Electron Capture Detectors Information for General Licensees
Contents
1. 5 Remove the two screws that hold the ECD cover and lift the cover off Information for General Licensees 51 Agilent Electron Capture Detectors Note the bare wire that comes out of the top of the ECD cell It connects to an L shaped bracket that is held in place by a single screw Remove the screw and straighten the wire so that the bracket is above the cell Use care to avoid breaking the wire particularly at the point where it attaches to the cell Now remove the single screw that holds the insulation cover Lift the cover up and over the L shaped bracket until it is free of the ECD You may have to compress the spring on the L shaped bracket to allow it to pass through the insulation cover Disconnect the tubing and elbow connect to the ECD vent This is the tube that extends to the left from the cell body Remove the two Pozidriv screws that hold the cell to the mounting block 10 Remove the threaded plug from the inlet fitting if present and check that no column is installed Grasp the upper part of the cell and pull it straight up It should come free with only moderate force If it is frozen contact your local Agilent Sales Office Do not attempt to force the cell loose 11 If the ECD is to be returned to Agilent Technologies see shipping instructions How to Package and Ship ECDs on page 53 12 Thoroughly wash your hands using a mild nonabrasive soap and water Do not disturb the four socket head bolts2. Formulas 56 G General License 12 15 General License Requirements 15 H High Wipes 56 Incidents 58 Installing ECDs 25 L Leak test 12 Lost ECD 58 Information for General Licensees M Maintenance 24 NRC Nuclear Regulatory Commission 12 NRC Offices 71 Radioactive Wipe Test 12 Regulatory Requirements 20 Removing Your ECD 28 S Safety Precautions 21 Samples 60 Sensitivity 61 Shipping ECDs 65 Specific License 12 14 Storing Your ECD 26 T Temperature Limitations 22 Thermal Cleaning 24 Transferring ECDs 23 V Venting Your ECD 26 wW Warnings 21 Wipe test 12 Wipe Test Companies 55 77 Index 78 Information for General Licensees hee Agilent Technologies Agilent Technologies Inc Printed in USA March 2013 5961 5664E
3. s instruction manual All malfunctions are reported to the Department of Nuclear Safety 32 Ill Adm Code 330 220 b 3 B C and E 7 Tests for contamination or leakage of radioactive material are performed at intervals specified on the device label and are analyzed by someone specifically licensed or otherwise authorized to do so Any leakage above regulatory limits is reported to the Department of Nuclear Safety 32 Il Adm Code 340 1260 and 330 220 b 3 B and C 8 All radioactive devices are labeled correctly and missing or damaged labels have been replaced 32 IH Adm Code 330 220 b 3 A 9 Records are maintained of receipt transfer use storage and disposal of devices and of the tests described above 32 IH Adm Code 310 40 and 330 220 0 3 D SIGNATURE OF RESPONSIBLE INDIVIDUAL Person named above as responsible for radioactive devices I hereby certify that to the best of my knowledge and belief compliance with the regulations is being maintained and the above information is complete and correct except as noted Name Print or Type Signature Date Information for General Licensees 75 E Self Inspection 76 Information for General Licensees Index A Agency 12 Agreement States 12 69 C Capping ECDs 22 CFR Title 10 67 Cleaning ECDs 25 Conversion Formulas 56 Converting a General License 17 Converting a Specific License 18 E ECD Description 19 ECD Properties 19 F
4. a uECD from a side mounted third detector box on page 32 Removing the detector cover 6890 7890 and 7820A Raise the GC s detector cover to the vertical position and lift off of instrument Removing the old style detector cover 6890 The top cover protects the detectors valve box and valve assembly 1 Tilt the front cover up 2 Squeeze the clip on the right hinge pull the clip toward you and pivot it up Information for General Licensees 25 Agilent Electron Capture Detectors 3 Push the metal pin behind the clip to the left 4 Slide the detector cover to the right and lift it off 5 To replace the top cover a Slide the plastic post on the left side of the cover into the hole on the injection port fan cover b Line up the hole in the tab on the right side of the cover with the metal pin and push the pin to the right through the hole c Pivot the clip back down and snap it back over the metal pin Removing the right side cover WARNING The electronics cover shields the high voltage components on the main board Turn off the main power switch and unplug the power cord before removing this cover CAUTION Be sure to wear an ESD strap grounded to the GC chassis while performing this procedure 1 Fully loosen the two captive screws Torx T 20 in the top of the cover for the 6890 and 7890 GCs and on the right side of the cover for the 7820A GC 2 Slide the side cover slightly to the
5. adapter 1 Inside the oven remove the insulation cup and disconnect the column from the makeup gas adapter 2 Usea9 16 inch wrench to loosen the 1 4 inch Swagelok nut on the makeup gas adapter from the bottom of the detector Slide the makeup gas adapter out of the bottom of the detector Removing the ECD Disconnect the ECD vent tube at the rubber sleeve 2 Disconnect the anode purge line at the pneumatics manifold Remove the one Torx T 20 screw securing the ECD detector top cover to the detector pallet and remove the cover 4 Disconnect the anode signal wire from the detector 5 Fully loosen the four Torx T 20 screws five screws for the 7820A GC on the detector pallet lift the pallet and turn on its right side 6 Thread the heater sensor leads out of the detector pallet and remove the rest of the detector from the pallet 7 For shipping or storage purposes cap the inlet anode purge and exhaust vent tubing Information for General Licensees 29 Agilent Electron Capture Detectors EPC fitting Detector top cover 7 p Anode purge line Remove ECD vent tube Detector pallet SE Se 6890 and 7890 ECD shown 30 Information for General Licensees Agilent Electron Capture Detectors 8 The ECD detector is now properly disassembled for return to Agilent Call the Technical Support number identified at the front of the booklet for further directions NN Ff A a XP WK i N BS i gt Information
6. for General Licensees 31 Agilent Electron Capture Detectors Instructions for removing a pECD from a side mounted third detector box Remove the detector box cover 1 Remove the third detector box cover from the side of the GC Remove the two T 20 Torx screws from the bottom of the cover panel PML TMT yu iti MITTIN LL wil ALALLAAN aii ALLL LALLA 6 Figure 4 Detector box cover removal 2 Lift the cover straight up and remove it 32 Information for General Licensees Agilent Electron Capture Detectors Disconnect the wires and plumbing 1 Unplug the heater sensor cable The heater sensor cable 2 Unplug the electrometer ribbon cable The electrometer ribbon cable Figure 6 33 Information for General Licensees Agilent Electron Capture Detectors Removing the makeup gas adapter 1 Open the oven door 2 Inside the oven remove the insulation cup and disconnect the column from the makeup gas adapter 3 Use a 9 16 inch wrench to loosen the 1 4 inch Swagelok nut on the makeup gas adapter from the bottom of the detector Slide the makeup gas adapter out of the bottom of the detector Figure 7 The nut warmer cup and insulation 4 Close the oven door Removing the ECD 1 Disconnect the ECD vent tube at the rubber sleeve Figure 8 Remove the tube shown here 34 Information for General Licensees Agilent Electron Capture Detectors 2 Disconnect the anode purge line at the p
7. for Specific License ECDs GC Gas chromatograph NRC Nuclear Regulatory Commission The Agency that regulates radioactive materials in the U S Refer to Appendix D to locate your local NRC office Radioactive Wipe Test This is also known as wipe test or leak test a test that is required on all Agilent ECDs at least every 6 months The wipe test is performed by wiping the outside of the ECD with either filter paper or a Information for General Licensees Agilent Electron Capture Detectors cotton swab The wipe is then analyzed by a liquid scintillation counter to determine the activity of the wipe Refer to Radioactive Wipe Tests on page 55 for additional information Regulations As used in this booklet this refers to the regulations of the NRC in the U S as published in Title 10 of the Code of Federal Regulations abbreviated as 10 CFR Customers located outside of the U S should contact their local Agency to determine the local Regulations Information for General Licensees 11 Agilent Electron Capture Detectors What is a Specific License 12 Customers in the U S can purchase either a General License or a Specific License ECD Specific and General Licenses ECDs are sold as either specific or general license The two types of ECD are physically identical except the model number and the detector label The General License ECD label contains additional warnings not required for the Spe
