Investigation of Silver Nanoparticle Sorption and Dissolution in Quartz Columns

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1 Investigation of Silver Nanoparticle Sorption and Dissolution in Quartz Columns Ashley Hart*, Hilary Emerson, O. Thompson Mefford, Brian A. Powell, Christopher L. Kitchens

2 Introduction Over 1600 consumer products contain nanomaterials 1 Growing concern of potential risk, transport and fate Numerous studies on ionic silver Design lab and field scale experiments to investigate AgNPs and other types of NPs AgNPs Size and surface chemistry dependent properties; Charge Stability Toxicity Levard, C., E. M. Hotze, et al. (2012). "Environmental Transformations of Silver Nanoparticles: Impact on Stability and Toxicity." Environmental Science & Technology 46(13):

3 Background Lysimeters Field apparatus for examining contaminant transport under natural conditions 1 year exposure Determine where NPs have traveled within tube Lysimeter Number Nanoparticle 1 Control no nanoparticles 2 Bare iron oxide nanoparticles, 6g 3 NOM stabilized iron oxide nanoparticles, 6g 4 NOM stabilized silver nanoparticles, 0.6g 5 Citrate stabilized silver nanoparticles, 0.6g 6 Thiol stabilized silver nanoparticles, 0.6g 3 Emerson, H. P., Hart, A. E., Mefford, O. T., Kitchens, C. L., Powell, B. A., ES&T. (2012), Under review.

4 Z (cm) from Source Z (cm) from Source Coring Results Silver Nanoparticles Lysimeters were segmented into 1 cm sections, acid digested and analyzed on ICPMS 0 Ag-Citrate Fraction of Source Ag-NOM Fraction of Source *99% of Ag in source travelled less than 5cm from source site Ag-NOM travels further than Ag-Citrate 4 Emerson, H. P., Hart, A. E., Mefford, O. T., Kitchens, C. L., Powell, B. A., ES&T. (2012), Under review.

5 Objective Gain insight as to why AgNPs are not mobile in soil Study transport of citrate and NOM AgNPs under ideal conditions Saturated flow Optimal ph Stationary phase that will not interact with nanoparticles One electrolyte at a time Design experiment that can be applied to other types of NPs 5

6 Column Study 8.3 cm Polycarbonate column Masterflex rotary pump Eldex Universal Fraction Collector Iota-8 ultra pure quartz powder 1 hour residence time Effluent analyzed on ICP-MS Nanoparticles: Citrate stabilized AgNPs Suwanee River Natural Organic Matter (NOM) stabilized AgNp Electrolytes: 0.001M, ph 6 NaCl (CH 3 ) 4 NClO 4 (TMAP) NaClO 4 6

7 Absorbance AgNP Synthesis & Characterization Ag + + NaBH 4 + A) Ag-Citrate 5.9 ± 2.5nm Ag-NOM Ag-Citrate B) Ag-NOM 7.6 ± 4.5nm Wavelength, nm 7 7

8 C/Co Ag-Citrate Column in 0.001M NaCl 1 Initial Breakthrough % 10.9% Second Breakthrough Diffusion Tail 43.9% Pore Volume, PV

9 C/Co Ag-Citrate Column Comparison Initial Breakthrough Ag Citrate NaCl Ag Citrate TMAP Ag Citrate NaClO4 AgNP Dissolution? Diffusion Tail No second breakthrough Pore Volume, PV

10 C/Co 1.0E E E E-01 C/Co 1.0E E E-03 Ionic Strength Flushes Citrate AgNPs/NaCl Citrate AgNPs/NaClO 4 1) DDI H 2 O 2) 0.1M NaCl 1) DDI H 2 O 2) 0.001M NaCl Pore Volumes, PV Pore Volumes, PV NaCl: increase with 0.1M NaCl flush NaClO 4 : Increase with H2O flush No trend seen in Citrate/TMAP or NOM columns 10

11 Log[Ag + ] [Cl - ]/[Ag + ] As ratio increases formation of soluble AgCl (x-1)- x thermodynamically favorable Ag mV Initial BT -7 AgCl 4 Diffusion Tail Second BT -8 Ag + AgCl AgCl 2 0.1M NaCl Log[Cl - ]

12 Log[Ag + ] ClO Ag Ag + Citrate/TMAP Log[ClO 4- ]

13 Ag Mass, ug Column Segmentation 10 Ag-Citrate Ag-Citrate NaCl 4.9% Ag-Citrate TMAP 0.48% Ag-Citrate NaClO4 0.41% Height in Column, cm 13

14 Recovery, % Ag-Citrate Recoveries NaCl TMAP NaClO Initial Breakthrough Diffusion Tail Second Breakthrough Quartz Powder Total Recovery

15 C/Co Ag-NOM Columns 1 Initial Breakthrough 78.1% Ag-NOM NaCl Ag-NOM TMAP % 0.5 % 39 % No second breakthrough Total Recoveries: 72.3 % 77 % Pore Volumes, PV

16 Ag Mass, ug 0.06 Column Segmentation Ag-NOM Ag-NOM NaCl 0.73% Ag-NOM TMAP 0.46% Height in Column, cm 16

17 Ag +, %, After 24 hours Batch Dissolution Centrifuged each NP/electrolyte solution in Millipore cellulose acetate 3000K cutoff filters 8000rpm for 3 min, discard filtrate 8000rpm for 45min, digest in 2% HNO 3 to measure [Ag] on ICP-MS Time zero, 3 hours, 24 hours, 10 days 35% 30% 25% 20% 15% 10% 5% 17 0% Citrate AgNP Control Citrate AgNP NaCl Citrate AgNP TMAP Citrate AgNP NaClO4 NOM AgNP control NOM AgNP NaCl NOM AgNP TMAP NOM AgNP NaClO4

18 Ag-Citrate Column NaCl Conclusions Low recovery in intial BT due to electrostatic screening Second breakthrough curve due to kinetics of formation and elution of dispersed AgCl ClO 4 not interacting with NPs Ag-NOM Columns Inhibiting dissolution Lack of second BT chelating Ag ions or preventing ionization Low recovery in initial breakthrough in NaCl TMAP Providing additional stabilization? 18

19 Acknowledgments Dr. Kitchens and Research Group Dr. O. T. Mefford Dr. B. A. Powell Hilary Emerson Sam Gorosh, Ian Gayman, Rebecca Lewis, Cody Davidson NSF CBET

20 Size by DLS, (nm) Zeta Potential, mv Max λ, nm Spike Characterization

21 Log[Ag + ] [Cl - ]/[Ag + ] As ratio increases formation of soluble AgCl (x-1)- x thermodynamically favorable Ag 0-4 Ag 0 /Ag + Ag 0 /AgCl -5-6 Ag 0 /Ag + Ag 0 /AgCl AgCl 4 400mV -7 AgCl 2 500mV -8-9 Ag + AgCl 600mV Citrate AgNP /NaCl Log[Cl - ]

22 Mass Balance &Retardation Factor NP Electrolyte Initial Breakthrough R % Diffusion Tail Second Breakthrough Quartz Powder Total % NaCl Ag- Citrate TMAP NaClO Ag- NOM NaCl TMAP

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