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
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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
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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
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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
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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
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UV–vis |
Cut textile sample from garment
Place sample in integrating sphere
Measure absorption spectra from 350 to 700 nm
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Cut textile sample from garment
Place sample in integrating sphere
Measure absorption spectra from 350 to 700 nm
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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
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SEM |
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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
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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
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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
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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
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DLS |
Gently shake product in original container
Pass sample through 1 μm hydrophilic Teflon filter
Thermally equilibrate sample in instrument, analyze
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Mix product
Add aliquot to 10 mM NaCl solution
Pass sample through 0.7 μm membrane filter
Thermally equilibrate sample in instrument, analyze
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ISE |
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Plastics |
ICP |
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SEM |
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