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6 protocols using nitric acid

1

Multi-Element Analysis Protocol

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Nitric acid (HNO3, 65% v/v) and hydrogen peroxide (H2O2, 30% v/v) were of Suprapure grade and purchased from J. T. Baker (Mallinckrodt Baker, Milan, Italy). Ultrapure water (<5 mg/L Total Organic Carbon (TOC) was supplied by Merck-Millipore (Darmstadt, Germany). The commercial standard solution of Re (internal standard), and the standards of Al, Cr, Mn, Fe, Co, Ni, Cu, Zn, As, Se, Mo, Cd and Pb used for the calibration curves came from Supelco (Bellefonte, PA, USA). For the element analysis, all the equipment for sample collection, handling and storage, as well as laboratory glassware and polytetrafluoroethylene (PTFE) digestion vessels, were washed with 5% HNO3 before use.
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2

Synthesis of Hybrid Organic-Inorganic Materials

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All materials were used as received. Anhydrous grades of toluene, n-butanol, tetrahydrofuran, chloroform, N,N-dimethylformamide and terpineol, 97% aluminum tri-sec-butoxide, >97% titanium isopropoxide, 20 wt % aluminum oxide nanoparticles in isopropanol (<50 nm, product number 702129), 57 wt % hydriodic acid in water, 33 wt % methylamine solution in ethanol, and lead chloride were obtained from Sigma-Aldrich. 70% nitric acid and 37% hydrochloric acid were obtained from Mallinckrodt Baker and EMD Millipore, respectively. 10 and 46 cP ethyl cellulose were obtained from TCI America.
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3

Histological Analysis Materials and Reagents

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All materials and reagents employed for the histological analyses were supplied by Bio-Optica Milano S.p.a. (Milan, Italy). The following reagents were all provided by Sigma-Aldrich (Milan, Italy): sulfuric acid (95–98% purity), sodium hydroxide, boric acid, hydrogen chloride, benzoic acid, and phosphate-buffered saline (PBS). The Kjeldahl catalyst was supplied by Carlo Erba (Milan, Italy). n-Heptane was purchased from PanReac AppliChem (Barcelona, Spain). Potassium hydroxide, chloroform, methanol, sodium carbonate anhydrous, Folin Ciocalteau’s reagent, stock standard solution of Re (1000 mg L−1 in 2% HNO3), gallic acid, and stock standard solutions of Sc, Ge, In, and Bi (1000 mg L−1 in 2% HNO3) were from Fluka (St. Gallen, Switzerland). Nitric acid (65%, v/v) was of Suprapur grade (Mallinckrodt Baker, Milan, Italy). Ultrapure water (<5 mg L−1 TOC) was obtained from a Barnstead Smart2Pure 12 water purification system (Thermo Scientific, Milan, Italy).
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4

Analytical Procedures for Food Characterization

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For crude protein, the Kjeldahl catalyst was supplied by Carlo Erba (Milan, Italy). Solvents, including n-hexane and n-heptane (reagent grade), and acetonitrile and methanol (HPLC grade), were from J.T. Baker (Phillipsburg, NJ, USA). Hydrogen peroxide (30% v/v) and nitric acid (65% v/v) (trace metal analysis grade) and ultrapure water (resistivity of 10 mΩ cm) were from Mallinckrodt Baker (Milan, Italy). Reference standards of fatty acids methyl esters (FAMEs, C4–C24) were purchased from Supelco (Bellefonte, PA, USA). Stock solutions of various inorganic elements (1000 mg/L in 2% HNO3, each) were supplied by Fluka (Milan, Italy), while reference standards of individual sugars and polyphenols were obtained from Sigma-Aldrich (St. Louis, MO, USA) and Extrasynthese (Genay, France).
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5

Synthesis and Characterization of Iron-CMC Composites

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Iron sulfate heptahydrate (FeSO4⋅7H2O) and CMC (MW = 90 000 in the sodium form, degree of substitution = 0.7) were purchased from Acros Organics (Morris Plains, NJ, USA). Sodium sulfide nonahydrate (Na2S·9H2O), hydrogen peroxide (H2O2), acetic acid, formalin and xylene were obtained from Fisher Scientific (Fair Lawn, NJ, USA). Nitric acid was obtained from Mallinckrodt Chemical (St. Louis, MO, USA). All chemicals are of the ACS reagent grade. All solutions were prepared with local tap water. To avoid effect of chlorine, the tap water was first dechlorinated under aeration at pH 6.0 for ~7 days. Table S1 in Supplementary Information (SI) gives the relevant water quality parameter.
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6

Analytical Procedures for Trace Element Determination

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Supra-pure-grade hydrogen peroxide (H2O2, 30% v/v) and nitric acid (HNO3, 65% v/v) were purchased from J.T. Baker (Mallinckrodt Baker, Milan, Italy), and hydrochloric acid (HCl, 37% v/v) and ultrapure water from Merck-Millipore (Darmstadt, Germany). The commercial standard solution of Re (internal standard), and the standards of Ag, Al, As, B, Ba, Be, Bi, Cd, Co, Cr, Cu, Fe, K, Li, Na, Mg, Mn, Mo, Ni, Pb, Sb, Se, Sr, Ti, Tl, V, Zn, used for the calibration curves, were purchased from Supelco (Bellefonte, PA, USA).
From Merck (Darmstadt, Germany) a Hg solution (1000 mg/L in 3% hydrochloric acid) was purchased. To clean the DMA-80 instrument, 3% HCl solution, prepared from concentrated HCl (37%), obtained from Merck (Darmstadt, Germany), was used.
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