8. rear of the GC and lift the cover out of the slot in the bottom of the chassis 26 Information for General Licensees Agilent Electron Capture Detectors Figure 2 Right side cover removal 6890 GC shown 7890 GC similar 6890 GC cover removal Hinge pin new dectector cover Rear locking tab not shown Notch Electronics cover Front locking tab 1 Remove the GC right side cover 2 Reach under the electronics cover and press the rear locking tab toward the front of the instrument Information for General Licensees 27 Agilent Electron Capture Detectors 3 While pressing the tab lift up the back of the electronics cover and slide the cover back up and out of the instrument 4 To reinstall the cover make sure that the notched edge of the cover faces the front left side of the instrument and snap it back into place 7890 GC cover removal 1 Remove the screws from the left side and the rear of the top electronics cover 2 Lift the electronics top cover up and away from the right side of the GC Disconnecting the cables 1 Disconnect the heater sensor cable from the connector on the right side of the GC 2 Disconnect the ribbon cable from the detector board Heater Sensor cable Ribbon cable Figure 3 Disconnect the cables 6890 GC shown 7890 and 7820A GCs similar 28 Information for General Licensees Agilent Electron Capture Detectors Removing the makeup gas
9. soap and water after handling the ECD If you are returning the ECD to Agilent Technologies refer to the shipping instructions in How to Package and Ship ECDs on page 53 If you should encounter any problems or complications when removing your ECD call your local Agilent customer engineer or the Agilent Response Center at 1 800 424 9759 Instructions for removing G1533A 6890 GC G2397A 6890 and 7890 GCs and G2397AE 7820A GC ECDs Safety All versions of ECD cells contain radioactive material Exposure to radioactive material is hazardous to human health Under no circumstances should an ECD cell be disassembled as this is in violation of the General License agreement ECDs must be returned to a licensed facility Agilent will accept only ECDs manufactured by either Hewlett Packard or Agilent Technologies Inc CAUTION Always allow time for the oven and heated zones to cool before turning off the gas supplies Failure to allow cooling may damage the ECD 24 Information for General Licensees Agilent Electron Capture Detectors WARNING Before proceeding turn off the oven and any heated zones and let them cool down When they have cooled turn off any detector gases at their supply then turn off the main power switch and unplug the power cord CAUTION Make sure you are properly grounded with an ESD strap before continuing Removing a left side mounted ECD from a 7890 See Instructions for removing
10. some conversion formulas and examples to put these numbers in perspective are found below C Wipe in CPMs counts per minute D Wipe in DPMs disintegrations per minute E Efficiency of the liquid scintillation counter LSC for that day F Wipe in microcuries uCi B Wipe in Becquerels Bq D C E F D 2 220 000 B D 60 1 Curie Ci 3 7 x 10 Becquerels Bq 37 000 MBq 1 Curie Ci 1 000 mCi millicuries 1 Curie Ci 1 000 000 uCi microcuries 1 Curie Ci 1 000 000 000 nCi nanocuries 1 Curie Ci 1 000 000 000 000 pCi picocuries Information for General Licensees 57 Agilent Electron Capture Detectors For example if you had a wipe of 9 435 CPM and the efficiency of the count is 85 you would convert the value to DPMs and microcuries as follows 9 435 CPMs 0 85 1 1 100 DPMs 11 100 DPMs 2 220 000 0 005 pCi 5 nCi 11 100 60 185 Bq 58 Information for General Licensees Incidents Agilent Electron Capture Detectors 10 CFR Sections 20 2202 31 5 c 5 and 20 2203 of the NRC Regulations referred to in Appendix B describe the reporting actions that must be taken if an incident occurs In this section an incident is any occurrence involving radioactive material that may have caused or threatens to cause e Exposure to dangerous levels of radiation e Release of dangerous amounts of radioactive materials Please refer to the NRC regulations for further details In
11. suggestions on the following page into your radiation safety program These suggestions may greatly assist you in building a good relationship with your state regulatory agency and the NRC Please feel free to contact the Agilent Radiation Safety Officer via 302 636 8262 if you have any questions Sincerely yours Agilent Technologies Information for General Licensees 7 Radiation Safety Program Suggestions 1 Develop and document a Radiation Safety Program that will be passed on to successive RSOs Customers purchasing Specific License ECDs are required to comply with the conditions of their license Contact your regional NRC office for specifics of a safety program Customers purchasing General License ECDs should use the information provided in the following sections of this manual to prepare a safety program These sections include Descriptions of specific and general licenses General License requirements General License restrictions Converting licenses Properties of an ECD Regulatory requirements Safety precautions ECD warnings Capping the ECD Temperature limitations Transferring an ECD ECD maintenance Thermal cleaning the ECD Installation venting storing and removing the ECD Packaging and shipping instructions Radioactive wipe tests Wipe test conversion formulas Incidents reporting and recording 2 Educate lab managers and ECD users to notify you as their RSO of all changes of ownership or transfers to o
12. your ECD must be tested for leakage of radioactive material at least every 6 months Customers outside of the U S should consult their local nuclear agency to determine the required frequency of wipe tests Records of all tests and their results must be maintained for possible inspection by the NRC or your local Agency Under severe usage conditions radioactivity leak tests during every column change will provide maximum security Although Agilent Technologies performs a wipe test on all ECDs prior to shipment all further 6 month wipe tests are the responsibility of the end user In addition customer wipe tests are not performed by Agilent service engineers are not included in any service contract and are not part of any preventative maintenance carried on by Agilent Technologies The procedure used is called the wipe test Wipe test kits are available for sale through Agilent P N 18713 60050 We recommend that disposable gloves be worn when performing this test If they are not used wash your hands thoroughly when you are finished The following are detailed instructions for performing the wipe test on Agilent ECDs This information is also provided in the service note contained in the wipe test kit 1 Select three information cards item 1 and fill them out completely 2 Select three pieces of filter paper item 2 and label them with a pencil as follows Sample 1 Det Entrance Fitting Sample 2 Det Housing Sample 3
13. 103A 103A 107A Other form 103A 10A 107A 64 Information for General Licensees A Instructions for Customer Return of ECDs per Compliance with IATA Regulations Air Transportation Instructions for Customer Return of ECDs per Compliance with U S DOT Regulations Surface Transportation other than Federal Express Procedures for packaging labeling and marking ECD packages for return to Agilent Technologies by common carrier 1 Plug the entrance fitting and cap the vent tube Place the ECD in a strong plastic bag seal it and pack it in a strong container with shock absorbing packing material a corrugated cardboard box in good condition and bubble wrap is a satisfactory combination 2 Completely remove or mark out any previous labels if the container chosen has previous shipping labels on it 3 This package must be marked with the appropriate Radioactive Material Excepted Packaging label Contact your Agilent Field Repair Center for the required label 4 Refer to page 53 and the regulations provided below for additional shipping information and instructions U S DOT Regulations The U S Department of Transportation U S DOT provides requirements for surface transportation of ECDs in 49 CFR Part 173 424 Excepted packages for radioactive instruments and articles Contact your qualified carrier or access the regulation on line at www dot gov for up to date instructions Information for General Licensees 65 A Instruct
14. 27 1554 New York Phone 518 457 1202 Fax 518 485 7406 North Carolina Phone 919 571 4141 Fax 919 571 4148 North Dakota Phone 701 328 5153 Fax 701 328 5200 Nebraska Phone 402 471 8566 Fax 402 471 9449 Nevada Phone 775 687 5394 Fax 775 687 5751 Ohio Phone 614 644 7860 Fax 614 466 0381 Became an Agreement State on 9 29 00 7 1 65 1 1 80 9 15 69 9 1 65 3 1 63 4 1 84 12 31 66 8 1 02 3 4 05 Oklahoma Phone 405 702 5155 Fax 405 702 5101 Oregon Phone 503 731 4014 Fax 503 731 4081 Rhode Island Phone 401 222 2438 Fax 401 222 2456 South Carolina Phone 803 896 4244 Fax 803 896 4242 Tennessee Phone 615 532 0360 Fax 615 532 7938 Texas Phone 512 834 6679 Fax 512 834 6708 Utah Phone 801 536 4250 Fax 801 533 4097 Washington Phone 360 236 3210 Fax 360 236 2255 Wisconsin Phone 608 267 4792 Fax 608 267 4799 Minnesota Phone 651 201 4602 Fax 651 201 4606 Information for General Licensees Agilent Electron Capture Detectors Information for General Licensees ee D United States Nuclear Regulatory 6 amp _ Commission Regional Offices e Office Address Telephone 24 hours Region 1 Connecticut Delaware USNRC 475 Allendale Road 610 337 5000 District of Columbia Maine Maryland King of Prussia PA 19406 Massachusetts New Hampshire New Jersey New York Pennsylvania Rhode Island and Vermont Region Il Alabama
