Valco Instruments Co. Inc. Pulsed Discharge Detector Models D-3-I-HP and D-3-I-7890 Instruction Manual D3.P65 Rev. 9/07 Printed in USA North America, South America, and Australia/Oceania contact: ® Valco Instruments Co. Inc. tel: 800 367-8424 fax: 713 688-8106 valco@vici.com Europe, Asia, and Africa contact: ® VICI AG International tel: + 41 41 925-6200 fax: + 41 41 925-6201 info@vici.
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Table of Contents Introduction Description and Operating Principles ............................................................ 1 Safety Notes and Information ........................................................................ 2 Symbols Installation Category Safety Components of the Detector System ............................................................. 3 System Requirements Components not Included with the Detector System ..................................... 4 System Purity ...................
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1 Introduction Description and Operating Principle The D3 is a non-radioactive pulsed discharge ionization detector (PDID), with models available for “plug and play” installation on the Agilent 6890 or 7890 GC. A schematic representation of the detector is shown in Figure 1. The D3 utilizes a stable, low power, pulsed DC discharge in helium as the ionization source.
Introduction 2 Safety Notes and Information Symbols ATTENTION Refer to the manual. Installation Category This equipment has been designed for installation category (overvoltage category) II, pollution degree 2. It has been approved for use only in heavy industrial environments and may not be used in the residential, commercial, or light-industrial environment. Safety This instrument left the factory in a safe condition.
Introduction 3 Components of the Detector System Components of the detector system are listed in Table 1 below. Check the contents of the packages to verify that everything is present. Contact the factory if anything is missing or damaged. (NOTE: damaged shipments must remain with the original packaging for freight company inspection.
Introduction 4 System Requirements Components Not Included with the Detector System • Helium (99.
Introduction 5 Gas Specifications Detector Mode PDHID Ar-PDPID Discharge gas Helium 2% Ar in He Carrier gas Helium * Kr-PDPID Xe-PDPID 1.5% Kr in He 0.8% Xe in He ** ** ** Any gas including He which has an ionization potential greater than 12 eV ** Any gas including He which has an ionization potential greater than 11 eV Purity Specifications • Helium (discharge and carrier gas) must have a minimum purity of 99.999%, with < 20 ppm Ne impurity.
6 Installation General Precautions • Do not use plastic/polymer or copper tubes for gas handling and interconnectons. Use only stainless steel tubing with Valco gold-plated ferrules. • Do not turn the discharge power on until the helium discharge gas is flowing through the detector. • Do not shut off or disconnect the discharge gas when the detector is hot, even if the GC is turned off. • Do not turn on the GC during detector installation. Checking the Firmware Version Agilent 6890 GC 1.
Installation 7 Agile A 7890 GC s logie chno nt Te MODEL D3 DETECTOR m Syste Figure 2: A D3 detector in the “Back” position on a 7890A CAPTIVE SCREWS (4) DISCHARGE GAS INLET (30 mL/min@60 psi) VENT HEATER/SENSOR CABLE TO D3 PULSER MODULE (PD-M2) HIGH VOLTAGE CABLE ELECROMETER RIBBON CABLE COLUMN INLET CAPILLARY COLUMN ADAPTER (Packed column adapter shown on page10) TO FID LOGIC BOARD Figure 3: Mounting and connecting the detector
Installation 8 CAUTION: A D-3-I-HP will not work on a 7890 GC, and a D-3-I-7890 will not work on a 6890. If you are not sure which model you have, call the VICI detector department with the detector serial number. Installing and Configuring the FID Logic Board Agilent 6890 GC (units without EPC) The D3 uses the electrometer portion of the Agilent FID logic board, which must be configured to ignore the ignitor circuit. HEATER/SENSOR CABLE CONNECTOR FID BOARD SCREW 1.
Installation 9 MODEL D3 IN BACK POSITION FRONT OF 7890 HEATER CABLE CONNECTIONS THUMBSCREW FID LOGIC BOARD FOR FRONT POSITION ELECTROMETER CABLE CONNECTIONS FID LOGIC BOARD FOR BACK POSITION B-DET CABLE CONNECTION F-D ET B-DET F-DET CABLE CONNECTION Figure 5: 7890 FID logic board 6. Press the key, then press or , corresponding to the location where the PDD will be installed. For this example we will select Back Det.
