2 5 5 1 4 1 4 1 4 1 4 2 4 1 4 2 1 4 2 1 4 2 2 4 2 3 Page 4 Introduction Installation Considerations Unpacking Instructions General Considerations Carrier Discharge Gas Considerations Installing and Purging of Gas Regulators Electrical Connections Rack Mount Specifications Gas Supplies and Connections Carrier Gas Supply Carrier Gas Purity Carrier Gas Purity Requirements Carrier Gas Connection Regeneration Hydrogen H2 Gas Supply H2 Gas Generators H2 Gas Cylinders Actuator Gas Supply Sample Gas Supply External Calibration Gas Supply Second Sample Supply Calibration Gas Connection for Analyzer with Internal Blender Span Gas Supply For Internal Span Gas Blender Standard Start up Procedure Quick Start Sequence Column Conditioning Detector Conditioning Energizing The PDHID Sample Analysis Calibration Establishing New Instrument Response Factors Shutdown and Transport Peak Performer Operator Interface Set up Screen Set up Screen Upper Section Set up Screen Upper Section Bu
48. e 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 Page 11 Peak Performer 1 Users Manual OPTIONAL STRINGE rl IAWECTION PORTS Co oo oG 8G amp Figure 3 Rack Mount Rear View with Dimensions Page 12 Peak Performer 1 Users Manual Ball Bearing Side ride Model 2507 26 or ulvaiert og anes long Figure 4 Rack Mount Top View with Dimensions 2 5 Gas Supplies and Connections CAUTION Never turn on the instrument without purified helium carrier gas flowing 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 ZF1 b Supply tubing is 1 16 O D x 0 03 I D cleaned and baked T300 stainless steel tubing Page 13 Peak Performer 1 Users Manual e 2 e 7 cou lt gt f SAMPLE 1 SAMPLE 1 ACTUATOR CARRIER FID FID IN OUT IN IN AIR H2 a2 tee m SAMPLE 2 SAMPLE 2 SPAN IN TO FROM ia IN OUT TRAP TRAP I then 90 120 VAC 50 60 Hz i C CO
49. e Zone Out of Range e Temperature Zone Disabled e Detector Zeroing Target Error e Vlamp Low Voltage Out of Range RCP Analyzers Only e FID Flame Temperature Out of Range FID Analyzers Only e Event Program Load Error e Stream Selector Program Error e System Parameters Corrupted e Parameter Change Update Needed e Detector Power Page 52 Peak Performer 1 Users Manual 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 Viewer Details 2014 02 19 15 03 Ioj x Print Name AR 358 2 20 6 2rd Variable BIA Peak Time Sec 191 4 Left Width sec 11 6 Right Width sec 20 Measured Area 10784016 Response Factor a39 F hea BEGEEEE TELL TELL TELL TELL iE T T width Snalysis Variable Flame Temperature Cycle Stream 1 System Alarm Figure 36 Viewer Detail screen showing raw analysis data The information on the screen is linked to run 15 29 displayed in figure 35 5 5 2 Start Menu on the Viewer Taskbar Ay PeakView Ver 5 08 File Stop Chrom View Event Info Upload Run T Single Run Cycle Run Stream Run Figure 37 Start menu on the taskbar Page 53 Peak Performer 1 Users Manual The Start menu contains the following commands ee Single Run selection commands the PP1 to start a Single Run Cycle Run Cycle Run option commands the PP1 to s
50. e half duplex communications only one unit may transmit at a time but allows up to 32 users on a party line network NOTE The RS 422 specification supports four wire full duplex communications two units may transmit at a time and also allows up to 32 users on a party line network The following information is provided to enable the users to install the Peak Performer 1 intoa RS 485 network This system diagram consists of the PP1 RS 232 to RS 485 converter and master host controller x lt PP1 COM2 RS232 to RS485 Converter Master Controller T Power me COM2 RS232 to RS485 al PP 1 Converter At Power Supply Figure 42 System configuration diagram with basic connections 6 6 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 Page 68 Peak Performer 1 Users Manual 7 0 Chromatographic Principles As an analytical system the PP1 PDHID performs four primary functions Sample injection Component separation Component analysis Integrated microprocessor system control with operator and data interface 7 1 Sample Injection A standard air actuated VICI injection valve is used to inject samples Standard PDHID analysis methods use stainless steel 0 2 cc sample loops 7 2 Carrier Gas Purification Chromatographic instrum
51. e the Date Time or Protocols Page Advances the user to the next screen Page 27 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 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 Allows the initialize the detector electronics and establish a consistent baseline signal ie Moves the cursor upwards Ie Moves the cursor downwards Edit Allows the user to energize each heater zone or change heater setpoint temperatures Heat Energizes all the heater zones Page Advances the user to the next screen Page 28 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 Figure 13 Screen Commands After Warm up 4 1 3 1 Set up Screen Middle Section Button Functions Normal Zero Allows the initialize the detector electronics and establish a consistent baseline signal is Moves the cursor upwards i Moves the cursor downwards Edit Allows the user t
52. ed metal getter purifier available for carrier gas purification This style of purifier typically has a hot catalyst element ahead of the heated getter material for complete removal of methane hydrocarbon CH3 a common contaminant in commercial nitrogen sources Hydrogen Carbon Monoxide Carbon Dioxide Hydrocarbons and Moisture carrier gas impurities are reduced to less than 10 ppt by this type of purifier Typical Heated Metallic Getter Purifier Specifications Type Heated Reactive Metal Getter Maximum Flowrate gt 300 cc min lt 5 L min Argon Concentration outlet lt 10 ppb THC Concentration outlet lt 10 ppt CO CO2 Concentration outlet De H2 H2O Concentration outlet Super Expected Life Consult Manufacturer Page 16 Peak Performer 1 Users Manual 2 5 1 2 Carrier Gas Purity Requirements Nitrogen Argon lt 100 ppt total carnier or Helium contaminants Sapa 350 sccm z ii UHP Grade 7 aa ion Hydrogen 25 psig sccm Heated reactive metal getters are the only proven reliable technique for generating the specified carrier gas purification Cold metallic getters and absorption getters do not reliably remove all common critical bulk gas contaminants 2 5 1 3 Carrier Gas Connection The PP1 carrier gas connection utilizes a 1 16 female VICI bulkhead labeled CARRIER IN on the front or rear panel 1 Connect purified He carrier gas supply gas to the carrier bulkhead and set the source regulator
