Home

Model 3480 Electrospray Aerosol Generator Manual

1. AC Power Connector Figure 3 2 Back Panel of the Model 3480 Electrospray Aerosol Generator Aerosol Exit Flexible tubing with a diameter slightly less than 4 or any 4 Swagelok type fitting can be attached to the aerosol exit Conductive tubing is supplied for use at the aerosol exit to minimize particle loss due to electrostatic charge Model 3480 Electrospray Aerosol Generator Analog Output The analog output is a standard 15 pin D sub connection that allows analog signals to be read by an external instrument to collect Electrospray voltage and current information The pin designations and signal connections are shown in Figure 3 3 and Table 3 1 respectively Note the conversion factors in Table 3 1 8765 43 2 1 gt y 10 06 66686 J 15 14 13 12 11 10 9 Figure 3 3 ANALOG OUTPUT Pin Designations Table 3 1 Signal Connections for Analog Output Configurations Pin Number s Signal 1 Voltage Output 1V 1 00 kV 2 Voltage GND 3 Current Output 1V 100 nA 4 Current GND 5 15 AC Power Connector The AC power connector accepts the line cord supplied to provide AC power to the instrument Line voltage can be 85 to 260 VAC 50 60 Hz single phase 3A max The connector has a built in on off switch Power consumption is 25 Watts max Note Make certain the line cord is plugged into a grounded power outlet Position the Electrospray so the power cord connect
2. Installing the Capillary Step 10 lists instructions for adjusting the position of the capillary tip Make sure to remove power from the instrument and turn off all flows before removing the cover from the instrument Adjusting the Position of the Capillary and the Platinum Wire in the Pressure Chamber In the pressure chamber the capillary and the platinum wire are positioned at the factory to extend near the bottom of a standard sample vial 1 7mL centrifuge tube In most cases the sample to be electrosprayed can be put into a standard sample vial however if a smaller vial must be used the following things must be done The electronic circuits within this instrument are susceptible to electrostatic discharge ESD damage Use ESD precautions to avoid damage a Use only a table top with a grounded conducting surface a Wear a grounded static discharging wrist strap High voltage is accessible in several locations within this instrument Make sure you unplug the power source before removing the cover or performing maintenance procedures Maintenance 5 15 Q Obtain a short piece of a non conductive piece of hollow tubing or a similar object to place in the bottom half of the pressure chamber to allow the smaller vial to be placed securely Q Cut the platinum high voltage wire to length or replace the platinum high voltage wire with a new platinum wire of desired shape and size To modify or replace the platinum high
3. Michelson D 1990 Electrostatic Atomization New York Adam Hilger Pui D Y H and B Y H Liu 1979 Technical paper Aerosol Generation and Calibration of Instruments Mechanical Engr Dept Univ of MN May June Model 3480 Electrospray Aerosol Generator Righetti P G G Tudor and K Ek 1981 Isoelectric Points and Molecular Weights of Proteins A New Table Chromatographic Reviews 149 J Chromatography 220 115 194 3 Wiedensohler A E L tkemeier M Feldpausch and C Helsper 1986 Investigation of the Bipolar Charge Distribution at Various Gas Conditions J Aerosol Sci 17 413 Willeke K and P A Baron 1993 Aerosol Measurement Principles Techniques and Applications New York Van Nostrand Reinhold Wiedensohler A 1988 Technical Note An Approximation of the Bipolar Charge Distribution for Particles in the Submicron Range J Aerosol Sci 10 3 387 389 Wiedensohler A and H J Fissan 1988 Aerosol Charging in High Purity Gases J Aerosol Sci Vol 19 Theory of Operation B 11 Index A AC power connector 3 5 AC POWER IN 2 3 acetic acid 4 3 adjustable conductivity 4 2 adjustable pH 4 2 adjusting capillary tip 5 15 aerosol exit 3 4 aerosol exit port cleaning 5 4 aerosols generating 4 6 air flow control B 7 air leak test 5 8 ammonium acetate 4 2 ammonium hydrozide 4 3 analog output 2 4 3 5 ANALOG OUTPUT 2 4 applying back p
4. for information related to the maintenance of these filters Model 3480 Electrospray Aerosol Generator CHAPTER 4 Operating the Electrospray Use the information in this chapter to become familiar with how to prepare liquid solutions and operate the Model 3480 Electrospray Aerosol Generator Preparing Samples Samples can be prepared and stored using commercially available materials handling procedures and storage equipment Typically a buffer solution is made the conductivity and pH are adjusted and a solid or nonvolatile liquid is dissolved in the buffer solution You may find it most convenient to prepare a large 500 mL buffer solution adjusted to the desired conductivity and pH and then dilute sample material with the buffer solution in a standard sample vial 1 7 mL centrifuge tube Any material or procedure mentioned in this manual is intended for use by qualified professionals familiar with potential chemical hazards and trained in safe laboratory procedures To slow the growth of contaminants in a buffer solution or sample solution refrigerate them when not in use In addition use caution when handling sample vials to avoid transferring contaminants to the vial 4 2 Preparing a Buffer Solution A buffer solution is intended for use in the Electrospray to clean the capillary either before after or between samples It is also useful to use a buffer solution as the solvent to dissolve solids or nonvolatile li
5. section should result in a stable generation of aerosol in the Cone Jet mode of the Electrospray see below for an explanation of the Cone Jet mode Once the liquid is flowing from the capillary tip the high voltage can be adjusted to achieve different Electrospray operating modes Four distinct modes see Figure 4 2 can be observed through the viewing window or by the current LED display as the electric field is increased by increasing the high voltage Dripping mode Pulsating mode Cone Jet mode Model 3480 Electrospray Aerosol Generator and Corona Discharge mode Figure 4 2 shows three photographs of the capillary tip viewed through the viewing window Figure 4 2 Three Views of Capillary Tip Through the Viewing Window 1 No liquid flow 2 Liquid flow but no electric field Dripping mode 3 Liquid flow and an electric field Cone Jet mode The third view illustrates stable electrospray operation Q Dripping mode view 2 in Figure 4 2 occurs when a primary droplet builds up on the end of the capillary until it becomes large enough to be pulled away by the weak electric field The current display is usually near zero in this mode Inspection through the viewing window shows the primary droplet increasing in size until it is pulled away at a very low frequency As the voltage is increased in this mode the primary droplet size decreases a In Pulsating mode the liquid at the tip of the capillary continues to drip but
6. 3480 Electrospray Aerosol Generator Filters 4 Interlock Switch PAS Power Supply High Voltage Supply Module q E Main a S lt S NA Electrospray Zor Chamber Capillary Sleeve Capillary High Voltage Fitting and Shield o o0 Figure 3 4 Main Internal Components Power Supply 15V is supplied to the main PCB by the 25W power supply The power supply contains no user serviceable parts Main PCB Controls all the electronics in the Electrospray This PCB is calibrated at the factory and there should be no need to make adjustments to its components under normal usage High Voltage Supply Module The high voltage supplied to the Electrospray chamber is generated by this component Two modules are available positive high voltage Controls Indicators and Connectors 3 7 3 8 standard and negative high voltage See Chapter 5 for instructions on servicing the high voltage supply module Interlock Switch The interlock switch is a safety measure to ensure that high voltage will not be supplied to any part of the instrument unless the instrument cover is in its proper position Filters These filters are used to clean the air and CO in various flow paths in the instrument See Appendix B Theory of Operation for a flow schematic of the Electrospray and see Chapter 5 Maintenance
7. Labels Description of Caution Warning Symbols The following symbol and an appropriate caution statement are used throughout the manual and on the Model 3480 to draw attention to any steps that require you to take cautionary measures when working with the Model 3480 Caution Caution means be careful lt means if you do not follow the procedures prescribed in this manual you may do something that might result in equipment damage or you might have to take something apart and start over again It also indicates that important information about the operation and maintenance of this instrument is included xii Model 3480 Electrospray Aerosol Generator Warning Warning means that unsafe use of the instrument could result in serious injury to you or cause irrevocable damage to the instrument Follow the procedures prescribed in this manual to use the instrument safely Caution or Warning Symbols The following symbols may accompany cautions and warnings to indicate the nature and consequences of hazards Warns you that uninsulated voltage within the instrument may have sufficient magnitude to cause electric shock Therefore it is dangerous to make any contact with any part inside the instrument Warns you that the instrument is susceptible to electro static dissipation ESD and ESD protection procedures should be followed to avoid damage Indicates the connector is connected to earth ground and cabinet ground Warns y
8. Ring 2501862 Figure 5 2 Viewing Window Assembly 7 Secure the lens by tightening the lens ring retainer using a coin Do not overtighten as it could damage the lens 8 Lightly grease the external O ring and wipe off any excess grease before replacing the viewing window mount in the Electrospray chamber If the view of the capillary tip is still unsatisfactory after focusing the lens see the section later in this chapter Cleaning the Electrospray Chamber Replacing the lonizer The use of controls adjustments or procedures other than those specified in this manual may result in exposure to hazardous radiation The ionizer does not need to be removed or cleaned under normal operating conditions However the ionizer should be removed if the Electrospray chamber needs to be cleaned or if the ionizer is more than twelve months old Use the following procedure to replace the ionizer Refer to Figure 2 2 if necessary Maintenance 5 5 1 Remove the ionizer retainer using the ionizer retainer tool supplied in the accessory kit Contact TSI for instructions on returning the ionizer 2 Place the new ionizer in the ionizer retainer The ionizer mesh side should be facing the open end of the ionizer retainer 3 Install the ionizer retainer making sure the O ring is between the ionization chamber and the ionizer retainer and tighten with the ionizer retainer tool Cleaning the Electrospray Chamber High volt
9. Shoreview MN 55126 U S A Fax 651 490 3824 E mail Address particle tsi com For current information www tsi com Model 3480 Electrospray Aerosol Generator CHAPTER 1 Product Overview This chapter describes the Model 3480 Electrospray Aerosol Generator and gives an overview of how it works Product Description The Model 3480 Electrospray Aerosol Generator shown in Figure 1 1 generates monodisperse aerosols in the size range of 2 to 100 nanometers Beginning with a liquid and adding a solute to form a solution or suspension the Electrospray converts the sample to an aerosol by charging the liquid pushing it through a capillary and exerting an electric field at the capillary tip The liquid evaporates from the droplets formed at the capillary tip while the charge on each droplet is reduced by an ionizer In addition to the vast combination of solutes that could be used in the Electrospray to generate aerosols the user has the ability to control the liquid flow rate through the capillary the intensity of the electric field at the capillary tip and the amount of time the aerosol is exposed to the ionizer Ts L ERT carauasy PESA once e aa 3 coo i Wee Presa ANAT saat ELECTROSPRAY AEROSOL GENERATOR Figure 1 1 Model 3480 Electrospray Aerosol Generator 1 1 Applications The successful use of the electrospray method to generate monodisperse aerosol has been documented in many publications
10. at TSI Incorporated 1 800 874 2811 USA or 651 490 2811 Q If the Electrospray does not operate properly or if you are returning the instrument for service contact TSI at 1 800 874 2811 USA or 651 490 2811 Returning the Electrospray for Service Call TSI at 1 800 874 2811 USA or 651 490 2811 for specific return instructions Customer Service will need this information when you call Q The instrument model number The instrument serial number A purchase order number unless under warranty A billing address A shipping address Oooo Prior to shipping any components to TSI for service or repair please utilize our convenient Return Material Authorization RMA Form which is available online at www tsi com 7 1 The Model P 2042 lonizer must be removed from the Electrospray prior to shipping the instrument See the section titled Replacing the lonizer in Chapter 5 for instructions on how to remove the ionizer Do not ship the ionizer to TSI if the instrument must be returned rather keep the ionizer and ship the instrument without the ionizer Note The ionizer must be replaced 12 months from the date on the ionizer label Contact TSI to order a new ionizer four weeks before the ionizer expiration date When returning an ionizer contact TSI for handling and shipping instructions 7 2 Model 3480 Electrospray Aerosol Generator APPENDIX A Model 3480 Specifications The following specifications
11. at a higher frequency than in dripping mode In addition a visual inspection shows a more cylindrical liquid profile with a cone shaped tip During operation the cylindrical liquid profile increases in length and the current display increases until the primary droplet is pulled away and the current display rapidly decreases As in the dripping mode as the voltage is increased the primary droplet size decreases while the frequency increases Q The Cone Jet mode view 3 in Figure 4 2 occurs when the electric field strength is balanced with the liquid properties A visual inspection shows the conical shape of the profile Taylor Cone but the jet of primary droplets cannot be seen since the primary droplets are very small As voltage is increased the profile does not change significantly while in this mode in addition the total current reading changes very little The cone jet mode is the most stable and useful mode for generating aerosols The voltage setting in this mode is typically 2 00 to 2 50 kV using a 20 mM ammonium acetate buffer solution Q As the voltage is increased further the electric field becomes too strong for the liquid and surrounding gas and the Corona Discharge mode occurs The strong electric field causes the tip of the liquid to become rounded Also the current reading is high because of the current traveling through the CO air sheath flow and erratic because of the instability of this mode Operating the Elec