15. Agilent Electron Capture Detectors Information for General Licensees Ee Agilent Technologies Notices Agilent Technologies Inc 2013 No part of this manual may be reproduced in any form or by any means including elec tronic storage and retrieval or translation into a foreign language without prior agree ment and written consent from Agilent Technologies Inc as governed by United States and international copyright laws Manual Part Number 5961 5664E Edition Fifth edition March 2013 Printed in USA Agilent Technologies Inc 2850 Centerville Road Wilmington DE 19808 1610 USA Safety Notices CAUTION A CAUTION notice denotes a haz ard It calls attention to an operat ing procedure practice or the like that if not correctly performed or adhered to could result in damage to the product or loss of important data Do not proceed beyond a CAUTION notice until the indicated conditions are fully understood and met A WARNING notice denotes a hazard It calls attention to an operating procedure practice or the like that if not correctly per formed or adhered to could result in personal injury or death Do not proceed beyond a WARNING notice until the indicated condi tions are fully understood and met Information for General Licensees What can we do to assist you Please call Radiation Safety Officer 302 636 8262 Technical Support 1 800 227 9770 Information for General Li
16. Agilent Technologies is not associated with and does not specifically endorse any one of these companies You may choose to use any of these companies or any other authorized company Customers outside of the U S please contact your local nuclear regulatory agency for an authorized company 9 You will receive a written report of the results from the wipe test company It is your responsibility to retain all wipe test results for possible inspection by your local Agency Wipe test companies Nuclear Radiation Developments Inc 2937 Alt Boulevard Grand Island New York 14072 716 773 7634 National Leak Test Center P O Box 1400 North Tonawanda New York 14120 716 693 0550 AEA Technologies 6765 Langley Drive Baton Rouge Louisiana 70809 225 751 5893 Detector Service Center Inc 9423 Chapel Hill Road Cary North Carolina 27513 919 469 0259 Information for General Licensees Agilent Electron Capture Detectors Spencer Scientific 13309 SE 159th Place Renton WA 98058 7802 425 204 6167 High wipes If the radioactive leak test indicates leakage of 0 005 microcuries or greater you must take the ECD out of service immediately and notify the NRC or the appropriate State agency within 5 days See Incidents on page 59 for additional reporting information Wipe test conversion formulas When you receive your wipe test results they will be defined as CPMs DPMs microcuries or Becquerels For your convenience
17. Det Exit 3 Disconnect the column from the ECD 4 Wipe the outside and inside of the ECD entrance fitting including column and adapter connections with the piece of filter paper labeled Sample 1 Det Entrance Fitting Immediately insert it and a filled out information card into one of the plastic bags item 3 and seal it closed 5 Wipe the ECD housing with the filter paper labeled Sample 2 Det Housing and insert it and a filled out information card into a second plastic bag 6 Disconnect the exit tubing from the ECD vent tube Wipe the side of the metal ECD exit tube and or the inside of the exit tubing with the filter Information for General Licensees 55 Agilent Electron Capture Detectors 56 paper labeled Sample 3 Det Exit Insert it and a completed information card in a third plastic bag If the ECD is installed in a GC reconnect the tubing to the ECD vent and inspect the vent line to verify that it is attached securely and vented properly 7 After completing wipe tests wash your hands thoroughly with mild soap and water 8 In the U S the ECD Wipe Samples must be analyzed by an NRC authorized company offering this service Below is a list of a few of the companies that provide this service We suggest that you contact them for cost of testing turnaround times and payment arrangements Please note that the listing of Wipe Test Companies is only provided as a courtesy to our customers and
18. ECD Install an empty unpacked clean glass metal column to maintain gas flow into and through the ECD Set the oven temperature to 250 C and the carrier flow to 30 to 90 mL min Raise the ECD temperature above your normal operating temperature but less than the maximum operating temperature allowed for your ECD For the 5880A GC the maximum ECD temperature is 370 C for 5890 6890 7890 and 7820A GC instruments the maximum ECD temperature is 400 C Maintain this bakeout condition for several 3 to 24 hours or until the ECD baseline has stabilized The total time necessary will depend on the type and degree of contamination as well as the normal operating temperature versus the bakeout temperature Baking the ECD at higher temperatures above the normal operating temperature and at higher purge flow rates will Information for General Licensees Agilent Electron Capture Detectors shorten the time necessary It is good practice to monitor the ECD signal baseline during the bakeout to help determine the time necessary A typical baseline trace might look similar to Figure 1 Amplitude 1 Baseline before start of bake out time 2 Baseline after bake out time continue until signal has stablized Time Figure 1 Typical baseline trace Cleaning the ECD thermally will most likely change its response characteristics so you will probably be required to recalibrate your ECD depending on the actual method Who can open th
19. Florida Georgia Sam Nunn Atlanta Federal Center Kentucky Mississippi North Carolina USNRC 61 Forsyth St SW Puerto Rico South Carolina Suite 23785 Tennessee Virgin Islands and West Atlanta GA 30323 Virginia Region Ill Illinois Indiana lowa Michigan USNRC 2443 Warrensville Road Minnesota Missouri Ohio and Suite 210 Wisconsin Lisle IL 60532 Region IV Alaska Arizona Arkansas USNRC 611 Ryan Plaza Drive California Colorado Hawaii Idaho Suite 400 Kansas Louisiana Montana Arlington TX 76011 Nebraska Nevada New Mexico North Dakota Oklahoma Oregon South Dakota Texas Utah Washington Wyoming and U S territories and possessions in the Pacific EE Agilent Technologies Fax 610 337 5269 404 562 4400 Fax 404 331 4449 630 829 9500 800 522 3025 Fax 630 515 1078 817 860 8100 Fax 817 860 8210 71 D United States Nuclear Regulatory Commission Regional Offices 72 Information for General Licensees Agilent Electron Capture Detectors P d n Information for General Licensees an 090 e0 0e 9209 on Inspection i i e e J e We strongly advise adding a periodic internal audit of your ECD management program Such an audit will greatly enhance your ability to maintain staff awareness of the regulatory requirements you face as a General Licensee Please refer to the next two pages for a suggested format The items identified in the audit are derived from the NRC s regulatio
20. Safety precautions to follow when handling ECDs 1 Never eat drink or smoke when handling ECDs 2 Always wear safety glasses when working with or near open ECDs 3 When handling ECDs wear protective clothing such as laboratory jackets safety glasses and gloves and follow good laboratory practices In addition wash hands thoroughly with a mild non abrasive cleaner after handling ECDs 4 Cap the inlet and outlet fittings when the ECD is not in use Connect the ECD exhaust vent to a fume hood or vent to the outside in some other acceptable manner whenever the ECD is in use ECD warnings Although beta particles at this energy level have little penetrating power the surface layer of the skin or a few sheets of paper will stop most of them they may be hazardous if the isotope is ingested or inhaled For this reason the cell must be handled with care radioactive leak tests must be performed at regular intervals the inlet and outlet fittings must be capped when the ECD is not in use corrosive chemicals must not be introduced into the ECD and the effluent from the ECD must be vented outside the laboratory environment WARNING Materials that may react with the 63Ni source either to form volatile products or to cause physical degradation of the plated film must be avoided These materials include oxidizing compounds acids wet halogens wet nitric acid anmonium hydroxide hydrogen sulfide PCPs and carbon monoxide This list is not e
