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. Author manuscript; available in PMC: 2015 Oct 7.
Published in final edited form as: Int J Hyg Environ Health. 2015 Feb 11;218(3):345–357. doi: 10.1016/j.ijheh.2015.02.002

Table 1.

Summary of detection and characterization methods used to evaluate silver content of consumer products.

Matrix Techniqueb Sample preparation and analysisa
EPA NIOSH
Textile ICP
  • Cut textile sample from fabric and weigh (500–1000 mg, air-dry mass)

  • Submerge sample in 5 mL HNO3 (concentrated, 69–71%, w/w) and 5 mL ultrapure water

  • Cover beaker with watch glass, heat to ~ 100°C

  • Digest in HNO3

  • Cool, add 3 mL H2O2 (30%)

  • Heat to ~100°C, add H2O2 until effervescence is minimal

  • Cool, filter through glass fiber filter

  • Dilute with ultrapure water

  • Analysis by ICP-MS

  • Cut textile sample from garment and weigh

  • Digest with 15.6 M HNO3 at 95 °C for 70min

  • Cool, add water + 30% H2O2

  • Heat, add H2O2 until effervescence stops

  • Continue to heat for 120 min

  • Cool, add 12.1 M HCl

  • Heat for 10 min

  • Cool, dilute with di water

  • Analysis by ICP-AES

  • MDL = 0.7mg Ag/kg textile


SEM
  • Cut small piece of fabric from product

  • Adhere fabric to SEM stub with carbon tape

  • Ash piece of material and dust onto carbon tape on SEM stub

  • Sputter coat with ~50 Å gold

  • Image at 10 kV accelerating voltage

  • Remove individual fibers from garment using tweezers

  • Mount fibers on carbon tape

  • Sputter coat with ~50 Å gold/palladium

  • Image at 20 kV accelerating voltage

  • Cut textile sample from garment

  • Ash at 350°C for 3 h in alumina crucible

  • Disperse residue in deionized water

  • Pass aliquot through 0.4 μm pore TEPC filter

  • Section filter, mount on carbon tape

  • Sputter coat with ~ 50 Å gold/palladium

  • Image at 20 kV accelerating voltage


TEM
  • Cut small piece of fabric from product

  • Ash at <550 °C in muffle furnace

  • Dust ashed sample onto carbon-coated TEM grids

  • Suspend ashed sample in distilled water, immerse in sonicating bath, evaporate droplets on carbon-coated TEM grids

  • Image at 120 kV using TEM

-

UV–vis
  • Cut textile sample from garment

  • Place sample in integrating sphere

  • Measure absorption spectra from 350 to 700 nm

  • Cut textile sample from garment

  • Place sample in integrating sphere

  • Measure absorption spectra from 350 to 700 nm


Liquids ICP
  • Gently shake product in original container

  • Withdraw sample of known volume

  • Dilute 1:10 with ultrapure water

  • Dilute 1:100 with ultrapure water, add NHO3 to acidify

  • Analysis by ICP-MS

  • Mix product and withdraw sample of known volume

  • Digest as described for textiles

  • Analysis by ICP-AES

  • MDL = 0.001 mg Ag/L


SEM -
  • Mix product

  • Pass aliquot through 0.1 μm pore TEPC filter

  • Section filter, mount on carbon tape

  • Sputter coat with ~ 50 Å gold/palladium

  • Image at 20 kV accelerating voltage


TEM
  • Place 10 μL droplet onto carbon-coated grid

  • Dry TEM grid in desiccator

  • Repeat until total sample volume reaches 20 μL

  • Image at 120 kV accelerating voltage

  • Mix product

  • Place 4 μL drop onto carbon-coated grid

  • Air dry

  • Image at 80 kV accelerating voltage


UV–vis
  • Gently shake product in original container

  • Dilute liquid with deionized water (as necessary)

  • Dispense sample in 1-cm path length plastic cuvette

  • Measure absorption spectra from 350 to 700 nm

  • Mix product

  • Dilute liquid with deionized water (as necessary)

  • Dispense sample in 1-cm path length plastic cuvette

  • Measure absorption spectra from 350 to 700 nm


DLS
  • Gently shake product in original container

  • Pass sample through 1 μm hydrophilic Teflon filter

  • Thermally equilibrate sample in instrument, analyze

  • Mix product

  • Add aliquot to 10 mM NaCl solution

  • Pass sample through 0.7 μm membrane filter

  • Thermally equilibrate sample in instrument, analyze


ISE -
  • Mix product

  • Dilute aliquot with deionized water (as necessary)

  • Add ionic strength adjuster (5 M NaNO3)1:50

  • MDL = 0.015 mg/L


Plastics ICP
  • Cut sample from plastic and weigh (500–1000 mg, air-dry mass)

  • Digest as described for textiles

  • Analysis by ICP-MS

-

SEM
  • Cut small piece from plastic

  • Prepare for microscopy as described for textiles

-
a

HNO3, nitric acid; H2O2, hydrogen peroxide; HCl, hydrochloric acid; MDL, method detection limit; TEPC, track-etched polycarbonate; NaCl, sodium chloride; NaNO3, sodium nitrate; -, matrix not evaluated.

b

ICP, inductively coupled plasma (AES, atomic emission spectroscopy; MS, mass spectroscopy); SEM, scanning electron microscopy; TEM, transmission electron microscopy; UV-vis, ultraviolet-visible absorption spectroscopy; DLS, dynamic light scattering (photon correlation spectroscopy); ISE, ion selective electrode.