Mercury intrusion porosimetry (MIP, Autopore IV 9520, Micromeritics, Norcross, GA, USA) was utilized to investigate the effect of TNTs addition on the total porosity and pore size distribution of the cement paste with w/c = 0.3. The cubic paste samples (5 × 5 × 5 mm3) subjected to 28 days of hydration were soaked in isopropanol and diethyl ether to stop further hydration. The treated samples were dried in a 40 °C oven for 48 h prior to the measurements. The maximum pressure was up to 33,000 psia, the density of mercury was 13.5335 g/mL, the contact angle was 130°, and the surface tension of mercury was 0.485 N/m.
Autopore 4 9520
Manufactured by Micromeritics
Sourced in United States
The AutoPore IV 9520 is a fully automated mercury intrusion porosimeter designed for the measurement of pore size distribution and porosity in a wide range of materials. It provides high-pressure analysis up to 60,000 psia and can characterize pores ranging from 0.003 to 900 micrometers in diameter. The instrument collects and analyzes data automatically, providing detailed information about the porous structure of the sample.
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Lab products found in correlation
Tga 4000, by PerkinElmer (2 mentions)
S 4300, by Hitachi (1 mentions)
Tensile tester, by Instron (1 mentions)
Fe sem s4300, by Hitachi (1 mentions)
Model 4465, by Instron (1 mentions)
Optima 8000, by PerkinElmer (1 mentions)
S 4800, by Hitachi (1 mentions)
Jec 3000fc, by JEOL (1 mentions)
D2 phaser x ray diffractometer, by Bruker (1 mentions)
Jsm 7900f, by JEOL (1 mentions)
Tga 550, by TA Instruments (1 mentions)
Ta q800, by TA Instruments (1 mentions)
Jsm 6701f, by JEOL (1 mentions)
11 protocols using autopore 4 9520
1
Porous Cement Characteristics by MIP
2
Analyzing Porous Structure and VCM Release
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The relationship between the pore structure and VCM release profiles of CPC/VCM and PMMA/VCM was analyzed and compared. CPC/VCM without implantation was immersed in 20 mL of acetone for 10 min for dehydration, removed, and dried at room temperature; this process was not necessary for PMMA/VCM. Thin sections (1-2 mm thickness) of each test specimen were prepared using a microtome for scanning electron microscopy (SEM) analysis (S-4300, Hitachi High-Technologies) and the analysis of pore size distribution using mercury porosimetry (AutoPore IV9520, Micromeritics, Norcross, GA, USA).
3
Morphology and Mechanical Analysis of Porous HDPE Scaffolds
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The surface morphology of the porous HDPE, HDPE/PEAA, and HDPE/PEAA/Col scaffolds was observed under a field emission scanning electron microscope (FE-SEM S4300; Hitachi, Japan) after sputter-coating with platinum. The chemical bonds and elemental composition were characterized by Fourier transform infrared (FT-IR; Mattson, Galaxy 7020A) spectroscopy and electron spectroscopy for chemical analysis (ESCA; ESCA LAB VIG microtech, Mt 500/1, and so forth, East Grinstead, UK), respectively.
Tensile properties were measured via a universal testing machine (Instron, model 4465) with a Zwick Roell tensile tester equipped with a 1 kgf load cell, at 25 °C with an extension speed of 10 mm/min. The tensile strength and Young’s modulus measure of each sample were calculated from the averages of 10 specimens.
The porosity of the porous scaffolds was determined by using a mercury intrusion porosimeter (AutoPore IV 9520; Micromeritics Co., USA). The advancing and retreating contact angles of mercury were taken to be 140° and the surface tension was taken as 0.480 N/m (480 dynes/cm).
Tensile properties were measured via a universal testing machine (Instron, model 4465) with a Zwick Roell tensile tester equipped with a 1 kgf load cell, at 25 °C with an extension speed of 10 mm/min. The tensile strength and Young’s modulus measure of each sample were calculated from the averages of 10 specimens.
The porosity of the porous scaffolds was determined by using a mercury intrusion porosimeter (AutoPore IV 9520; Micromeritics Co., USA). The advancing and retreating contact angles of mercury were taken to be 140° and the surface tension was taken as 0.480 N/m (480 dynes/cm).
4
Pore Structure Analysis of Concrete
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Divide the parallel sample of unconfined compressive strength test into upper, middle and lower parts. Take 10 g blocks with a size of about 7 mm from the three parts, dry them at a low temperature blast at 40 °C for 24 h, and test the pore structure distribution of the sample with an Auto pore IV 9520(Micromeritics, Norcross, GA, UAS). The test pressure range is 25–3300 psi, and the corresponding hole diameter range is about 340 μm–6.0 nm.
5
Mercury Intrusion Pore Analysis
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The core plugs, which were used for measurement of matrix density using the pycnometer, were also used for the application of the mercury intrusion (MI) method. Each core plug was weighed again prior to the MI method application. In order to make mercury intrusion into the pores of the core plug, we used the equipment of AutoPore IV 9520 (Micromeritics co.) which has two separate pressure ports for the measurement of different pressure intervals: the lower pressure port for 0.10–30 psia and the higher pressure port for 30–60,000 psia. This equipment can provide us with a cumulative record of mercury intrusion volume increasing with ambient pressure rise from 0.10 psia up to 60,000 psia, i.e., a continuous record of mercury increments to intrude the pores decreasing in size from 360 μm down to 0.003 μm, inversely to the increasing pressure. Hence the maximum intrusion volume can be read on the cumulative curve, i.e., it is indicated by the point on the curve with no more increase in mercury intrusion volume even under further increase in pressure.
