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12 protocols using acrylic acid aac

1

Thermoresponsive Polymer Synthesis and Characterization

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N-Isopropylacrylamide (NIPAAm, Sigma-Aldrich, St. Louis, MO, USA, >99%) was purified by recrystallisation in hexane and dried in vacuo. Acrylic acid (AAc, Sigma-Aldrich, >99%) was vacuum-distilled to remove the inhibitor MEHQ (hydroquinone monomethyl ether) and possible oligomer content. 4,4 -Azobis-4-cyanopentanoic acid (ACPA, 98%), N,N -methylenbisacrylamide (MBAm, 99%), 2-(dodecylthiocarbonothioylthio)-2-methylpropionic acid (TTCA, 98%), 1,4-dioxane (anhydrous, 99.8%), 1,3,5-trioxane (>99%), ethanol (99.8%) were all purchased from Sigma-Aldrich and used as received. Sodium chloride (99.5%) and diethyl ether (99%) were obtained from Acros Organics, Geel, Belgium. The water used throughout this study was deionised water from a Milli-Q system (Millipore, Burlington, MA, USA).
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2

Synthesis and Purification of Polymers

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N-isopropylacrylamide (NIPAm, 99%) was purchased from Acros Organics and was recrystallized from n-hexane. N,N′-methylenebis(acrylamide) (BA, 99%) was purchased from Alfa Aesar and was recrystallized from methanol. Acrylic acid (AAc, 99+%) was obtained from Sigma Aldrich and was purified by vacuum distillation prior usage. Sodium dodecyl sulfate (SDS, 99%+) was received from Sigma Aldrich and was purified by recrystallization from absolute ethanol. Ammonium persulfate (APS, ACS Grade) was purchased from Amresco VWR and was used as received. N-(3-Dimethylaminopropyl)-N′-ethylcarbodiimide hydrochloride (EDC, BioXtra), 2-(N-Morpholino)ethanesulfonic acid hydrate (MES, BioXtra), and Cadaverine dihydrochloride (CAD, Sigma Aldrich, Burlington, MA, USA) were used as received. All solutions were prepared in ultrapure MilliQ water (Total Organic Content ≤ 5 ppb, Resistivity ≥ 18 MΩcm).
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3

Pectin-Acrylic Acid Biomaterial Synthesis

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Pectin (from citrus fruits, galacturonic acid content 93.5%, methoxy content 9.4%, Sigma-Aldrich, St. Louis, MO, USA) and acrylic acid (AAc) of purity 99.9% (Sigma-Aldrich, St. Louis, MO, USA) were used. Other chemicals, such as buffers and dye were purchased from El-Nasr Co. for Chemical Industries, Nasr City, Egypt and used without further purification.
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4

Hydrogel Synthesis from HPMC and Acrylic Acid

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Hydroxypropyl methyl cellulose (HPMC) powder (composition: hydroxypropoxy content ~9%, viscosity: ~15 mPa.s for 2% (w/w) polymer in H2O at 25 °C), acrylic acid (AAc, 99%), N,N′-methylenebisacrylamide (MBA, 99%), tetramethylethylenediamine (TEMED, 99%) and potassium persulfate (K2S2O8, 99%) were purchased from Sigma-Aldrich, Sydney, Australia.
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5

Synthesis of NIPAM-AAc Microgels

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Example 1

N-Isopropylacrylamide (NIPAm) (Sigma) was recrystallized with hexanes heated to 60° C. for 1 hr and 0.22 μm filtered after cooling. NIPAm (95% of a 140 mM monomer solution by weight) was dissolved completely with agitation (1 hr) then filtered in ultrapure water into a 3-neck reaction vessel heated in silicon oil, stirred at 450 rpm, and fluxed at 70° C. A condenser with running cold water was attached to the middle neck, nitrogen was bubbled through the monomer solution via a side neck, and a temperature probe connected to a hot plate through a feedback loop was in the 3rd neck. NIPAm was fluxed 50 min before adding co-monomer Acrylic acid (AAc) (Sigma) (5% by weight) to flux an additional 10 minutes prior to initiation. The nitrogen was removed to add 1 mM ammonium persulfate (APS) to initiate the reaction and the nitrogen was then gently blown over the surface of the solution. The reaction proceeded for 6 hours, while stirring, with water flow through condenser. The reaction vessel was removed from the oil and stirred to cool overnight. Microgels were purified by filtering over glass wool to remove large aggregates and by dialysis to remove excess monomers in 1000 kDa MWCO cellulose ester dialysis tubing (spectrum) against ultrapure water (40× volume with 2 water changes over 48 hr).