12. manual did you find most helpful 5 Rate your level of experience with the product Beginning Intermediate Expert 6 Please provide us with the following information Name Address Title Company TSI Incorporated 500 Cardigan Road Shoreview MN 55126 U S A USA Tel 1 800 874 2811 UK Tel 44 149 4 459200 France Tel 33 491 95 21 90 Germany Tel 49 241 523030 Sweden Tel 46 8595 13230 India Tel 91 80 41132470 China Tel 86 10 8260 1595 Contact your local TS Distributor or visit our website www tsi com for more detailed specifications E mail particle tsi com E mail tsiuk tsi com E mail tsifrance tsi com E mail tsigmbh tsi com E mail tsiab tsi com E mail tsi india tsi com E mail tsibeijing tsi com Website Website Website Website Website P N 1933793 RevE Copyright 2008 by TS Incorporated www tsi com www tsiinc co uk www tsiinc fr www tsiinc de www tsi se Printed in U S A q yo SCIENCE INNOVATION
13. plate into the ionization chamber and the placement of the ionizer cause the droplets to encounter the ions nearly immediately upon their formation Model 3480 Electrospray Aerosol Generator Equilibrium Charging Theory The equilibrium charge distribution generated by the ionizer of the Electrospray can be represented by a theoretical model developed by Wiedensohler 1986 which is an approximation of the Fuchs 1963 diffusion theory for particle sizes in the submicrometer regime Figure B 2 shows the measured data of Wiedensohler 1986 and theoretical curves based on the theory of Fuchs 1963 and calculated by Wiedensohler 1988 The theoretically determined charge distribution agrees well with experimental data It can be seen from the figure that the fraction of positively charged particles is different from the fraction of negatively charged particles Table B 2 lists the fractions of particles in air that carry 1 2 3 and 4 charge units E AS ETTE EA teal mrss O K N Ladung K E e N positive F R o N negative N 2 papa bea eel E A AT a Figure B 2 Bipolar Particle Charge Distribution in Air Wiedensohler and Fissan 1988 Theory of Operation B 5 Table B 2 Midpoint Particle Diameters and Fraction of Total Particle Concentration that Carries 1 2 3 and 4 Elementary Charges Fraction of Total Particle Particle Concentration That Carries This Diameter Number 1 4 of Posit
14. the capillary is 3 7 psi 4 atm and the viscosity of water at 20 C is 0 89E 2 poise Given these conditions the nominal liquid flow rate is 66 nL min Table B 1 lists values of the liquid flow rate as a function of B 2 Model 3480 Electrospray Aerosol Generator pressure and capillary diameter Also included in the table is the volume of the capillary residence time of the liquid in the capillary and the length of time for 1 mL to flow through the capillary Table B 1 Capillary Flow Characteristics for Water at 20 C Capillary Capillary Inner Liquid Flow Capillary Liquid Sample Time Pressure Drop Diameter rate Volume Residence Time AP psi D um Q nL min V nL t Sec ts days mL Theory of Operation B 3 Calculating Primary Droplet Diameter As the liquid reaches the end of the capillary the electric field induces a surface charge on the liquid The electrostatic charge of the liquid produces forces that cause the liquid to disperse into a fine spray of charged droplets The diameter of the charged droplet as it first leaves the tip of the capillary is referred to as the primary droplet diameter After the primary droplet is generated the liquid from the primary droplet evaporates in the ionization chamber and an aerosol particle remains If a sucrose solution is used to generate an aerosol the sucrose concentration can be varied to generate different particle diameters For any sucrose particle diameter D the primar
15. vial as shown in Figure 4 1 Use caution not to contaminate the sample 4 Replace the bottom half of the pressure chamber by aligning the grooves to the pins in the top half and pushing the bottom half upwards making sure the capillary and platinum wire are aligned with the sample vial As the pins enter the grooves continue pushing upwards while turning the bottom half clockwise until the bottom half locks in place The capillary and platinum wire are adjusted for use with a 1 7 mL centrifuge tube if it is necessary to use a different sized vial see Chapter 5 Maintenance for instructions on adjusting the capillary and platinum wire positions to avoid breaking the capillary or damaging the platinum wire Operating the Electrospray 4 5 Sample Vial Pressure Chamber Bottom Half Figure 4 1 Inserting a Sample Vial into the Pressure Chamber 5 Turn the pressure regulator knob clockwise until the pressure gauge reads 3 7 psi 6 Turn the air rotameter knob counterclockwise to reach 1 0 L min 7 Turn the CO rotameter knob counterclockwise to reach 0 1 L min 8 Turn the voltage adjustment knob clockwise to reach 2 30 kV 9 Within two minutes the liquid should be exiting the capillary See Chapter 6 Troubleshooting if the liquid has not made it through the capillary after two minutes Generating Aerosols 4 6 The Electrospray operating parameters set in the Starting Up the Electrospray
16. voltage wire use the instructions earlier in this chapter titled Cleaning the Pressure Chamber to remove the capillary and the high voltage fitting The platinum high voltage wire is soldered to the inside of the brass pin on the bottom of the high voltage fitting and can be removed by heating with a soldering iron Finally solder the new platinum wire to the inside of the brass pin and replace the high voltage fitting Q Reinstall the capillary using the instructions earlier in this chapter titled Installing the Capillary Reversing the High Voltage Polarity The electronic circuits within this instrument are susceptible to electrostatic discharge ESD damage Use ESD precautions to avoid damage a Use only a table top with a grounded conducting surface a Wear a grounded static discharging wrist strap High voltage is accessible in several locations within this instrument Make sure you unplug the power source before removing the cover or performing maintenance procedures Note Refer to Figure 5 6 and note the location of the high voltage power supply to determine whether a high voltage module has a positive or negative polarity In a positive module shown the high voltage power supply is located on the exposed side of the high voltage PCB In a negative module the high voltage power supply is located on the opposite side of the high voltage PCB Model 3480 Electrospray Aerosol Generator High Vo
17. was removed from the discussion and reader was referred to a related publication for more information Part Number Copyright Address Fax No E mail Address Limitation of Warranty and Liability effective July 2000 Service Policy Warranty 1933793 Revision E March 2007 TSI Incorporated 2008 All rights reserved TSI Incorporated 500 Cardigan Road Shoreview MN 55126 USA 651 490 3824 particle tsi com Seller warrants the goods sold hereunder under normal use and service as described in the operator s manual shall be free from defects in workmanship and material for 12 months or the length of time specified in the operator s manual from the date of shipment to the customer This warranty period is inclusive of any statutory warranty This limited warranty is subject to the following exclusions a Hot wire or hot film sensors used with research anemometers and certain other components when indicated in specifications are warranted for 90 days from the date of shipment b Parts repaired or replaced as a result of repair services are warranted to be free from defects in workmanship and material under normal use for 90 days from the date of shipment c Seller does not provide any warranty on finished goods manufactured by others or on any fuses batteries or other consumable materials Only the original manufacturer s warranty applies d Unless specifically authorized in a separate writing by Selle
18. which are subject to change list the most important features of the Model 3480 Electrospray Aerosol Generator Table A 1 Specifications of the Model 3480 Electrospray Aerosol Generator Mode of operation Generation of aerosols from liquid solutions or suspensions using an electrospray method Capillary dimension 25 pm 250 mm length Particle type Solids or nonvolatile liquids soluble in 20 mM ammonium acetate solution in ultrapure water or 0 05 trifluoroacetic acid in ultrapure water Suspensions in some solvents up to a particle size of 100 nm Initial droplet diameter 150 nm nominal Particle generation rate gt 10 particles cm Particle size range 2 to 100 nm Liquid conductivity 0 2 S m nominal Liquid flow rate 66 nL min nominal Differential pressure O to 5 psi 3 7 psi nominal Flow rates AMD 0 2 to 2 5 L min 1 L min nominal O 0 05 to 0 5 L min 0 1 L min nominal Aerosol 0 25 to 3 L min determined by the sum of air and CO flow rates TOMIZER 0 25226 22002520 500nrenrneesre Bipolar Po 210 5 millicurie half life of 138 days shipped separately Front panel displays LED 3 5 digit voltage and current displays Ports Air Inlet 2000063050 0003 505002 Ya in OD Swagelok con
19. 1016 O Ring Orifice Plate 2901014 Figure 5 1 Inlet Fitting 1 Remove power from the instrument and turn off all flows 2 Remove the cover by loosening the four screws securing the cover they do not have to be removed and pulling the cover upward while pushing down on the top of the front panel of the instrument or on the viewing window mount 3 Remove the screw that holds the inlet fitting in place 4 Pull the inlet fitting out of the Electrospray chamber Use a twisting motion if necessary Maintenance 5 3 5 Detach the capillary from the inlet fitting see Removing the Capillary later in this chapter 6 Remove the O rings using a tweezers or similar tool Inspect the O rings for damage and replace if necessary 7 Use a soft cloth soaked in alcohol or a mild solvent to clean the outside of the inlet fitting and flush the inside of the inlet fitting with alcohol or a mild solvent to clear any deposits that may have formed 8 Rinse the inlet fitting with clean water 9 Blow clean dry air through and on the inlet fitting to evaporate the water 10 Replace the O rings and lightly apply the vacuum grease supplied with the instrument Remove any excess grease 11 Replace the inlet fitting and reinstall the capillary see Installing the Capillary later in this chapter 12 Replace the cover on the instrument and tighten the four screws that secure the cover Cleaning the Aerosol Exit
20. 3 changing samples 4 8 cleaning aerosol exit port 5 4 Electrospray chamber 5 6 viewing window lens 5 4 CO inlet 3 5 CO Input 2 4 connectors 3 1 controls 3 1 Electrospray chamber 3 6 filter Index 1 Electrospray Aerosol Generator continued replacing 5 19 filtered air inlet 3 5 filtered air input 2 4 filters 3 8 front panel 3 1 generating aerosols 4 6 high voltage fitting and shield 3 6 high voltage supply module 3 7 indicators 3 1 3 2 inlet fitting 5 3 interlock switch 3 8 internal components 3 6 drawing 3 7 ionizer 2 5 Ionizer retainer 3 3 isolating leaks 5 10 leak checking 5 9 Electrospray chamber and pressure chamber 5 9 LED display 3 1 main PCB 3 7 maintenance 5 1 5 12 periodic 5 1 schedule 5 1 measuring and adjusting conductivity 4 2 measuring and adjusting pH 4 3 mounting 2 2 operating 4 1 operating temperature xiv operation 1 2 operation unstable 6 1 packing list 2 1 photograph 1 1 power connection 2 3 power supply 3 7 preparing a buffer solution 4 2 preparing samples 4 1 pressure chamber 3 3 adjusting capillary 5 15 adjusting platinum wire 5 15 cleaning 5 10 5 11 pressure regulator cleaning 5 19 pressure regulator and gauge 3 3 product overview 1 1 proteins 4 4 PSL 4 4 purging the capillary 5 1 replacement parts 5 19 returning for service 7 1 rotameter 3 3 cleaning 5 19 safety xi chemical xiv electrical xv labels xi radi
21. 4 Cleaning the Pressure Chamber Maintenance 5 11 5 Generously grease the O ring on the bottom half of the pressure chamber and the pin grooves using the vacuum grease supplied in the accessory kit Remove excess grease and insert the bottom half into the top half of the pressure chamber Reapply vacuum grease to the O ring and pin grooves if necessary 6 Reinstall the high voltage fitting using caution not to bend or damage the platinum high voltage wire 7 Reattach the high voltage cable to the inlet fitting and install the capillary using the instructions in the next section titled Installing the Capillary Special Maintenance Removing the Capillary The capillary needs to be removed when cleaning any part of the Electrospray chamber or if the capillary becomes damaged or the capillary tip becomes dirty Use the following steps and Figure 5 5 to remove the capillary High voltage is accessible in several locations within this instrument Make sure you unplug the power source before removing the cover or performing maintenance procedures 1 Remove power from the instrument and turn off all flows 2 Remove the cover by loosening the four screws securing the cover they do not have to be removed and pulling the cover upward while pushing down on the top of the front panel of the instrument or on the viewing window mount 5 12 Model 3480 Electrospray Aerosol Generator High Voltage Shield Capillary Sl
22. 5 psi forward pressure drop across the capillary and finally try cleaning the capillary tip or purging the capillary see Chapter 5 If the capillary is still plugged it should be discarded and replaced see Chapter 5 Table 6 2 Troubleshooting if the Capillary has Become Plugged Reason Solution A contaminant or large Back pressure the capillary using the particle in the sample vial procedure listed below has plugged the capillary inlet Residue has built up on the Purge the capillary see Chapter 5 inner walls of the capillary Residue has built up on the Clean the capillary tip see Chapter 5 capillary tip The capillary has not been Purge the capillary see Chapter 5 cleaned properly when shutting down the Electrospray The capillary tip has become Replace the capillary see Chapter 5 broken during maintenance Removing the Capillary and or handling procedures Installing the Capillary Applying Back Pressure to the Capillary If the capillary becomes plugged the first attempt to unplug the capillary should be to apply back pressure to the capillary The following procedure should unplug the capillary if a contaminant or large particle in the sample vial has plugged the capillary inlet 1 Remove power from the instrument and turn off all flows 2 Connect a compressed air source capable of generating 5 psi pressure or a large syringe gt 50 cc to the aerosol exit Do not exceed 5 psi since
