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7 protocols using kaucl4

1

Systematic Synthesis of AuNPs on PEGylated RNTs

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The formation of AuNPs on PEGylated RNTs was studied in a systematic fashion by altering the ratios of reactants used (Table 1). The PEGylated RNTs used in the synthesis method were prepared using a strategy previously developed by the authors.13 (link)–17 (link) A solution of PEGylated RNTs was treated with potassium tetrachloroaurate (KAuCl4, Sigma) solution. The resulting solution was aged in the dark at room temperature for 24 hrs then treated with hydrazine hydrate (Acros Organics). The final solution was stored in the dark at room temperature for an additional 4 days.

Concentration of PEG-RNTs, KAuCl4, (NH2)2-H2O, and the ratios of PEG-RNTs/KAuCl4/(NH2)2-H2O used for gold deposition studies

SamplePEG-RNTsKAuCl4 Solution(NH2)2,H2O
Au-PEG-RNT-11 mg/mL, 930 μM, 1 mL3.77 mg/mL, 10 mM, 9.3 μL, 1 eq32.1 μg/mL, 1 mM, 9.3 μL, 0.1 eq
Au-PEG-RNT-21 mg/mL, 930 μM, 1 mL3.77 mg/mL, 10 mM, 18.6 μL, 2 eq32.1 μg/mL, 1 mM, 18.6 μL, 0.2 eq
Au-PEG-RNT-31 mg/mL, 930 μM, 1 mL3.77 mg/mL, 10 mM, 37.2 μL, 4 eq32.1 μg/mL, 1 mM, 37.2 μL, 4 eq
Au-PEG-RNT-41 mg/mL, 930 μM, 1 mL3.77 mg/mL, 10 mM, 74.4 μL, 8 eq32.1 μg/mL, 1 mM, 74.4 μL, 8 eq
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2

Synthesis and Characterization of Organometallic Complexes

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Fluorophenylthiols (HSRF), Pb(CH3COO)2, K[AuCl4], tetrahydrothiophene (tht), and 1,3-bis(diphenylphosphano) propane were purchased from Sigma-Aldrich and used without additional treatment. Solvents were obtained from JT Baker and used without previous treatment.
IR spectra were obtained using a Perkin-Elmer Spectrum 400 (PerkinElmer, Inc., Waltham, MA, USA) in the range of 4000 to 400 cm−1 using attenuated total reflectance (ATR-FTIR). Elemental analysis was performed with a Thermo Scientific Flash 200 (Thermo Fisher Scientific., Waltham, MA, USA) at 950 °C. NMR spectra were recorded on a 9.4 T Varian VNMRS spectrometer (Varian, Inc., Palo Alto, CA, USA) in CDCl3. Chemical shifts are reported in ppm relative to internal TMS δ = 0 ppm (1H, 13C) and to external references of CFCl3 (for 19F) and H3PO4 (for 31P) at 0 ppm. Positive-ion fast atom bombardment mass spectrometry (FAB+MS) spectra were measured on an MStation JMS-700 (JEOL, Ltd., Tokyo, Japan). Crystals were grown by slow (1 week) evaporation of solutions of the compounds in chloroform.
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3

Gold Nanoparticle Synthesis via UV-Assisted Deposition

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A quartz glass slide was placed on top of the substrate after a drop of about 10 µL of water was applied. The assembly was then exposed for 4 min to deep UV light (254 nm, 85 W). After this step, the substrate was placed in an aqueous solution of enthanolamine (2 mM, Sigma-Aldrich) and potassium gold(III) chloride (KAuCl4, 0.1 wt %, Sigma-Aldrich), to grow the gold precursor particles with the electroless deposition process. Reactive ion etching (Oxford Plasmalab 80 Plus) was used to remove the polymer with an oxygen plasma treatment with the following settings: process pressure 100 mTorr, power 100 W, temperature 20 °C and duration of the etching process 60 s. To measure the inter-particle spacing and sizes of the gold nanoparticles in this work we used a Scanning Electron Microscope (SEM) (Hitachi SU 8030).
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4