21. These hold the cell halves together removing or disturbing them is a violation of the terms of the General License and could create a safety hazard 52 Information for General Licensees Agilent Electron Capture Detectors How to Package and Ship ECDs Shipping radioactive materials in the U S is regulated by the U S Department of Transportation DOT for surface transport and by the International Air Transport Association IATA for air transport Appendix A contains e Instructions for Customer Return of ECDs per Compliance with IATA Regulations for shipping ECDs via Air Transportation e Instructions for Customer Return of ECDs per Compliance with U S DOT Regulations for shipping ECDs via Surface Transportation Prior to shipping radioactive materials you should contact your transportation officer and or your carrier to determine which regulations are pertinent to your shipment 1 Using a clean dry cloth remove any external chemicals or debris that may be on the ECD 2 Insert the threaded plug in the entrance fitting and cap the vent tube These measures keep foreign materials out of the ECD cavity and keep any loose fragments in 3 Place the ECD in a strong plastic bag and seal the bag 4 Pack the bag in a strong container corrugated cardboard is satisfactory with a shock absorbing packing material bubble pack if available and seal the box carefully If possible try to retain the original ECD box for retu
22. apture Detectors 10 With the lower right side of the cover pushed in lift the right side of the cover and slide it to the right to remove the top cover and lid shaft as a unit Electronics carrier top cover Information for General Licensees 47 Agilent Electron Capture Detectors 11 Remove the electronics carrier top cover by grasping it at the rear and lifting upward until its catch releases then pulling it toward the rear of the instrument Screws Right side panel Screws 12 Remove the right side panel by removing four screws two each along its upper and lower edges 13 Using a Pozidriv screwdriver remove the three screws securing the ECD cover to the thermal strap 14 Remove the ECD cover 15 Disconnect any tubing attached to the vent exhaust tube 16 Disconnect the cell collector lead from the PCB interconnect 48 Information for General Licensees Agilent Electron Capture Detectors 17 Loosen the screws securing the clamps that hold the interconnect in place Cell collector lead Clamps PCB interconnect Thermal strap CAUTION The following steps require protection against ESD electrostatic discharge Use a grounded wrist strap part no 9300 0969 large or 9300 0970 small connected to a suitable ground Failure to heed this caution may result in damage to the instrument CAUTION When storing or between handling of PCBs printed circui
23. apture Detectors Information for General Licensees C Agreement States Revised 2 07 Ref www nrc stp orn gov for more detail Became an Agreement State on 10 1 66 5 15 67 7 1 62 9 1 62 2 1 68 7 1 64 12 15 69 Alabama Phone 334 206 5391 Fax 334 206 5387 Arizona Phone 602 255 4845 Fax 602 437 0705 Arkansas Phone 501 661 2301 Fax 501 661 2468 California Phone 916 445 0931 Fax 916 324 3610 Colorado Phone 303 692 3036 Fax 303 343 3692 Florida Phone 850 487 1004 Fax 850 487 0435 Georgia Phone 404 362 2675 Fax 404 362 2653 Became an Agreement State on 6 15 87 1 1 86 1 1 65 3 26 62 5 1 67 4 1 92 1 1 71 Illinois Phone 217 785 9868 Fax 217 524 4724 lowa Phone 515 281 3478 Fax 515 725 0318 Kansas Phone 785 296 1561 Fax 785 296 0984 Kentucky Phone 502 564 3700 Fax 502 564 6533 Louisiana Phone 225 765 0108 Fax 225 765 0222 Maine Phone 207 287 5698 Fax 207 287 4172 Maryland Phone 410 631 3300 Fax 410 631 3198 Apg Agilent Technologies 69 C Agreement States Revised 2 07 Became an Agreement State on 3 1 97 7 1 62 5 16 66 5 1 74 10 15 62 8 1 64 9 1 69 10 1 66 7 1 12 7 31 99 Massachusetts Phone 617 727 6214 Fax 617 727 2098 Mississippi Phone 601 987 6894 Fax 601 987 6887 New Hampshire Phone 603 271 4588 Fax 603 225 2325 New Mexico Phone 505 827 1557 Fax 505 8
24. censees Information for General Licensees Contents Important Information For General License Holders Please Read 7 Reference ECD control 7 Radiation Safety Program Suggestions 8 Agilent Electron Capture Detectors Information for General Licensees Introduction 9 Definitions 10 What is a Specific License 12 What is a General License 13 General License requirements 13 General License restrictions 14 Description ofthe ECD 15 Properties ofan ECD 15 Regulatory Requirements 16 Safety precautions to follow when handling ECDs 17 ECD warnings 17 Capping yourECD 18 Temperature limitations 18 Who cantransferanECD 19 Maintenance 20 Thermal cleaning 20 Who can open their ECD for cleaning 21 Installation 21 Venting yourECD 22 Storing yourECD 22 Removing yourECD 24 Instructions for removing G1533A 6890 GC G2397A 6890 and 7890 GCs and G2397AE 7820A GC ECDs 24 Removing the detector cover 6890 7890 and 7820A 25 Instructions for removing a HECD from a side mounted third detector box 32 Instructions for removing G1223A and G1224A ECDs 5890 GC 38 Instructions for removing 19233 and 19235 ECDs 5890 GC 44 Instructions for removing 19303 and 19312 ECDs 5880 GC 51 How to Package and Ship ECDs 53 Radioactive Wipe Tests 55 Wipe test companies 56 High wipes 57 Wipe test conversion formulas 57 Incidents 59 Principle of Operation 61 What types of samples do ECDs detect 61 Sensitivity 62 In
25. cific License ECDs Specific License ECDs require the end user to have a Materials License from the NRC or their local State Agency which permits them to possess the applicable type and quantities of radioactive material Customers with a Specific License have more flexibility with their ECD They can typically ship sell or transfer their ECD to any other company or location with a valid Specific License depending on actual license conditions They also have more responsibilities These will be defined in the customer s License and other Regulatory Guidelines Owners of Specific License ECDs are required to comply with the conditions of their license If you would like to obtain a Specific License contact your local Agency Information for General Licensees Agilent Electron Capture Detectors What is a General License General License ECDs do not require end users to have a Materials License Agilent Technologies has a Distribution License with the NRC that allows us to distribute Generally Licensed materials Before customers can order a General License ECD they must complete and return a General License Registration Form By completing and signing the form customers certify that they will adhere to the instructions safety warnings and regulatory requirements for Agilent ECDs as specified in the NRC regulations identified at the time of sale General License customers may only operate the ECD at the location specified on th
26. e General License Registration Form They cannot open or clean the detector internally They can only ship the ECD back to Agilent Technologies or another organization licensed to receive radioactive by product material If customers with a General Licensed ECD wish to sell or transfer their ECD to another location that does not possess a radioactive materials license the ECD may only be shipped to the new location via Agilent Technologies Agilent Technologies files reports of ECDs sold to U S and U S district customers to the NRC and applicable Agreement States every 3 months These quarterly reports contain end user s names company names addresses serial numbers model numbers and ECD shipment dates during the previous quarter General License requirements You become a General Licensee automatically when you purchase a General License ECD whether it is mounted in a GC or purchased as an add on accessory You do not have to apply for a General License from the NRC or State Agency However if you reside in an Agreement State you may be required to register your ECD within that state and you may be expected to pay a state tax or fee to support your state s nuclear regulatory program To determine if your state is an Agreement State or to obtain the addresses contact persons and telephone numbers of the agreement states refer to Appendix C at the end of this booklet Information for General Licensees 13 Agilent El
27. ectron Capture Detectors 14 General License restrictions Certain restrictions apply to General Licenses They are 1 2 3 Owners shall not open the ECD cell Owners shall not modify the cell in any manner Owners shall not use any solvent including water to internally clean the cell see Thermal cleaning on page 20 Owners shall not interfere with or attempt to defeat the overheat circuitry that may be supplied with the ECD Owners shall not transfer the ECD to another person or another location except as described in the applicable Regulations See Who can transfer an ECD on page 19 for additional information Owners must perform a radioactive leak test at least every 6 months Owners must maintain records as required by your local Agency see Appendix C and Appendix D Owners must notify the Agency in case of incidents or failures that might lead to a hazardous condition Information for General Licensees Agilent Electron Capture Detectors Description of the ECD The ECD can be purchased as an option with the instrument in which case it is installed in your GC at the factory or as an add on accessory to be installed by you or by Agilent Technologies The ECD consists of the detector cell the thermal insulation that surrounds it mounting hardware the ECD cover and associated overheat protection circuitry if appropriate The two halves of the ECD body are joined by tamper proof sc
