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6 protocols using n n dimethyl p toluidine dmpt

1

PMMA/HA Microsphere Composites for Bone Cement

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PMMA/HA microsphere composites with various HA contents (5 vol %, 20 vol %, and 40 vol %) were prepared by mixing HA microspheres with PMMA/MMA mixtures. Pre-polymerized PMMA beads (Sunjin Chemical, Ansan, Korea) with a size range of 10–20 µm in diameter were used. An MMA (Yakuri Pure Chemicals Co., Kyoto, Japan) monomer with a purity of 95% was used to complete the polymerization. Benzoyl peroxide (BPO; Sigma Aldrich, St. Louis, MO, USA) and N,N-dimethyl-p-toluidine (DMPT, Sigma Aldrich, St. Louis, MO, USA) were used as initiator and activator of free radical polymerization, respectively. PMMA prepolymer beads and a liquid MMA monomer containing 1 wt % of BPO powder and liquid DMPT activator were hand-mixed at a 2:1 weight ratio. The mixtures were placed into a cylindrical polyester mold with a diameter of 6 mm. The PMMA/HA composites were then cured in a 70% humidified incubator at 37 °C for 24 h to evaporate the residual MMA monomer. For comparison purposes, PMMA bone cements with HA powders or barium sulfate powders (BaSO4, Sigma Aldrich, St. Louis, MO, USA) as an additive were also produced in a similar way.
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2

Experimental Dental Composite Synthesis

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Two paste experimental composites were prepared using the powder to liquid ratio of 2:1. The initiator liquid (Table 1) consisted of urethane dimethacrylate (UDMA, Lot no. MKCG8230, Sigma Aldrich, St. Louis, MO, USA), triethyleneglycol dimethacrylate (TEGDMA, Lot no. STBF9549V, Sigma Aldrich), 2-hydroxyethyl methacrylate (HEMA, Lot no. STBG9652, Sigma Aldrich), 4-methacryloyloxyethyl trimellitic anhydride (4-META, Lot no. A766387 Polysciene, Warrington, PA, USA), camphorquinone (CQ, Lot no. 09003AQV, Sigma Aldrich), benzoyl peroxide (BP, Lot no. MKCF7091, Sigma Aldrich), and N, N-dimethyl-p-toluidine (DMPT, Lot no. MKBX9809V, Sigma Aldrich).
The composition of powder phase of each experimental composite is provided in Table 2. The powder phase consisted of silanated dental glass (33 wt% BaO, 50 wt% SiO2 and 9 wt% BO, Lot no. 806335, Esstech, Essington, PA, USA), monocalcium phosphate monohydrate (MCPM, Lot no. MCP-444950, Himed, Bethpage, NY, USA), and nisin Z (nisin, Lot no. 030220190415, Handary, Brussel, Belgium).
Powder and liquid phases were weighed and hand mixed using a plastic spatula. The mixed initiator and activator pastes were loaded into the double-barrel syringe and was injected using mixing tip and mixing gun (MIXPAC, Sulzer, Winterthur, Switzerland). Commercial self-adhesive dental composite (VF, Vertise flow, Kerr) was used as a comparison (Table 3) 5) .
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3

Dental Composite Resin Formulation

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Methyl methacrylate (MMA), 2-(diethylamino) ethyl acrylate (DEAEA), 2-(diethylamino) ethyl methacrylate (DEAEM), benzoyl peroxide (BPO), and chitosan from shrimp shells with a molecular weight between 190–310 KDa and deacetylation degree of 88% were all purchased from Sigma-Aldrich (Sigma-Aldrich, Palo Alto, CA, USA). N,N-dimethyl p-toluidine (DMPT) was purchased from Merck (Merck, Burlington, MA, USA). Barium sulfate was purchased from Alfa Aesar (BaSO4) (Alfa Aesar, Tewksbury, MA, USA). PMMA powder beads were purchased from Veracryl (New Stetic SA, Medellin, Colombia).
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4

Synthesis and Characterization of ABC Microparticles

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The solid phase of ABCs was composed of PMMA microparticles acquired from New Stetic S.A. (Medellin, Colombia), barium sulphate (BaSO4) from Alfa Aesar (Tewksbury, MA, USA), and benzoyl peroxide (BPO). The chitosan sheets were from shrimp shells (Mw = 190 000–310 000 and a deacetylation degree of 88%) from Sigma-Aldrich, with CAS number 9012-76-4 and MDL number MFCD00161512 (Palo Alto, CA, USA). CS spheres with a maximum diameter of 1 mm were obtained from the transformation of chitosan sheets by the coacervation method based on the methodology reported by Dias and Queiroz.20 (link) CS spheres were also used in the preparation of the solid phase.
The liquid phase was composed of methyl methacrylate (MMA), 2-(diethylamino)ethyl acrylate (DEAEA), 2-(diethylamino)ethyl methacrylate (DEAEM) (Sigma-Aldrich, Palo Alto, CA, USA), and N,N-dimethyl p-toluidine (DMPT) (Merck, Burlington, MA, USA), according to Table 1. All materials were used as received from the supplier, except for BPO, which was recrystallized from methanol.
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5

Synthesis and Characterization of Graphene Oxide and Acrylate-Based ABC

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Flake graphite (325 mesh, Alfa Aesar, Tewksbury, MA, USA), sulfuric acid ((H2SO4), potassium permanganate (KMnO4), hydrogen peroxide (H2O2), and 2-propanol (Merck, Burlington, MA, USA) were used for the synthesis of the GO. PMMA microparticles (New Stetic SA, Medellin, Colombia), barium sulfate (BaSO4,) (Alfa Aesar, Tewksbury, MA, USA), benzoyl peroxide (BPO), and chitosan from shrimp shells (Mw = 190.000–310.000 g/mol and a deacetylation degree of 88%, Sigma-Aldrich, Palo Alto, CA, USA) were used in the preparation of the solid phase of ABCs. Methyl methacrylate (MMA), 2-(diethylamino) ethyl acrylate (DEAEA), 2-(diethylamino) ethyl methacrylate (DEAEM) (Sigma-Aldrich, Palo Alto, CA, USA), and N,N-dimethyl p-toluidine (DMPT) (Merck, Burlington, MA, USA) were used in the liquid phase. All materials were used as received from the supplier, except for the BPO, which was recrystallized from methanol, and the CS, which was purified by dissolving in a 0.5 M solution of acetic acid, precipitation in a 2 M sodium hydroxide solution, and washing in water:ethanol solutions with decreasing concentrations (1:9, 3:7, 1:1, 2:1, 1:0, 1:0). Then it was frozen, lyophilized, and finally milled and passed through a 150 μm sieve.
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6

Barium Sulfate-PMMA Composite Synthesis

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The solid phase was composed of PMMA beads (New Stetic SA, Medellin, Colombia), barium sulfate (BaSO4) (Alfa Aesar, Tewksbury, MA, USA), and benzoyl peroxide (BPO) (Sigma-Aldrich, Palo Alto, CA, USA). The liquid phase was composed of methyl methacrylate (MMA), 2-(diethylamino) ethyl acrylate (DEAEA), 2-(diethylamino) ethyl methacrylate (DEAEM) (Sigma-Aldrich, Palo Alto, CA, USA), N,N-dimethyl p-toluidine (DMPT) (Merck, Burlington, MA, USA), and GO synthetized by a Hummers method modified.
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