53. en THC Concentration lt 10 ppm CO Concentration lt 10 ppm CO Concentration lt 10 ppm H20 Concentration lt 100 ppm CAUTION High moisture content in the H gas supply has been shown to irreversibily damage the Oz Trap 2 5 2 1 H Gas Generators Peak recommends only the use of Palladium Transfer Tube or Regenerative Drying Hydrogen Generators Hydrogen produced by electrolytic decomposition of water is extremely humid at nearly 100 relative humidity H generators using only single stage gas H2 dryers molecular sieves will saturate with moisture within a week or two of normal use and therefore require frequent manual exchange and regeneration to maintain acceptable H gas quality 2 5 2 2 H2 Gas Cylinders Cylinder sources suitable for use as regeneration H2 include UHP and Zero Quality grades See Section 2 5 2 for detailed specifications Page 18 Peak Performer 1 Users Manual 2 5 3 Actuator Gas Supply In addition to feeding the actuator the helium from the actuator supply is internally used to purge the internal system NO additional helium purge specific connections need to be considered It is NOT necessary to use purified helium as actuator gas The actuator supply is attached at the rear panel of the instrument Attach the Helium gas actuator supply to ACTUATOR IN port on the rear panel Preset the source to 60 80 psig i Nominal 2 2 5 4 Sample Ga
54. ent detection limit is directly related to carrier gas purity Improved carrier gas purity enables improved sensitivity Typical 99 9999 Helium Carrier Gas Specifications Pre Purification ee ee Dewar Consequently the analyzer s minimum detectable quantity MDQ would be quite high gt 10 ppm unless the carrier gas is purified Peak recommends use of the best quality heated metal getter purifier available for carrier gas purification This style of purifier typically has a hot catalyst element ahead of the heated getter material for complete removed of methane hydrocarbon CH4 a common contaminant in commercial nitrogen sources Hydrogen Carbon Monoxide Carbon Dioxide Hydrocarbons and Moisture carrier gas impurities are reduced to less than 10 ppt by this type of purifier Page 69 Peak Performer 1 Users Manual Gas Purifier Specifications Heated Reactive Metal Getter Maximum Flowrate gt 300 cc min lt 5 L min Gases Purified Helium Argon Concentration outlet lt 10 ppb THC Concentration outlet lt 10 ppt CO CO Concentration outlet ae H2 H2O Concentration outlet SOPPI Expected Life Consult Manufacturer 7 3 Component Separation Component separation is normally performed by isothermal packed analytical columns Column materials vary by application and are noted in the test report documentation Please contact Peak Laboratories for additional details specific to your application In general
55. er Go beyond finger tight but do not tighten the nut all the way some leakage is required for the purging operation 3 Turn the output pressure regulating knob completely counterclockwise 4 Open the cylinder on off valve slightly and quickly close it again 5 Adjust the tightness of the regulator connecting nut to allow a pressure reduction of 690 kPa sec 100 psi sec With a new bottle the gauge should start out at about 14 MPa 2000 psi 6 When the pressure drops into the 1 4 3 4 MPa 200 500 psi range open the cylinder on off valve slightly and quickly close it again 7 Repeat Step 5 eight or ten times to be certain that all the air is purged On the final purge tighten the regulator connecting nut very securely as the pressure approaches the 2 1 3 4 MPa 300 500 psi range 8 Open the cylinder valve to pressurize the regulator once again Close the valve and observe the needle of the high pressure gauge for 15 minutes If it doesnt move there is no critical leak on the high pressure side of the regulator CAUTION Never use leak detecting fluids on any part of this system Page 10 Peak Performer 1 Users Manual 2 3 Electrical Connections Verify the correct operating voltage as marked on the rear of the analyzer at the main power switch Attach a standard power cable to the rear of the instrument see Figure 1 and connect to an appropriately grounded outlet Power Cord PP1 Power Entry
56. er as text files suffixed chm The text files can be imported into most common laboratory analysis soreadsheet and word processor programs as needed Data points in the chromatogram file are time sequenced at 0 2 seconds per data point The filename of the chromatogram file is generated by time of day on the host computer and the file is stored in a folder that corresponds to the date of collection A corresponding Viewer data file is created and or updated at the time the chromatogram file is created As an example the fourth chromatogram shown in Figure 36 would be archived on the host computer as follows Main directory C Viewer Sub directory 2013 12 05 YYYY MM DD of archive creation Viewer filename 2013 12 05 csv Filename 0851 chm 5 5 4 2 File Menu on the Chrom Viewer Taskbar BA Chrom iewer 2014 02 19 1503 chm Ioj xj Fie viewer Analysis DB Open ATTEN 5A SPAH Saves ake al ak Bn a Send To Analyzer Receive from nalyzer H2 AR D Figure 39 Baseline Selected Page 55 Peak Performer 1 Users Manual PA Chrom iewer 27014 02 195 1503 chm ioj x File viewer Analysis DB Open ATTEN 512 SFAH 500 Saves 4 gt 4 Send To Analyzer Receive from Analyzer Figure 40 Baseline Deselected The File menu offers the following commands j Funetion avert Opens a chromatogram file Use this command to open and load the chromatogram data for display
