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44

Model 5380 PFPD Operator’s Manual
Rev. 3.1

11. Split the air supply using a T-connector and attach one arm of the split supply

to the AUX 4 connector and the other arm to the AUX 5 connector using a

Q

/

i

" nut and ferrule. Make sure that the gas lines are pushed into the connector

as far as they will go before tightening the nuts onto the connectors. Securely
tighten the 

Q

/

i

" nuts using a 

U

/

qy

" wrench.

12. Remove the preassembled AUX EPC pneumatics kit for the PFPD (Part

#286344) from its container, taking care not to bend any of the previously
formed gas lines.

13. Install the AUX EPC pneumatics kit in the open compartment behind the

auxiliary EPC manifold module. Secure its aluminum bracket to the pneumat-
ics compartment using the two supplied Torx T-20 screws (Part #252585).

14. Remove the protective covers from the ends of the preformed gas lines

leading from the AUX EPC pneumatics kit.

15. Attach these lines to the corresponding gas outlet on the OI gas outlet block

(see Figure 4.10) using a 

Q

/

qy

" nut (Part #223057) and ferrule (Part #216358).

Make sure that the number on each gas line and gas outlet to which the gas
line is attached correspond. Make sure that the gas lines are pushed into the
connector as far as they will go before tightening the nuts into the gas outlet
block. Securely tighten the nuts using a 

T

/

qy

" wrench.

16. Cut the nylon tyraps holding the 

Q

/

qy

" stainless steel gas lines from the PFPD

together. Do not remove the nylon tags designating the COMB and WALL
gas lines. Unroll the gas lines without kinking them.

17. Route the gas lines to the pneumatics compartment in the back of the GC.

18. Remove the plastic protector caps on the ends of the COMB and WALL gas

lines leading from the base of the PFPD, and the protector plugs from the
COMB and WALL gas connectors in the compartment behind the Agilent
6890 GC’s gas control module.

19. Connect the COMB gas line from the base of the PFPD assembly to the open

port below the fine adjust needle marked COMB and the WALL gas line to
the open port on the T-connector marked WALL using a 

Q

/

qy

" nut and ferrule

in both cases (Figure 4.10). Make sure that the gas lines are pushed into the
connector as far as they will go before tightening the nuts onto the connector.
Securely tighten the nut using a 

T

/

qy

" wrench.

20. Gently turn the fine adjust needle valve (Part #282491) protruding from the

top of the GC’s gas control module to the OFF position (clockwise) (see
Figure 4.10). Do not tighten down as this can damage the needle. Then open
two full turns counterclockwise.

21. Replace the flame arrestor located on top of the detector cap with the barbed

fitting (Part #202077) included in the PFPD Start-up Kit. Attach a gas flow-
meter to the barbed end of the fitting.

!

CAUTION:  Do

not use the

needle valve as

an On/Off valve.

Overtightening

can distort the

needle valve’s

seal and make it

unreliable.

Содержание 5380

Страница 1: ...R 1 AIR 2 FINE ADJUST ON AUX Model 5380 Pulsed Flame Photometric Detector PFPD Operator s Manual 151 Graham Road P O Box 9010 College Station Texas 77842 9010 USA Toll Free 800 653 1711 Tel 979 690 17...

Страница 2: ...erformance or use of this material No part of this document may be reproduced photocopied or translated to another lan guage without the prior written consent of OI Analytical Revision 3 1 December 20...

Страница 3: ...instructions when properly installed on that CPU OI Analytical does not warrant that the operation of the CPU software or firmware will be uninterrupted or error free Consumables columns lamps and hig...

Страница 4: ...g the Model 5380 PFPD Assembly 29 Installing the Model 5380 PFPD in the Agilent 6890 Valve Box 32 Installing the Model 5380 Detector Controller 35 Installing the Pneumatics 36 Preparing the PFPD for O...

Страница 5: ...bliography 99 Appendix A Photomultiplier Tube and Filter Configurations 101 Appendix B Definition of Detectivity 103 Appendix C Dual Gate Capability and Calculation of Alpha 105 Appendix D Noise Sourc...

Страница 6: ...Controller or within the pneumatics com partment of the GC system Principle of Operation Operation of the Pulsed Flame Photometric Detector is based on a propagating flame that terminates within a fu...