23. 50 C Excess temperatures may damage the ionizer resulting in radioactive contamination Q The ionizer must be returned after 12 months Contact TSI for information and instructions on returning the ionizer Q Do not remove any parts from the Electrospray unless you are specifically told to do so in this manual Chemical Safety Observe these warnings when operating the Electrospray Aerosol Generator Any material or procedure mentioned in this manual is intended for use by qualified professionals familiar with potential chemical hazards and trained in safe laboratory procedures Corrosive materials can degrade the stainless steel and aluminum chamber inside the Electrospray Aerosol Generator Do not operate the Electrospray with chemicals that corrode stainless steel or aluminum xiv Model 3480 Electrospray Aerosol Generator High concentrations of aerosols can be hazardous Use a filter at the Electrospray exit if the generated aerosol is not being used by another instrument or in another application Electrical Safety The Electrospray Aerosol Generator contains a high voltage source on the inside of the instrument Under normal circumstances you will not come into contact with hazardous voltage However always remove power from the Electrospray before removing the cover from the instrument High voltage is accessible in several locations within this instrument Make sure you unplug the power source before re
24. 956 2 27E9D pkT E N In Hz e m e Zi 47 2e0D p kT 2 a kl e S N Equation B 5 where l elementary charge 1 60217733E 19 coulomb Es dielectric constant 8 854187817E 12 farad m for air D particle diameter m k Boltzmann s constant 1 380658E 23 joule K for air T Temperature K N number of elementary charge units Z Z ion mobility ratio 0 875 Wiedensohler Air and CO Flow Control This section describes the flow of air and CO through the Electrospray A flow schematic is shown in Figure B 3 Theory of Operation B 7 B 8 DIFFERENTIAL PRESSURE REGULATOR FILTER ORIFICE TO PRESSURE CHAMBER ROTAMETER FILTER CHAMBER FILTER ROTAMETER Figure B 3 Electrospray Flow Schematic The differential pressure regulator is used to maintain the pressure drop across the Electrospray capillary therefore if the flow rates of the air and CO into the Electrospray chamber are changed the capillary pressure drop will not change The high pressure tap for the pressure gauge is connected to the output of the pressure regulator which is at the same pressure as the pressure chamber The low pressure tap is connected in the same orientation as the air CO mixture inlet to the ionization chamber which is immediately upstream of the capillary tip The orifice leading to the pressure chamber is used to allow the quick release pressure chamber bottom to be removed withou
25. Although the basic principles are well understood many of the details explaining how different operating parameters affect the electrospray method remain to be discovered Known applications for this instrument include Q Studies of nano aerosols Q Instrument calibration Q Dispersion of nanometer sized powders for nano powder sizing a Aerosol analysis in the macromolecular and submicrometer range a Research involving parameters that influence the electrospray method How the Electrospray Operates 1 2 A sample solution is stored in a cone shaped vial enclosed in a cylindrical pressure chamber The chamber accommodates a capillary and a high voltage platinum wire both of which are immersed in the solution A differential pressure causes the solution to be pushed through the capillary An electrical field pulls the charged solution out of the capillary exit forming droplets that are mixed with clean air and CO This produces a sheath flow which transports the droplets to the Electrospray chamber The highly charged droplets are neutralized by a radioactive ionizer Polonium 210 and the liquid is evaporated before the aerosol exits the instrument Model 3480 Electrospray Aerosol Generator Packing List CHAPTER 2 Unpacking and Setting Up the System Use this information in this chapter to unpack and set up the Model 3480 Electrospray Aerosol Generator As you unpack the shipping container make certain the sh
26. How the Electrospray Operates oocccoccnoccnoccnnccnnannnacnnnananacaneno 1 2 CHAPTER 2 Unpacking and Setting Up the System 2 1 Packing TIS roio ise ien eA AA E 2 1 Mounting the Instrument rsresrrsrierisrisna rieres iaaea 2 2 Ventilation Requirements rn o e ea AEEA NA 2 2 Checking the Zero of the Pressure Gauge coooccconccnnncccnnnncnns 2 3 Power Connection ita ai avs EEE E degen deve eee 2 3 Analog Output tr dai rE a Seeded A T 2 4 Filtered Air Input sertar EE AAE TSAS 2 4 eieae EET EEE clos ies teins EE E E A 2 4 Inistalling The Ionizer yds ser cia riada ENA E E 2 5 CHAPTER 3 Controls Indicators and Connectors 3 1 Pront Panel O tetas aeees 3 1 LED Displays vz vsscveseltensevannsseevessays er ans O Enar EEOAE NERA R 3 1 Voltage Adjustment Knob ooccoocnniocnnocnnncnnncnnncnnncnnaconacanicanoso 3 2 Indicators saioren eaa AE AE OAE ed 3 2 Rotameters yi iaee re EE E EE TEE E S AS NE S 3 3 Pressure Regulator and Gauge sssssessesessrsrrrserreeseeresses 3 3 Pressure Chamber 3 3 Viewing WIN O We siesreto sista cece na siea renina cnesdecbedny rasa nde cian 3 3 lonizer Retainer scaricare ed 3 3 Back Panel occitano 3 4 Aerosol Eta dadas 3 4 Analog OULPUts ecos rororsranooeo nds aae iaae E Aa 3 5 vii AC Power CoOmnectolr ccccccecccsceccceseeceescceetecseeeeeseesseceense 3 5 Filtered Air Inlet 2 siisocodziatig ada 3 5 COSUDE vencio id a 3 5 Intertial Components a a T NEE 3 6 Capilla
27. Maintenance Periodic cleaning of several parts of the Electrospray is necessary to ensure proper performance The capillary should be cleaned after each day s use to prevent buildup of solutes If aerosol deposits accumulate on the orifice plate the orifice could be reduced in size or eventually plugged In addition aerosol deposits will buildup on the Electrospray chamber and viewing window optics although at a lesser frequency than on the orifice plate The service intervals depend on the type and concentration of aerosols generated with the Electrospray The following maintenance schedule is suggested for the Electrospray Table 5 1 Maintenance Schedule Maintenance Task momen Replacing the ionizer 12 months Cleaning the Electrospray chamber Performing an air leak test If you clean the Electrospray chamber or the viewing window lens Cleaning the pressure chamber Purging the Capillary The capillary should be purged after each day s use to keep solutes from building up on the inside of the capillary It may need to be purged more often depending on the chemicals you are using or if you suspect the capillary has become partially or fully plugged see also page 6 3 Any material or procedure mentioned in this manual is intended for use by qualified professionals familiar with potential chemical hazards and trained in safe laboratory procedures To purge the capillary place one of the following solutions
28. Po AR TeG ae Aerosol Generators Model 3480 Electrospray Aerosol Generator User s Manual P N 1933793 Revision E March 2008 4 yo SCIENCE INNOVATION TSE Model 3480 Electrospray Aerosol Generator User s Manual Product Overview Unpacking and Setting Up the System Controls Indicators and Connectors Operating the Electrospray Maintenance Troubleshooting Contacting Customer Service Appendixes Manual History The following is a manual history of the Model 3480 Electrospray Aerosol Generator Part Number 1933793 Revision Date Preliminary Version March 1999 Final May 1999 A July 2000 B February 2002 C October 2002 D October 2003 E March 2008 In Revision A TSI s Limitation of Warranty and Liability was updated In Revision B Table 2 1 was updated Appendix C was removed and a few minor corrections were made throughout manual In Revision C TSI s phone numbers and address were updated Front and back manual covers were updated In Revision D directions for replacing the capillaries were updated due to a change to the capillary design Miscellaneous changes were made throughout manual and pictures were updated In Revision E manual was updated with new logo and look The equation used for calculating final particle diameter D when using a sucrose solution with the Electrospray was corrected and simplified Relationship between viscosity of solution and concentration
29. Port The aerosol exit port can be cleaned as needed without disassembling the instrument Simply remove power and turn off all flows to the instrument and use a cotton swab moistened with alcohol or a mild detergent to clean the inside of the aerosol exit port see Figure 3 2 Cleaning the Viewing Window Lens If the viewing window lens becomes dirty it can be cleaned without removing the cover from the instrument First try cleaning the lens without disassembling the instrument by using a cotton swab soaked in alcohol a mild detergent or a lens cleaner If the lens is still dirty use the following procedure to clean the viewing window lens 1 Remove power from the instrument and turn off all flows 2 Using Figure 5 2 as a guide unscrew the viewing window mount by hand and remove the lens ring retainer using a coin 3 Turn the viewing window mount upside down to remove the lens 4 Clean the lens using a soft cloth soaked in alcohol a mild detergent or a lens cleaner 5 If necessary the O rings can be removed from the viewing window mount and the viewing window mount can be cleaned using a soft cloth soaked in alcohol or a mild detergent Model 3480 Electrospray Aerosol Generator 6 Replace the lens in the viewing window mount making sure the O rings are installed properly The flat side of the lens should be facing the O ring Lens Ring Retainer Lens be T O Ring 2501010 Viewing Window Mount O
30. a relief valve is attached to the Electrospray chamber If the relief valve opens remove all pressure from the Electrospray chamber and the relief valve will reset automatically Troubleshooting 6 3 Applying more than 5 psi pressure to the Electrospray chamber will cause a relief valve to open If the relief valve opens remove all pressure from the Electrospray chamber and the relief valve will reset automatically 3 With a sample solution installed in the bottom half of the pressure chamber apply up to 5 psi pressure to the aerosol exit for 15 seconds 4 Remove pressure from the aerosol exit and run the Electrospray under normal operating conditions to check if the capillary is unplugged If not repeat steps 1 4 except apply back pressure for several minutes until bubbles can be seen exiting the capillary into the sample vial If bubbles are not seen after 5 minutes at 5 psi back pressure refer to the alternative solutions mentioned earlier in this chapter to unplug the capillary 6 4 Model 3480 Electrospray Aerosol Generator CHAPTER 7 Contacting Customer Service This chapter gives directions for contacting people at TSI Incorporated for technical information and directions for returning the Model 3480 Electrospray for service Technical Contacts Q Ifyou have any difficulty setting up or operating the Electrospray or if you have technical or application questions about this system contact an applications engineer
31. acking List oocooncoccocinccnccnnconconconcnnacaninnnono 2 1 Signal Connections for Analog Output Configurations 3 5 Selected Proteins and Their Diameters c cee 4 5 Maintenance Schedule sisser a na Sa 5 1 Replacement Parts piisi ih ii k rea ieS 5 19 Troubleshooting if the Electrospray Operation is Unstable Grosero a saad A wend EE E EA vente 6 2 Troubleshooting if the Capillary has Become Plugged 6 3 Specifications of the Model 3480 Electrospray Aerosol GEODETI oec aa A E E 8 1 Capillary Flow Characteristics for Water at 20 C B 3 Midpoint Particle Diameters and Fraction of Total Particle Concentration that Carries 1 2 3 and 4 Elementary Charges oocoooccnoconoconiconaconaconaccnancnnacaninono B 6 Coefficients for Equation B 4 occcoocccnnnccnnnccnnnnccnnonanininnnnns B 7 Model 3480 Electrospray Aerosol Generator Labels Safety This section gives instructions to promote safe and proper handling of the Model 3480 Electrospray Aerosol Generator There are no user serviceable parts inside the instrument Refer all repair and maintenance to a qualified technician All maintenance and repair information in this manual is included for use by a qualified technician To prevent problems take these precautions a Do not remove any parts from the instrument unless you are specifically told to do so in this manual Q Do not remove the instrument housing or covers while power
32. age is accessible in several locations within this instrument Make sure you unplug the power source before removing the cover or performing maintenance procedures The Electrospray chamber should not need cleaning as often as the orifice plate under most operating conditions However the Electrospray chamber should be checked periodically for corrosion or aerosol deposits depending on the nature of the chemicals used in the Electrospray It is easiest to clean the Electrospray chamber while cleaning the orifice plate Refer to Figure 5 3 and use the following procedure to clean the Electrospray chamber 1 Follow steps 1 through 10 in the section Cleaning the Orifice Plate earlier in this chapter In addition you may want to remove the capillary to avoid damage while cleaning the Electrospray chamber See the section Removing the Capillary later in this chapter for details 2 Remove the ionizer using the ionizer retainer tool supplied in the accessory kit and place the ionizer in a safe place Use Figure 2 2 as a guide if necessary Model 3480 Electrospray Aerosol Generator Aerosol Exit Tube gt lt Exit Manifold Block O Ring 2501029 a lonization Chamber Inlet Manifold Block Viewing Window Lens Assembly Hex Nut Inlet Fitting Capillary Inserts Here Figure 5 3 Cleaning the Electrospray Chamber 3 Remove the common ground screw on the side of the Electrospray chamber Also detac