57. eset Single Register Packet Example In the next example the PP1 s Modbus slave address is 143 and the master requests to write the value of 3 to Modbus register 40004 In accordance with the Modbus protocol register 40004 is numbered as address 3 when requested Slave Address 143 8F Hex Modbus Function 06 06 Hex Starting Register 3 0003 Hex Preset Data 3 0002 Hex Request Packet non shaded background denotes the DATA field of the packet LRC Slave Modbus mae Register Response Packet LRC Slave Modbus es Register As you can see from the response packet above the response is the echo of the requested packet Page 63 Peak Performer 1 Users Manual 6 4 4 Modbus Data Format The PP1 is capable of exporting all holding registers into the Modbus protocol The PP1 data available in a contiguous set of Modbus holding registers The PP1 output registers are located in the Modbus register map from 40001 to 40099 The actual location is defined in table 3 below Six Data Formats Used in the PP1 Analyzer UINT16 16 bit unsigned integer 0 to 65 535 INT 16 16 bit signed integer 32 768 to 32 767 UINT32 32 bit unsigned integer 0 to 4 294 967 295 INT32 32 bit signed integer 2 147 483 648 to 2 147 483 647 Boolean Packed Boolean Format 8CharString 8 character string format 16 bit Integer Format Unsigned and signed 16 bit integer formats are the simplest formats Each PP1 addre
58. gas flowing CAUTION Do not exceed 210 C of column oven temperature Temperatures in excess of 210 C can destroy column material 1 Connect the front jumper tube between SAMPLE IN and BYPASS OUT 2 Use the t and keys to navigate and alter the SET value for the Column heater zone to 180 to 200 C 3 After 8 to 12 hours of stable conditioning temperature the column temperature may be restored to the original factory setting 4 After normal operating temperature is achieved the front jumper tube may be reconnected between SAMPLE IN and SAMPLE OUT 5 After a 5 10 minute detector re equilibration period samples may be run Normal operating temperatures vary with specific application Consult the Final Test Data for special settings special reconditioning requirements etc for your application 3 3 Detector Conditioning CAUTION The maximum detector operating temperatures for the PDHID is 150 C The PDHID does not normally require conditioning treatment however it does require 8 to 12 hours at normal operating temperature to achieve optimum stable performance Normal detector operating temperature for the PDHID is 100 C although operating temperatures may vary with the specific application See Section 8 for details concerning the effects of operating parameters temperature and flow on PDHID detector performance 3 4 Energizing the PDHID 1 Verify that Carrier and Actuator
59. he current decreases there is a leak at that connection Tighten the fitting and test it again repeating as necessary until there is no change in the standing current 3 Reconnect the column When the standing current reaches an acceptable level the detector is ready for use If the current stays high use this method to check for leaks at the column detector connection internal and external plumbing 4 A portable helium detector eg Gow Mac model 21 070 can be used to check for gross leaks Page 90 Peak Performer 1 Users Manual 9 0 Analyzer PDHID Maintenance and Service Procedures Figure 59 Chassis Overview PEAK PERFORMER 1 PDHID COMPONENT LAYOUT LCD TOUCHSCREEN ASSEMBLY MCPU PCB ASSEMBLY VALVE 1 6 PORT FLOW CONTROL NEEDLE VALVE ASSSEMBLY COLOMN OVEN WITHOUT COVER VALVE 2 6 PORT PDHID CONTROLLER PCB ASSEMBLY WITH COVER PDHID ASSEMBLY REAR PANEL PCB ASSEMBLY INCLUDES MAIN DC POWER SUPPLY ee ee ae ae a Page 91 Peak Performer 1 Users Manual 9 1 Peak Performer 1 System Block Diagram Detector Module e m e i o a l l l Toco c 1 SWA LINE Al WOU CUVUOSE a al aH aroa L ZmmaAQw Figure 77 PP1 Functional Block and Interconnect Diagram Page 92 Peak Performer 1 Users Manual 9 2 Monitor Regulator Pressures Gas supply settings should not vary Carrier Actuator and H2 settings may shift when supply cylinders run low and should be checked period
60. he request packet The PP1 only supports Modbus functions 03 and 06 The address referenced in the data field is an invalid address for the specified function This can also indicate that the registers requested are not within the valid register range of the PP1 a The value referenced in the data field is not allowed for the referenced register Oo M The LRC checksum is invalid Table 2 Exception Codes supported by the PP1 Exception Response Packet Slave Modbus l SSS o i e Page 65 Peak Performer 1 Users Manual PP1 Modbus Registers Map The PP1 Modbus holding register map defines a set of parameters which are treated as holding registers having addresses 4XXXX According to the Modbus protocol in response to a request for register 4XXXX of a particular slave device the Modbus master reads register XXXX 1from the slave For example Modbus register 40054 corresponds to holding register 53 There are two classes of Modbus registers within the PP1 Modbus Output Registers and External Control Registers See Table 3 below PP1 Modbus Holding Registers Map 40001 Unit serial number UINT16 40002 Main controller software version UINT16 40003 Detector type RCP FID PDD TCD UINT16 aeons Run Mode Idle Single Cycle UINT16 Stream 40014 40039 _ Sp are SSS o o o o Compound 1 Concentration bose 40048 40049 Spare oo o oo Compound 2 Concentration 40058 40059 Spare C CSC C dNSCOCOC
61. ically to maintain consistent flame settings and peak retention times Varying carrier pressures can cause peaks to shift out of set retention times and not be flagged 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 9 4 ALTERING THE ANALYTICAL RANGE OF THE INSTRUMENT Sample loops are very easy to customize 1 Determine the desired loop volume Analytical range is directly proportional to sample loop size 2 Select tubing tube internal diameter to use In general use the largest ID tube possible to avoid flow restrictions Guidelines 0 040 ID for 3 8 cc to 2 cc loops 0 030 ID for 3 16 cc to 1 2 cc loops 0 020 ID for 50 uL to 1 4 cc loops Note the shortest practical length of tubing for a sample