Страница 7: ...is gas mixture reaches the glowing ignitor coil The flame then propagates from the ignitor region through a convoluted pathway to prevent light from the ignitor reaching the PMT and down into the comb...

Страница 8: ...combustor and ignitor regions are controlled by a fine adjust needle valve Figure 1 2 Four Phase Cycle of Propagating Flame Replenishment Ignition Combustion Extinction Gas Outlets Combustor Gas COMB...

Страница 9: ...magnitude and lifetime of the chemiluminescence resulting from combustion Refer to Chapter 5 Operation for a discussion of pneumatic settings that optimize the operating efficiency of the PFPD The em...

Страница 10: ...age developed by OI Analytical WinPulse permits the operator to set up and optimize all of the PFPD s operating parameters After these parameters have been uploaded to the Detector Controller the soft...

Страница 11: ...ers of signal response Phosphorus First order linear over five orders of magnitude Detectivity Sulfur 1 pg S sec Phosphorus 100 fg P sec Selectivity at Optimum Detectivity Levels Sulfur 106 S C or gre...

Страница 12: ...Requirements Carrier helium nitrogen or hydrogen 80 psig 99 999 purity or better Air 60 psig Zero Air 99 999 purity or better Hydrogen 60 psig 99 999 or better Electrolytic Grade Recommended Use of h...

Страница 13: ...r this unit to function properly Operator Precautions For operator safety pay attention to WARNING and CAUTION statements throughout the manual A WARNING indicates a condition or possible situation th...

Страница 14: ...te parts that are not OI Analytical original parts to the instrument To prevent burns verify that all heated areas have cooled before handling or wear adequate hand protection Compressed Gas Cylinders...

Страница 15: ...instrument and throughout the manual Warning Caution see accompanying instruction for more information Indicates a hot surface Indicates hazardous voltages and risk of shock Indicates earth ground te...

Страница 16: ...r connects to the PMT HV high voltage connector on the back of the Model 5380 Detector Controller Ignitor Cable connects to the ignitor connector on the back of the Model 5380 Detector Controller Sign...

Страница 17: ...detector base Combustor is a transparent quartz tube within which the GC column effluent combusts Combustor Support mounts into the base with the combustor support washer The combustor support positio...

Страница 18: ...the PFPD assembly to the top of the GC oven using mounting screws Optical Filter mounts inside the PMT housing An O ring is used to keep the filter from moving and to ensure that all the light from th...

Страница 19: ...e external wall of the combustor and ignitor volume AUX LED red is for future use Fine Adjust Needle Valve proportions the flow of Air 1 and H2 between the combustor and the wall flow paths H2 control...

Страница 20: ...re use PMT HV Connector SHV connector connects the PMT HV high voltage cable to the Detector Controller PMT Signal Connector BNC connector connects the PMT signal cable to the Detector Controller LIN...

Страница 21: ...tor Controller in order to synchronize the PFPD timed events with the start of the GC s analytical run Scope Outlet BNC connector connects to an oscilloscope optional Serial I O Port 9 pin D sub conne...

Страница 22: ...nPulse Overview of Main WinPulse Screen The Main Screen consists of a menu bar the chemiluminescence signal and several screen manipulation and data recording features along the right and bottom of th...

Страница 23: ...ence signal from the screen Attenuation Adjust Adjusts the signal attenuation on the WinPulse Main Screen The setting is independent of the attenuation values set in the Gate Parameters and Timed Even...

Страница 24: ...o o Z r a b l o o T r a B s u t a t S s r e t e m a r a P s e d o M s e t a G l e n n a h C d r a o B s t l u a f e D o t t e S s t n e v E s t n e v E d e m i T t e S s d n a m m o C y d a e R o t D...

Страница 25: ...to preview the data that will be printed to the file or printer before executing the print command Print Setup Allows the operator to set up the printer Exit Exits WinPulse View Menu Zoom Modifies vi...

Страница 26: ...s upon powering up Utilities Menu Set Preferences Displays a dialog box in which the operator can indicate preferences such as minimum limit for available disk space during a run and a maximum data fi...

Страница 27: ...the Gate Parameters List and change the desired parameters The function of each field in the Current Mode box is as follows Mode Modifies a current mode or adds a mode Gate mode identifi cation label...

Страница 28: ...nal for a specified mode is a function of the selected operator op the specified value of the Alpha scaling factor and the integration results for gates A and B which are determined by the specified s...

