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13 protocols using ammonium nitrate

1

Synthesis of Multifunctional Magnetic Nanoparticles

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Iron(III) chloride hexahydrate (FeCl3.6H2O, 97.0−102.0%), iron(II) chloride hydrate (FeCl2.H2O, 99%), ammonium nitrate (NH4NO3, 99.999%), N-hydroxysuccinimide (NHS, 98+%), ethylenediaminetetraacetic acid tetrasodium salt hydrate (EDTA, 98%) and tetraethyl orthosilicate (TEOS, ≥99.999% metals basis) were bought at AlfaAesar. The n-Cetyltrimethylammonium bromide (CTAB), (3-aminopropyl) triethoxysilane (APTES, ≥98%), thioglycolic acid (≥99.9%), succinic anhydride (≥99% GC), (+)-sodium L-ascorbate (crystalline, ≥98%), N-3-dimethylaminopropyl-n-ethylcarbodiimide hydrochloride (EDC, ≥97%), acetone (≥99.5% GC), 4-morpholineethanesulfonic acid (MES, ≥99%), TRIS (hydroxymethyl)aminomethane hydrochloride (TRIS HCl) and phosphate-buffered saline (PBS, tablets) were purchased from Sigma Aldrich. Ethanol absolute (EtOH, extra pure), hydrochloric acid (HCl, 37%) and sodium hydroxide (NaOH) were bought at Scharlab, SL. Oleic acid (OA, 65.0–88.0 %) was acquired from Honeywell Fluka and sodium chloride (NaCl, 99.0–100.5%) at PanReac AppliChem. BactoTM Glycerol was bought from Becton Dickinson&Co (Sparks, MD, USA). Muller Hinton Broth (MHB) and Trypto Casein-Soy Broth (TSB) were obtained from Biokar Diagnostics. All reagents were used as acquired, without any further purification, and all solutions, unless otherwise indicated, were prepared with deionized Millipore miliQ water.
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2

Synthesis and Characterization of Nanoparticles

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Thioglycolic acid (TGA, C2H4O2S, ≥99%), cadmium acetate dihydrate (Cd(CH3COO)2·2H2O, 99.5%), (3-aminopropyl)triethoxysilane (APTES, H2N(CH2)3Si(OC2H5)3, 99%), tetraethyl orthosilicate (TEOS, SiC8H20O4, 98%), ammonia (NH3, ≥99.9%), cetyltrimethylammonium bromide (CTAB, C19H42BrN, ≥98%), poly(ethylene glycol) BioUltra 3000, poly(ethylene glycol) BioUltra 6000, poly(ethylene glycol) BioUltra 8000, p-toluenesulfonyl chloride (CH3C6H4SO2Cl, ≥98%), hydrochloric acid (HCl, 37%), magnesium sulfate (MgSO4, ≥99.5%), sodium ascorbate, bovine serum albumin (BSA), lysozyme (LYS), carbonic anhydrase (CA), ovalbumin (OVA), hemoglobin (Hb), myoglobin (Myb), and cytochrome c (CYT) were purchased from Sigma-Aldrich (Lisbon, Portugal). Sodium hydroxide (NaOH, ≥98%) was produced by Panreac. Sodium tellurite (Na2TeO3, 99.5%) and ammonium nitrate (NH4NO3, 99.9%) were purchased from Alfa Aesar. Sodium borohydride (NaBH4, 99%), ethylene glycol (C2H6O2, ≥99.5%) and (3-isocyanatopropyl)triethoxysilane (IPTES, (C2H5O)3Si(CH2)3NCO, 95%) were produced by Fluka. Methanol (MeOH), ethanol (EtOH), tetrahydrofuran (THF, C4H8O, ≥99.9%), and chloroform (CHCl3) were purchased by Carlo Erba Reagents. All the reagents and solvents were of analytical reagent grade and were used as received. All cell culture reagents were purchased from Gibco (Alfagene, Lisbon, Portugal) unless stated otherwise.
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3