62. igh Background Current Checking for leaks in the Discharge Gas Plumbing Analyzer PDHID Maintenance and Service Procedures Peak Performer 1 System Block Diagram Monitor Regulator Pressures Verifying Valve Integrity Carrier Blank Zero Gas Altering the Analytical Range of the Instrument Testing the Heater Resistance Adjusting the Display Contrast Adjusting the 5 Volt DC Power Supply Main DC Power Supply Replacement COM 1 Connections on Multiple Analyzers to a Single Oxygen Trap Regeneration Procedure Peak Performer 1 Users Manual PEAK PERFORMER 1 1 0 Introduction The Peak Laboratories Peak Performer 1 PP1 gas analyzer is a trace level gas analysis system capable of detecting impurities 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 Sampling hardware 4 6 and 10 port VICI valves Covered Helium Purged Isothermal Mandrel Heating Single or Multiple 1 8 Packed Capacity Columns or 0 53 mm Capillary Columns Temperature range A
63. igidly established only by the Peak Database parameters Figure 62 Baseline as Established in Baseline Mode Peaks quantified using this method are denoted with an B in the last column of the data report 7 6 2 Peak Quantification Fixed Width Mode The Fixed Width Mode is enabled when the maximum detector peak signal value 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 82 Peak Performer 1 Users Manual The time associated with the peak maximum signal must be within the time regime of interest PkCen 12 PkWin for any peak quantification to occur In Fixed Width Mode the normal detector baseline is calculated based upon the peak maximum signal time value rather than the PkCen value Peak start time Peak end time Peak signal maximum time value LW Peak signal maximum time value RW E E 3 co a Figure 63 Baseline as Established in Fixed Width Mode Peaks are quantified using this method are denoted with a F 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 a
64. ion to perform Similarly the function field of a response packet tells the master what function the addressed slave has just performed On page 5 lists the Modbus functions supported by the PP1 when acting as slave please refer to Table 2 Modbus Functions Supported by the PP1 as Slave Data Field The data field of a Modbus request is variable length and depends on the function This field contains information required by the slave device to perform the command specified in a request packet or data being passed back by the slave device ina response packet Data in this field is contained in 16 bit registers Registers are transmitted in the order of high order byte first low order byte second Example e A 16 bit register contains the value 62BE Hex four ASCII characters e High order byte 62 Hex two ASCII characters e Low order byte BE Hex two ASCII characters e This register is transmitted in the order 6 2 B E four ASCII characters e Error Check Field LRC Checksum two ASCII characters Error Check Field In Modbus ASCII mode an 8 bit Longitudinal Redundancy Check LRC algorithm is used to compute the checksum byte The checksum field enables the receiving device to determine if a packet is corrupted with transmission errors The sending device calculates the checksum 8 bit value based on every byte in the packet using the LRC algorithm The calculated value is inserted in the error check field The receiving device
65. le valve will enable the operator to minimize baseline drift and create a smooth chromatogram 4 to Ez L EA pace i i Fo feu Lice R gt WP oe FS al Fi a Ee ee ee a eas a i Figure 51 Properly Flow Balanced Detector Baseline Page 74 Peak Performer 1 Users Manual LY fat gf ba far IP 2 JFE al l Figure 52 High PDHID flow from NV1 note rise after the V2 CCW command E SPAN in Cone pow on ois if fat f br oe fe ae jpe o pi l cea Flame Temp Analysis Type Figure 53 Low PDHID flow from NV1 note drop after the V2 CCW command Differences in COLUMN flow during normal and venting valve positions will be expressed as shifts in peak retention time compared to a chromatogram without any venting action Page 75 Peak Performer 1 Users Manual a W2 Flow 59 sccm o a AW Flow 39 sccm NY Flow 79 sccm o L I N TTR r A md Y Rj f TNE ENAN went D 20 40 60 60 100 120 140 160 180 200 220 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 chrom
66. ls generated from this information appear on the rear panel s green DIN terminal blocks See Figure 5 or 19 lt eee e e e a e oeae a eme e Channel Figure 18 Analog Interface Screen Page 33 Peak Performer 1 Users Manual 4 2 1 Analog Interface Screen Button Function Page 34 Range Manset Page Moves the cursor upwards Moves the cursor downwards Allows the user to select the full scale concentration range associated with the maximum 1 00 VDC signal for each compound The ranges are manually set from 0 gt 999999 ppb e g 0 1000 ppb readings in the analyzer 0 1 00 VDC output scale where a 500 ppb value would output 0 5 VDC 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 In lieu of a specific concentrations range the RANGE buiton for the recorder function toggles through choices of raw signal attenuation X1 X2 X4 X8 X16 X64 This function is similar to the RANGE switch on a chart recorder This function only affects the recorder output not the individual compound trends Temporarily over rides the signal output with a known output voltage for test purposes Four MANSET options are available 0 00 VDC 0 25 VDC 0 5 VDC and 1 VDC There is not any zero offset or full voltage scale adjustment within the PP1 if this function is a