Страница 29: ...hey set parameters used to digitize the PMT signal before it is sent to the output handling device Two channels are provided because the Detector Controller can simultaneously process and send two sig...

Страница 30: ...g between observed output values from each pulse to derive a higher output data fre quency Linear provides point to point interpolation and Spline provides piecewise cubic smooth interpolation Attenua...

Страница 31: ...ocated on the toolbar See Figure 3 4 Timed events are initiated through the Detector Controller s remote start which is activated by a contact closure supplied either by the GC or an external remote s...

Страница 32: ...e Sqrt selection set specified in the Gate Param eters screen Enabling this option allows the operator to linearize quadratic response signals associated with some modes e g sulfur mode S Gate Specifi...

Страница 33: ...28 Model 5380 PFPD Operator s Manual Rev 3 1 Change Modifies current timed event without adding a new mode to the Event List Delete Deletes the selected timed event...

Страница 34: ...ch the internal parts of the PFPD without latex gloves Use clean lab tissues the Teflon extractor device or Teflon coated forceps to remove or replace internal detector parts Place removed parts on a...

Страница 35: ...mounting position in the GC s detector area Figure 4 1 Set the insulation plug aside for later use 7 Cut a hole in the top right GC cover as in Figure 4 2 8 Place a paper towel or tissue paper on the...

Страница 36: ...te Part 280735 for Agilent 6890 GC Part 245464 for Agilent 5890 GC Insert the heater element larger diameter metal probe and temperature sensor smaller diameter white porcelain probe into the appropri...

Страница 37: ...e When mounted the PMT protrudes to the right side of the GC If this orientation of the detector needs to be changed refer to Installing the Combustor and Reassembling the PFPD in this chapter Install...

Страница 38: ...e Part 296350 After cutting away the insulation carefully remove all the insulation material debris and the paper towel 4 Cut a hole approximately 1 25 mm in diameter in the previously removed insulat...

Страница 39: ...r located in the electronics area above the GC motherboard see Figure 4 4 9 If both detector ports are occupied by existing detectors the heater assembly must be plugged in and controlled by the valve...

Страница 40: ...ard GC right side disconnect the brown plug J10 and remove the clear plastic housing Unplug the brown plug J9 on the far right of the motherboard by squeezing its two locking levers Press the two heat...

Страница 41: ...nto the 8 pin MINI DIN connector marked EXT EVNT located on the back of the GC Valve 8 will need to be programmed as an External Start event in the Agilent 6890 GC see the Agilent 6890 Series Gas Chro...

Страница 42: ...using a U qy wrench 6 Cut the nylon tyraps holding the Q qy stainless steel gas lines from the PFPD assembly together Do not remove the nylon tags designating the COMB and WALL gas lines Unroll the g...

Страница 43: ...starts to flow It is suggested that the initial gas flows to operate the PFPD be set at this point in the following way If any flow controllers were turned on turn them off again Note Allow a few minu...

Страница 44: ...supply from the OIM gas flow module to the PFPD The required parts are included in the supplied detector gas kit Part 312678 1 Ensure that all gas supply lines to be used for the PFPD pneumatic syste...

Страница 45: ...itting 14 Attach the needle valve bracket to the GC using the screws Part 252585 provided in the detector gas kit 15 Cut the nylon tyraps holding the Q qy stainless steel gas lines from the PFPD toget...

Страница 46: ...alve Then open two full turns counterclockwise 21 Replace the flame arrestor located on top of the detector cap with the barbed fitting Part 202077 included in the PFPD Start up Kit Attach a gas flow...

Страница 47: ...well regulated pressure supply of H2 and air Pressure in the 50 70 maximum 90 psig range is acceptable 2 Shut off all gas supply lines to be used for the PFPD s pneumatic system 3 All gas line tubing...

Страница 48: ...ock the connector by moving the tabs to the center of the connector until they click into place See the Agilent 6890 GC Auxiliary Pressure Control Manifold Installation Guide for further instruction 9...

Страница 49: ...nch 16 Cut the nylon tyraps holding the Q qy stainless steel gas lines from the PFPD together Do not remove the nylon tags designating the COMB and WALL gas lines Unroll the gas lines without kinking...