33. age wire through the groove in the bottom edge of the high voltage shield and tightening the mounting screw 8 Turn on the power to the instrument If the cover is removed high voltage will not be supplied to the instrument but the capillary viewing window LED will turn on Model 3480 Electrospray Aerosol Generator 9 Carefully insert the capillary tip into the capillary guide While looking through the viewing window continue pushing the capillary into the capillary guide until the tip of the capillary first appears then tighten the hex nut on the inlet fitting 10 If the capillary is centered in the viewing window installation is complete If not loosen the hex nut on the inlet fitting adjust the position of the capillary and retighten the hex nut Note Due to variations in the dimensions of the viewing window components the capillary may appear slightly off center in the direction transverse to the capillary axis This is not a cause for concern however because the center of the orifice plate is aligned to the inlet fitting axis at the factory 11 Replace and secure the cabinet cover The Electrospray is now ready for use See Chapter 4 Operating the Electrospray Adjusting the Position of the Capillary Tip If the capillary does not appear in the center of the viewing window or you wish to move the capillary closer or further from the orifice plate refer to the instruction preceding this subsection titled
34. ain PCB 3 7 maintenance 5 1 periodic 5 1 pressure regulator A 2 removing capillary 5 12 rotameter A 3 schedule 5 1 special 5 12 manual about xvii manual history iv measuring and adjusting conductivity 4 2 measuring and adjusting pH 4 3 Model 3074B Filtered Air Supply 2 4 Model 3480 Electrospray Aerosol Generator see Electrospray Aerosol Generator Model P 2042 Nuclespot Local Air Ionizer xiii xiv 2 5 3 3 replacing 5 5 monodisperse aerosol size range 1 1 O operation 1 2 4 1 preparing a buffer solution 4 2 preparing samples 4 1 operation unstable 6 1 orifice plate cleaning 5 3 P Q packing list 2 1 pH meter 4 3 Polonium 210 xiii 2 1 2 5 3 3 power connection 2 3 power supply 3 7 pressure chamber 3 3 adjusting capillary 5 15 adjusting platinum wire 5 15 cleaning 5 10 5 11 leak checking 5 9 pressure gauge checking the zero 2 3 pressure regulator cleaning 5 19 maintenance A 2 pressure regulator and gauge 3 3 proteins 4 4 PSL 4 4 pulsating mode 4 7 purging the capillary 5 1 5 2 R radiation safety xiii references theory of operation B 9 replacement parts 5 19 replacing filter 5 19 returning for service 7 1 rotameter 3 3 cleaning 5 19 maintenance A 3 S safety xi chemical xiv electrical xv labels xi radiation xiii service policy v setting up the Generator 2 1 shutting down the Electrospray 4 8 specifications A 1 starting up the El
35. amber and Pressure Chamber 1 Remove power from the instrument 2 Remove the cover by loosening the four screws securing the cover they do not have to be removed and pulling the cover upward while pushing down on the top of the front panel of the instrument or on the viewing window mount 3 Make sure a capillary is installed 4 Disconnect the tubing from the barbed fitting on the pressure chamber and the two barbed fittings on the Electrospray chamber Maintenance 5 9 5 10 5 Plug all three barbed fittings Connect a pressure gauge or manometer between the aerosol exit port and a leak tight valve The valve should be closed 7 Connect the valve to a vacuum source or a vacuum pump capable of drawing 18 inHg vacuum 8 Turn on the vacuum pump or vacuum system and slowly open the valve Allow the vacuum gauge reading to become stable and then close the valve 9 Observe the gauge reading The reading should not change by more the 0 5 inHg in 1 minute 10 If the instrument does leak follow the steps below under Isolating Leaks Isolating Leaks 1 Isolate the leak by wetting suspected joints with clean isopropyl alcohol while the system is under vacuum The alcohol will be drawn into a leaky joint and evaporate 2 After isolating the leak repair it usually by greasing or replacing an O ring or by sealing a fitting 3 Blow clean dry air through the repaired section to evaporate and remove any le
36. anley L Kaufman 1995 Electrospraying of Conducting Liquids for Monodisperse Aerosol Generation in the 4 nm to 1 8 pm Diameter Range J Aerosol Sci 26 963 977 Cloupeau M 1994 Recipes for Use of EHD Spraying in Cone Jet Mode and Notes on Corona Discharge Effects J Aerosol Sci 25 1143 1158 Cloupeau M and Prunet Foch B 1994 Electrohydrodynamic Spraying Functioning Modes A Critical Review J Aerosol Sci 25 1021 1036 Cloupeau M and Prunet Foch B 1989 Electrostatic Spraying of Liquids in Cone Jet Mode J Electrostatics 22 135 159 Fuchs N A 1963 On the Stationary Charge Distribution on Aerosol Particles in a Bipolar Ionic Atmosphere Geophys Pura Appl 56 185 Grace J M and Dunn P F 1992 Electrohydrodynamic Droplet Mixing J Aerosol Sci 23 5213 S216 Grace J M and Marijnissen J C M 1994 A Review of Liquid Atomization by Electrical Means J Aerosol Sci 25 1005 1020 Hinds W C 1982 Aerosol Technology Properties Behavior and Measurement of Airborne Particles New York John Wiley amp Sons Hussin A H G Scheibel K H Becker and J Porstendorfer 1983 Bipolar Diffusion Charging of Aerosol Particles I Experimental Results Within the Diameter Range of 4 30 nm J Aerosol Sci 14 671 Joffre G H and Cloupeau M 1986 Characteristic Forms of Electrified Menisci Emitting Charges J Electrostatics 18 147 161
37. ard surface so that the intake air can move freely under the base of the cabinet Model 3480 Electrospray Aerosol Generator Checking the Zero of the Pressure Gauge The pressure gauge is adjusted to the zero position at the factory however if the needle is not lined up with the left side of the zero box marked on the gauge you will need to re zero the pressure gauge see Figure 3 1 If zeroing is required follow the steps below to reset the gauge 1 You will need a palm sized square of soft clean rubber to grip the front surface of the gauge and a 050 inch hex wrench included in the accessory kit 2 Hold the cabinet for support and grip the front surface of the gauge with the square of rubber in the palm of your hand 3 Unscrew the front cover of the gauge in a counter clockwise direction 4 A sockethead setscrew is located under the bottom of the gauge panel where it is marked zero 5 Adjust the setscrew until the needle lines up with the left side of the zero box marked on the gauge 6 Reassemble the front cover of the gauge Power Connection Connect the AC power cord supplied to the AC POWER IN connection on the back of the Electrospray and then into an available power outlet It is not necessary to select the correct voltage the instrument accepts line voltages of 85 to 260 VAC 50 60 Hz 25 W max single phase The connector has a built in on off switch Note Make certain the line cord is plug
38. ation xiii schematic diagram B 2 setting up 2 1 Electrospray Aerosol Generator continued shutting down 4 8 specifications A 1 starting up 4 5 sucrose 4 3 system description B 1 theory of operation B 1 troubleshooting 6 1 typical solutes 4 3 unpacking 2 1 ventilation requirements 2 2 viewing window 3 3 viewing window assembly 5 5 voltage adjustment knob 3 2 Electrospray chamber 3 6 cleaning 5 6 5 7 leak checking 5 9 theory of operation B 4 F filter replacing 5 19 FILTERED AIR IN 2 4 filtered air inlet 3 5 filtered air input 2 4 filters 3 8 Fluka address 5 2 front panel 3 1 G generating aerosols 4 6 H help xvii high voltage fitting and shield 3 6 High voltage polarity determining 5 17 reversing 5 16 high voltage supply module 3 7 I J K indicators 3 1 3 2 inlet fitting 5 3 installing the capillary 5 14 interlock switch 3 8 internal components 3 6 capillary 3 6 drawing 3 7 Electrospray chamber 3 6 filters 3 8 high voltage fitting and shield 3 6 high voltage supply module 3 7 interlock switch 3 8 main PCB 3 7 power supply 3 7 Ionizer see also Model P 2042 Nuclespot Local Air Ionizer installing 2 5 drawing 2 6 replacing 5 5 Index 2 Model 3480 Electrospray Aerosol Generator Ionizer see also Model P 2042 Nuclespot Local Air Ionizer continued retainer 3 3 isolating leaks 5 10 L leaks isolating 5 10 LED displays 3 1 M N m
39. by pushing the black tab clockwise on the base of the knob Viewing Window lonizer Retainer Pressure Chamber Pressure Regulator Pressure Gauge Figure 3 1 Front Panel of the Model 3480 Electrospray Aerosol Generator Indicators There are two status LED s on the Electrospray power and high voltage a The green power LED indicates that power is supplied to the instrument a The high voltage LED indicates that high voltage is being applied to the platinum wire The high voltage is turned off if the cover is off the instrument or the bottom half of the pressure chamber is not installed Model 3480 Electrospray Aerosol Generator Rotameters The rotameters regulate the flow rates of air and CO to the Electrospray chamber The air and CO flow rates are typically 1 0 and 0 1 L min respectively Pressure Regulator and Gauge The pressure drop across the capillary is regulated and measured with these two components See Appendix B Theory of Operation for details on how the pressure drop is measured and how it can be used to approximate the flow rate of the liquid through the capillary Pressure Chamber The pressure chamber holds a sample vial which contains the liquid solution to be electrosprayed A platinum wire and capillary extend from the top half of the pressure chamber into the liquid solution to charge and transport the liquid solution respectively To change the
40. e Electrospray to avoid deposits on the inside of the capillary Follow the procedure below see Starting Up the Electrospray for details to shut down the Electrospray 4 8 Model 3480 Electrospray Aerosol Generator Buffer should be run before shutting down the Electrospray to clean the capillary Subsequently the Electrospray should be run without a sample to allow the air to clear the capillary of liquid Follow the procedure in this section to prolong capillary life and to avoid deposits on the inside of the capillary 1 Purge the capillary see section Purging the Capillary in Chapter 5 Maintenance 2 Remove the bottom half of the pressure chamber Close the lid of the vial and remove it 4 Replace the bottom half of the pressure chamber without inserting a vial to clear the liquid from the capillary and run air through it 5 View the capillary through the viewing window to determine when the liquid has been cleared from the capillary This process takes approximately 5 minutes with a standard buffer solution 6 Turn the pressure regulator knob until the pressure gauge reads zero psi 7 Turn the air and CO rotameters to read zero L min 8 Turn the voltage knob counterclockwise until it reaches its stopped position 9 Turn the power switch off Operating the Electrospray 4 9 CHAPTER 5 Maintenance This chapter gives maintenance and service procedures for the Electrospray Periodic
41. e back panel it flows through a filter before entering the CO rotameter therefore the CO rotameter should not need to be cleaned under normal operating conditions However if you suspect the CO rotameter has become dirty refer to Appendix A for the manufacturer s specifications and instructions for maintaining the CO rotameter Replacing the Filters Because the level of contaminants entering the Electrospray in the air and CO is low the four internal filters in the Model 3480 do not need to be replaced under normal operating conditions Replacement Parts This subsection contains information on replacement parts available from TSI and their part numbers See also the section in Chapter 2 for information on parts included in the accessory kit which are also available as replacement parts Table 5 2 Replacement Parts Part Description Part Number Shield High Voltage Fitting 2904157 Wire High Voltage Platinum 3301754 Maintenance 5 19 Part Description Part Number Tubing Silicone 4 Barb 3001257 High Voltage Module 1035907 please specify positive or negative Capillaries 25 um 25 per pack 3900124 5 20 Model 3480 Electrospray Aerosol Generator CHAPTER 6 Troubleshooting This chapter lists potential problems and their solutions Electrospray Operation is Unstable If the Electrospray is not operating in the Cone Jet mode see Chapter 4 Operating the Electrospray or the current display is n
42. ectrospray 4 5 sucrose 4 3 Swagelok 2 4 3 4 T theory of operation B 1 Electrospray chamber B 4 references B 9 troubleshooting 6 1 TSI contacting v 7 1 7 2 getting help xvii submitting comments xviii Tween 5 2 typical solutes 4 3 U ultrapure water 4 2 unpacking the Generator 2 1 unplugging capillary 6 3 unstable operation 6 1 V ventilation requirements 2 2 viewing window 3 3 cleaning lens 5 4 viewing window assembly 5 5 volatile solution 4 2 voltage adjustment knob 3 2 voltage measurement B 9 W X Y Z warning description xiii water ultrapure 4 2 Model 3480 Electrospray Aerosol Generator Index 3 Index 4 Model 3480 Electrospray Aerosol Generator Reader s Comments Please help us improve our manuals by completing and returning this questionnaire to the address listed in the About This Manual section Feel free to attach a separate sheet of comments Manual Title Model 3480 Electrospray Aerosol Generator P N 1933793 Rev E 1 Was the manual easy to understand and use Yes No Please identify any problem area s 2 Was there any incorrect or missing information please explain 3 Please rate the manual according to the following features Good Adequate Poor Readability Accuracy Completeness is everything there Organization finding what you need Quality and number of illustrations Quality and number of examples Comments 4 Which part s of this
43. eeve High Voltage Fitting Figure 5 5 Removing or Installing the Capillary 3 Loosen the hex nut on the inlet fitting but do not remove it 4 Carefully pull the capillary from the capillary guide leaving the guide behind When removing the capillary from the inlet fitting the capillary can become damaged if not removed carefully Read the note below for hints on removing the capillary without damage Note When removing the capillary slowly the capillary tip will have a tendency to hit the edge of the hex nut on the inlet fitting if it is not pulled straight out from the inlet fitting To prevent damage to the capillary use a steady hand and pull the capillary straight out from the inlet fitting or pull the capillary out slowly until it is almost removed and then pull quickly to completely remove the capillary One alternative solution is to remove the inlet fitting before removing the capillary Another is to perform steps 5 7 before steps 3 and 4 5 Remove the high voltage shield by loosening the mounting screw and pulling the high voltage shield upward until it clears the capillary 6 Loosen the hex nut on the high voltage fitting but do not remove it Maintenance 5 13 5 14 7 Pull the capillary straight up until it clears the high voltage fitting 8 Store the capillary in the case provided to prevent breakage Cleaning the Capillary Tip If the capillary tip appears dirty remove the capillary u