67. mbient 50 C gt 295 C Temperature stability 0 5 C Page 7 Peak Performer 1 Users Manual Pulse Discharge lonization Detector PDHID 930 Series The Peak Performer PDHID uses Peak Laboratories standard process interface GC platform and electronics integrated with Valco Instruments www vici com D 2 detector and pulse module in PDHID mode The GC is optimized to measure ppb levels of argon and or nitrogen impurities in a variety of UHP ultra high purity matrix gases The PDHID is a universal detector and the utmost care must be used to integrate the system free from leaks Final product performance will depend on the quality of components used to delivery both sample and support gases We always recommend best install practices and high purity components to maximize product performance The table below illustrates some typical compounds and detection capabilities of the PDHID Detection limits vary with matrix gas and impurities specified Detected Compound Typical Detection Limit 1 10 ppb aan Page 8 Peak Performer 1 Users Manual 2 0 2 1 2 2 Installation Considerations Unpacking Instructions Remove the Peak Performer 1 from the packing material or traveling case taking care to not scar the exterior surfaces of the analyzer set the analyzer on a firm even surface and remove the protective plastic wrap Each analyzer ships with adequate supplies for installation Be certain to rem
68. nts for software versions 4 and above Page 96 Peak Performer 1 Users Manual 9 7 Adjusting the 5 Volt DC Supply Adjust this potentiometer so that the volatge is between the RED and BLACK wires at 5 1 to 5 2 VDC Tha a gt Tama Poy DC DET P PU a Lal TP 5 e 7 i i i E gt EN AO 12V AC SSR3 ha YP gt 1 DE 3 J2 RCP LAMP ull Figure 66 Adjusting the 5 Volt DC Supply Page 97 Peak Performer 1 Users Manual 9 8 Main DC Power Supply Replacement 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 LA 7 aae Wt i sg FG TD i ws f Z AY Av vant be 9 ee i ig XY a ASS y a ak Figure 67a 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 2 Figure 84b Main DC Power Page 98 Peak Performer 1 Users Manual i gt fale Ni am OHHH ES g a a RCP T Figure 68 Main DC Power Supply with Shield Removed Unscrew the 4 each 14 standoffs
69. nvolution is one such method Convolution rolls two waveforms together as the product of data matrices with the resulting new waveform having exaggerated characteristics Detector Baseline Cross Multiplied by the Convolution Filter Yields the Resultant Baseline Figure 61 Convolution to Enhance Signal Characteristics As seen in Figure 61 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 Consequenily there are several different convolving Page 81 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 of the optimum filter width is best performed by re processing chromatograms representing typical peaks 7 6 1 Peak Quantification Baseline Mode When the PkHgt variable is set to zero the Baseline 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 determinations are disabled and the normal detector baseline is r
70. o energize de energize each heater zone or change heater setpoint temperatures Page Advances the user to the next screen Page 29 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 eleven individual error conditions that can cause the status LED on the front panel to glow red Detector Communication Error Temperature Zone Out of Range Temperature Zone Disabled Detector Zeroing Target Error Page 30 Light Turns Green When Alarm is Cleared Peak Performer 1 Users Manual Vlamp Low Voltage Out of Range FID Flame Temperature Out of Range Event Program Load Error Stream Selector Program Error system Parameters Corrupted Parameter Change Update Needed Detector Power off For PDHID amp TCD Analyzers Only 4 1 4 2 Clearing Error Messages on the Set up Screen Lower Section Figure 15 Typical PDHID 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 e
71. ove 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 Analyzer size is 26 L x 17 W x 7 H Maximum operating environment for the PP1 analyzer is 30 C Minimum operating environment for PP1 analyzer is 15 C Power consumption is 160 watts maximum Fuse size is 2 5 ampere 250 VAC 5 x 20 mm SLO BLO Free air flow for adequate ventilation to the rear of the unit is required Communication between the PP1 and your PC is via 9 pin straight through cable connection to COM 1 and COM 2 Analog outputs are available from the DIN screw terminal strips on the rear panel H venting He shut off valving and H2 supply safety equipment must be supplied by customer Do not use plastic polymer or copper tubes for gas handling and interconnections Use only stainless steel tubing Do not turn the unit on until the helium carrier gas is flowing through the detector Do not shut off or disconnect the discharge gas when the detector is hot even if the unit is turned off Turn off power switches and allow the detector to cool down naturally before disconnecting or shutting off the discharge gas 1 hour Do not cover the unit with materials or devices which would restrict
72. requirement Peak Labs recommends the use of standard commercial voltage converters attached externally to the analyzer Advances the user to the next screen Peak Performer 1 Users Manual 4 2 2 Analog Interface Connections and Wiring All analog interface connections are made via the rear panel DIN connector To make a proper connection strip all wires back approx 3 8 unscrew the terminal locking screw fully insert the wire and tighten A common error is insufficient length of bare wire creating the condition where the terminal contacts only the wire insulation ANALOG 1 ANALOG 2 ANALOG 3 ANALOG4 ANALOG 5 ANALOG 6 RECORDER REMOTE START FID FLAME GEN ALARM 00 00000000 0000000000 COMMON GND COMMON GND COMMON GND COMMON GND COMMON GND COMMON GND COMMON GND COMMON GND FID FLAME GEN ALARM 200 240 VAC 50 60 Hz 160 WATTS Figure 19 Analog Output Connections NOTE The analog outputs are locked if the Port 1 Protocol on the MAIN SCREEN is set to DETECTOR See Section 4 1 1 4 2 3 Analog Interface Wiring Breakdown There are 10 total terminal connectors from the top the connectors ID s are Terminals 1 6 e Impurity Trends All channels are mapped to the calibration database All channels are 0 1 VDC All channels signals are updated at the end of run and held All channels are manually scalable on the ANALOG INTERFACE SCREEN e g 0