Страница 50: ...12 psi and adjust it until the gas flow for Air 1 reaches 9 5 mL min Finally set the pressure for Aux 5 Air 2 to 16 psi and adjust it until the gas flow for Air 2 reaches 10 mL min Once these flow ra...

Страница 51: ...ly press its conical tip into the top of the combustor which is located just below the upper surface of the detector body Carefully extract the combustor and immediately reinsert the combustor extract...

Страница 52: ...shape or poor reproducibility are observed To minimize degradation of the column tip do not operate the detector at temperatures that exceed the recommended maximum temperature of the capillary column...

Страница 53: ...y that the top of the column is correctly positioned 0 5 mm to 1 5 mm above the top of the combustor support Note For optimal performance the column must be 0 5 1 5 mm above the combustor support Wall...

Страница 54: ...column with the tapered end facing into the GC column nut see Figure 4 13 3 With the ferrule and nut on the column insert the column end into the detec tor base Gently push the column up well beyond...

Страница 55: ...n the column nut The column will likely move slightly upwards when the column nut is tightened Observe whether or not the insertion tool moves and adjust accordingly Often it is only required to move...

Страница 56: ...assembly facing left into the center of the detector area but the detector can also be oriented with the PMT housing assembly facing toward the back of the detector area To change the orientation of t...

Страница 57: ...ing the WinPulse Software Before installing the WinPulse software confirm that the minimum hardware and software specifications required to run WinPulse exist in the PC on which WinPulse is to be inst...

Страница 58: ...ed PC by double clicking on the WinPulse icon After the WinPulse Mode Initialization screen appears click on the Online operation mode This accesses the Main Screen 3 Go to the Parameters menu and sel...

Страница 59: ...PFPD has already been set on the GC then either the column gas flow should be set to zero or the amount of the column gas flow should be added to each of the preceding initial flow rates Replace the...

Страница 60: ...propagating fully in the combustor The fine adjust needle valve may have to be turned counterclockwise to increase the H2 Air 1 mixture flowing through the combustor The flow rate of Air 2 may also h...

Страница 61: ...re delayed more than phosphorus and have a longer lifetime This description focuses on maximizing the lifetime of phosphorus and sulfur chemiluminescence emissions Figure 5 1 illustrates a background...

Страница 62: ...nd emission intensity see Figure 5 2 Slowly decreasing the H2 flow will result in the sulfur emission building back up to a maximum of emission amplitude and lifetime A similar dynamic is observed wit...

Страница 63: ...urs to obtain detectable emission Once a steady permeation rate has been achieved the PFPD response can be easily optimized In order to optimize the operation of the PFPD the column flow should be set...

Страница 64: ...t 4 5 Hz the display on the WinPulse screen will turn red indicating that the data generat ing frequency has exceeded the PFPD s data handling capacity The pulse rate can be easily changed by adjustin...

Страница 65: ...With slower computers it may be possible that only every alternate tick tock emission is observed 13 Disconnect the permeation source from the injector or detector and reconnect the GC column to the...

Страница 66: ...e to slightly air rich 4 Use WinPulse to archive data for comparison purposes when making multiple manual injections The optional PFPDView program must be used to observe the stored data 5 After the o...

Страница 67: ...obtained with the appropriate filters and PMTs to match a given application For assistance in properly configuring the PFPD to a specific application call OI Analytical s Technical Support Department...

Страница 68: ...lysis sulfur concentration within the combustor and the PFPD s detectivity for sulfur can be increased in the following way 1 Use the 2 mm combustor See Installing the Combustor and Reassembling the P...

Страница 69: ...sulfur can be maximized as follows 1 Decrease sensitivity by decreasing the PMT voltage range and or amplitude settings in WinPulse 2 If the emission starts to collapse i e does not extend beyond 20...

Страница 70: ...nterferences from other analytes heteroatoms thus increasing selectivity for the analyte of interest Selectivity for analytes with overlapping chemiluminescence lifetimes can also be enhanced through...

Страница 71: ...lectivity for sulfur over carbon the following steps are necessary 1 Ensure that the carbon concentration is not so high that it quenches the sulfur response Quenching can be observed by a collapsing...

Страница 72: ...ents to gate settings for optimal phosphorus detectivity see Appendix C for further details Maximizing Sulfur to Phosphorus Selectivity 1 Use an optical filter in the PMT assembly that is optimal for...

