Size-exclusion liquid chromatography for effective purification of amphiphilic trinuclear gold(I) pyrazolate complex

Jalani, Mohamad Azani; Yuliati, Leny; Lee, Siew Ling; Lintang, Hendrik Oktendy

doi:10.11113/mjfas.v14n1-2.953

Cited by 3 publications

(5 citation statements)

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“…3. Moreover, the variable-temperature SAXS analysis is in good agreement with the DSC results [23] showing a wide liquid crystalline property within room-temperature range (-7.2 to 43 °C). In sharp contrast with our work, gold pyrazolate complexes typically displayed a narrow liquid crystalline property above the roomtemperature (more 25 °C) [12][13].…”

Section: Liquid Crystalline Properties [Au3pz3]c10tegsupporting

confidence: 79%

“…The successful synthesis and purification of [Au3Pz3]C10TEG has been discussed in detail in our previous works [17,23], while its liquid crystalline property was firstly confirmed by using DSC as being reported elsewhere [14,23]. Later, in-depth characterizations using variable-temperature POM and SAXS analysis were also carried out to further study the mesogenic behavior of [Au3Pz3]C10TEG as described in this work.…”

Section: Liquid Crystalline Properties [Au3pz3]c10tegmentioning

confidence: 65%

“…The collected solution was transferred in a flask and evaporated to dryness in order to remove the solvent. The residue was firstly purified by using column gravity chromatography before being further purified by using recycling size exclusion chromatography to give [Au3Pz3]C10TEG as a pale-yellow sticky solid (150.00 mg, 0.03 mmol) as being reported in our previous work [17,23].…”

Section: Synthesis and Purification Of [Au3pz3]c10tegmentioning

confidence: 99%

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Temperature-Dependent X-Ray Studies of Discotic Hexagonal Columnar Mesophases in Trinuclear Gold(I) Pyrazolate Complex

Jalani

Lintang²,

Lee³

et al. 2021

Mal. J. Fund. Appl. Sci.

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Gold(I) pyrazolate complex ([Au3Pz3]C10TEG) has been widely studied due to its interesting liquid crystalline properties by exhibiting the discotic hexagonal columnar arrangement. Generally, the liquid crystalline properties of the gold complex were confirmed based on their differential scanning calorimetry thermogram and polarized optical microscopy (POM) images. However, there is still no in-depth study on the phase transition in liquid crystals of [Au3Pz3]C10TEG especially on its structural change at variable temperature. In this study, the resulting liquid crystalline properties of [Au3Pz3]C10TEG upon being heated and cooled was extensively demonstrated via variable-temperature POM (VT-POM) and small angle X-ray scattering (VT-SAXS). Based on the VT-POM images, it was indicated that [Au3Pz3]C10TEG displayed a fan-shaped texture for typical arrangements of discotic hexagonal columnar of liquid crystals. Moreover, VT-SAXS results was in good agreement with the VT-POM images as it showed that [Au3Pz3]C10TEG might consist of two types of stacking system, which are ordered and disordered hexagonal discotic arrangements. Likewise, VT-SAXS analysis also demonstrated that hexagonal columnar mesophase of [Au3Pz3]C10TEG could be recovered even after the heating and cooling for two cycles.

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Section: Liquid Crystalline Properties [Au3pz3]c10tegsupporting

confidence: 79%

Section: Liquid Crystalline Properties [Au3pz3]c10tegmentioning

confidence: 65%

Section: Synthesis and Purification Of [Au3pz3]c10tegmentioning

confidence: 99%

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Temperature-Dependent X-Ray Studies of Discotic Hexagonal Columnar Mesophases in Trinuclear Gold(I) Pyrazolate Complex

Jalani

Lintang²,

Lee³

et al. 2021

Mal. J. Fund. Appl. Sci.

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“…Gold(I) pyrazolate complex/silica ([Au3Pz3]C10TEG/silica) film composite was firstly synthesized via sol-gel synthesis after the formation of columnar structures consisting of gold(I) pyrazolate complex as the template [16][17][18]. Firstly, a medium comprised of dry ethanol (61.6 mg, 1.25 mmol), deionized water (11.9 mg, 0.70 mmol) and hydrochloric acid (0.30 mg, 2.99 x 10 -3 mmol) was prepared before being added to gold pyrazolate complex (10 mg, 2.49 x 10 -3 mmol).…”

Section: B Experiments and Characterisationmentioning

confidence: 99%

Facile Preparation of Gold Nanoparticles Silica Composite Film Embedded in Anodized Aluminium Oxide-Glass Substrate