73. rt self powered Hub Inland 08302 or equivalent 5 2 Installing the Peak View Software 1 Place Peak View software CD ROM disk into CD ROM drive 2 If Autorun is enabled follow the installation screen prompts 3 If the CD ROM does not automatically launch select SETUP from CD ROM disk 4 The installation software will auto install the Viewer in a folder under the PC s main drive as the default The user has options from the installation process to create a new folder and install in a new location 5 3 Starting the Peak View Software 1 Double click the Peak View icon on the Desktop or 2 Select START button on the bottom Taskbar 3 Select PROGRAMS select PEAK VIEW and double click to launch move to Peak View 5 4 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 See Section 6 for details on communications protocols Page 48 Peak Performer 1 Users Manual 5 5 Viewer Software Window The Viewer window shown in Figure 33 shows the main Viewer screen with a RED DOT in the upper right corner This RED DOT signifies that there is a connection problem with the PC and the PP1 Verifying the following can solve this connection problem Communication Settings Connection of 9 pin cable between PC and PP1 RS 232 cable plugged into the PP1 s COM 1 port P
74. s 31 Go back to the Viewer window 32 Under File on toolbar select Port Settings 33 Enter COM number assigned to second USB to DB9 adapter probably COMS 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 103 Peak Performer 1 Users Manual 9 10 Oxygen Trap Regeneration Procedure For those PP1 analyzers using the Oxygen Trap module this procedure is used when the Peak Laboratories PDHID oxygen trap has been exhausted from multiple injections of pure oxygen samples Frequency of the regeneration cycle will depend on the volume of the injections and number of injections Once oxygen breaks through the trap the Argon impurity or calibration peak will be buried in the oxygen upset making trace lt 1 ppm analysis impossible in bulk Os H vent He supply and associated safety must be supplied by customer during regeneration cycle Once the oxygen trap capacity is exhauste
75. s 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 Higher sample pressures can be used if a fixed restrictor is set and calibrated to the incoming pressure Please contact the factory for sample handling instructions if these input conditions are not available SAMPLE GAS SUPPLY FLOW RESTRICTOR 30 60 seem ATMOSPHERIC PRESSURE QO TOPP e 8h T ni Figure 7 Sample Supply Flow Schematic Page 19 Peak Performer 1 Users Manual 2 5 4 1 External Calibration Gas Supply Certified calibration standards must be connected periodically to the PP1 for verification of analyzer response When using a mobile calibration gas source such as high pressure cylinder the plumbing arrangement shown in figure 7 is recommended The calibration source can be connected to the SAMPLE IN port on the analyzer front panel or alternatively make sure the front panel jumper between SAMPLE OUT and SAMPLE IN is installed and connect the calibration source to the rear panel SAMPLE IN port The SAMPLE OUT port must be unrestricted when using either method 2 5 4 2 Second Sample Gas Supply Peak Labs offers an optional second
76. ss corresponds to one Modbus Holding Register If the format is unsigned the value range for the output registers is 0 to 65535 If the format is signed the value range is 32767 to 32767 32 bit Integer Format To accommodate values that can reach beyond the 16 bit range the Modbus Slave provides 32 bit integer format as an output option In signed and unsigned 32 bit integer formats each PP1 address corresponds to two 16 bit Modbus Holding Registers A 32 bit register represented in 32 bit integer format is passed via communications as two 16 bit registers High Order Register value 65536 Low Order Register value modulus 65536 Example Unsigned 32 bit Value 12345678 is passed in unsigned 32 bit integer format 12345678 OOBC614E Hex High Order OOBCHex Low Order 614EHex Example Signed 32 bit Value 12345678 is passed in signed 32 bit integer format 12345678 FF439EB2 Hex High Order FF43 Hex Low Order 9EB2 Hex Packed Boolean Format Boolean registers are packed into a single Modbus register The boolean outputs corresponds to one bit in the single output register of the module The relationship is left to right the first input register corresponds to the left most bit in the 16 bit output register etc Page 64 Peak Performer 1 Users Manual Example Packed Boolean Format Six Boolean registers are linked to a single Modbus register which is configured for Packed Boole
77. ssion indicator is a STX character 02 hex and the end of transmission indicator is a ETX character 03 hex The fields within each record are defined as follows lt STX gt SSS YYYY MM DD HH MM S S E X N AREA CONC N AREA CONG N AREA CONC lt ETX gt SSS Serial Number of Unit This is also used as the RS 485 unit ID YYYY MM DD Date 2013 12 05 HH MM SS Time 12 23 44 12 hours 23 minutes 44 seconds E General Error Alarm 0 No Error 1 Error X Stream Number e N Name of Impurity x6 e AREA Are of Impurity x6 e CONC Concentration of Impurity x6 NOTE The least significant decimal of the concentration resolution represents 0 1 ppb CONC reading of 1 represents a 0 1 ppb concentration level 6 4 Modbus Protocol and Register Map for Peak Laboratories Devices This section describes the Modbus protocol for Peak Laboratories PP1 analyzer It is assumed that the reader is familiar with the Modbus protocol and serial communications in general The following rules define the protocol for information transfer between a Modbus MASTER device and the Modbus SLAVE The MASTER initiates and controls all information transfer on the communications channel A SLAVE device never initiates a communications sequence All communications activity occurs in the form of PACKETS A packet is a serial string of 7 bit ASCII bytes All PACKETS transmitted by the MASTER are REQUESTS All PACKETS transmitte