Страница 73: ...us and Sulfur Simultaneously 1 Install optical filter UV34 Part 310623 See Replacing the Optical Components in Chapter 6 2 Decide which element sensitivity is more important to determine the combus to...

Страница 74: ...ng C L and phosphorus 1 ng P L If the configuration is for the phosphorus mode a standard mix containing 100 pg P L 10 ng C L and 10 ng S L should be used 3 Inject the standard test solution into the...

Страница 75: ...0 32 mm diameter and 0 25 m film thickness Temperatures settings are Splitless isothermal injector set at 250 C GC oven is programmed as follows Initial temperature set to 60 C held for 0 50 min Incr...

Страница 76: ...his section will be used to define the directory and file name for the recorded WinPulse files 2 Click on the button Select a location and name for the WinPulse files The file name may be up to five c...

Страница 77: ...ck on Add Click on OK to save the timed events WinPulse is now programed to begin recording at the specified times See Timed Events Screen in Chapter 3 for more information Note WinPulse files tend to...

Страница 78: ...part names and numbers Note Before changing the combustor bakeout the PFPD overnight at 350 C Observe the carbon emission to see if the combustor has been cleaned In most cases this procedure may be...

Страница 79: ...chapter Examining the Column Tip 1 Verify that the combustor has been removed 2 Remove the detector body mounting screws Part 295295C using a U yr Allen wrench Place the screws on a clean lab tissue 3...

Страница 80: ...Place the combustor support onto a clean lab tissue or store in a clean sealable plastic bag 3 Loosen the column nut Part 223057 in the GC oven and pull the column down 4 Using clean forceps replace t...

Страница 81: ...is properly installed when the top of it sits approximately 0 05 below the surface of the detector body 2 If the large aluminum washer between the detector body and the detector cap was dislodged cen...

Страница 82: ...the ignitor assembly 5 Using the ohm volt meter measure the resistance between one lead and the top of the detector cap to see if it is shorted to the detector cap If it appears shorted look through...

Страница 83: ...hands when installing the PFPD optics Never handle tool parts used to remove or replace internal parts of the detector Always use clean latex gloves and use Teflon coated forceps to remove and replac...

Страница 84: ...ilter rattles when the cap has been fully screwed on an additional Viton O ring Part 288084 is required to take up excess space between the PMT and the filter If this is the case remove the PMT again...

Страница 85: ...lter s in the PMT housing 7 Verify that the PMT is not broken and is properly mounted in its socket Carefully screw the PMT housing cap back onto the body of the PMT hous ing Lightly tighten the PMT c...

Страница 86: ...rotruding from inside the detector body to remove all glass fragments Discard the cotton swab in an appropriate waste container 6 After checking that there are no glass fragments in the combustor cham...

Страница 87: ...he PMT signal cable and the PMT HV cable to their respective connectors at the back of the Detector Controller 15 Using WinPulse reset the PMT voltage to its appropriate voltage e g nominally 600 V 16...

Страница 88: ...he baking process can be done after reassembling the PFPD through a staged heating process The stage process used by OI Analytical includes setting the initial detector temperature to 200 C increasing...

Страница 89: ...84 Model 5380 PFPD Operator s Manual Rev 3 1 Notes...

Страница 90: ...ice Department at 800 336 1911 or 409 690 1711 with the following three printouts available 1 WinPulse screen showing a peak emission signal To capture a peak re sponse during a chromatographic run ac...

Страница 91: ...Gently turn the needle valve counterclockwise until seated and then turn it clockwise one half a turn Replace the knob and retighten the lock screw Set the GC oven to the highest temperature that the...

Страница 92: ...window in WinPulse Reduce the PMT voltage Examine the emission profile for response due to contamination Replace the combustor if necessary Verify that the output signal zero is enabled Check that hyd...

Страница 93: ...zero via WinPulse Optimize PMT voltage for noise measurements see Appendix D for details Adjust needle valve to tick tock operation Back off Q r to Q w turn Increase PMT voltage setting 50 V higher a...

Страница 94: ...ceed the recommended maximum tempera ture for the column Check the column end protruding beyond the combustor support to verify full flame propagation into the combustor Increase detector temperature...

Страница 95: ...90 Model 5380 PFPD Operator s Manual Rev 3 1 Notes...