28. eir ECD for cleaning e Customers must have a current Specific License issued by either the NRC or the applicable Agreement State and The license must specify that they are qualified to clean ECDs Installation ECDs ordered as an option to an Agilent GC are installed at the factory If the ECD is purchased as an add on accessory the ECD will be shipped with detailed installation instructions WARNING 5880 GCs Only To prevent possible creation of a hazardous situation the instructions must be followed exactly Pay special attention to those sections concerning the overheat protection board and the thermal measurement board Information for General Licensees 21 Agilent Electron Capture Detectors 22 The instructions include a procedure for verifying correct operation of the overheat protection circuitry If this circuitry does not function correctly turn the instrument off notify your local Agilent service organization immediately and do not attempt to use the instrument When installing an ECD always remember to vent the detector in accordance with the procedure specified in Venting your ECD on page 22 and remember to install all labels as instructed Venting your ECD The instrument in which the ECD is mounted must be placed where the ECD effluent can be vented The ECD shall not be vented into the laboratory environment A vent line to a fume hood is a convenient way to accomplish this This precaution is ta
29. ge gas through an ECD in storage or purging the ECD well and sealing an inert gas inside to prevent air oxygen and water from diffusing into the Information for General Licensees Agilent Electron Capture Detectors active area of the cell Nitrogen by itself is not a problem but in combination with oxygen very corrosive components could be formed An inert gas such as argon or helium would probably be best for this purge gas The 6 month wipe tests for leakage of radioactive material see Radioactive Wipe Tests on page 55 must continue during periods of inactivity or storage Information for General Licensees 23 Agilent Electron Capture Detectors Removing your ECD You will need to remove the ECD if you wish to reposition it on the GC or return it to Agilent Technologies The ECD consists of two parts the ECD cell and the heated block Under no conditions is the ECD cell to be disassembled Begin by turning the heated zone off and allowing the instrument to cool to room temperature When the ECD has cooled turn all gas flows off remove the column to which the detector is connected and turn the main instrument power off Disconnect the main power cord from the wall receptacle The instructions for removing the ECD from your chromatograph vary with the GC model Determine which model ECD you have and follow the appropriate instructions When removing the ECD wear disposable gloves and wash your hands thoroughly with mild
30. h all current regulations including requirements for training packaging labeling and documentation procedures Most primary carriers use the IATA regulations however consult with your selected carrier for additional information ca Agilent Technologies 63 A Instructions for Customer Return of ECDs per Compliance with IATA Regulations Air Transportation Definition of Excepted Quantities Excerpted from IATA 2 7 Very small quantities of dangerous goods may be transported in sucha manner that they may be excepted from the marking loading and documentation of these Regulations When they are transported under these provisions such goods are called Dangerous Goods in Excepted Quantities In the case of radioactive material the requirements for radioactive material in excepted packages is found in IATA 10 5 9 Excepted Package Activity Limits for ECD Returns Calculated from Table 10 5 A The activity of an ECD cell an item in Table 10 5 A is below the limit of 800 mCi for Ni A2 800 Ci therefore 800 Ci x 0 01 8 Ci or 8000 mCi This qualifies all packages containing a single ECD at 15 mCi as an excepted quantity Table 10 5 4 Excepted Package Activity Limits 10 5 9 4 Nature of Contents Materials Instruments and articles Package limits Item limits Package limits Solids Special form 103A 107A Ay Other form 103A 107A Ay Liquids 104A 103A 101A Gases Tritium 2x107A 2x107A 2x10 A Special form
31. ions for Customer Return of ECDs per Compliance with IATA Regulations Air Transportation 66 Information for General Licensees Agilent Electron Capture Detectors Information for General Licensees ee B CODE OF FEDERAL REGULATIONS s TITLE 10 ENERGY CHAPTER 1 NUCLEAR REGULATORY COMMISSION Please access the NRC s home page at www nrc gov Open the Reference Library icon and then Title 10 of the Code of Federal Regulations Topics of interest include PART 20 STANDARDS FOR PROTECTION AGAINST RADIATION Section 20 2201 Reports of theft or loss of licensed material Section 20 2202 Notification of incidents Section 20 2203 Reports of exposure exceeding constraints or limits PART 30 RULES OF GENERAL APPLICATION TO DOMESTIC LICENSING OF BYPRODUCT MATERIAL Section 30 34 Terms and conditions of licenses Section 30 51 Records Section 30 52 Inspections Section 30 53 Tests Section 30 61 Modification and revocation of licenses PART 31 GENERAL DOMESTIC LICENSES FOR BY PRODUCT MATERIAL Section 31 2 Terms and conditions Section 31 5 Certain measuring gauging or controlling devices Only a portion of the standards mentioned above have been identified You may wish to browse other sections of Part 20 for further information Agilent Technologies 67 B CODE OF FEDERAL REGULATIONS TITLE 10 ENERGY CHAPTER 1 NUCLEAR REGULATORY COMMISSION 68 Information for General Licensees Agilent Electron C
32. ken to avoid radioactive contamination of the laboratory if an abnormal condition should occur Agilent Technologies recommends a vent line running to a fume hood The inside diameter should be 6 mm 1 4 inch or greater to prevent back pressure which might cause noise in the ECD signal With a line of this diameter the length of the tubing is not critical Storing your ECD Depending on the needs of the laboratory it may be good practice to have an extra ECD on site to provide rapid turnaround for a contaminated ECD This would be particularly true in laboratories with a very high workload or sample throughput where instrument operation must be maintained This spare ECD cell operation is quite possible with the Agilent design but some precautions may be necessary for trouble free operation when the spare ECD is put into service Due to the extremely chemically active atmosphere inside the ECD it is advisable to keep air and moisture out of the cell The carrier gas flow does this when the detector is in use but storage for an extended period will result in an ECD that does not perform as desired when restored to service This may be due to the formation of corrosive compounds such as nitric acid from the ionized components of air inside the cell To our knowledge this has not been proven but such components would likely be quite detrimental to the ECD if they were present To prevent this occurrence we suggest providing a slow pur
33. lent Electron Capture Detectors Instructions for removing 19233 and 19235 ECDs 5890 GC WARNING Hazardous voltages are present in the instrument when the power cord is connected Avoid a potentially dangerous shock hazard by disconnecting the power cord before working on the instrument 1 Set the main power line switch to the off position Red o visible 2 Disconnect the power cable from its receptacle 3 Allow time for the oven and heated zones to cool 44 Information for General Licensees Agilent Electron Capture Detectors 4 When the heated zones are cool turn off all gas supplies Makeup gas adapter 5 Inside the column oven at the bottom of the ECD to be removed remove the column and hardware associated with the detector s liner column liner nuts ferrules makeup gas adapter etc 6 Remove the injection port cover by grasping its back edge and lifting it upward Lift the hinged top cover at its front edge exposing the detector area Remove the 1 4 inch screw and washer securing the cover at its right side hinge point Information for General Licensees 45 46 Agilent Electron Capture Detectors 9 Remove the screw securing the ground strap to the hinged top cover Injection port cover Top cover Lid shaft Press here to free cover 1 4 inch screw and washer Information for General Licensees Agilent Electron C
