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29 protocols using 1 3 5 benzenetricarboxylic acid

1

Synthesis of Gadolinium-Iron Metal-Organic Frameworks

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Example 27

Two Synthetic Conditions are Possible:

Synthesis 1:

0.028 g (0.5 mmol) of metallic iron powder Fe° (Riedel-de Haën, 99%), 0.225 g of gadolinium(III) nitrate hexahydrate (0.5 mmol, Aldrich, 99.9%) and 0.140 g of 1,3,5-benzenetricarboxylic acid (0.666 mmol, Aldrich, 95%) dispersed in 10 ml of deionized water, the whole left for 24 hours at 180° C. in a 23 ml Teflon body placed in a Paar metallic bomb. The solid is then filtered off and washed with water and then with ethanol.

Synthesis 2:

0.065 g (˜0.5 mmol per 1 iron per trimer) of iron(III) acetate (prepared according to the synthesis described in Example 1), 0.225 g of gadolinium(III) nitrate hexahydrate (0.5 mmol, Aldrich, 99.9%) and 0.140 g of 1,3,5-benzenetricarboxylic acid (0.666 mmol, Aldrich, 95%) dispersed in 10 ml of deionized water (or methanol or ethanol or dimethylformamide), the whole left for 12 hours at 150° C. in a 23 ml Teflon body placed in a Paar metallic bomb. The solid is then filtered off and washed with water and then with ethanol.

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2

Synthesis of Gadolinium-Iron Metal-Organic Frameworks

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Example 27

Two synthetic conditions are possible:

Synthesis 1:

0.028 g (0.5 mmol) of metallic iron powder Fe0 (Riedel-de Haën, 99%), 0.225 g of gadolinium(III) nitrate hexahydrate (0.5 mmol, Aldrich, 99.9%) and 0.140 g of 1,3,5-benzenetricarboxylic acid (0.666 mmol, Aldrich, 95%) dispersed in 10 ml of deionized water, the whole left for 24 hours at 180° C. in a 23 ml Teflon body placed in a Paar metallic bomb. The solid is then filtered off and washed with water and then with ethanol.

Synthesis 2:

0.065 g (˜0.5 mmol per 1 iron per trimer) of iron(III) acetate (prepared according to the synthesis described in Example 1), 0.225 μg of gadolinium(III) nitrate hexahydrate (0.5 mmol, Aldrich, 99.9%) and 0.140 g of 1,3,5-benzenetricarboxylic acid (0.666 mmol, Aldrich, 95%) dispersed in 10 ml of deionized water (or methanol or ethanol or dimethylformamide), the whole left for 12 hours at 150° C. in a 23 ml Teflon body placed in a Paar metallic bomb. The solid is then filtered off and washed with water and then with ethanol.

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3

VEGF-Based Protein Conjugation Protocol

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Human recombinant VEGF165, anti-VEGF165 antibody, N-hydroxysuccinimide (NHS), 1-ethyl-3-(3-dimethylaminopropyl)carbodiimide hydrochloride (EDC), dimethylformamide (DMF) and ethanol (95%) were purchased from Sigma-Aldrich, India. Just to highlight that anti-VEGF antibody and VEGF165 were stored at 4 °C and −20 °C, respectively, before use. Freshly aqueous solutions of EDC and NHS were prepared before using. All solutions were prepared using deionized water (DI) from a Millipore system. Cobaltous chloride, potassium ferricyanide, 1,3,5-benzenetricarboxylic acid (BTC) and GO were purchased from Merck. Sodium dihydrogen orthophosphate dehydrate (Merck) and sodium phosphate dibasic dehydrate (Sigma-Aldrich) were used to prepare a 0.1 M phosphate buffer of different pH to carry out pH study. All chemicals were of analytical grade and used without any further purification.
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4

Synthesis of Metal Complexes

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All used materials including, acetonitrile, Lithium perchlorate, 4-Amino Benzoic acid, Sodium nitrite, Methanol, 1,3,5-benzene tricarboxylic acid, and alcohols were purchased from Merck. Hydrochloric acid, Potassium tetrafluoroborate, Co(NO3)2. 6H2O, Dimethylformamide were purchased from Sigma-Aldrich. All chemicals have been used without further purification.
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5

BTC Synthesis and Characterization

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The chemical reagents used were of analytical grade, and solutions were prepared with twice-distilled water (from here on out, “water”).
To begin, 1,3,5-Benzenetricarboxylic acid (≥95%) (BTC) was supplied by Merck (Darmstadt, Germany). Hydrochloric acid 37% (HCl), hydroquinone and sodium hydroxide (NaOH) were obtained from PanReac Química (Castellar del Vallès, Barcelona, Spain). Acetonitrile, acrolein (≥95.0%, ~0.2% hydroquinone as stabilizer), deuterium oxide (D2O), and 3-(trimethylsilyl)-2,2,3,3-tetradeuteropropionic acid sodium salt (TSP) were purchased from Sigma-Aldrich (St. Louis, MO, USA).
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6