Страница 96: ...5890 170093 ea Combustor 2 mm 282939C ea Combustor 3 mm 282913C ea Combustor Sleeve 283093C ea Combustor Support 2 mm 280461C ea Combustor Support 3 mm 280453C ea Detector Base 301325 ea Detector Bod...

Страница 97: ...e Handshake for Agilent 5890 185868 ea Cable PFPD Remote Start for Agilent 5890 6890 288902 ea Cable PFPD Remote Start for Shimadzu 17A 288977 ea Cable Signal Output to Spadelugs 215962 ea Cable Signa...

Страница 98: ...WinPulse Software Kit 286302 ea ANNUAL REPLACEMENT PARTS PART UM Req Yr Cable Ignitor Assembly 282624 ea 1 Combustor 2 mm 282939C ea 1 Combustor 3 mm 282913C ea 1 Ferrules as required Fitting Q qy Co...

Страница 99: ...94 Model 5380 PFPD Operator s Manual Rev 3 1 Notes...

Страница 100: ...the attenuation Auto Zero Output signal zero value automatically set by WinPulse This is activated at a specified time during an analytical run Channel Corresponds to a specified PFPD output signal Co...

Страница 101: ...dle Valve Controls the proportion of the H2 Air 1 mixture that flows to the combustor and wall gas pathways Gate Time segment during the flame propagation lifetime used to initiate and stop the integr...

Страница 102: ...erates in a periodic fashion generating emission waveforms Photomultiplier Tube Converts the chemiluminescence energy resulting PMT from the combustion of the GC effluent into an electrical current PM...

Страница 103: ...ture Tick Tock Occurs when the propagating flame alternately termi nates at the top and bottom of the combustor because the propagating flame reaches the top of the combus tor before the combustor gas...

Страница 104: ...em 1991 63 2061 2064 Introductory paper on the PFPD Cheskis S Atar E and Amirav A Pulsed Flame Photometer A Novel Gas Chromatography Detector Anal Chem 1993 65 539 555 Excellent description of princip...

Страница 105: ...A Combined Pulsed Flame Photometric Ionization Detector Anal Chem 1995 67 167 173 Other Important References Zainullin R F and Berezkin V G Flame Photometric Detectors in Chromatogra phy A Review Crit...

Страница 106: ...2 t r a P 5 2 9 1 R 6 0 1 0 9 2 t r a P 0 7 0 5 R 1 2 9 2 8 2 t r a P w o l l e Y 5 9 4 G G 5 1 0 0 9 2 t r a P e u l B t L 9 3 G B n e g o r t i N 9 4 0 0 9 2 t r a P 5 2 9 1 R 6 0 1 0 9 2 t r a P 0...

Страница 107: ...102 Model 5380 PFPD Operator s Manual Rev 3 1 Notes...

Страница 108: ...eak to peak noise level and is calculated from the measured sensitivity and noise level DP 2NP SP 1 where DP minimum detectability for phosphorus pgP sec NP peak to peak noise level in phosphorus mode...

Страница 109: ...low rate of sulfur atoms into the flame the sulfur sensitiv ity can be determined as follows SS Ai mS 1 mS 5 where SS sulfur sensitivity response Amp pgS s 2 Ai integrated peak area Amp sec mS mass of...

Страница 110: ...fficiently large differences in the emission time domain of each species to allow specification of discrete gates each of which incorporates a substantial segment of the time domain of one emitting sp...

Страница 111: ...e as much of the phosphorus chemiluminescence time domain as possible while at the same time minimizing the carbon and or sulfur chemiluminescence time domain In Figure C 1 the phosphorus gate is set...

Страница 112: ...sing dual gate enhancements The first left peak in each chromatogram in Figure C 3 represents the compound with only sulfur i e THT which contains no phosphorus The reason why a sulfur peak appears in...

Страница 113: ...igure the GC for a test run to analyze a suitable test standard containing both phosphorus and sulfur Ensure that each compound incorporated in the test standard contains only one of the heteroatoms o...

Страница 114: ...wo peaks above zero see Figure C 3 7 Using the values obtained from case 1 2 and 3 the Alpha value for the phosphorus and sulfur modes can be easily obtained as follows From Case 1 and 2 Calculate sma...

Страница 115: ...occurs the Alpha values entered in the Gate Parameters screen will have to be adjusted to get the desired peak elimination The use of OI Analytical s optional PFPDView software program which was used...