78. ssociated 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 83 Peak Performer 1 Users Manual z Oo Oo 2 2 N N Figure 64 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 64 The hypothetical calculation of the peak start time is labeled LW in Figure 65 Peak Maximum s S So aed N N PEAK START Figure 65 Progression of Peak Start Time Calculation After calculating the hypothetical peak area based upon the L and R values the mathematics package makes another peak area calculation using a slightly earlier time value The peak areas of the two calculations are compared and if the peak area increases by more than 0 5 the mathematics package repeats the process The net effect is illustrated in Figure 65 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 84 Peak Performer 1 Users Manual The trial evaluation of peak area continues for the peak ending point again using a fixed percentage of the L
79. tart 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 5 3 Stop Menu on the Viewer Taskbar The Stop Command selection instantly sends a command the PP1 to terminate the current run immediately 5 5 4 Chrom View Menu and Chromatograph Viewer Window The Chrom View menu selection opens the Chromatograph Viewer window Two methods can open the Chrom Viewer window 1 The first method is to select the Chrom View menu selection from the Viewer taskbar and then select a chm file to display 2 The second method of opening the Chrom Viewer is double clicking one of the concentration values displayed in the Viewer window Using either method after the chromatogram data is loaded the display can be adjusted by the Offset Attenuation and Span scroll bars zmizi File viewer Analysis DB Open ATTEN 512 SPAN 500 Saves 4 r 4 gt Send To Analyzer Receive from Analyzer gt N2 AR i E Figure 38 Chromatogram Viewer Window Page 54 Peak Performer 1 Users Manual 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 5 4 1 Chromatogram Files Chromatograms are archived on the host comput
80. 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 Page 38 Peak Performer 1 Users Manual 4 4 Analysis Database Screen The Analysis Database screen stores critical information regarding peak identification and quantification parameters Figure 22 Analysis Database Screen 4 4 1 Analysis Database Parameters Name The peak identification tag expressed as 5 alphanumeric characters A Z 0 9 PkCen The normally expected peak retention time in seconds used for assigning the appropriate Name LW The typical time span measured from the start of the peak s baseline rise to the peak apex PkCen in seconds Minimum value is 3 maximum is 35 RW The typical time span measured from the peak s apex PkCen to the end of the peak s baseline decline in seconds Minimum value is 3 maximum is 35 PkWin Total tolerance window in seconds for assignment of a Name to a quantified chromatographic peak
81. the next run HEAT ON Not currently in use HEAT OFF Not currently in use 4 5 2 Event Editor Screen Button Function Tz Moves the cursor upwards J 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 Purchased Option Peak offers a dual sample stream option for most analyzers The selection and timing of sample streams can be pre programmed on this screen NOTE This screen will only appear when the STREAM method of analysis is selected on the RUN screen FTT 12914 7 Stream Selector Program Editor Marual Select Figure 25 Stream Selector Sequence Screen Page 42 Peak Performer 1 Users Manual 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 before switching to other stream 4 6 2 Stream Selector Program Editor Screen Button Function T Moves the cursor upwards J 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
82. tinuous 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 Page 45 Peak Performer 1 Users Manual 4 7 3 Manual Screen Sub Screen of the Run Screen The Manual sub screen allows the operator to invoke all the event program commands on demand Figure 29 Run Manual screen 4 7 3 1 Manual Screen Button Functions Zero Pressing this key will electronically zero the detector Ignite Pressing this button applies power to the Pulse Supply Module Bias Toggles the high voltage within the PDHID to ON BIAS or OFF V1 Toggles Valve 1 between CW and CCW positions V2 Toggles Valve 2 between CW and CCW positions Esc Exits from the Manual sub screen to the Run screen Page 46 Peak Performer 1 Users Manual 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
83. to approximately 60 psig 2 There are no internal regulators in the standard PP1 PDHID all gas pressures are controlled by external regulators customer supplied 3 Verify the BYPASS OUT port is flowing approximately 25 35 sccm Carrier flow within the analyzer is split with a portion of the flow passing through a gas sampling valve the other portion passes through a restrictor tube terminating at the location of the BYPASS OUT port Under normal operating conditions this port is plugged During column reconditioning the plug may be removed and the SAMPLE IN switched to the bypass flow In this manner column reconditioning may be performed without requiring a shutdown of the sample gas flow avoiding the lengthy re equilibration period 2 5 2 Regeneration Hydrogen H2 Gas Supply H venting He shut off valving and H2 supply safety equipment must be supplied by customer Some PP1 PDHID units come with an O Trap Module The O Trap Module has an H gas connection utilizing 1 16 female VICI bulkhead fittings Page 17 Peak Performer 1 Users Manual 1 Connect the Hydrogen gas supply to the bulkhead and set the source regulator to approximately 25 psig 2 There are no internal regulators in the standard O2 Trap Module all gas pressures are controlled by external regulators customer supplied Regeneration Hydrogen Gas Specifications High Pressure Cylinder or Hydrogen Generator Gas Type Hydrog