34. llustrations and more detailed instructions see your service manual 1 Remove the top cover of the instrument over the ECD area a Ifthe instrument has an automatic sampler installed the top cover is in two parts Only the left part must be removed If the sampler is a 7671 remove all sample vials from the tray If it is a 7672 sampler remove the sample cassette Rotate the sampler to the right until it rests on the right top edge of the mainframe The sampler is heavy so use care to avoid injury or damage to the sampler Do not hold it by the door Remove the two screws at the rear of the left part of the top cover and slide it back and off the instrument b If there is no sampler the top cover is in one piece Remove the two screws at the rear raise the rear of the cover and slide it back and off the instrument 2 Remove the two screws at the top of the right side instrument cover Tilt the cover out and lift it free of the tabs at the bottom 3 Locate the printed circuit board for the detector you are going to remove These are the small boards at the upper left as you look into the right side of the mainframe They are in the same order as the detector locations on the top of the oven ECD boards are labeled NICKEL 63 ELECTRON CAPTURE near the outer edge 4 Use the plastic board puller tabs at the top and bottom to pull the board free of its connector It is not necessary to remove the board just pull it out about 25 mm 1 inch
35. n 10 CFR 31 5 c the entire portion of which may be accessed on the world wide web by following the pathway below www nrc gov Reference Library Title 10 of the Code of Federal Regulations Part 31 31 5 31 5 c Certain measuring gauging or controlling devices stii Agilent Technologies 73 E Self Inspection 74 SELF INSPECTION FORM FOR GENERAL LICENSEES Please print or type Registration No Company Name Address City State ____ Zip Chief Executive Officer Person Responsible for or Plant Manager Radioactive Devices Job Title of Responsible Person Telephone Fax E Mail Address Address where Radioactive Devices Are Used Address City Zip REVIEW OF DEVICE RDS Do not include static eliminators containing polonium 210 Number of radioactive devices possessed at time of previous report n Total number of devices shown on Inventory Verification Form Number of radioactive devices received since previous report eccseeeereee Number of radioactive devices transferred since previous TepOrt ssseeeeeees Fill out transfer report below for devices transferred Number of radioactive devices possessed NOW ccscssescsssssasscessensenseneecesnennneenee Explanation of any discrepancies in the above REPORT OF DEVICE TRANSFERS Note that a general licensee may transfer a radioactive device only to a specific licensee A general licensee may transfer a device t
36. n shipping such occurrences must be reported per 10 CFR 20 2201 Information for General Licensees 59 Agilent Electron Capture Detectors This list is not exhaustive It is intended to illustrate the range of occurrences that could be considered reportable incidents or failures In dealing with radioactive isotopes it is advisable to be overly cautious particularly if you do not have the equipment to make an accurate assessment of the situation Incidents and failures should also be reported to Agilent Technologies Attn Radiation Safety Officer 2850 Centerville Road Wilmington Delaware 19808 1610 60 Information for General Licensees Agilent Electron Capture Detectors Principle of Operation The radioactive source in this ECD produces high energy electrons called beta particles These beta particles collide and interact with the carrier gas molecules causing a multiplication of the number of electrons and a decrease in their energy Each beta particle produces approximately 100 of these low energy electrons also known as free electrons When a sample molecule comes in contact with the free electrons a free electron may be captured by a sample molecule to create a negatively charged ion The voltage across the cell electrodes is pulsed to collect the surviving free electrons while the heavier ions are relatively unaffected and swept out the vent with the carrier gas flow The measured cell current is compared to a refere
37. nce current The pulse rate is adjusted to keep the two currents equal The more free electrons there are the lower the pulse frequency required to match the reference current When a component that captures electrons passes through the cell it causes a decrease in the electron concentration and an increase in the pulse rate This pulse rate is converted to a voltage and recorded What types of samples do ECDs detect The ECD is used for low level detection of electron capturing substances These include mono and poly halogenated compounds nitro derivatives and anhydrides The ECD produces little or no response to hydrocarbons ethers and esters or to aliphatic alcohols ketones and amines Hydrocarbons ethers and esters in that order are the preferred solvents for ECD analysis Because of the combination of very high sensitivity and selectivity provided by the ECD it is widely used for trace level analysis of halogenated particularly chlorinated components A major application is the detection and quantitation of pesticide residues many of which are chlorinated Information for General Licensees 61 Agilent Electron Capture Detectors 62 Sensitivity The response of the ECD depends upon the molecular composition of the analyte and its concentration your ECD the cell cleanliness the column the inlet and the instrument setpoints temperature flow rates and reference current It is important to create calibration curves
38. neumatics manifold Figure 9 The anode purge line Information for General Licensees 35 Agilent Electron Capture Detectors 36 3 Fully loosen the four Torx T 20 screws on the detector pallet s Pi 4 Pull straight out on the detector pallet to remove it from the GC Figure 10 Screws securing the detector pallet 5 Remove the one Torx T 20 screw securing the ECD detector top cover to the detector pallet and remove the cover 6 Disconnect the anode signal wire from the detector 7 Thread the heater sensor leads out of the detector pallet and remove the rest of the detector from the pallet 8 For shipping or storage purposes cap the inlet anode purge and exhaust vent tubing Information for General Licensees Agilent Electron Capture Detectors ji N Detector top cover Anode purge line A i Remove ECD vent tube Remove anode signal wire Detector pallet 9 The ECD detector is now properly disassembled for return to Agilent Call the Technical Support number identified at the front of the booklet for further directions Information for General Licensees 37 Agilent Electron Capture Detectors Instructions for removing G1223A and G1224A ECDs 5890 GC WARNING Hazardous voltages are present in the instrument when the power cord is connected Avoid a potentially dangerous shock hazard by disconnecting the power cord before working on the instrument 1 Set
39. o another general licensee if the device remains in use at the same location See 32 Ill Adm Code 330 220 6 3 H No report is required if a radioactive device is transferred to a specific licensee in order to obtain a replacement device Device Reference Number s Transfer Date Name of Specific Licensee Contact Person Telephone Address City State Zip Information for General Licensees E Self Inspection SELF INSPECTION FORM FOR GENERAL LICENSEES Page 2 of 2 CERTIFICATION OF COMPLIANCE WITH LICENSING REQUIREMENTS 1 Radioactive devices have not been will not be abandoned 32 Il Adm Code 330 220 b 3 F 2 Radioactive devices have been will be transferred to authorized recipients only 32 Hl Adm Code 330 220 6 3 G 3 Theft or loss of a radioactive device or transfer other than for trade in or replacement has been will be reported to the Department of Nuclear Safety 32 Ill Adm Code 340 1210 4 Installation removal and servicing involving radioactive material or its shielding or containment are performed by persons specifically licensed or otherwise authorized to do so 32 Ill Adm Code 330 220 b 3 C 5 Plant relocations or address changes will be reported to the Department of Nuclear Safety 32 Ill Adm Code 320 10 a 6 If applicable to the types of radioactive devices possessed tests for proper operation of an on off mechanism and indicator are performed in accordance with the manufacturer
40. ommission NRC or if your state is an Agreement State the responsible state agency Refer to Appendix C to determine if you are located in an Agreement State or an NRC State Customers located outside of the U S should contact their local Agency to determine the applicable regulations Agreement States The Nuclear Regulatory Commission NRC is the Agency in the U S that regulates radioactive materials However in certain states these regulations by agreement with the NRC are enforced by a State Agency Refer to Appendix C to determine if you are located in an Agreement State or an NRC State ECD Electron capture detector General License ECD This is an ECD that customers in the U S can purchase without having their own radioactive materials license General License ECDs are covered under Agilent Technologies distribution license General License customers are required to complete and sign the General License Registration Card provided at the time of sale and to comply with the requirements of this booklet Specific License ECD This is an ECD that requires customers to possess their own radioactive materials license issued by their local nuclear agency which is valid for the applicable material and quantities A Specific License ECD is physically identical to a General License ECD except for the model number and the detector labeling The General License ECD label contains additional warnings not required
