Size distribution analysis with the Nanoparticle Nebulizer Model 3485 in combination with an SMPS (spray characterisation)

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SOP: Size distributin analysis with the Nanparticle Nebulizer Mdel 3485 in cmbinatin with an SMPS (spray characterisatin) Date 28.05.2016 Versin 1.

1 SOP: Size distributin analysis with the Nanparticle Nebulizer Mdel 3485 in cmbinatin with an SMPS (spray characterisatin) Date Versin 1.0 English Cntent 1 Scpe 2 2 Basics Nanparticle Nebulizer 2 3 Instrumentatin 3 4 Instrumentatin preparatin Nanparticle Nebulizer SMPS 4 5 Preparatin fr sampling 6 6 Measurements 6 7 Interpretatin 7 8 Quality assurance 8 Page 1 f 9

2 1 Scpe The scpe f this standard peratin prcedure is the descriptin f the prcedure f the particle measurements with the Nanparticle Nebulizer (Mdel 3485, TSI) in cmbinatin with a Scanning Mbility Particle Sizer (SMPS Mdel 3963, TSI). 2 Basics Nanparticle Nebulizer The Nanparticle Nebulizer Mdel 3485 aerslizes aqueus suspensins f particles fr analysis by a TSI SMPS r ther gas phase particle instrument. The liquid sample is metered int the instrument via a peristaltic pump, cmbined with a knwn rati f pure water fr nline dilutin, and atmized int ultrafine drplets using a Venturi effect at a cntrlled temperature. An impactin pin psitined within 0.1 mm f the nebulizer nzzle remves the largest liquid drplets. The remaining wet aersl has a nminal drplet size f 300 nm. The aersl is cnditined at an elevated temperature t evaprate liquid, leaving nly the particles and disslved residue within the sample. The particles are cmbined with dry, filtered, make-up air. Up t 2 l/min f dry aersl flw can be drawn frm the aersl utlet. Figure 1: Flwsheet Nebulizer Page 2 f 9

3 3 Instrumentatin Instrumentatin used fr the particle measurements with particle number cncentratin and particle size distributin (suitable sampling carriers are t be used fr the imaging prcesses (TEM, REM, EDX, etc.)): Nanparticle Nebulizer Mdel 3485 SMPS spectrmeter Mdel 3936 with main cmpnents: Aersl inlet with impactr fr pre-separatin f larger particles SMPS Classifier Mdel 3080 with neutralizer Mdel 3077 (Kryptn 85) and DMA (Differential Mbility Analyzer) Mdel 3081 r NanDMA Mdel 3085 CPC (Cndensatin Particle Cunter) Mdel 3786 (here used, but ther CPCs are als suitable) Flw equalizer assembly t adjust the sample flw, depending n the CPC used PC r laptp t data cllectin and lgging NAS Nanmeter Aersl Sampler Mdel 3089 Pssibly Sensrs fr temperature, relative Humidity, pressure 4 Instrumentatin preparatin 4.1 Nanparticle Nebulizer Fill in the pressurised water cntainer accrding manufacturers' instructins with distilled water. After clsing, cnnect it with the water tube t the nebulizer. Cnnect the pressure water cntainer t the cmpressed air supply and set it t at least 14.7 psi (~ 1 bar). Cnnect the nebulizer t the cmpressed air supply and set it t at least 60 psi (~4.1 bar). Cnnect the waste water tube t the nebulizer and cnnect it with a waste water cntainer (with manually regular dispsal) r the labratry waste water system. Switch n the nebulizer after cnnectin t the pwer supply. The warm-up perid is apprximately 15 minutes. After warm-up the status screen shuld display fllwing temperatures: Nebulizer Temp 15 C Evapratr Temp 55 C Set the wrking pressures with the pressure regulatrs n the back panel f the nebulizer t: Air Pressure 35 PSIG Liquid Pressure 18 PSIG Setting f peristaltic pump cassette pressure Unscrew the sample bttle and pen the cassette lever, then press the cassette lever dwn until n lnger any drips frm the needle are seen. Press the cassette lever up tw mre clicks. Page 3 f 9