44. els 5 xii Model 3480 Electrospray Aerosol Generator 068 1 1 Bottom View of Electrospray Aerosol Generator Showing Location of Rubber Feet oooccconccnnnnconnnccnnnnconnnccnnnnncnnnonos 2 2 Installing the lOniZers esere ae anida dni tadas dei bes 2 6 Front Panel of the Model 3480 Electrospray Aerosol CHETICLALOL a 3 2 Back Panel of the Model 3480 Electrospray Aerosol O a E AL as dosis 3 4 ANALOG OUTPUT Pin Designations c cece cece eeees 3 5 Main Internal Components occcnccnnccnnccnaccnnncnnaconiacanicnnncnnno 3 7 Inserting a Sample Vial into the Pressure Chamber 4 6 Three Views of Capillary Tip Through the Viewing WAT Wisin rd oe 4 7 ilet Fitin Ren TO 5 3 Viewing Window Assembly sessesseereseessessesreereeresseseese 5 5 Cleaning the Electrospray Chambetf cccccsesseeeseeeeee 5 7 Cleaning the Pressure Chamber oooccncccnccnnncnnconocacocinocono 5 11 Removing or Installing the Capillary eee 5 13 Determination of High Voltage Polarity ee 5 17 Reversing the High Voltage Polarity ccc eees 5 18 Schematic Diagram of the Electrospray e cesses B 2 Bipolar Particle Charge Distribution in Air Wiedensohler and Fissan 1988 cccccceeeeseeeeeeees B 5 Electrospray Flow SchematiC oocccocccoconioconcconaccnncnnnncnnannno B 8 Contents ix Tables 2 1 3 1 4 1 5 1 5 2 6 1 Electrospray P
45. f the aerosol exit tube that faces the inside of the Electrospray chamber 7 Clean the inside of the ionization chamber using a soft cloth or cotton swab moistened with alcohol or a mild detergent 8 Reassemble the inlet and exit manifolds to the ionization chamber and connect the Electrospray chamber to the cabinet 9 Reattach the viewing window LED connector to the main PCB and reconnect the three ground wires to the ionization chamber 10 Place the ionizer in the ionizer retainer The ionizer mesh side should be facing the open end of the ionizer retainer 11 Install the ionizer retainer making sure the O ring is between the ionization chamber and the ionizer retainer and tighten with the ionizer retainer tool 12 Replace the inlet fitting If needed refer to step 11 in the section Cleaning the Orifice Plate earlier in this chapter 13 Install the capillary tube using the instructions later in this chapter titled Installing the Capillary 14 Perform and air leak test using the instructions below Performing an Air Leak Test Whenever an air leak is suspected or a significant part of the Electrospray chamber has been reassembled perform a leak test to assure proper operation Use these steps to check the entire instrument for leaks Skip to the next section if you want to isolate the Electrospray chamber and check it for leaks Model 3480 Electrospray Aerosol Generator High voltage is accessible in
46. ftover alcohol 4 If you cannot find the leak or cannot repair the leak please contact TSI for assistance Cleaning the Pressure Chamber The pressure chamber can be cleaned if the surfaces appear dirty or the sample vial is difficult to see clearly Refer to Figure 5 4 and use the following procedure to clean the pressure chamber High voltage is accessible in several locations within this instrument Make sure you unplug the power source before removing the cover or performing maintenance procedures 1 Remove power from the instrument and turn off all flows 2 Remove the capillary using the instructions in the next section titled Removing the Capillary 3 Remove the screw attaching the high voltage cable to the fitting on top of the pressure chamber The fitting can then be removed by twisting counter clockwise using caution not to bend or damage the platinum high voltage wire Model 3480 Electrospray Aerosol Generator When removing the fitting on top of the pressure chamber use caution not to bend or damage the platinum high voltage wire 4 Clean the top and bottom of the pressure chamber using a soft cloth or cotton swab moistened with alcohol or a mild detergent High Voltage Cable A A E Hex Nut A High Voltage Fitting A Platinum High Voltage Wire O Pressure Chamber Top Half HS Le Pressure Chamber eC Ll Bottom Half Pin Groove 2X O Ring 2501024 Figure 5
47. g Back Pressure to the Capillary 6 3 CHAPTER 7 Contacting Customer Service cscscessseees 7 1 Technical Contacts cenit is de rd iii 7 1 Returning the Electrospray for Service coooccconoccnnnccnonccnnnnnnns 7 1 viii Model 3480 Electrospray Aerosol Generator APPENDIX A Model 3480 Specifications csseeceees A 1 Pressure Regulator Maintenance oocooccocnncnncnnncnncnncnncnncnncnns A 2 Rotameter MaintenanCe ooocococccnooncnnnocnnnnnonnnncnonacnnnoncncnncnnons A 3 APPENDIX B Theory of Operation cscssccsscssecsceeevees B 1 System DESCA PUO oocooccocnocnncnncnncnnanoncnncnncnncnnncnncnnconcnncnninns B 1 Capillary Flow CharacteristicS oooccocccnccnnocnnncnnncnnoconacanicanoso B 2 Calculating Primary Droplet Diameter ooocccncccnncnnccnnicnnccnns B 4 Electrospray Chambers scsi arnoa er r E E ETT este B 4 Equilibrium Charging Theory coocccncccnccnnaconaconiconacnnncnanacanono B 5 Air and CO Flow Control ooocccconccccnccnonnnnncncononanonanaconanicnanass B 7 Voltage and Current Measurement oocccoccnnccnoconocinocinacninnicon B 9 Voltage Measurement iremen aieeao an En dens RET B 9 Current Measurement erone ekari AE EiT B 9 Selected Referente Sisir isicsiskcccsscssstendvesscotsatsadscdsuesececscenveaes B 9 Index Reader s Comments Figures 2 2 3 1 3 2 3 3 3 4 4 1 4 2 5 1 5 2 5 3 5 4 5 5 5 6 5 7 B 1 B 2 Location of Warning and Information Lab
48. ged into a grounded earth grounded power outlet Position the Electrospray so the power cord connector is not blocked and is easily accessible Note The Electrospray power supply contains no user serviceable parts If the power supply is not operating correctly use the information in Chapter 7 to contact TSI This instrument should not be used in a manner not specified by the manufacturer Toggle the on off switch at the AC POWER IN connection to the on position to verify the instrument has power Unpacking and Setting Up the System 2 3 Analog Output The Electrospray has a single 15 pin D subminiature connector port on the back panel labeled ANALOG OUTPUT that can be used to measure signals that represent the voltage and current output on the front panel meters of the instrument See Chapter 3 fora detailed list of the signal connections Filtered Air Input The back panel of the Electrospray has an input marked FILTERED AIR IN 25 PSI MAX that is a 1 4 Swagelok tube fitting with nylon ferrules Insert the supplied polyethylene tubing or a similar tubing and tighten the Swagelok nut finger tight plus 4 turn with a wrench This will provide a secure connection and allow the tubing to be removed without damaging the ferrules A regulated compressed air supply that furnishes HEPA filtered clean dry air must be used to supply filtered air to the Electrospray TSI Model 3074B Filtered Air Supply is recommended and may be pu
49. h the viewing window LED connector from the main PCB 4 Detach the Electrospray chamber from the cabinet by removing the two screws on the back panel of the instrument behind the Electrospray chamber not shown in Figure 5 3 5 Remove the eight screws that fasten the two white manifold blocks to the inlet and exit of the ionization chamber The viewing window lens can be cleaned if necessary by following the instructions in the section Cleaning the Viewing Window Lens earlier in this chapter The viewing window LED mount can also be removed to clean the optical window it holds in place by using the following procedure a Unscrew the viewing window LED mount The optical window and an O ring will fall out of the inlet manifold Maintenance 5 7 5 8 b Clean the optical window using a soft cloth or cotton swab moistened with alcohol a mild detergent or a lens cleaner Before replacing the viewing window LED mount make sure the optical window is flush with the O ring Failure to do so could result in breakage of the optical window as the viewing window LED mount is screwed into the inlet manifold c Place the O ring and optical window in the inlet manifold making sure the optical window is flush with the O ring surface then replace the viewing window LED mount 6 Use a soft cloth or cotton swab moistened with alcohol or a mild detergent to clean the inside of the aerosol exit tube and the stainless steel surface o
50. h ultrapure or distilled water to 0 5 a 20 mM KOH solution A 20 mM potassium hydroxide solution in ultrapure or distilled water is a low enough concentration to clean the capillary with little etching of the capillary walls This solution should not be run for more than 10 minutes because capillary etching may become significant a 0 1 M KOH solution For heavy buildup a 0 1 M potassium hydroxide solution in ultrapure or distilled water can be used however this solution should not be run for more than 2 minutes because capillary etching may become significant more quickly than for the 20 mM KOH solution OTWEEN is a registered trademark of Uniqema a business unit of ICI Americas Inc 5 2 Model 3480 Electrospray Aerosol Generator Cleaning the Orifice Plate High voltage is accessible in several locations within this instrument Make sure you unplug the power source before removing the cover or performing maintenance procedures The orifice plate is permanently attached to the inlet fitting of the Electrospray chamber to ensure electrical contact Since the aerosol is generated inside the inlet fitting and then passes through the orifice plate the inlet fitting will need to be cleaned more frequently than other components through which the aerosol passes Figure 5 1 shows a view of the inlet fitting inside the cabinet Use the following steps to clean the inlet fitting and orifice plate O Ring Capillary Sleeve 250
51. in a sample vial and use it as if you were generating an aerosol see the section in Chapter 4 Operating the Electrospray When shutting down the instrument always rinse the capillary with a buffer solution and flush the capillary with air after purging the capillary to prevent deposits from forming on the capillary Four different solutions have been used with the Electrospray to purge the capillary They include o 20 mM ammonium acetate buffer solution see the section in Chapter 4 Preparing Samples This solution is convenient to use because it is the same solution recommended for use between samples to prevent sample contamination However this solution rinses the capillary but does not contain cleaning agents If you suspect the capillary walls are dirty use one of the three solutions listed below to clean the capillary and then a buffer solution to rinse the capillary 20 mM ammonium acetate buffer solution or a similar buffer solution should be run to rinse the capillary after using any detergent such as Tween 80 or any strong alkali such as KOH to purge the capillary After the capillary is rinsed with the buffer solution and before turning off the instrument run air through the capillary to prevent deposits from forming if the buffer solution were left in the capillary to evaporate Q 0 5 Tween 80 solution a detergent 10 Tween 80 solution P8192 Sigma Aldrich Co St Louis MO is useful if diluted wit
52. ing of this manual and the safety information provided with the ionizer The use of controls adjustments or procedures other than those specified in this manual may result in exposure to hazardous radiation Use this procedure to install the ionizer 1 Remove the ionizer retainer shown in Figure 2 2 using the ionizer retainer tool supplied in the accessory kit and set the dummy source aside 2 Place the ionizer in the ionizer retainer in place of the dummy source The ionizer mesh side should be facing the open end of the ionizer retainer 3 Install the ionizer retainer making sure the O ring is between the ionization chamber and the ionizer retainer and tighten with the ionizer retainer tool Note The ionizer must be replaced 12 months from the date on the ionizer label Contact TSI to order a new ionizer four weeks before the ionizer expiration date When returning an ionizer contact TSI for handling and shipping instructions Unpacking and Setting Up the System 2 5 2 6 Y yy ae Figure 2 2 Installing the lonizer Model 3480 Electrospray Aerosol Generator lonization Chamber Dummy Source O Ring 2501027 G lonizer Retainer Front Panel CHAPTER 3 Controls Indicators and Connectors Use the information in this chapter to familiarize yourself with the location and function of controls indicators and connectors on the Model 3480 Electrospray Aerosol Generator Thi
53. ipment is complete Table 2 1 gives a packing list for the Electrospray Table 2 1 Electrospray Packing List Qty Description 1 Model 3480 Electrospray Aerosol Generator Electrospray Accessory Kit Including Capillaries 25 um 25 per pack Ionizer Retainer Tool Tee Connector with Filter L Key Hex Wrench 050 in Cable Power Supply Instruction Manual Ferrules Nylon Front s in tube Ferrules Nylon Back s in tube O rings 1 009 FSI O rings 1 010 EPDM O rings 1 013 FSI O rings 1 014 EPDM O rings 1 016 EPDM O rings 1 020 EPDM O rings 1 024 BUNA O rings 1 027 EPDM O rings 1 029 EPDM Vacuum Grease 50 Vial 1 5 ml Center Tube Poly 5 ft 1 5 m Tubing Silicone Conductive in OD 10 ft 3 m Tubing Polyethylene 4 in OD h m y ga F NNNNNNNONNN rn Part No 348000 3900124 3012062 1030023 3305003 1303053 1933793 1611252 1611253 2501899 2501520 2501567 2501528 2501602 2501073 2501024 2501603 2501072 1101063 3002003 3001903 3929436 Power cable listed is for U S A use only Note A Polonium 210 ionizer is shipped separately from the Electrospray instrument and accessory kit The ionizer must be installed for the Electrospray to operate properly See the instructions later in this chapter for installing the ionizer 2 1 Mounting the Instrument 2 2 The Electrospray has no special mounting requirements other than providing good ventilation see below The cabinet has f
54. is supplied to the instrument If the Model 3480 is used in a manner not specified by the manufacturer the protection provided by the equipment may be impaired High voltage is accessible in several locations within this instrument Make sure you unplug the power source before removing the cover or performing maintenance procedures The Electrospray has the eight labels shown in Figure S 1 They are described below starting from the bottom right and moving clockwise 1 High Voltage Symbol Label interior on high voltage power supply shield High Voltage Symbol Label interior on power supply High Voltage Symbol Label interior on power entry module Ground Symbol Label interior bottom next to ground stud A sala D N Caution No User Serviceable Parts Label back of cabinet xi 6 Customer Service Label back of cabinet 7 Serial Number Label back of cabinet 8 High Voltage Symbol Label interior on high voltage fitting shield o000000000 oOo00000000 0000000000 Di of oe El KE o iS For Service and Information Ei er Service TSI Particle Instrument Division 651 490 3893 1 800 874 3893 500 Cardigan Road TSI Shoreview MN 55126 USA q q TO AVOID ELECTRICAL SHOCK Pol CONNECTED TO EARTH GROUND Figure S 1 Location of Warning and Information