Mohamad Azani Abd Khadir Jalani,

Juan Matmin,

Siew Ling Lee

et al. 2024

MJoSHT

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Thin film based on gold nanoparticles or AuNPs is typically used as catalyst in the industrial processes due to their high stability and good reusability. In this work, a thin AuNPs-silica composite film was fabricated firstly from sol-gel method by mixing gold pyrazolate complex to a medium comprised of ethanol, deionized water, and hydrochloric acid followed by addition of tetrabutyl orthosilicate as silica source. Next, 70 microliters of the sol-gel solution were spin-coated on several type of substrates such as glass, anodized aluminium oxide or AAO, and combination of both to yield gold complex-silica composite film. It was found that gold complex-silica composite film fabricated on combination of both AAO-glass substrate gave the best quality based on its surface thickness, layer uniformity and film brittleness. Later, the film was selected and subjected to thermal hydrogen reduction at 210 degrees Celsius for 2 hours to facilitate the formation of gold nanoparticles to give AuNPs-silica in AAO-glass film. Before the heat treatment, the light-brownish colour of the original gold complex-silica in AAO-glass film in daylight will appear as a pinkish red film under UV light, suggesting the interaction between gold atoms and supported by its luminescence spectrum at 692 nm. Upon heat treatment, the resulting AuNPs-silica in AAO-glass film gave a deep-red colour indicating the successful formation of AuNPs. The presence of AuNPs in the film was further confirmed based on the absorption peak at 545 nm, X-ray diffraction pattern at 38.20 degrees for d111 plane in wide-angle region, transmission electron microscopy images showing a small and sphere shape particles as well as its elemental composition in energy dispersive X-ray analysis. Moreover, scanning electron microscope images also suggested that the AAO pores is fully filled with the composite and is in accordance with its surface roughness study via atomic force microscopy analysis.

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“…Recently, mesoporous silica nanomaterials were not only used as a support to control the size of the AuNPs [28], but also to enhance the thermal stability after heat treatment at high temperature [29]. In our previous works, high purity [Au 3 Pz 3 ] C10TEG [30] was used to fabricate [Au 3 Pz 3 ] C10TEG /silica hex for synthesizing AuNPs in the nanocomposites via calcination ([AuNPs] cal /silica hex ) [31] and thermal hydrogen reduction methods ([AuNPs] red /silica hex ) [32]. However, the resulting quality of the mesoporous silica nanomaterials was quite low based on their characteristic diffraction peaks and microscopy images.…”

Section: Introductionmentioning

confidence: 99%

Highly ordered mesoporous silica film nanocomposites containing gold nanoparticles for the catalytic reduction of 4-nitrophenol

Jalani

Yuliati

Lee

et al. 2019

Beilstein J. Nanotechnol.

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We report that transparent mesostructured silica/gold nanocomposite materials with an interpore distance of 4.1 nm, as-synthesized from a templated sol–gel synthesis method using discotic trinuclear gold(I) pyrazolate complex, were successfully utilized for the fabrication of thin film mesoporous silica nanocomposites containing gold nanoparticles. The material exhibited a highly ordered hexagonal structure when subjected to a thermal hydrogen reduction treatment at 210 °C. In contrast, when the material was subjected to calcination as a heat treatment from 190 to 450 °C, the thin film nanocomposites showed an intense d 100 X-ray diffraction peak. Moreover, gold nanoparticles inside the thin film nanocomposites were confirmed by the presence of the d 111 diffraction peak at 2θ = 38.2°, a surface plasmon resonance peak between 500–580 nm, and the spherical shape observed in the transmission electron microscope images, as well as the visual change in color from pink to purple. Interestingly, by simply dipping the material into a reaction solution of 4-nitrophenol at room temperature, the highly ordered structure of the as-fabricated silica/gold nanoparticle thin film composite after thermal hydrogen reduction at 210 °C resulted in an improved catalytic activity for the reduction of 4-nitrophenol to 4-aminophenol compared to the material calcined at 250 °C. Such catalytic activity is due to the presence of gold nanoparticles of smaller size in the silicate channels of the highly ordered mesoporous film nanocomposites.

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Size-exclusion liquid chromatography for effective purification of amphiphilic trinuclear gold(I) pyrazolate complex

Cited by 3 publications

References 0 publications

Temperature-Dependent X-Ray Studies of Discotic Hexagonal Columnar Mesophases in Trinuclear Gold(I) Pyrazolate Complex

Temperature-Dependent X-Ray Studies of Discotic Hexagonal Columnar Mesophases in Trinuclear Gold(I) Pyrazolate Complex

Facile Preparation of Gold Nanoparticles Silica Composite Film Embedded in Anodized Aluminium Oxide-Glass Substrate

Highly ordered mesoporous silica film nanocomposites containing gold nanoparticles for the catalytic reduction of 4-nitrophenol

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