Страница 116: ...ith upper and Without lower the use of Calculated Alpha Values Phosphorus Gate Channel 1 Output P 0 Phosphorus Gate Channel 1 Output P 0 370 Sulfur peak eliminated 0 0 Sulfur Gate Channel 2 Output S 0...

Страница 117: ...112 Model 5380 PFPD Operator s Manual Rev 3 1 Notes...

Страница 118: ...caled by the attenuation setting The scaled digital signal is converted to a 0 1 V signal by a digital to analog converter DAC and the 0 1 V signal is sent out of the back of the Detector Controller t...

Страница 119: ...set these signal scaling factors appro priately may result in artificially high background noise or insufficient dynamic range for signal output Table D 1 and Figure D 1 show the effects of changing r...

Страница 120: ...56 2 38 238 1 0 039 0 60 060 10 256 1 0000 15 26 15 259 1 0 A 10V 64 0 2500 3 82 3 815 16 0 0625 0 094 945 4 0 0156 0 24 238 0 1 0 0039 0 06 060 1 256 0 10000 1 526 15 259 0 1 A 10V 64 0 02500 382 3 8...

Страница 121: ...ve 32 would undersample and thereby incorrectly display the noise amplitude while decreasing the attenuation below 32 would only reduce the dynamic range available for signal display A general rule fo...

Страница 122: ...ttenuation Setting on Noise to DAC Step Relationship Range 100 Attentuation 256 DAC Steps 2 Range 100 Attentuation 256 128 64 32 16 DAC Steps 1 2 3 6 13 Att 16 Att 32 Att 256 Att 256 Att 128 Att 64 Au...

Страница 123: ...o isolate and solve this problem Flexing of the PMT signal cable can create relatively large current spikes and therefore add to noise To minimize cable noise do not use auxiliary cables to connect th...

Страница 124: ...Ignitor Assembly 282624 Light Pipe 282608C Light Pipe Clamp 245563C PMT Housing 286096 Photomultiplier Tube PMT See Appendix A Washer 288076 Detector Base 301325 O ring 288084 Optical Filter See Appen...

Страница 125: ...120 Model 5380 PFPD Operator s Manual Rev 3 1 Notes...

Страница 126: ...Manifold 42 B Bibliography 99 Board Channel 20 Board Channel Parameters Window 24 C Cable HV 11 Ignitor 11 PMT HV 97 PMT Signal 97 Signal 11 Channel 27 95 Channel 1 Connector 15 Channel 2 Connector 1...

Страница 127: ...fault Settings Change 55 Detectivity 6 95 103 119 Detector Base 12 96 Detector Body 12 96 Reinstalling 76 Detector Cap 13 96 Detector Controller 1 96 Detector Controller Setting Up 35 Detector Design...

Страница 128: ...Parameters List 22 Gate Parameters Window 22 Gate Start 96 Gate Stop 96 Gates Modes 20 GC Column 43 96 Glossary 95 H H2 14 H2 Flow 96 H2 Inlet Connector 15 Hardware Requirements 7 Heater Assembly 31...

Страница 129: ...lamp 13 M Main Screen WinPulse 17 Maintenance 73 Manual Gas Flow Control 37 Marker Adjust 18 Menu Features 20 Mode 22 25 97 Mounting Plate 13 Mounting the PFPD 31 Multiple Manual Injections 61 N Noise...

Страница 130: ...e 13 97 Replacing 79 PMT 13 PMT Housing 13 97 PMT HV Connector 15 PMT Signal Connector 15 PMT Socket 13 97 PMT Voltage 24 97 Pneumatic System 2 Pneumatics 97 Pneumatics HP 6890 GC 42 Pneumatics Instal...

Страница 131: ...ing 105 Sensitivity 103 Sensor Temperature 98 Serial I O Port 16 Set Communications Port 21 Set Preferences 21 Set Timed Events 21 Signal Cable 11 Signal Output 98 Specifications 6 Split Set Control 2...

Страница 132: ...gger Level 24 98 Troubleshooting 85 U Use DataView 21 Utilities Menu 21 V Value 27 View Menu 20 View Run Log 21 Viton O ring 13 98 W Wall Gas Connector 16 WinPulse 98 Dual Gate 105 Installing 52 Main...

Страница 133: ...P O Box 9010 College Station TX 77842 9010 Tel 979 690 1711 FAX 979 690 0440 www oico com...

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