55. ive Charges Midpoint nm 1 2 3 4 10 0 0411 0 0 0 11 0 0460 0 0 0 12 0 0514 0 0 0 14 0 0573 o 0 0 15 0 0638 0 0 0 17 0 0709 0 0 0 18 0 0784 0 0 0 21 0 0866 0 00012 0 o 23 0 0953 0 00023 0 0 25 0 1041 0 00041 0 0 28 0 1145 0 0007 0 0 31 0 1241 0 0011 0 0 35 0 1343 0 0018 0 0 38 0 1446 0 0027 0 0 43 0 1550 0 0040 0 o 48 0 1650 0 0056 0 0 53 0 1748 0 0078 0 0 59 0 1841 0 0105 0 0 66 0 1925 0 0138 0 0 74 0 2000 0 0180 0 00045 0 83 0 2064 0 0225 0 00089 0 93 0 2113 0 0279 0 0016 0 104 0 2148 0 0339 0 0028 0 117 0 2167 0 0406 0 0046 0 00014 132 0 2167 0 0477 0 0072 0 00031 150 0 2149 0 0552 0 0105 0 00064 170 0 2113 0 0627 0 0149 0 0012 The formulas used to calculate Table B 2 are shown below They are taken from Wiedensohler 1988 To calculate the fraction of particles carrying zero one or two charges use Equation B 4 which is an approximation of the Fuchs model Equation B 4 is valid for size ranges 1 nm lt D lt 1000 nm for N 1 0 1 for 20 nm lt D lt 1000 nm for N 2 2 and for D lt 20 nm for N lt 1 Cs 5 Di i f N 10 Equation B 4 Model 3480 Electrospray Aerosol Generator Table B 3 Coefficients for Equation B 4 26 3328 44 4756 35 9044 79 3772 21 4608 62 8900 7 0867 26 4492 1 3088 E 5 7480 0 1051 0 5049 For the fraction of particles carrying three or more charges use Equation B 5 which is based on an derivation by Gunn from 1
56. lary see Chapter 5 Clean the capillary tip Chapter 5 Adjust the position of the capillary see Chapter 5 Installing the Capillary Clean the inlet fitting see Chapter 5 Increase the conductivity of the sample see Chapter 4 Decrease the voltage setting Decrease the capillary pressure drop Increase the CO flow rate Purge the capillary see Chapter 5 Clean the capillary tip see Chapter 5 Adjust the position of the capillary see Chapter 5 Installing the Capillary Clean the inlet fitting see Chapter 5 Decrease the conductivity of the sample see Chapter 4 Make sure the voltage pressure and flow rates are adjusted properly Make sure the capillary is immersed in the sample vial solution See the section below Unplugging the Capillary Make sure the voltage pressure and flow rates are adjusted properly Make sure the capillary is immersed in the sample vial solution Make sure the platinum wire is immersed in the sample vial solution Model 3480 Electrospray Aerosol Generator Unplugging the Capillary Each capillary is checked before leaving the factory to ensure proper operation However a capillary can become fully or partially plugged due to several reasons including those listed in Table 6 2 As a general rule if the capillary becomes plugged and the capillary tip is not broken first try applying back pressure to the capillary see the procedure listed below then try applying a
57. ltage Module High Voltage PCB High Voltage Power Supply Figure 5 6 Determination of High Voltage Polarity The standard Electrospray is equipped with a positive high voltage module which causes the generated droplets to initially have a high positive charge However if initially negatively charged droplets are desired a negative high voltage module is available from TSI Reversing the high voltage polarity is a procedure that should only be performed by a qualified electronics technician observing ESD precautions To replace one high voltage module with another refer to Figure 5 7 and proceed as follows 1 Remove power from the instrument and turn off all flows 2 Remove the cover by loosening the four screws securing the cover they do not have to be removed and pulling the cover upward while pushing down on the top of the front panel of the instrument or on the viewing window mount Maintenance 5 17 5 18 ett Main PCB High Voltage Module Captive Screw 2X High Voltage Cable Connector Figure 5 7 Reversing the High Voltage Polarity 3 Disconnect the high voltage cable from the high voltage module by gripping the connector and twisting the collar turn clockwise The connector should then separate easily from the socket 4 Loosen the two captive screws attached to the high voltage module until the screws pop out 5 Pull the high voltage module straight out until it clears the spacers used to
58. lution is outlined here 1 Dissolve 0 77 grams of ammonium acetate in 500 milliliters of ultrapure or de ionized water 2 Assuming the solution has an initial pH of 6 7 add 0 75 milliliters of 1M ammonium hydroxide 3 See the following sections for measurement and adjustment of the buffer solution conductivity and pH Measuring and Adjusting Conductivity A conductivity meter is useful for measuring the conductivity of a buffer solution The conductivity can be increased or decreased by adding ammonium acetate or ultrapure water respectively to the buffer solution Although the Electrospray will operate at a wide Model 3480 Electrospray Aerosol Generator range of conductivities a 0 2 S m buffer solution is typically used An experimental analysis of the useful range of liquid conductivity as a function of liquid flow rate using an electrospray method is discussed in the following journal article Chen Da Ren David Y H Pui and Stanley L Kaufman 1995 Electrospraying of Conducting Liquids for Monodisperse Aerosol Generation in the 4 nm to 1 8 pm Diameter Range J Aerosol Sci 26 963 977 Measuring and Adjusting pH A pH meter is useful for measuring the pH of a buffer solution Ammonium hydroxide or acetic acid can be added to the buffer solution to increase or decrease the pH value respectively Since the pH value should be greater than the pl value for proteins a useful reference for pI values of selected
59. may not be amended modified or its terms waived except by writing signed by an Officer of Seller Knowing that inoperative or defective instruments are as detrimental to TSI as they are to our customers our service policy is designed to give prompt attention to any problems If any malfunction is discovered please contact your nearest sales office or representative or call TSI s Customer Service department at 1 800 874 2811 USA or 651 490 2811 Contents Manual History scccsccccscccccccccccccccceccccccececcssececcececeseece iv WAITANLY ccecccccccccccccccccccecccccccceecceescseenescessseesseeseseenesseees Vv Safety NTRA IT xi Tea DOlS iiss tbe he di tenet nets bootie taba Mea ets xi Description of Caution Warning Symbols ce cesses xii CAUTION vie ects erect eethead A oa xii Warning isso do Ea eta lite aa xiii Caution or Warning SymbolS ocoocccnoccnocnnicnnioconacnnaccnncnnnins xiii Radiation Safety eieren anai sient ters len cette elite ads tes xiii Chemical Sada aa xiv Electrical Safety eiieeii aE ari AE ETE XV About This Manual cccccscsccscscscecscecscscccsccsscesscesseeees xvii Purposes a e E tate Pate ASS xvii Related Product Literature oocooconcnoconcnncnnccnocnncnnconconcnnacnnon xvii O xvii Submitting Comments crearte ninia xviii CHAPTER 1 Product Overview cccccesscescccscscscecscececess 1 1 Product Description e inexes 1 1 ApplicatioAS id aa 1 2
60. minating the need to clean the pressure regulator However if you suspect the regulator has become dirty use Figure A 1 and the instructions provided by the manufacturer below to disassemble and clean the regulator Remove air supply pressure and bleed off output pressure prior to performing maintenance To disassemble the pressure regulator loosen adjusting handwheel 1 until spring tension is relieved Remove six screws 9 and lift off bonnet 5 spring plate 6 spring 7 and diaphragm assembly 8 To remove nozzle assembly 10 use socket wrench to remove nozzle assembly to avoid damage to the nozzle All parts may be cleaned by immersion in a suitable solvent and blowing dry with air stream To reassemble replace nozzle assembly 10 and place diaphragm assembly 8 over body 11 with diaphragm plate up Place spring 7 and spring plate 6 on diaphragm assembly 8 re install bonnet 5 and tighten six screws 9 The six screws should be tightened alternately Figure A 1 Pressure Regulator Assembly A 2 Model 3480 Electrospray Aerosol Generator Rotameter Maintenance If you suspect either rotameter has become dirty refer to Figure A 2 and the instructions provided by the manufacturer below to clean either rotameter Remove air supply pressure and bleed off output pressure prior to performing maintenance RETAINING CLIP Occasional cleaning may become necessary if dirt appears in the flowme
61. moving the cover or performing maintenance procedures Safety XV Purpose About This Manual This is an instruction manual for the operation and handling of the Model 3480 Electrospray Aerosol Generator Related Product Literature Getting Help Q Model 3080 Electrostatic Classifier Manual part number 1933792 TSI Incorporated Q Model 3010 Condensation Particle Counter Manual part number 1933010 TSI Incorporated Q Model 3022A Condensation Particle Counter Manual part number 1933763 TSI Incorporated Q Model 3025A Ultrafine Condensation Particle Counter Manual part number 1933762 TSI Incorporated Q Model 3936 SMPS Scanning Mobility Particle Sizer Manual part number 1933796 TSI Incorporated Q Model 3068 Aerosol Electrometer Manual part number 1933068 TSI Incorporated To obtain assistance with this product or to submit suggestions please contact TSI TSI Incorporated 500 Cardigan Road Shoreview MN 55126 U S A Fax 651 490 3824 Telephone 1 800 874 2811 USA or 651 490 2811 E mail Address particle tsi com xvii Submitting Comments xviii TSI values your comments and suggestions on this manual Please use the comment sheet on the last page of this manual to send us your opinion on the manual s usability to suggest specific improvements or to report any technical errors If the comment sheet has already been used send your comments to TSI Incorporated 500 Cardigan Road
62. ndependent of sample concentration Protein samples can be prepared using the following method 1 Dissolve 1 mg protein per 1 milliliter buffer solution 2 Dilute the 1mg mL solution to obtain a 10 pg mL solution This concentration is sufficient for most proteins when analyzing the size distribution of the protein aerosol Selected proteins and their diameters are listed in Table 4 1 This is a very limited sample of the numerous proteins available Some proteins may be dangerous to emit into the environment Filter dangerous aerosols before emitting them into the environment Model 3480 Electrospray Aerosol Generator Table 4 1 Selected Proteins and Their Diameters Protein Diameter nm Ubiquitin 3 Bovine Serum Albumin 6 5 Ferritin 12 Starting Up the Electrospray After the Electrospray system has been set up see Chapter 2 Unpacking and Setting Up the System and samples have been made follow this procedure to begin generating aerosols 1 Turn on the power switch on the back panel Make sure the power and high voltage LED s are on and check the viewing window to make sure the capillary tip is near the center of the viewing window 2 Remove the bottom half of the pressure chamber by twisting it s turn counterclockwise The bottom half can then be removed by pulling downward Note High voltage is turned off if the bottom half of the pressure chamber is removed 3 Insert and open the sample
63. nection CO inlet 0066 Ya in OD Swagelok connection Aerosol outlet Ya in OD Stainless Steel tube Voltage range 0 5 to 3 5 kV 2 0 to 2 5 kV nominal negative high voltage module available Current range O to 2000 nA 280 to 320 nA nominal Dimensions LWH 20 3 cm x 40 4 cm x 25 7 cm 8 0 in x 15 9 in x 10 1 in 6 8 kg 15 Ib 85 to 260 VAC 50 60 Hz 25 W maximum Fuse not replaceable by user 2 5A 250 V type 5x20 mm not replaceable by operator A 1 Environmental Conditions Indoor use Altitude up to 2000 m 6500 ft Ambient temperature 10 50 C Ambient humidity 0 90 RH non condensing Over voltage category II Pollution degree II TSI Incorporated is authorized by the United States Nuclear Regulatory Commission to distribute these lonizers If your location is within the United States no other federal license is required Check local regulations for your own protection Ionizers are shipped separately End user name and address is required Contact TSI to return used ionizers or obtain replacements Specifications are subject to change without notice TSI and the TSI logo are registered trademarks of TSI Incorporated Pressure Regulator Maintenance The air supplied to the pressure regulator should always be from a clean dry air supply eli
64. oncentration influencing the flow rate and thereby the primary droplet size Refer to Morison 2002 for more information Operating the Electrospray 4 3 44 Sucrose solutions can be made using the following method 1 Dissolve 1 58 grams sucrose per 10 milliliters buffer to make a 10 V V solution 2 For lower concentrations of sucrose dilute the 10 V V solution with buffer solution accordingly Ken R Morison Department of Chemical and Process Engineering University of Canterbury Christchurch New Zealand Viscosity Equations for Sucrose Solutions Old and New Paper 984 The Asian Pacific Confederation of Chemical Engineering APCChE Conference 2002 PSL Polystyrene Latex PSL is used to generate test aerosols in a wide size range from 20 nm to 160 pm the Electrospray is useful on the low end of this range from 20 to 100 nm PSL is commercially available as aqueous suspensions in 15 mL dropper bottles and samples can be easily made by adding one drop 50pL of PSL to 1 mL of buffer solution in a standard sample vial Unlike sucrose PSL size is independent of concentration Higher aerosol concentrations can be obtained by adding more PSL which may become necessary with larger PSL sizes Proteins Most proteins that have been used with the Electrospray range from 3 to 12 nm in diameter Most are commercially available from many chemical companies The diameters of particles generated from proteins are i
65. oniconiconiconanos 5 4 Cleaning the Viewing Window Lens occcoccnoccnoconoconiconinnnanes 5 4 Replacing the lonizer cccoocccoccnoccnocnnnnnnnanonacanaconaconaronaconanos 5 5 Cleaning the Electrospray Chamber ccooccnoccnoconioconiconinnnanos 5 6 Performing an Air Leak Test ooooonccnnoccnnnccnnnncnnnnrcnnnnrnnonccnnns 5 8 Cleaning the Pressure ChambeT ccocccnocnniccnnicnnicnnccnnccnnicono 5 10 Special MAIMLENANCE cise dcrgirss aduenen doce vadestoedeeteiarovatercdeseanens 5 12 Removing the Capillary srera roesini i niie 5 12 Cleaning the Capillary Tip oonccoccnnccnnocnnncnnocnnncnnncnnccnnninns 5 14 Installing the Capillary iesenii cece innr En TReni 5 14 Adjusting the Position of the Capillary Tip ee 5 15 Adjusting the Position of the Capillary and the Platinum Wire in the Pressure Chambet 0000004 5 15 Reversing the High Voltage Polarity oocccoccnnccnnccnnacinicinos 5 16 Cleaning the Pressure Regulator ooccocccncccnncnnccnnccnnccnnnnnns 5 19 Cleaning the Rotameters occoocccnccnoccnoconaconacinacinaninancnnacon 5 19 Replacing the Milters soircas nese i E tana 5 19 Replacement Parts cccssasivsestevcrnneveatassewedeestedsectevanseenavavevenes 5 19 CHAPTER 6 Troubleshooting cccsccesscececscecececccesceess 6 1 Electrospray Operation is Unstable coocccncccnccnnocnnicanaconanos 6 1 Unplugging the Capillary oooccocccnocnniocnnionnnonnnnncnnnanananunacacnono 6 3 Applyin