84. tton 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 Error Messages on the Set up Screen Lower Section Clearing Error Messages on the Set up Screen Lower Section 31 Set up Screen Lower Section Button Functions Analog Interface Trend and Recorder Output Screen Analog Interface Screen Button Function Analog Interface Connections and Wiring Analog Interface Wiring Breakdown 6 4 4 Page 5 Peak Performer 1 Users Manual Calibration Database Screen Calibration Screen Button Functions Calibration Establishing New instrument Response Factors Analysis Database Screen Analysis Screen Parameters Analysis Screen Button Function Event Program Editor Screen Event Program Commands Event Editor Screen Button Function Stream Selector Sequence Editor Screen Stream Selector Commands Stream Selector Program Editor Screen Button Function Run Chromatogram Screen Run Screen Button Functions Run Screen Continuous Monitoring Analysis Manual Screen Sub Screen of Run Screen Manual Screen Button Functions Display Screen Sub screen of Run Screen Display Screen Button Functions Viewer Software System Requirements Installing the Viewer Software Starting the Viewer Software COM1 COM2 Port and Cable Wiring Viewer Software Window File Men
85. u on the Viewer Taskbar Communication Setting Window Viewer Line Details Window Start Menu on the Viewer Taskbar Stop Command on the Viewer Taskbar Chrom View Window and Chromatogram Viewer Window Chromatogram Files File Menu on the Chrom Viewer Taskbar Viewer Menu on the Chrom Viewer Taskbar Communication Port Protocols and Data Formats COM1 COM2 Port and Cable Wiring Port 1 Protocol COM 1 Port Settings Peak View Output Format Format of columns in CSV file 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 PLC Output Format Trend Analog Output Format Mode Transmission Modbus Packet Structure Packet Communications Modbus Data Format Page 6 Peak Performer 1 Users Manual Broadcast Packets Trend Analog Outputs Setting up a RS485 Network RS232 to RS485 Converters Chromatographic Principles Sample Injection Carrier Gas Purification Component Separation Venting and Flow Balancing Effects of Temperature and Flow on Analytical Columns Peak Identification and Quantification Peak Quantification Baseline Mode Peak Quantification Fixed Width Mode Peak Quantification Variable Mode Pulse Discharge Helium lonization Detector PDHID Helium lonization Detector Principles Temperature Effects Within the PDHID Tower Detector Flow Rate Effects Troubleshooting H
86. uld 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 H venting He shut off valve and H2 supply safety equipment must be supplied by customer Page 2 Peak Performer 1 Users Manual Glossary and Terms PDHID HSD Molecular Sieve Unibeads Purity Span Gas Response Factor Name PkCen LW RW PkWin PkHgt Fit VICI Page 3 Pulsed Discharge Helium lonization Detector HayeSep D column packing material Zeolite column packing material Silica column packing material Amount of undesired elements in a gas supply Gas supply with known certified amounts of specific compounds Proportionality factor between area count units and concentration units Peak identification tag Expected peak retention time in seconds Typical time span measured from the start of the peak s baseline rise to the peak apex PkCen in seconds Typical time span measured from the peak s apex PkCen to the end of the peak s baseline decline in seconds Total tolerance window in seconds for assignment of a Name to a quantified chromatographic 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 Variabl
87. ur computer 8 Follow installation instructions that come with USB to DB9 adapter I confirm that it is okay to click the Continue anyway box 9 Your computer may prompt to install the USB to DBY 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 it s COM4 on most computers 16 Go back to the Viewer window 17 Under File on toolbar select Port Settings 18 Enter COM number assigned to first USB to DB9 adapter probably COM4 check that Baud Rate 38400 Data Bits 8 Stop Bits 1 19 Click OK box to save these settings 20 Communications settings for that USB to DB9 adapter will be saved in the folder and will be
88. xist the error message may re appear Accept Allows the user to acknowledge and clear error messages E Moves the cursor upwards Moves the cursor downwards Page Advances the user to the next screen Page 31 Peak Performer 1 Users Manual 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 Figure 16 Parameter Change Error Message Accept Allows the user to initiate permanent updates to non volatile memory ie Moves the cursor upwards he Moves the cursor downwards Page Advances the user to the next screen Pressing the ACCEPT button alters the screen appearance Page 32 Peak Performer 1 Users Manual Figure 17 Parameter Change Prompt 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 Analog signa
89. y to maintain pure gas flow to the detector This pure gas flow is provided by an additional branch on the internal carrier gas main line feeding other ports on the valve Ultra high purity flow control components can be bulky and expensive To diminish installed cost of flow control components Peak has chosen a different method based upon flow restrictors to create a flow divider A typical flow divider is shown in Figure 50 Page 73 Peak Performer 1 Users Manual CARRIER GAS MAIN LINE FLOW ADJUSTMENT NEEDLE VALVE MAIN FLOW LIMITER 110 sccm 60 PSIG EXCESS FLOW VENT TO DETECTOR DETECTOR BALANCE RESTRICTOR Figure 50 Flow Divider Schematic The gas flow path to the detector is extremely clean and free of moving parts The gas passing from the main flow limiting restrictor can be split to follow both gas paths Studying the schematic it can be seen that the detector flow can be adjusted by changing the amount of gas that is allowed to exit via the excess flow vent as more gas exits the excess flow vent less gas is available to flow towards the detector The controlling needle valves for detector flow rate and column venting are co mounted in the chassis for convenience see Figure 61 The detector flow control needle valve is color coded red Differences in DETECTOR flow during normal and venting valve positions can be expressed as shifts in detector baseline Careful adjustment of the detector flow control need

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