Synthesis of Multifunctional Nanoparticles

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1,6-diaminohexane (98%), Acetic Acid (HOAc ≥ 99.7%), Acetone, Borate Buffered Saline (tablets), Dichloromethane (DCM, reagent grade), DiEthyl Ether, Dimethylformamide (DMF, reagent grade), Ethyl Ether (reagent grade), Hydrochloric Acid (≥37%), Hydrogen Peroxide (30%), N-Hydroxysulfosuccinimide sodium salt (NHS-Sulfo), N-N'- disuccinimidyl carbonate (DSC, ≥98%), Ofloxacin, Phosphate Buffered Saline (tablets), Pluronic F-127, Rhodamine B base (≥98%), Silver Nitrate (99%), Sodium Borohydride (99%), Sodium Citrate tribasic dehydrate (99%), Tetraethyl Orthosilicate (TEOS, 99.99%), Tetrahydrofuran (THF), Trimethylchlorosilane (TMSCl, ≥98%), Toluene were purchased from Sigma Aldrich. 3-(triethoxysilyl)propyl isocyanate (≥95%), Sodium Chloride, Piperazine (≥98%), Triethylamine (≥99.5 %) were purchased from Fluka. Absolute Ethanol, Dimethyl Sulfoxide (DMSO), Ethylene Glycol were purchased from Carlo Erba Reagents. Ammonium Nitrate, Hexadecyltrimethylammonium bromide (CTAB, 98%) were purchased from Alfa Aesar. Potassium Bromide and Sodium Hydroxide were purchased from Panreac. All reagents were used without further purification.
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4

Characterization of Organic Acids and Compounds

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The following chemicals, including their sources, purity, and CAS numbers, were used: citric acid monohydrate, Fisher, ACS grade, 5949-29-1; ᴅʟ-malic acid, Alfa Aesar, 98%, 6915-15-7; ᴅʟ-isocitric acid, trisodium salt hydrate, Acros Organics, 95%, 1637-73-6; ᴅʟ-lactic acid, TCI, >85%, 50-21-5; ᴅʟ-glyceric acid, TCI, 20% in water (ca. 2 mol/L), 473-81-4; ᴅʟ-tartaric acid, TCI, >99%, 133-37-9; glutaric acid, Acros Organics, 99% 110-94-1; tricarballylic acid, Alfa Aesar, 98%, 99-14-9; adipic acid, Sigma, 99%, 124-04-9; acetic acid, Sigma, ACS grade, 64-19-7; pimelic acid, Alfa Aesar; >98%, 111-16-0; succinic acid, TCI, >99%, 110-15-6; tartronic acid, Sigma, >97%, 80-69-3; sodium mesoxalate monohydrate, Chemodex, >98%, 31635-99-1; ᴅʟ-2-hydroxybutyric acid sodium salt, Alfa Aesar, >97%, 5094-24-6; ᴅʟ-3-hydroxybutyric acid sodium salt, Chem Impex Int’l Inc., 100.3%, 150-83-4/306-31-0; ascorbic acid, TCI, >99%, 50-81-7; ammonium nitrate, Fisher, ACS grade, 6484-52-2; sodium nitrate, VWR, ACS grade, 7631-99-4; sodium hydroxide, VWR, ACS grade, 1310-73-2; nitric acid, Sigma, ACS grade, 7697-37-2; and sodium azide, Sigma, 99.8%, 26628-22-8. Lacey carbon, 300 mesh, copper grids (product #01895) from Ted Pella, Inc. were used for electron microscopy.
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5

Screening Organic Acids and Peroxidase Activity

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The chemicals, their sources, purity, and CAS #s were: adipic acid, TCI, ≥ 99%, 124-04-9; ammonium nitrate, Fisher, ACS grade, 6484-52-2; citric acid monohydrate, Fisher, ACS grade, 5949-29-1; DL-3-hydroxybutyric acid sodium salt, Chem Impex Int’l Inc., 100.30%, 150-83-4 & 306-31-0; DL-malic acid, Alfa Aesar, 98%, 6915-15-7; glutaric acid, Acros organics, 99%, 110-94-1; hydrogen peroxide 3% W/W, BDH chemicals, 7722-84-1; horseradish peroxide type II, Sigma, 150-250 U/mg, 9003-99-0; lactic acid, TCI, ≥ 85%, 50-21-5; pimelic acid, Alfa Aesar, 98+%, 111-16-0; sodium acetate, VWR, ACS grade, 127-09-3; sodium azide, Sigma, 99.8%, 26628-22-8; sodium nitrate, BDH chemicals, ACS grade, 7631-99-4; succinic acid, TCI America, ≥ 99%,110-15-6; and tricarballylic acid, Alfa Aesar, 98%, 99-14-9. For electron microscopy, hexagonal copper square grids with 200 mesh carbon support film from Electron Microscopy Sciences were used. Pierce Biotechnology’s 2 kD MWCO Slide-A-Lyzer™ dialysis cassettes were used.
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6