66. or is easily accessible Filtered Air Inlet The filtered air inlet connection is described in Chapter 2 Unpacking and Setting Up the System CO Inlet The CO inlet connection is described in Chapter 2 Unpacking and Setting Up the System Controls Indicators and Connectors 3 5 Internal Components 3 6 The main internal components are shown in Figure 3 4 A brief description of each follows Capillary The capillary transports the liquid to be electrosprayed from the sample vial to the Electrospray chamber More information on the liquid flow through a capillary can be found in Appendix B Theory of Operation Information on the maintenance of the capillary can be found in Chapter 5 Maintenance Electrospray Chamber The aerosol is generated inside the Electrospray chamber See Chapter 5 Maintenance for instructions on how to clean and maintain the Electrospray chamber Appendix B Theory of Operation contains information on the theory of operation of the Electrospray chamber High Voltage Fitting and Shield The high voltage fitting is attached to the top half of the pressure vessel High voltage is supplied to the fitting which is connected to a platinum high voltage wire that is immersed in the liquid contained in the sample vial hence charging the liquid The high voltage shield covers the high voltage fitting to protect the user from accidental electrical shock Model
67. ot stable first try decreasing the voltage setting to its minimum value and then increase the voltage setting until the Cone Jet mode appears in the viewing window If the Cone Jet mode appears the current display should be stable If this procedure does not resolve your problem use Table 6 1 to pinpoint possible solutions 6 1 Table 6 1 Troubleshooting if the Electrospray Operation is Unstable Problem Solutions ss Electrospray is operating in the Dripping mode see Chapter 4 Operating the Electrospray or Current display is much lower and more unstable than normal Electrospray is operating in the Pulsating mode see Chapter 4 Operating the Electrospray or Current display is lower and more unstable than normal Electrospray is operating in the Corona Discharge mode see Chapter 4 Operating the Electrospray or Current display is higher and more unstable than normal No liquid is flowing through the capillary There is no current reading 6 2 Increase the voltage setting Increase the capillary pressure drop Increase the air flow rate Purge the capillary see Chapter 5 Clean the capillary tip see Chapter 5 Adjust the position of the capillary see Chapter 5 Installing the Capillary Clean the inlet fitting see Chapter 5 Increase the conductivity of the sample see Chapter 4 Increase the voltage setting Increase the capillary pressure drop Purge the capil
68. ou that the Model P 2042 Nuclespot Local Air lonizer which is installed inside the Model 3480 Electrospray Aerosol Generator contains Polonium 210 a radioactive material that is subject to the regulations of the U S Nuclear Regulatory Commission and local regulations Carefully read the Model P 2042 Literature provided with the ionizer to determine your legal responsibilities regarding the ionizer Radiation Safety The Electrospray Aerosol Generator contains a Model P 2042 Nuclespot Local Air Ionizer with a Polonium 210 source Under normal circumstances you will not come into contact with hazardous radiation However take these precautions when operating the Electrospray Safety xiii The Model P 2042 Nuclespot Local Air lonizer with a Polonium 210 AA source must be installed in the Electrospray for it to operate properly a Po 210 is subject to the regulations of the U S Nuclear Regulatory Commission and local regulations Carefully read the safety information provided with the ionizer to determine your legal responsibilities regarding the ionizer AA The use of controls adjustments or procedures other than those A specified in this manual may result in exposure to hazardous radiation Q Corrosive materials can degrade the protective coating of gold on the ionizer inside the Electrospray Do not operate the Aerosol Generator with chemicals that corrode gold Q Do not operate the Aerosol Generator at temperatures above
69. our non marking rubber feet that give the instrument a good grip on clean level surfaces The rubber feet Figure 2 1 are installed in the cabinet using integrated 8 32 UNC threaded fasteners and can be removed by unscrewing to allow other mounting fasteners to be used Note If the cabinet is mounted to a plate drill holes in the plate to match the ventilation holes in the bottom of the cabinet or use standoffs to raise the bottom of the cabinet at least Ya inch 1 2 cm above the mounting plate 10 50 266 7 68 17 3 1 50 38 1 FF Panag E Orin AN q q OOOO OOO OOO 6 00 152 4 000000000000 7 99 202 8 DOOOOOTOOO OO JE y oo T 15 86 402 8 Figure 2 1 Bottom View of Electrospray Aerosol Generator Showing Location of Rubber Feet Feet can be removed to provide mounting points on cabinet Dimensions are in inches mm Ventilation Requirements The Electrospray cabinet is designed to be cooled by natural convection of room air drawn through the bottom of the cabinet and exhausted through the back of the cabinet The cabinet should be installed with at least 2 inch 50 mm clearance between the back panel and any other surface Also the cabinet should be set on a clean h
70. pillary exit which pulls the charged solution out of the capillary forming droplets that are mixed with clean air and CO This produces a sheath flow which transports the droplets to the Electrospray chamber The highly charged droplets are neutralized by a Polonium 210 source and the liquid is evaporated before the aerosol exits the instrument The remainder of this section discusses liquid flow in the capillary the Electrospray chamber design aerosol neutralization the flow control system and the high voltage control and current measurement methods used in the Electrospray Clean air CO2 mixture in lonizer Capillary 1 Particles gt Aerosol out Tube High Voltage Wire Pressure Chamber Top Regulated gt clean air in Vial with particle liquid solution Pressure Chamber Bottom quick release Figure B 1 Schematic Diagram of the Electrospray Capillary Flow Characteristics The liquid flow rate Q nL min through the capillary is governed by the following equation for Poiseuille flow in a circular tube 4 g c 2e a A Equation B 1 2 S U L where D is the capillary inner diameter um p is the liquid viscosity poise AP is the pressure across the capillary psi Lis the length of the capillary cm cis a constant to account for all unit conversions 4 14E4 The capillary in the Electrospray has a diameter of 25 2 pm anda length of 25 cm a typical pressure across
71. proteins is Righetti P G G Tudor and K Ek 1981 Isoelectric Points and Molecular Weights of Proteins A New Table Chromatographic Reviews 149 J Chromatography 220 115 194 Typical Solutes Any solid or nonvolatile liquid that is soluble in a buffer solution can be used to make a sample for use with the Electrospray With a standard buffer solution useful solutes include sucrose PSL and proteins The properties of each solute and methods of preparing each sample are discussed below Sucrose The sucrose concentration of a sample can be varied to create continuously variable particle sizes For a given conductivity and flow rate the diameter of the primary droplets produced by the Electrospray will remain the same Once the liquid evaporates from the primary droplet the sucrose contained within the volume of the primary droplet will determine the resulting particle diameter The resulting particle diameter D may be calculated using the formula D 150 q where 150 being the primary droplet size in nm and being the sucrose volume fraction per unit volume buffer For example at q 0 1 10 volume sucrose per unit volume buffer the resulting particle diameter will be 69 nm At q 0 001 the particle diameter will be 15 nm The maximum particle diameter that may be created is 78 nm at q 0 143 reflecting smaller droplet sizes at higher concentrations The viscosity of sucrose solutions may vary by c
72. quids when preparing samples Key guidelines for choosing a buffer solution include the following Q volatile solution the solution must evaporate in the Electrospray chamber Q chemical buffer the pH of the solution should not change significantly when a sample is made a adjustable pH when making certain samples such as proteins the pH value of the solution must be greater than the isoelectric point pI value for the protein or the sample will stick to the capillary walls Q adjustable conductivity the primary droplet size produced by the Electrospray is inversely proportional to the cube root of the conductivity therefore there is a finite range of conductivities over which the Electrospray will operate A buffer solution used extensively in the Electrospray is 20 mM ammonium acetate created by dissolving ammonium acetate in ultrapure water De ionized water can be used in place of ultrapure water if necessary however ultrapure water is recommended to reduce the chances of buffer or sample contamination growth 20 mM ammonium acetate is volatile a weak buffer and has an adjustable pH and conductivity As an example to get started using the Electrospray a 20 mM ammonium acetate buffer solution with a conductivity of 0 2 S m adjusted to pH 8 is useful for dissolving solutes such as sucrose PSL and proteins to name a few The procedure for making this buffer solution subsequently referred to as the standard buffer so
73. r Seller makes no warranty with respect to and shall have no liability in connection with goods which are incorporated into other products or equipment or which are modified by any person other than Seller The foregoing is IN LIEU OF all other warranties and is subject to the LIMITATIONS stated herein NO OTHER EXPRESS OR IMPLIED WARRANTY OF FITNESS FOR PARTICULAR PURPOSE OR MERCHANTABILITY IS MADE TO THE EXTENT PERMITTED BY LAW THE EXCLUSIVE REMEDY OF THE USER OR BUYER AND THE LIMIT OF SELLER S LIABILITY FOR ANY AND ALL LOSSES INJURIES OR DAMAGES CONCERNING THE GOODS INCLUDING CLAIMS BASED ON CONTRACT NEGLIGENCE TORT STRICT LIABILITY OR OTHERWISE SHALL BE THE RETURN OF GOODS TO SELLER AND THE REFUND OF THE PURCHASE PRICE OR AT THE OPTION OF SELLER THE REPAIR OR REPLACEMENT OF THE GOODS IN NO EVENT SHALL SELLER BE LIABLE FOR ANY SPECIAL CONSEQUENTIAL OR INCIDENTAL DAMAGES SELLER SHALL NOT BE RESPONSIBLE FOR INSTALLATION DISMANTLING OR REINSTALLATION COSTS OR CHARGES No Action regardless of form may be brought against Seller more than 12 months after a cause of action has accrued The goods returned under warranty to Seller s factory shall be at Buyer s risk of loss and will be returned if at all at Seller s risk of loss Buyer and all users are deemed to have accepted this LIMITATION OF WARRANTY AND LIABILITY which contains the complete and exclusive limited warranty of Seller This LIMITATION OF WARRANTY AND LIABILITY
74. rchased separately The recommended pressure of the filtered air supply used with the Electrospray is 15 psi Supplying more than 25 PSI air pressure could result in damage to the internal components of the Electrospray and decreased sensitivity of the pressure regulator and air rotameter CO Input Above the filtered air input is an identical input marked CO IN 15 PSI MAX Connect the supplied polyethylene tubing in the manner described for the Filtered Air Input using a commercial CO compressed gas tank to supply CO to the Electrospray Commercial CO tanks and accessories are available from most compressed gas suppliers in denominations ranging from 2 5 to 50 lb The recommended pressure of the CO supply used with the Electrospray is 5 psi swagelok is a registered trademark of Swagelok Company 2 4 Model 3480 Electrospray Aerosol Generator Supplying more than 15 PSI CO pressure will cause the internal silicone tubing to disconnect from the CO rotameter fitting In addition a higher CO inlet pressure makes it more difficult to adjust the CO flow rate lonizer Installing the A Model P 2042 Nuclespot Local Air Ionizer with a Polonium 210 source is shipped separately because of regulations that govern packaging and shipping requirements for radioactive materials The ionizer must be installed for the Electrospray to operate properly Before installing the ionizer read the safety information at the beginn
75. ressure to capillary 6 3 B back panel 3 4 drawing 3 4 buffer solution 4 2 preparing 4 2 C capillary 3 6 adjusting position of tip 5 15 applying back pressure 6 3 cleaning tip 5 14 flow characteristics B 2 installing 5 14 removing 5 12 unplugging 6 3 caution description xii changing samples 4 8 chemical buffer 4 2 chemical safety xiv cleaning aerosol exit port 5 4 capillary tip 5 14 Electrospray chamber 5 6 5 7 orifice plate 5 3 pressure chamber 5 10 pressure regulator 5 19 rotameter 5 19 viewing window lens 5 4 CO flow control B 7 CO IN 15 PSI MAX 2 4 CO inlet 3 5 CO input 2 4 components capillary 3 6 Electrospray chamber 3 6 filters 3 8 high voltage fitting and shield 3 6 high voltage supply module 3 7 interlock switch 3 8 internal 3 6 main PCB 3 7 power supply 3 7 conductivity meter 4 2 cone jet mode 4 7 connectors 3 1 contacting TSI v 7 2 controls 3 1 corona discharge mode 4 7 current measurement B 9 customer service v 7 1 cylindrical pressure chamber 1 2 D dripping mode 4 7 droplet diameter calculating B 4 E electrical safety xv Electrospray Aerosol Generator 1 1 5 3 AC power connector 3 5 aerosol exit 3 4 air leak test 5 8 analog output 2 4 3 5 applications 1 2 back panel 3 4 drawing 3 4 bottom view 2 2 capillary 3 6 adjusting position of tip 5 15 cleaning tip 5 14 installing 5 14 unplugging 6
76. ry a TN 3 6 Electrospray Chamber asan aE tees a A ER 3 6 High Voltage Fitting and Shield cece cece eens 3 6 POWEL SUPPLY oi a rana 3 7 Main PCB sciisiizssces focos atenten eno Ade a a ii e 3 7 High Voltage Supply Module occoocccnccnnccnnccnnaconiconaconicnnnans 3 7 Interlock SwitCh esise ieren eraa enS AEn aS SEST EIREANN EEEE 3 8 Filters it a a a O E E N E E Ri 3 8 CHAPTER 4 Operating the Electrospray scsesesssseees 4 1 Preparing Samples rencon siena eaa aR aa are es i 4 1 Preparing a Buffer Solution oooccconnccnnncnnnnncnnnncnnnnarononccnnno 4 2 Measuring and Adjusting Conductivity c ees 4 2 Measuring and Adjusting PH eee eee eee tere eee need 4 3 TYPICAL SOMMES ws ensina peee vas beacon aeneonsdedeaassasaneseeseenss 4 3 Starting Up the Electrospray ooccocccocccnccnnccnnaconacanicanacanicananes 4 5 Generating ASrosolS oskai erre e op tent svennys ph dsaibataed samenaiees 4 6 Changing Samples smesh Mave wwe ai cag spaasssyices el venules Gav true be tbe tye ee 4 8 Shutting Down the Electrospray cocccocccnccnnocanacanaconacaniconanes 4 8 CHAPTER 5 Maintenance ccccccceccceccecccescccsccescecscecese 5 1 Periodic Maintenance wrona eiiiai cde ddden tens yada sue neve tebe 5 1 Purging the Capillary sccviien iiss sctecs stein to tenen sli se 5 1 Cleaning the Orifice Plate ooccoonccnnncccnnocnnnnccnnnnrnnnnccnnnarons 5 3 Cleaning the Aerosol Exit Port ocoooccncconoconocnnac