Peanut Shell-derived Adsorbent for Water Purification

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Peanut shells were purchased from a grocery store and used as the raw materials. Sodium hypochlorite solution (6–14%), copper nitrate trihydrate (Cu(NO3)2·3H2O), sulfuric acid (95–98 wt%), 1,3,5-benzene tricarboxylic acid (BTC), N,N'-methylene bisacrylamide (MBA), and other reagents (NaOH, HNO3, CHCl3, EtOH, t-butyl alcohol and Congo Red) were all purchased from Merck. Deionized water (resistivity 18.2 MΩ/cm) was used in all cases. All the chemicals in this study were used as received without any further purification.
FTIR measurements were conducted on Nicolet 6700 Fourier transform infrared spectrometer. Scanning electron microscopy (SEM) measurements were conducted on Hitachi S-4800 instruments operated at 2 kV for gold-sputtered samples. XRD patterns were recorded on a Bruker D8 ADVANCE X-ray diffractometer with a Cu Ka radiation (λ = 1.5418 Å). The powder was leveled on sample holders and scanned with a 2θ angle from 5° to 50° with a step speed of 5°/min. The concentration of the contaminated water was determined using a DU 800 UV–Vis spectrophotometer. The amounts of Mn2+ and Mn7+ were determined by Inductively Coupled Plasma (ICP) analysis on sequential plasma spectrometer, Shimadzu (ICPS-7000).
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7

Synthesis of NENU-5 Nanocrystals

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All chemicals were purchased and used without further purification. In a typical synthesis, 1 mmol of copper (II) acetate monohydrate (Sigma-Aldrich), 0.5 mmol of L-glutamic acid (Sigma-Aldrich) and 0.3 g of phosphomolybdic acid hydrate (Sigma-Aldrich) were dissolved in 40 ml of deionized water and stirred at ambient condition for 20 min. After that, 0.67 mmol of 1,3,5-benzenetricarboxylic acid (Merck) completely dissolved in 40 ml of ethanol was poured into the above solution under continuous stirring. The solution immediately turns turbid due to the rapid formation of NENU-5 nanocrystals. After stirring for 14 h at ambient condition, the green precipitate was collected by centrifugation and washed twice with ethanol. The product was dried at 70 °C overnight for further experiment and characterizations. The size of the NENU-5 particles can be easily tuned by varying the added amount of L-glutamic acid.
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8

Functionalization of Wood Samples

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European beech (Fagus sylvatica), American basswood (Tilia americana), and Norway spruce (Picea abies) wood samples were cut into cuboids with the dimensions 10 × 10 × 5 mm3 (radial × tangential × longitudinal, R × T × L). Tangential cut beech samples with a thickness of 6 mm, a length of 6 cm, and a width of 2 cm were used. Zinc nitrate hexahydrate (Zn(NO3)2·6H20, 98%), copper(II) acetate (Cu(OAc)2, 98%), triethylamine (C3H9N, ≥99%), and sodium chloroacetate (ClCH2COONa, 98%) were purchased from Sigma‐Aldrich. 2‐Methylimidazole (2‐MeIm, C6H6N2, 97%) and sodium hydroxide (NaOH) were supplied by Thermo Fisher GmbH. 1,3,5‐benzenetricarboxylic acid was obtained from EMD Millipore Corporation. Methanol (≥99.9%), ethanol (≥99.8%), and N,N‐dimethyformamide (DMF, ≥99.8%, Sigma‐Aldrich) were used as solvents. All chemicals were used as received.
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9

Lanthanide-based Metal-Organic Framework Synthesis

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Yttrium(III) acetate hydrate and Europium(III) acetate hydrate were purchased from STREM Chemicals, and the 1,3,5-benzenetricarboxylic acid was purchased from Sigma-Aldrich. All the reagents were used without other purifications. Two different sets of syntheses have been performed. Scheme 1 provides a summary of the process.
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10

Synthesis of Metal-Organic Frameworks

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All chemicals and reagents were utilized, without additional purification. Ni(NO3)2·6H2O; 1,3,5-benzenetricarboxylic acid (BTC), terephthalic acid (TPA), 2-aminoterephthalic acid (ATPA), 2,5-dihydroxyterephthalic acid (DHTPA), dimethylformamide (DMF), ethanol, KOH, methanol, acetone, absolute ethanol (99.9%), acetic acid, ethylene glycol, 1-ethyl-3-methylimidazolium tetrafluoroborate, fluorine doped tin oxide (FTO) coated soda-lime glass substrate (SLG), were pursed from Sigma Aldrich, Germany.
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