41. on all compounds and evaluate ECD response on a regular basis Even with frequent calibration you can expect the ECD response to change when operating conditions change for instance when analyzing dirty samples that contaminate the ECD Information for General Licensees Agilent Electron Capture Detectors P Information for General Licensees Instructions for Customer Return of 3 ECDs per Compliance with IATA Regulations Air Transportation K n oo e0 ce A 20 Procedures for Packaging Labeling and Marking ECD Packages for Return to Agilent Technologies by Air 1 Plug the entrance fitting and cap the vent tube Place the ECD in a strong plastic bag seal it and pack it in a strong container with shock absorbing packing material a corrugated cardboard box in good condition and bubble wrap is a satisfactory combination 2 This package must be marked with the appropriate Radioactive Material Excepted Packaging label Contact your Agilent Field Repair Center for the required label 3 The Air Bill Air Waybill must list this as Radioactive material excepted package articles UN2911 4 Refer to page 65 for a further explanation of shipping information and instructions IATA Regulations The following are references and excerpts from the International Air Transport Association IATA Dangerous Goods Regulations This information is provided for your convenience It is your responsibility to comply wit
42. onnect the cell anode lead from the PCB interconnect 15 Loosen the locking screw on the ECD cover 40 Information for General Licensees Agilent Electron Capture Detectors 16 Slide the locking tab on the ECD cover back freeing the cover from the anode shaft of the cell Top cover ECD cover Anode lead Cell 17 Carefully slide the ECD cover over the anode shaft and anode and remove it from the ECD 18 Cap the base of the ECD inside the column oven to avoid damage or contamination of the ECD 19 Remove the two Pozidriv screws securing the upper and lower heated blocks to the cell 20 Remove the upper heated block from the cell Information for General Licensees 41 Agilent Electron Capture Detectors 21 Disengage the cell from the lower block Screw Upper heated block Fold lines loosely Do not crimp Anode Cap Socket screw Upper cell body Plated lower body Cap 22 For shipping or storage purposes cap the inlet purge and exhaust vent tubing 42 Information for General Licensees Agilent Electron Capture Detectors 23 The ECD detector is now properly disassembled for return to Agilent Call the Technical Support number identified at the front of the booklet for further directions Fold line loosely do not clamp Cap Gang fitting cap G1533 20520 Information for General Licensees 43 Agi
43. rews that require a special tool for removal This tool is not provided with the ECD It is only supplied to Specific License customers who have a license that permits them to work with open sources Properties of an ECD The radiation source used in the ECD is Ni This material is plated onto the inner surface of the cell body It is a solid at temperatures used in chromatography Some of its properties are listed here e Half life 101 1 years e Emission 65 87 keV maximum beta radiation e Melting point 1453 C e Nominal dimensions of the active part of the ECD Inside diameter 1 2 cm Height 1 cm e Nominal dimensions of the active part of the uECD Inside diameter 6 mm Height 4 2 mm e Activity Refer to the Characteristics of the Sealed Source for the individual model number maximum activity Information for General Licensees 15 Agilent Electron Capture Detectors Regulatory Requirements The full text of the pertinent sections of the NRC Regulations is posted on the World Wide Web See Appendix B for more information In general the following are the regulatory requirements relating to the possession and use of ECDs However it is your responsibility to ensure compliance with the current NRC requirements or your local nuclear Agency requirements 1 2 You must not remove the metal tag attached by wire to the ECD You must comply with the instructions provided in this booklet and any other manuals or instruc
44. rn shipment 5 Determine the carrier s means of transportation to Agilent Technologies 2850 Centerville Rd Wilmington DE 19808 1610 See Appendix A for Procedures to package label and mark ECDs for return to Agilent Technologies by air or ground transportation for shipment by Federal Express use IATA instructions 6 If available affix the preprinted address label originally provided with the ECD If you are using our address label ensure that our current Wilmington Delaware address is on the label All ECDs should be sent to Agilent Technologies Attention ECD Lab 2850 Centerville Road Wilmington DE 19808 1610 Information for General Licensees 53 Agilent Electron Capture Detectors 54 7 All ECDs must be shipped via a licensed common carrier with tracking capabilities we recommend Federal Express ECDs should not be shipped via regular mail because regular mail is not traceable and ECDs should never be hand delivered 8 Regulations cited in this manual were valid at the time of this revision Agilent Technologies accepts no liability for transportation compliance For additional regulatory information regarding shipping ECDs refer to the domestic and or international regulatory requirements in Appendix A Consult with your appropriate transportation officer for changes since the date of this revision Information for General Licensees Agilent Electron Capture Detectors Radioactive Wipe Tests In the U S
45. structions for Customer Return of ECDs per Compliance with IATA Regulations Air Transportation 63 CODE OF FEDERAL REGULATIONS TITLE 10 ENERGY CHAPTER 1 NUCLEAR REGULATORY COMMISSION 67 Agreement States Revised 2 07 69 United States Nuclear Regulatory Commission Regional Offices 71 Self Inspection 73 Index 77 Information for General Licensees Important Information For General License Holders Please Read Reference ECD control Dear Agilent Customer We wish to bring an issue to your attention that a number of our customers and regulatory agencies have shared with us relative to the Nuclear Regulatory Commission s requirements for controlling Electron Capture Detectors ECDs As you are probably aware the ownership and locations of ECDs frequently change as a result of internal equipment lab personnel and company transfers As a result of these changes the awareness of the responsibilities associated with ECD control and monitoring is sometimes lost and an RSO or lab manager may potentially be faced with being unable to provide ownership records when confronted by regulatory inspectors The Nuclear Regulatory Commission NRC your individual state agency and Agilent Technologies have a great interest in your being able to prevent any possible conflict and embarrassment to you or your company Because of this concern we strongly urge you and your company s Radiation Safety Officer RSO to consider incorporating the
46. t boards always place them in static control envelopes or enclosures Information for General Licensees 49 Agilent Electron Capture Detectors 18 Remove the ECDs PCB from the right side of the instrument by grasping it in the center area along its outer edge and pulling it straight out This will draw the interconnect out of the ECD clamps on the thermal strap Shield Thermal strap Insulation Screw ECD cell Heated block 19 Remove the five screws securing the thermal strap and shield to the instrument 20 Remove the shield from the thermal strap by working it over the collector lead and exhaust vent tube carefully Depending on the ECDs location it may be necessary to bend the shield to remove and install it Avoid excessive bending as this will fatigue the metal shield shortening its life 50 Information for General Licensees Agilent Electron Capture Detectors 21 Remove the thermal strap working it carefully over the collector lead and exhaust vent tube 22 Cap the base of the ECD inside the column oven to avoid damage or contamination of the ECD 23 Remove the insulation around the ECD cell to expose the two Pozidriv screws that secure the cell to the heated block Remove the screws 24 Remove the ECD cell from the heated block 25 For shipping or storage purposes cap the inlet purge and exhaust vent tubing Instructions for removing 19303 and 19312 ECDs 5880 GC For i