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6

Acrylic Acid and Gelatin Hydrogel Synthesis

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All chemicals, including acrylic acid (AAc) and gelatin (G), were obtained from Sigma Aldrich (St. Louis, MO, USA).
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7

Hydrogel Composite Synthesis and Fabrication

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N-Isopropylacrylamide monomer
(NIPAM, Scientific Polymer Products Inc.), poly-N-isopropylacrylamide (pNIPAM, MW 300 000, Scientific Polymer
Products Inc.), N,N′-methylenebis-acrylamide
(BIS, Sigma-Aldrich), n-butanol (Sigma-Aldrich), acrylic acid (AAc,
Sigma-Aldrich), diethyl fumarate (DEF, Sigma-Aldrich), 80% hydrolyzed
poly(vinyl alcohol) (PVA, MW 9–10 kDa, Sigma-Aldrich), iron(III)
oxide (Sigma-Aldrich), Irgacure 2100 (Ciba), 1827 photoresist (Microchem),
351 developer (Microchem), and three inch silicon (Si) wafers (WRS)
were used as is without further modification.
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8

Bioactive Hydrogel Synthesis and Characterization

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The ®-Glucan (BG) was purchased from DSP Gokyo Food and Chemical Co. Ltd., Osaka Japan. Acrylic acid (AAc) and N,N’-methylene-bis-acrylamide (N, N-MBA), n-HAp powder (<100 nm particle size), and AgNO3 were purchased from Sigma-Aldrich, Selangor, Malaysia. The phosphate buffer saline (PBS) solution was prepared using sodium hydrogen phosphate, potassium chloride, sodium chloride, di-potassium hydrogen phosphate, and hydrochloric acid obtained from Merck, Darmstadt, Germany and used without any purification.
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9

Fabrication of NIPAM Hydrogel Sensors

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Materials N-isopropylacrylamide (NIPAm) was purchased from TCI (Portland, Oregon) and puried by recrystallization from hexanes (ACS reagent grade, EMD, Gibbstown, NJ) prior to use. N,N 0 -Methylenebisacrylamide (BIS) (99%), acrylic acid (AAc) (99%), and ammonium persulfate (APS) (98+%) were obtained from Sigma-Aldrich (St. Louis, MO) and were used as received. Tris (4-(dimethylamino)phenyl)methylium chloride (Crystal Violet, CV) and tetraethyl orthosilicate (TEOS, 98%) were obtained from Sigma-Aldrich (St. Louis, MO). Sodium chloride was obtained from EMD (Millipore, Billerica, MA), and deionized (DI) water with a resistivity of 18.2 MU cm was used. Cr/Au annealing was done in a Thermolyne muffle furnace from ThermoFisher Scientic (Ottawa, Ontario). Anhydrous ethanol was obtained from Commercial Alcohols (Brampton, Ontario). Sodium hydroxide (NaOH, 99.8%) and hydrochloric acid were purchased from Caledon Chemicals (Georgetown, Ontario) and were used as received. Fisher's nest glass coverslips were 25 Â 25 mm and obtained from Fisher Scientic (Ottawa, Ontario). Cr was 99.999% and obtained from ESPI as akes (Ashland, OR), while Au was 99.99% and obtained from MRCS Canada (Edmonton, AB).
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10

Synthesis of Thermosensitive Hydrogels

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The monomer N-isopropylacrylamide (NIPAm) was purchased from TCI (Portland, OR) and purified by recrystallization from hexanes (ACS reagent grade, EMD, Gibbstown, NJ). N,N′-Methylenebisacrylamide (BIS) (99%), acrylic acid (AAc) (99%), ammonium persulfate (APS) (98%), silver nitrate, sodium borohydride and hydrogen peroxide were obtained from Sigma-Aldrich (Oakville, Ontario) and were used as received. All other chemicals were of analytical grade. Deionized (DI) water with a resistivity of 18.2 MΩ cm was obtained from a Milli-Q Plus system from Millipore (Billerica, MA), and filtered through a 0.2 μm filter prior to use.
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