6
High-Pressure Mercury Intrusion Analysis
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High-pressure mercury intrusion (HPMI) experiments were conducted with a Micromeritics AutoPore IV 9520 system at the Beijing Centre for Physical and Chemical Analysis. The maximum intrusion pressure was 30,000 psia (206.8 MPa), corresponding to a pore throat diameter of 6.6 nm. The experimental process was as follows: samples were loaded into the core chamber and vacuum pumped for 1 h. After mercury had filled the core chamber, measuring valves and balance valves were opened. Then, mercury was injected gradually under an applied pressure to measure the capillary pressure. Once a maximum pressure of 30,000 psia was reached, the pressure started to decrease progressively, and mercury was extruded from the sample. Capillary pressure curves were derived by Micromeritics AutoPore IV 9520 software. The pore size distribution (PSD) was calculated according to the Washburn equation. The laboratory procedure followed Standard GB-T 21650.1-2008.
7
Comprehensive Scaffold Characterization
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The surface morphology and calcium deposition of the scaffolds were observed by FE‐SEM. The mechanical property of the scaffolds was analyzed by a universal testing machine (UTM; Instron‐4464, MA, USA) with 1 N load cell. The porosity of the scaffolds was measured using a mercury intrusion porosimeter (AutoPore IV 9520, Micromeritics, GA, USA). The thermal property of the scaffolds was estimated using a thermogravimetric analyzer (TGA, TGA 4000, Perkin Elmer, MA, USA). Mass and pH changes were measured in 500 µL of PBS solution (pH 7.4) for 70 days to evaluate neutralizing ability of the scaffolds. The elemental mapping was executed using FE‐SEM (S‐4800, Hitachi, Japan) equipped with energy dispersive spectroscopy (EDS). The elemental compositions of scaffolds such as zinc, magnesium, calcium, and phosphorous were measured by inductively coupled plasma‐optical emission spectroscopy (ICP‐OES, Optima 8000, Perkin Elmer, MA, USA). The release of the BMP2 was determined using an ELISA (RHF913CKX, Antigenix America, NY, USA). The release of the ALN and ZO was determined using ICP‐OES.
8
Comprehensive Characterization of BioMOFs
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SEM analysis was performed using a JEOL JSM-7900F field emission SEM. The samples were freeze-dried prior to the analysis; a small fraction of the dried samples were then fixed onto a metallic holder using adhesive carbon tape. The samples were coated by a thin layer of Pt/Pd alloy using a fine auto-coater JEOL JEC-3000FC prior to the SEM imaging. N 2 sorption isotherm was performed at 77 K using a Quadrasorb SI analyzer. The samples were degassed at 423 K for at least 6 h before measurement. The porosity analysis was done by modeling the isotherm data using Bruneuer-Emmett-Teller (BET) model. MIP analysis was conducted with micromeritics AutoPore IV 9520. The XPS spectra of the BioMOFs were obtained by using Thermo Scientific VG ESCALAB 250 Xray photoelectron spectrophotometer (XPS) and analyzed by using XPSPEAK41 software. XRD analysis was conducted using a Bruker D2 Phaser X-ray diffractometer with a CuKα radiation λ = 1.5418 Amstrong. FTIR analysis was performed using a Bio-Rad FTS-3500 GX at wavenumber range from 4000 to 400 cm -1 ; the spectra were collected from 128 scans with a resolution of 4 cm -1 . TG/DTG analysis was conducted using a TA instrument TGA 550 at a temperature range of 30 to 600 • C. The compressive strength of the materials was analyzed by a Universal testing machine (UTM, Testometric M500-25AT/M500-25CT)
9
Characterization of Polymer Separator Films
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Structural identification, thermal properties, and porosity have been detailed in previous reports [26 (link)]. The surface morphology of the fibers was observed using field emission electron microscopy (SEM, JSM-6701F, JEOL, Tokyo, Japan). Thermogravimetric analysis (TGA, TGA 4000, Perkin Elmer, Washington, MA, USA) was used to detect the thermal degradation temperature of the polymer, which was raised from room temperature to 800 °C at 10 °C min−1 under a nitrogen atmosphere. A dynamic mechanical analysis instrument (DMA, TA Q 800, TA Instruments, New Castle, DE, USA) was operated at 1 Hz from 100 °C to 450 °C at 5 °C min−1 in a nitrogen atmosphere. A mercury porosimeter was used to measure the film’s porosity and pore size distribution (AutoPore® IV 9520, Micromeritics, Norcross, GA, USA). A universal tensile machine (Al-7000-S, Gotech testing machines, Inc., Taichung, Taiwan) was used to measure the mechanical properties, and the test plates were cut into 150 mm × 5 mm and tested at a tensile rate of 12.5 mm min−1. The electrolyte absorptivity was measured by immersing the film in the LIB electrolyte for 30 min and calculated according to Equation (1) [27 (link)]:
where W0 is the dry separator and W1 is the soaked one.
where W0 is the dry separator and W1 is the soaked one.
10
Fabric Pore Size Characterization
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The pore sizes and distribution of the above-produced fabrics were measured using a mercury porosimeter, following the Washburn equation (AutoPore IV 9520, Micromeritics, USA). Pressure ranging from 1.38 kPa to 206.8 MPa was applied, and each fabric was equilibrated for 20 s at each pressure.
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