4 Befre running a sample, r between running different samples, it is necessary t purge the sample needle and bttle. Screw the sample bttle int the base f the purge manifld (ver the needle) On the display screen, press SETUP. Verify that the pump cntrl is set t BOT- TLE and that the bttle size is set apprpriately (8 r 30 ml). Press HOME, then press the purge buttn at the tp right f the screen. A purge valve pens, the sample needle is purged with ml/min f dilutin water, and the peristaltic pump tube runs frward at maximum speed. The screen displays the time remaining fr the purge. Nte: The purge fr the 30 ml sample bttle takes 85 s and the purge fr the 8 ml bttle takes 22 s. Fllwing a purge, the nebulizer is in STANDBY mde. The instrument is ready t use. 4.2 SMPS Cnnect the SMPS spectrmeter accrding t the manufacturers' instructins with tubes and data cables. Install the impactr with the desired rifice (cut ff) and grease the impactr plate slightly, and then cnnect the impactr with the aersl inlet. Fill in the CPC Mdel 3786 accrding manufacturers' instructins with distilled water. Fr the measurement data lgging, cnnect the CPC via Universal Serial Bus (Mdel 3786) and cmputer cable with the PC r laptp. Switch n all devices (Classifier, CPC, and PC) after cnnectin t the pwer supply. The CPC Mdel 3786 warm-up perid is apprximately 15 minutes. After CPC warmup the status screen shuld display fllwing temperatures (in C): Optc GT 75.0 (Optics) 75.0 (Grwth Tube) SAT 12.0 (Saturatr) T check the status f these temperatures n the CPC display during the warm-up, select the Status Screen with the display buttn n the frnt panel. Once warm-up is cmplete, the CPC display shws the Primary Cncentratin Screen. Hardware adjustments On the classifier, the vltage cntrl shuld be set t Analg Ctrl t allw the DMA vltage t be cntrlled by the CPC. T d s, rtate the black cntrl knb until the Ctrl-Pane in the Classifier LCD Display is highlighted, and then press the knb t change frm Panel Ctrl t Analg Ctrl. The vlume flws have t be set depending n the particle size range used. Accrding t the manufacturers' instructins, the rati f the sheath air t aersl flw rates is nrmally set t 10:1. Fr example, the cvered particle size range is 13.5 t 750 nm mbility particle diameter fr the settings f sheath flw 3.0 l/min and aersl sample flw 0.3 l/min. Sheath Flw adjustment Rtate the black cntrl knb until the Sheath Flw pane in the Classifier LCD is highlighted. Click the cntrl knb by pushing in. Page 4 f 9

5 Scrll the cntrl knb until the crrect sheath flw is indicated, here 3 l/min Click the cntrl knb by pushing in. The sheath flw will then be updated with the actual flw The Sheath Flw LED lights up when the sheath flw is stabilized at set flw Sample Flw adjustment Cnnect a suitable flw meter (e. g. Gilibratr) t the aersl inlet Install the flw equalizer assembly accrding t the manufacturers' instructins between DMA and CPC. If sample flw is set t 0.6 l/min, the flw equalizer assembly is unnecessary and sheath flw shuld be set t 6.0 l/min. Turn n the CPC pump by pushing the Pump buttn Adjust the filter valve until the crrect aersl flw f 0.3 l/min is indicated n the flw meter Sftware adjustments The TSI sftware Aersl Instrument Manager is used fr measurement data lgging. After starting the sftware, pen a new file with File New, data type SMPS Data file (*.S80) and select a filename. The desktp pens in 4-Pane Layut (predetermined aut-fit) with the windws Size Data Graph, Size Data Table, SMPS-Sample List, and Statistics Table. With the Windw menu and 2-Pane Layut nly the windws Size Data Graph and SMPS- Sample List are displayed. A user-defined layut f the windws is pssible, t. With File Prperties, Run Prperties r muse buttn right after clicking New Sample in windw SMPS-Sample List and selecting prperties pen the dialg bx SMPS Prperties. Hardware Setting Classifier Mdel: 3080 DMA: 3081 r 3085 Impactr type: depending n use CPC: 3786 (depending n CPC mdel) DMA Flw Rate: Enter the Sheath and Aersl Flw td: Use the calculated value frm the hardware settings by using 10 inch tubing. (td is the time taken by the aersl t flw thrugh the classifier and the cnnectin tubing between the DMA and the CPC, which is assumed t be 10 inches (25.4 cm) lng.) Size Range Bunds: Enter the minimum and maximum size range t be sampled using the Lwer and Upper Diameter pull-dwn lists r select the buttn Set t Max Range t the maximum range based n current DMA and flw settings. Scan Time: Up (range is 30 t 300 s) 120 s Retrace (range is 10 t 300 s) 15 s Scheduling Sample: Scans per Sample and Number f Samples, if desired Scheduled: Select Only Once t cllect ne set f samples. Fr cntinuus mnitring, select the Repeat Every and enter interval starting time, here 3 min Start At Time: If desired, select the check bx and enter the clck time at which the sampling shuld begin Page 5 f 9