Analytical Characterization of Organic Compounds

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The chemicals, their sources, purity, and CAS numbers were adipic acid,
TCI, ≥ 99%, 124-04-9; ammonium nitrate, Fisher, ACS grade, 6484-52-2;
citric acid monohydrate, Fisher, ACS grade, 5949-29-1; DL-3-hydroxybutyric acid
sodium salt, Chem Impex Int’l Inc., 100.30%, 150-83-4 & 306-31-0;
DL-malic acid, Alfa Aesar, 98%, 6915-15-7; glutaric acid, Acros organics,
99%,110-94-1; hydrogen peroxide 3% W/W, BDH chemicals, 7722-84-1; horseradish
peroxide type II, Sigma, 150-250 U/mg, 9003-99-0; lactic acid, TCI, ≥
85%, 50-21-5; pimelic acid, Alfa Aesar, 98+%, 111-16-0; sodium acetate, VWR, ACS
grade, 127-09-3; sodium azide, Sigma, 99.8%, 26628-22-8; sodium nitrate, BDH
chemicals, ACS grade, 7631-99-4; succinic acid, TCI America, ≥
99%,110-15-6; and tricarballylic acid, Alfa Aesar, 98%, 99-14-9. The electron
microscopy grids were 200 mesh carbon support film on hexagonal copper square
grids from Electron Microscopy Sciences. Pierce Biotechnology’s 2 kD MWCO
Slide-A-Lyzer™ dialysis cassettes were used. Trace metal grade
concentrated nitric acid was from Fisher. ICP/DCP Ce ion standard solution was
from Aldrich.
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7

Protonation and Calcination of ZSM-5 Zeolite

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Zeolite ZSM-5 was purchased from Sigma Aldrich (St. Louis, MO, USA). A weight of 100 g of ZSM-5 was mixed with 400 mL of ammonium nitrate (1 mol L−1) (Fisher, Polk County, MN, USA) and the mixture was heated at 80 °C for 1 h using a rotary evaporator (Biobase model RE100-Pro) with continuous stirring at 60 rpm, which allowed us to increase the protonation of the zeolite before its impregnation. After that, several washes with distilled water were performed and excess solvent was removed by vacuum filtration. The obtained solid was dried at 120 °C for 2 h and then consecutively calcined at 250 °C for one hour, at 400 °C for an additional hour and finally for 12 h at 500 °C.
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8

Surfactant-Assisted Silica Synthesis

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Tetraethyl orthosilicate (TEOS), cetyltrimethylammonium bromide (CTAB), and triethanol amine were purchased from Across Organics. Methyltrimethoxysilane (MTMS) was purchased from TCI Chemicals. Pluronic F127 polymer was purchased from Anatrace, Inc. Ethanol was purchased from Decon Laboratories. Ammonium nitrate, hydrochloric acid (HCl, 37%) and cyclohexane were purchased from Fisher Scientific. Sodium hydroxide and ammonium hydroxide solution (28–30%) were purchased from Macron Chemicals. Bovine serum albumin (BSA) was purchased from USBiological Life Sciences. All materials were used as received.
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9

Synthesis and Activation of H-ZSM-5 Zeolite Crystals

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Large coffin-shaped zeolite H-ZSM-5
crystals (Figure 1a) with an average size of
∼20 × 20 × 100
μm3 and a bulk Si/Al ratio of 17 were used as provided
by ExxonMobil (Machelen, Belgium). The synthesis procedure has been
reported elsewhere.45 (link) Organic template
molecules (tetrapropylammonium, TPA) were removed by careful calcination
(1 °C/min) at 550 °C for 8 h. After template removal, the
zeolite crystals were converted into their acidic form by a triple
ion-exchange with 10 wt % ammonium nitrate (99+%, Acros Organics)
at 80 °C, followed by 6 h calcination at 500 °C. To avoid
residual fluorescence, prior to use, the crystals were activated at
500 °C (1 °C/min) for 24 h in static air.
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10

Synthesis of Large Zeolite H-ZSM-5 Crystals

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Large zeolite H-ZSM-5 crystals (dimensions:
100 × 20 × 20 μm3) were used as provided
by ExxonMobil (Machelen, Belgium). The synthesis has been reported
elsewhere.59 (link),61 (link) Tetrapropylammonium as template
was removed by calcination at 823 K for 8 h (1 K/min). The crystals
were subsequently converted into their acidic form by a triple ion
exchange with 10 wt % ammonium nitrate (99+% Acros Organics) at 353
K, followed by 6 h calcination at 773 K. The steamed zeolite H-ZSM-5
was treated at 773 K in a water-saturated N2 flow (150
mL/min) for 5 h. The resulting crystals were previously characterized
in detail by Aramburo et al.61 (link)
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