47. the appropriate authorities General License ECDs Customers cannot transfer their General License ECDs to another company or site within the same company except through Agilent Technologies or a company licensed to redistribute generally licensed materials The receiving entity assumes responsibility for local licensing requirements Information for General Licensees 19 Agilent Electron Capture Detectors Maintenance Customer maintenance of the ECD is limited to installation radioactivity leak testing thermal cleaning and removal of the ECD We recommend that the ECD be returned to the factory for thorough inspection on a periodic basis suggested 5 year intervals One of the easiest ways to monitor the proper operation of the ECD is to monitor the signal baseline See your Operators Manual for specific information Leaks can adversely affect the performance of your ECD It is important to locate and fix any gas leaks Complete instructions for performing leak tests can be found in the Maintenance and Troubleshooting Manual provided with your instrument Instructions for removal of the ECD can be found in this manual Thermal cleaning Thermal cleaning is the only cleaning procedure permitted under the General License Do not introduce any liquid solvent into the ECD cell 20 The ECD effluent must be vented properly during the thermal cleaning process Remove any existing column between the injection port and the
48. the absence of radiation measuring equipment all incidents or significant failures should be reported and the ECD should be taken out of service immediately Because a General Licensee is not required to maintain radiation measurement capability and may not have access to one when needed the following criteria are offered to aid in recognizing possible incidents and other failures High wipe If the leak wipe test results for your ECD exceeds the 0 005 microcuries limit a notification of failure must be reported per 10 CFR 31 5 Temperature runaway A failure in the temperature control circuits of the instrument accompanied by failure of the overheat protection circuits could cause the heating of the detectors to exceed their limits This must be reported if it causes failure or damage to the ECD e Physical damage If the ECD is involved in a fire flood or any other event that may cause harm to the ECD it must be reported per 10 CFR 31 5 e Modification of the ECD Changes to the ECD including drilling welding soldering sawing or other operations are prohibited under a General License If this occurs it must be reported per 10 CFR 31 5 Breakage of the ECD If the inlet fitting or vent tube of the ECD should break off take the ECD out of service immediately and report this failure to the appropriate agency e Lost ECD If you should lose misplace accidentally dispose of an ECD or if an ECD gets lost i
49. the main power line switch to the off position Red o visible 2 Disconnect the power cable from its receptacle 3 Allow time for the oven and heated zones to cool 4 When the heated zones are cool turn off all gas supplies 38 Information for General Licensees Agilent Electron Capture Detectors 5 Inside the column oven at the bottom of the detector to be removed remove the column and hardware associated with the detector liner column liner nuts ferrules makeup gas adapter etc Makeup gas adapter 6 Remove the injection port cover by grasping its back edge and lifting it upward Lift the hinged top cover at its front edge exposing the detector area Remove the 1 4 inch screw and washer securing the cover at its right side hinge point Information for General Licensees 39 Agilent Electron Capture Detectors 9 Remove the screw securing the ground strap to the hinged top cover Injection port cover Top cover Lid shaft Press here to free cover 1 4 inch screw and washer 10 With the lower right side of the cover pushed in lift the right side of the cover and slide it to the right to remove the top cover and lid shaft as a unit 11 Using a Pozidriv screwdriver remove the screw securing the detector top cover to the thermal strap 12 Remove the ECD top cover 13 Disconnect any tubing attached to the ECD purge and vent tubes 14 Disc
50. ther locations or companies You must then notify your state nuclear regulatory agency and regional NRC office listed by state in the Information for General Licensees manual of those changes Indicates extremely important information 8 Information for General Licensees Introduction Agilent Electron Capture Detectors Information for General Licensees This publication describes proper installation operation and maintenance of Agilent electron capture detectors ECDs It also discusses the regulations that govern their use and the safety precautions that must be observed to help avoid radiological hazards The material contained in this booklet concerning regulations is accurate as of the date of writing However regulations may change It is the user s responsibility to maintain compliance according to the latest regulations For customers located outside of the United States The information contained in this booklet relates to the regulations in the U S Though following the safety precautions and many of the requirements in this booklet is a good practice it is your responsibility to comply with your local regulations oa Agilent Technologies Agilent Electron Capture Detectors Definitions 10 Agency This applies to your local organization that regulates the use of radioactive materials in your country state etc As used in this booklet the Agency requirements refer to the Nuclear Regulatory C
51. tions provided that pertain to ECDs If an ECD has been lost or stolen you must notify your local Agency per the guidelines established in 10 CFR 20 2201 Reports of theft or loss of licensed material If there is any evidence of damage to the ECD you must stop using it immediately and notify your local Agency You must perform or have performed a radioactive leak test at least every 6 months If the results of the radioactive leak test indicate radioactivity leakage of 0 005 microcuries or greater you must stop using the ECD immediately and notify your local Agency You must maintain records containing the date the ECD was received dates it was transferred to some other person including return to the factory for repair etc and the results of the radioactivity leak tests These records are subject to inspection by your local Agency You may not transfer the ECD except in accordance with 10 CFR Part 31 See Appendix B for additional information You may not modify the ECD cell by cutting drilling welding or any other destructive or damaging operation under any circumstances 10 Corrosive chemicals must not be introduced to the ECD 11 Disassembly of the ECD is a violation of your General License and is 16 prohibited Only customers who have a Specific License which allows them to do so are permitted to open their ECD Information for General Licensees Agilent Electron Capture Detectors
52. umn is not attached In addition the metal vent tube exiting from the side of the ECD must be capped whenever the vent line is disconnected If the ECD is not going to be used or will be stored see Storing your ECD on page 22 Temperature limitations 18 The maximum detector temperature limit is 400 C 350 C for 5790 and 5880 GCs and the ECD must not be heated above these limits This limit is built into the 5890 6890 7890 and 7820A GCs temperature control systems If a malfunction should occur and the temperature of the ECD should rise to 425 C the instrument s main thermal control system will turn off all the thermal zones For the 5790 and the 5880 GCs if the temperature should rise above 350 C whether due to an incorrect setpoint entry or because of an instrument malfunction a safety circuit will turn the heater power off at 370 10 C Information for General Licensees Agilent Electron Capture Detectors If the ECD heater s should be deactivated a hardware problem may exist in the instrument Consult the instrument manual for information on diagnosing and correcting the problem Who can transfer an ECD Specific License ECDs Customers who own a Specific License ECD can sell lend or transfer their ECD to another company or site depending on the provisions of that site s license Specific License customers are required to maintain records of transfers and report such transfers as required to
53. xhaustive but indicates the kinds of compounds that may cause damage to 63 i detectors WARNING In the extremely unlikely event that both the oven and the ECD heated zone should go into thermal runaway maximum uncontrolled heating in excess of 400 C at the same time and that the ECD remains exposed to this condition for more than 12 hours the following must be done e After turning off the main power and allowing the instrument to cool cap ECD inlet and exhaust vent openings Wear disposable plastic gloves and observe normal safety precautions Information for General Licensees 17 Agilent Electron Capture Detectors e Call the Technical Support number identified at the front of this booklet It is unlikely even in this very unusual situation that radioactive material will escape from the cell However permanent damage to the 63Ni plating within the cell is possible and therefore the cell must be returned to Agilent Do not use solvents to clean the ECD You may not open the ECD cell unless authorized to do so by your local nuclear regulatory agency Do not disturb the four socket head bolts These hold the cell halves together Removing or disturbing them is a violation of the terms of the General License and could create a safety hazard Capping your ECD Overheating or chemical damage could cause radioactive particles to drop from the inlet fitting The ECD inlet fitting must be capped whenever a col
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