Installation 10 11. Scroll to select the second line and press . The display will read: CAUTION: Instrument power must be turned off and back on for set point to take effect. 12. Do not turn off the GC; instead press . The display should read: CONFIGURE BACK DETECTOR Configured: Channel Partner Ignore Ready = False [B-det] = (Signal) (FID) 13. Turn off the GC and power it back up. Verify the configuration by pressing . The display should read: Back detector (CP) Temperature xx. .
Installation 11 Gas Connections Remember these three points discussed earlier: (1) all surfaces that contact the gas stream must be glass or stainless steel; (2) do not use copper tubing or brass fittings; and (3) all tubes must be thoroughly cleaned and baked before use. The installation instructions below assume that the detector discharge gas will be supplied from a nearby cylinder of helium of the proper purity. If your installation is different, you may need to modify the instructions appropriately.
Installation 12 7. 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 doesn’t 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. Installing and Purging the Helium Purifier 1.
Installation 13 Initial Power-Up CAUTION: Always make sure that discharge gas is flowing before heating and powering up the detector. 1. Before installing the column, set the gas flow to 30 ml/min (measured at the detector vent). Let it flow for 15 minutes so that all air is purged from the helium purifiers. 2. Plug in the helium purifiers and turn on the GC. 3. Set the detector temperature to 100°C and allow time for the detector and helium purifiers to reach the set temperature. 4.
Installation 14 Capillary Column Connection If the capillary column adapter is installed in the column inlet: 1. Make a mark on the column 10.3 cm from the end. COLUMN INLET 10.3 cm CAPILLARY COLUMN ADAPTER (IZERA1.5) 2. Remove the knurled nut and plug from the capillary column adapter in the column inlet at the bottom of the detector. (Figure 3) Slide the nut over the end of the column, followed by the appropriate column ferrule (FS.4 or FS.5, or ZF.5V for megabore). COLUMN FERRULE 3.
Installation 15 3. Set aside the 1/8" wrench and completely remove the adapter from the column inlet. 4. Screw the packed column adapter into the column inlet by hand. Exercise caution, as the tip of the adapter is very fragile. Then tighten the adapter with a 1/4" wrench, using an additional wrench on the flats of the column inlet to support the detector. 5. Connect the 1/8" column to the packed column adapter with the EZRU21 reducing union supplied in the fittings kit.
16 Mode Selection and Setup Helium Ionization Mode Since the PDHID mode provides a better indication of the cleanliness and the integrity (leak tightness) of the system, that mode is utilized for initial testing and startup. If the system is operating according to the parameters described thus far, it is ready for operation in the PDHID mode. Selective Photoionization Mode To maximize detector lifetime, turn off the discharge power when the GC is not actually analyzing samples.
Mode Selection and Setup 17 Ar-PDPID Changing the discharge gas from helium to a mixture of 2% argon in helium changes the photon energy level from the 17 - 13.5 eV range to the 11.8 - 9.8 eV range. The argon emission consists of resonance radiation at 11.8 eV and 11.6 eV and the diatomic Ar2 emission in the range of 9.2 - 10.3 eV. Except for fixed gases and a few organic compounds like CH4 (IP = 12.5 eV), CH3CN (IP = 12.
18 Troubleshooting High Background Current The detector isn’t leaking. Check for column bleed and/or leaks in the GC setup.
Troubleshooting 19 High Noise Level If the noise lievel is high: 1. See if it improves with the GC fan turned off. 2. Check the column insertion position (10.3 cm for capillary columns, 8.7 cm for packed columns.) 3. If the noise level is still high, do a hydrogen leak test, described below. 4. If there are no leaks found, or leaks are found and repaired and the noise level is still high, consult Valco.
20 Warranty This Limited Warranty gives the Buyer specific legal rights, and a Buyer may also have other rights that vary from state to state. For a period of 365 calendar days from the date of shipment, Valco Instruments Company, Inc. (hereinafter Seller) warrants the goods to be free from defect in material and workmanship to the original purchaser.
21 Detector Performance Log In addition to the occasions indicated in the Comments area of the table below (see Initial Power-Up, page 13), the standing current should be observed and logged after any system change. Logging the standing current (with and without the column) on a regular basis is also an effective monitor of system integrity (leaktightness and cleanliness). To check sensitivity continuity, we recommend tracking the internal standard (quantity on column/area count).