77. s chapter is organized into three sections describing aspects of the instrument Front Panel Back Panel and Internal Components The main components of the front panel are shown in Figure 3 1 They include the voltage and current LED displays the voltage adjustment knob the power and high voltage LED indicators the CO and air rotameters the pressure regulator and gauge and the pressure chamber In addition the viewing window and ionizer retainer are integrated with the cover and are included in this section LED Displays There are two LED displays on the Model 3480 Voltage kV and Current nA Q The voltage LED display is a measure of the high voltage applied to the platinum wire which charges the liquid in the vial and capillary A positive high voltage is standard but a negative high voltage module is available in place of or in addition to the positive high voltage module Q The current LED display is a measure of the status and stability of the Electrospray Aerosol Generator See Chapter 4 Operating the Electrospray for more information on how the current reading aids in determining the status of the Electrospray and Appendix B Theory of Operation for more detail on how the current is measured Current LED Display Voltage LED Display Voltage Adjustment Knob This knob is used to change the high voltage applied to the liquid used in the electrospray process It can be locked
78. sample vial the bottom half of the pressure chamber can be removed by twisting turn counterclockwise High voltage is not supplied to the platinum wire if the bottom half of the pressure chamber is removed In addition an in line orifice provides a pressure drop equal to the differential pressure set point eliminating the need to reduce the pressure when changing samples See Chapter 4 Operating the Electrospray for detailed instructions for handling or changing the sample vial Viewing Window The viewing window provides a visual inspection of the capillary tip This is useful when observing the different operating modes of the Electrospray and when installing a capillary It is also a good tool for troubleshooting the Electrospray The viewing window is backlit by a green LED and the lens can be adjusted to focus on the capillary tip by rotating the lens mount lonizer Retainer The ionizer retainer allows a Model P 2042 Polonium 210 radioactive ionizer to be installed in the Electrospray chamber to meet all radiation safety requirements The ionizer reduces the charge on the droplets produced by the Electrospray to increase the exit aerosol concentration Controls Indicators and Connectors 3 3 Back Panel Aerosol Exit 3 4 As shown in Figure 3 2 the back panel has power and data connections as well as air and CO inlets and the aerosol exit COginlet Filtered Air Inlet Analog Output
79. secure the main PCB 6 Install the high voltage module with the desired polarity in the same orientation as the high voltage module that was removed making sure the six connector pins on the main PCB are aligned with the six sockets on the high voltage PCB Tighten the two captive screws finger tight 7 Reconnect the high voltage cable by pushing the connector into the socket There is a turn spring locking connect that secures the connector when it is seated properly 8 Replace the cover on the instrument and tighten the four screws that secure the cover Model 3480 Electrospray Aerosol Generator Cleaning the Pressure Regulator The air supplied to the pressure regulator should always be from a clean dry air supply eliminating the need to clean the pressure regulator However if you suspect the regulator has become dirty refer to Appendix A for the manufacturer s specifications and instructions for maintaining the pressure regulator Cleaning the Rotameters The air supplied to the air rotameter should always be from a clean dry air supply eliminating the need to clean the air rotameter However if you suspect the air rotameter has become dirty refer to Appendix A for the manufacturer s specifications and instructions for maintaining the air rotameter The CO supplied to the CO rotameter should be supplied from a compressed gas cylinder containing dry CO gas After the CO enters the Electrospray instrument from th
80. several locations within this instrument Make sure you unplug the power source before removing the cover or performing maintenance procedures Leak Checking the Entire Electrospray Instrument 1 Remove power from the instrument and turn off all flows 2 Remove the cover by loosening the four screws securing the cover they do not have to be removed and pulling the cover upward while pushing down on the top of the front panel of the instrument or on the viewing window mount 3 Make sure a capillary is installed and all internal tubing is connected properly see the flow schematic in Appendix B 4 Turn off the external air and CO supplies or disconnect the external air and CO connections and plug each port 5 Plug the exhaust filter inside the instrument Connect a pressure gauge or manometer between the aerosol exit port and a leak tight valve The valve should be closed 7 Connect the valve to a vacuum source or a vacuum pump capable of drawing 18 inHg vacuum 8 Turn on the vacuum pump or vacuum system and slowly open the valve Allow the vacuum gauge reading to become stable and then close the valve 9 Observe the gauge reading The reading should not change by more the 0 5 inHg in 1 minute 10 If the instrument does leak follow the steps below under Isolating Leaks or continue with the section Leak Checking the Electrospray Chamber and Pressure Chamber Leak Checking the Electrospray Ch
81. sing the instructions above and rinse or soak the capillary tip in alcohol or a mild detergent until the contaminants are removed Then install the capillary using the instructions in the next section Installing the Capillary High voltage is accessible in several locations within this instrument Make sure you unplug the power source before removing the cover or performing maintenance procedures To install the capillary refer back to Figure 5 5 and use the following instructions 1 Remove power from the instrument and turn off all flows 2 Remove the cover by loosening the four screws securing the cover they do not have to be removed and pulling the cover upward while pushing down on the top of the front panel of the instrument or on the viewing window mount 3 Loosen the hex nut on the inlet fitting but do not remove it 4 Remove the high voltage shield by loosening the mounting screw and pulling the high voltage shield upward 5 Loosen the hex nut on the high voltage capillary guide but do not remove it 6 Insert the long end of the capillary into the high voltage capillary guide until the end of the capillary reaches the end of the platinum wire Twist the capillary until it becomes retained by the corkscrew of the platinum wire then tighten the hex nut on the high voltage fitting 7 Attach the high voltage shield to the cabinet by sliding the capillary through the high voltage shield routing the high volt
82. t changing the position of the differential pressure regulator knob The exhaust orifice is used to provide bleed and relief features to the differential pressure regulator This increases the regulator stability and responsiveness by keeping the regulator in a dynamic state It also provides a quicker exhaust when the regulator output pressure exceeds the set point pressure The air and CO rotameters provide separate controls for each flow before the flows are mixed together immediately upon exit of the rotameter The filter provides a final clean of the sheath flow as well as a means to mix the air and CO thoroughly before the entrance to the ionization chamber Model 3480 Electrospray Aerosol Generator Voltage and Current Measurement The voltage and current of the Electrospray circuit are displayed on the digital front panel meters This section describes how the voltage and current displays are measured Voltage Measurement The voltage at the output of the high voltage supply is divided down through series resistors Two 10 MQ resistors are used to reduce the maximum current of the high voltage supply If a person comes into contact with the high voltage fitting of the Electrospray the maximum current is 0 25 mA A further divider of two 50 MQ and one 100 kQ resistor divides the voltage of the Electrospray down by a factor of 1000 The sense voltage is picked up at the 100 kQ resistor and buffered through an OP 27 follo
83. ter or if float movement is restricted To clean rotate Retaining Clip Located in the back of flowmeter counter clockwise to align clip with slot and then pull out Then remove top plug ring if required outlet fitting and float only Tube does not need to be removed Wash tapered hole float outlet fitting and top plug with clean water and a soft brush Rinse all parts with clean water and dry thoroughly Avoid use of solvents and strong bases for cleaning Reassemble by reversing above Figure A 2 Rotameter Back View Model 3480 Specifications A 3 APPENDIX B Theory of Operation This appendix describes theories of operation for the Electrospray Aerosol Generator System Description The Electrospray consists of three main subsystems that are used to generate a monodisperse aerosol Q Pressure chamber capillary Electrospray chamber a Air and CO flow control a High voltage control The pressure chamber capillary Electrospray chamber schematic is shown in Figure B 1 A description of how the Electrospray generates aerosol follows A sample solution is stored in a cone shaped vial enclosed in a cylindrical pressure chamber The chamber accommodates a capillary and a platinum high voltage wire both of which are immersed in the solution Maintaining a differential pressure causes the solution to be pushed through the capillary The high voltage control regulates an electrical field exerted at the ca
84. trospray 4 7 Changing Samples Caution must be used when changing samples to avoid contaminating either of the samples A buffer solution should be run in the Electrospray between samples to clear the capillary of possible contaminants Follow the procedure below see Starting Up the Electrospray earlier in this chapter for details to change samples To avoid contaminating samples a buffer solution should be run between samples to clear the capillary of possible contaminants Remove the bottom half of the pressure chamber Close the lid of the vial and remove it Insert a vial containing buffer solution Replace the bottom half of the pressure chamber Or e amp Do Run buffer solution for one minute Note The residence time in a capillary using a standard buffer solution at 3 7 psi is approximately 112 seconds For most applications running a buffer solution for GO seconds will sufficiently prevent sample contamination however using a highly viscous fluid or a low capillary pressure drop will increase the residence time See Appendix B Theory of Operation for an analysis of liquid flow in the capillary 6 Repeat steps 1 4 using a sample vial rather than a buffer solution 7 Aerosol should be produced after a time equal to the residence time of the particular sample and operating conditions Shutting Down the Electrospray The capillary should be cleaned and cleared of liquid before shutting down th
85. wer Two IN 457 low leakage diodes are used as clamping diodes across the op amp inputs In order to reduce the voltage for the 2 V voltmeter display the voltage is further divided down by a factor of 10 This also provides the opportunity to balance any divider tolerance on the high voltage divider A capacitor of 0 1 pF on the input of a second op amp follower with the resistors provides a filter for any noise Current Measurement To measure the current of the Electrospray an op amp operation as a current to voltage converter is used The current path measured goes from the positive high voltage supply side into the current to voltage converter and then into the analog ground From the analog ground the current path continues through the grounded electrospray side through the Electrospray in the form of charged droplets through the liquid in the capillary through a 20 MQ protection resistor and into the negative high voltage supply side Selected References The following list contains papers that are referenced in this appendix as well as other references that may be interesting to the reader Adachi M K Okuyama and T Kousaka 1985 Electrical Neutralization of Charged Aerosol Particles by Bipolar Ions Journal of Chemical Engineering Japan 16 229 Theory of Operation B 9 B 10 Bailey Adrian G 1988 Electrostatic Spraying of Liquids New York John Wiley amp Sons Chen Da Ren David Y H Pui and St
86. y droplet diameter D can be calculated if the sucrose concentration C expressed as a decimal is known by using the following expression 1 Dg D c 1 3 P Equation B 2 Empirical formulas expressing the particle diameter from which the primary droplet diameter can be calculated of a 0 1 V V sucrose solution as a function of Q K where Q is the liquid flow rate and K is the electrical conductivity of the liquid have been reported in publications such as Chen Da Ren David Y H Pui and Stanley L Kaufman 1995 Electrospraying of Conducting Liquids for Monodisperse Aerosol Generation in the 4 nm to 1 8 pm Diameter Range J Aerosol Sci 26 963 977 Electrospray Chamber B 4 Immediately after the highly charged primary droplets are generated at the capillary tip they are transported by an air CO sheath flow mixture through an orifice plate to the ionization chamber This must be done quickly because after the primary droplet is generated the liquid begins to evaporate which decreases the surface area of the droplet thereby increasing the surface charge density If the surface charge density becomes too large the Coulombic repulsive forces on the droplet will cause Rayleigh disintegration resulting in a less monodisperse aerosol To reduce the charge on each primary droplet the Electrospray chamber houses a Polonium 210 radioactive alpha emitter ionizer The nature of the flow through the orifice

Model 3480 Electrospray Aerosol Generator Manual

Contents

Download Pdf Manuals

Related Search

Related Contents