6 Physical Prperties Gas Prperties: Enter the Gas Viscsity and Mean Free Path (Default settings fr Air at K and kpa) Particle Density: Enter the density, if knwn Crrectin Flags and Values: Multiple Charge Crrectin: Fr the crrectin f multiple charged particles Diffusin Crrectin: Fr the crrectin f particle lsses caused by diffusin nly within the SMPS. This des nt accunt fr the particle lsses in sample tubes! Nanparticle Aggregate Mbility Analysis: Fr the crrectin frm spheres t aggregates. These crrectins are mathematically based n the identified raw cunts and can be switched n r ff retrspectively, t, i. e. after sampling By pressing the OK buttn the prgram retains the current settings. 5 Preparatin fr sampling Befre sampling start, the CPC shuld be drained manually t reduce measurement data lsses by draining the reservir (pump will be turned ff during draining). T d s, press the Drain/Prime buttn fr ne secnd t select the drain mde and press the Drain/Prime key again fr 2 s t start draining, duratin 1 min. Cnnect a sample tube frm the aersl utlet f the nebulizer t the aersl inlet (impactr) f the SMPS. Screw the sampling bttle (8 r 30 ml) with the particle suspensin t be measured int the base f the purge manifld (pssibly pre-treatments are shaking, dispersin in an ultrasnic bath, dispersing with ultrasund finger, etc.). Set the sampling flw ( ml/min) by pressing SETUP and SAMPLE FLOW depending n the dilutin. The dilutin depends f the dilutin flw ( ml/min) and is set later adjusted with the help f the dilutin ratis. The Start Display appears by pressing HOME. T sample particles t be used fr the imaging prcesses (REM, EDX) prepare the NAS with suitable sampling carriers (depending n the material t be examined) (see nangem SOP NAS). 6 Measurements Press the Start buttn n the HOME screen and the sample will be injected int the instrument. The nebulized sample will begin exiting the aersl utlet within 30 s. Press STATUS t shw the status display. Set the dilutin rati by adjusting the Dilutin Flw Cntrl (silver dilutin cntrl knb next the Purge Manifld). Pssibly a readjustment f Air Pressure and/r Liquid Pressure is required (indicated by the red VALUE errr message in the STATUS display). Nte values f STATUS display. Page 6 f 9

7 If the check bx by Prperties Scheduling Start at Time is marked and a clck time is entered, the sampling starts at the entered start time. Otherwise select Run Start Data Cllectin t start the sampling immediately. At least 5 measurement scans shuld be measured after stabilizatin f the particle size distributin and particle cncentratin. Select Run Finish Current Sample t stp the cntinuus mnitring after the current sample. Select Run Abrt Current Sample t stp the current sampling immediately and the data fr the current sample is discarded. Nte: Regularly apprpriate dispse f the waste water during run f the peristaltic pump. After finishing the measurement series change the particle suspensin dilutin by turning the Dilutin Flw Cntrl and start a new measurement series. Otherwise stp particle generatin by pressing Stp n the HOME screen. After stpping and finishing particle generatin unscrew the sampling bttle f the Purge Manifld. Stre the sampling bttle as a retained sample r dispse the sampling bttle and/r their cntent apprpriate. Screw a sampling bttle with distilled water int the Purge Manifld and press the purge buttn t purge the system (see als 4.1). Measure all particle suspensins accrding the described prcedure. 7 Interpretatin Simple data analysis with the 4-Pane-Layut: Select the sample in the SMPS-Sample List with muse click The windw Size Data Graph displays the particle size distributin f the selected sample The lwer and upper size limit can be changed with the muse pinter and pressing left muse buttn (pinter becmes a hand). Psitin the pinter n a bar (depending n type f graph that is active) and the pinter becmes a hand. By clicking the left muse buttn the values diameter and cncentratin are displayed. The displayed size distributin can be zmed in by placing the pinter at ne pint f the area t be enlarged by pressing the left muse buttn and dragging the muse t the ppsite pint f the data. Release the left Page 7 f 9

8 muse buttn and the selected area is enlarged. T zm ut, select Frmat Und Zm and the enlarged area is returned t nrmal view. The windw Size Data Table displays the cllected measurement data fr each size class in table frm. The windw Statistics Table displays the different diameters, deviatins, and the ttal cncentratins. Fr further data interpretatin: Select the samples, which shuld be exprted in the SMPS-Sample List. With File Exprt the samples can be exprted in a file. In the dialg bx Exprt Parameters, select the data types. After selecting a filename, the data can be exprted as a text file, and then imprted int a spreadsheet prgram. 8 Quality assurance Measures fr quality assurance: Zer tests: Peridical checking f adjusted vlume flws (sheath and aersl flw) with a suitable flw meter. By adjusting the vltage t zer V at the cllectr rd, the airstream flwing ut f the mndisperse aersl cnnectr shuld be particle free and the CPC shuld nt detect particles. Peridical testing fr leaks and sampling with filtered air (HEPA filter); the CPC shuld nt detect particles. Rutine checking f the calibratin with particles f certified aerdynamic diameters (PSL) Peridical checking f the system nebulizer-smps with the TSI standard 30 nm (supplied by the manufacturer). Realizatin and reprting f the maintenance f nebulizer und SMPS accrding t manufacturer and manual. Reprting f anmalies during sampling r maintenance Page 8 f 9

9 Title: This SOP is valid frm: This SOP replaces the SOP frm: Primary versin (1.0) Respnsible fr the implementatin f this SOP: Measurement persnal Previus changes: Primary (1.0) Signature/Date Authr: Apprved:, Dipl. Ing. H. Kaminski, Dr. rer. nat. B. Hellack Page 9 f 9

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