Nitazoxanide and Metal Complexes Characterization

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Nitazoxanide with 99 % purity (NTZ) and the metal salts of RuCl3·3H2O, KAuCl4 and AgNO2 were purchased from Sigma Aldrich and used without further purification. Human serum albumin (HSA, A1887; globulin and fatty acid free) and calf thymus DNA (Ct-DNA) were used for the biological study and purchased from Sigma Aldrich.
Infrared spectra (IR) for the ligand and metal complexes were recorded on a Bruker infrared spectrophotometer in the range of 400–4000 cm−1. The molar conductance of the 10−3 M complex solution in DMF was measured on a HACH conductivity meter. A Bruker 600 MHz spectrometer was used to record the 1H NMR spectra in DMSO d6 solution. Electronic spectra of the metal complexes were obtained with a Shimadzu UV/Vis spectrometer in the range of 200–800, while fluorescence experiments were carried out on a Cary Eclipse spectrofluorometer from 300 to 600 nm. Thermogravimetric analysis TG-DTG experiments were conducted using a NETZSCH STA 449F1 thermal analysis system under air at a flow rate of 30 mL/min and a 10 °C/min heating rate for the temperature range of 25–800 °C, and the data were analyzed by Proteus software. The percentage of the metal ions was calculated thermogravimetrically as metal oxides.
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5

Synthesis of Gold Nanostructures

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Glycine (≥99%), KAuCl4 (98%), Na2B4O7 (≥99.5%), NaOH (≥98%), 1-decanethiol (C10S) (99%), 1-octanethiol (C8S) (≥98.5%), 1,8-octanedithiol (C8S2) (≥97%), 4,4′-bis(mercaptomethyl)biphenyl (BMMBP) (97%), 2-aminoethanethiol (AET) (98%), methanol (99.8%), toluene (99.8%), and hexane (95%) were purchased from Sigma-Aldrich (St. Louis, MO). Au slugs (99.999%) were purchased from Alfa Aesar (Ward Hill, MA). Ethanol (99.99%) was purchased from Gold Shield Chemical (Hayward, CA). Water (≥18.2 MΩ) was generated from a Milli-Q system (Q-GARD 2, Millipore, Billerica, MA) and used for dilution and washing. Nitrogen gas (99.999%) was purchased from Praxair (Danbury, CT). Tungsten wire (99.95%) was purchased from California Fine Wire (Grover Beach, CA). All chemicals and materials were used without further purification.
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6

Substrate Pretreatment and Metal Deposition

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Pretreatment of silicon substrate and metal deposition. The starting substrate was a Si(100) n-type substrate with ρ = 3–5 Ω cm. Prior to plating, each sample was cut into squares of 1.5 × 1.5 cm and degreased in acetone at 60 °C and then placed in an ultrasonic bath for 6 min. This was followed by immersion in DHF (6% HF) for 10 s or 240 s. The substrates were then thoroughly washed with deionized water and blow-dried in air. Gold deposition was carried out by manually soaking each sample in a solution containing 1 mM KAuCl4 (99.995% trace metal, Sigma-Aldrich) and 10% HF (diluted HF, GPR RECTAPUR 40%, VWR) at room temperature, under ambient light conditions and without stirring. Then the samples were rinsed in water to remove all surfactants and products. They received an additional cleaning in acetone and were dried in air.
TEM sample preparation. For plan view, the samples were mechanically thinned from the backside to less than a micrometer. Then they were milled with a Gatan PIPS II device, according to a low-energy procedure. Gentle milling was performed at low temperature (less than −100 °C with LN2 cooling) at a 6° milling angle and with beam energy of 1 keV and current of 30 µA at the beginning and of 0.1 keV and 25 µA for final polishing.
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7

Electrochemical Deposition of Gold

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Au electrochemical deposition solutions were prepared from potassium tetrachloroaurate (KAuCl4, 99.99%, Sigma-Aldrich) with perchloric acid (HClO4, 99.99%, Sigma Aldrich) as a supporting electrolyte in ultra-pure Milli-Q water (18.2 MΩ cm, Millipore Corp., U.S.) at 20 °C. All chemicals were used as received without further purification. Au 3+ deposition solutions contained 1  10 -3 M [AuCl4] -in 0.1 M HClO4 (pH = 1.09) which was deaerated with Argon (Ar) for 20 minutes before electrodeposition to exclude oxygen. Ar flow was maintained over the solution during the experiment.
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