The texture properties (pore size distribution, BET and pore volume) of the sample were characterized using a ASAP 2020 surface analyzer (Micromeritics ASAP 2020). The crystal phase was identified by an X-ray diffraction analyzer (XRD; Rigaku RINT2000), and the morphology of the samples was discovered by scanning electron microscopy (SEM; ZEISS Merlin) and transmission electron microscopy (TEM; FEI Tecnai G2 F30). X-ray photoelectron spectroscopy (XPS, Thermo Scientific Escalab 250Xi) and diffuse reflectance infrared Fourier transform spectroscopy (FT-IR, BRUKER TENSOR II) spectra were obtained to identify the surface functionalities. Moreover, the ultimate analysis was analyzed by an Elementar instrument (Elementar vario MICRO).
Vario micro
Manufactured by Elementar
Sourced in Germany
The Vario Micro is a compact and fully automated elemental analyzer designed for the determination of carbon, hydrogen, nitrogen, and sulfur in solid and liquid samples. It provides accurate and reliable measurements with high sample throughput.
Automatically generated - may contain errors
Lab products found in correlation
Vertex 70, by Bruker (2 mentions)
Merlin, by Zeiss (1 mentions)
Tecnai g2 f30, by Thermo Fisher Scientific (1 mentions)
Rint 2000, by Rigaku (1 mentions)
Asap 2020, by Micromeritics (1 mentions)
Escalab 250xi, by Bruker (1 mentions)
Delta 5 plus, by Thermo Fisher Scientific (1 mentions)
D8 diffractometer, by Bruker (1 mentions)
Icap 6500, by Thermo Fisher Scientific (1 mentions)
Nova 3200e, by Anton Paar (1 mentions)
S 4800, by Hitachi (1 mentions)
Ft ir 4100, by Jasco (1 mentions)
Tecnai g2 s twin, by Thermo Fisher Scientific (1 mentions)
Zetasizer nano zs90, by Malvern Panalytical (1 mentions)
Jsm 6700f, by JEOL (1 mentions)
Ifs 66v s spectrometer, by Bruker (1 mentions)
13 protocols using vario micro
1
Comprehensive Characterization of Material
2
Elemental Analysis of Organic Samples
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Elemental analysis was performed on Elementar Vario MICRO (Elementar Analysensysteme GmbH, Frankfurt, Germany). The instrument hardware was configured for the analysis of 4 elements (C, H, N and S). An amount of 1.2 ± 0.2 mg of sample material was loaded into a tin foil crucible and combusted at 1150 °C with oxygen dosing time of 80 s and total O2 flow rate of 30 mL/min. Ultra-high purity grade helium (BOC, 99.999%) and oxygen (BOC, 99.995%) were employed as working fluids in all cases. Pure sulfanilamide was employed as a standard with quality control samples added into the workflow every 10–20 runs. The follow-up data analysis was performed using a custom peak picking and integration algorithm written in Python 3.11.
3
Biochar Characterization via Advanced Analytics
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The biochar samples’ content of carbon (C), hydrogen (H), nitrogen (N) and oxygen (O) were analyzed in triplicate with an elemental analyzer (Vario MICRO, Elementar, Germany). The Brunauer–Emmett–Teller surface area (SBET), total pore volume (Vtot), and pore size distribution of the biochar samples were analyzed in triplicate using N2 adsorption at 77 K with an Autosorb-IQC gas analyzer (Quantachrome, USA). Functional groups in the biochar samples were determined using Fourier transform infrared (FTIR) spectrometry (VERTEX 70, BRUKER, Germany).
4
Isotopic Analysis of Milk Proteins
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Total 15 N and 2 H enrichments Milk proteins and gastrointestinal samples were freeze-dried prior to analysis. Nitrogen percentage and 15 N enrichment in protein isolate, digestive samples and meal were determined using an isotopic ratio mass spectrometer (IRMS; Isoprime, GV Instrument, Manchester, UK) coupled with an elemental analyser (EA; Vario Micro, Elementar, Lyon, France).
Hydrogen percentage and 2 H enrichment in milk protein isolate, digestive samples and meal were determined using a high temperature conversion elemental analyser (ThermoFisher Scientific) coupled to IRMS (Delta V Plus, ThermoFisher Scientific).
Hydrogen percentage and 2 H enrichment in milk protein isolate, digestive samples and meal were determined using a high temperature conversion elemental analyser (ThermoFisher Scientific) coupled to IRMS (Delta V Plus, ThermoFisher Scientific).
5
Biochar Characterization via Elemental, Surface, and Functional Analysis
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Elemental (C, H, O and N) analysis was conducted using an elemental analyzer (Vario MICRO, Elementar, Germany). The Brunauer–Emmett–Teller surface area (SBET) and pore structure parameters of the biochar samples were obtained using an Autosorb-IQC gas analyzer (Quantachrome, USA) with N2 physical adsorption at 77 K. Fourier transform infrared (FTIR) spectroscopy (VERTEX 70, BRUKER, Germany) was used to identify functional groups on the biochar surfaces.
6
Radiocarbon Dating of Cytochrome b Sequences
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The age of 22 samples from which we successfully obtained whole cytb sequences was determined by radiocarbon dating. It was performed with the accelerator mass spectrometry method (AMS) at Gliwice Absolute Dating Methods Centre (GADAM). The collagen extraction from bones was performed according to the modified Longin’s protocol37 ,38 (link). The bone samples were cleaned in an ultrasonic bath in demineralized water, then dried and ground in a ball mill. The powdered bone was treated with 0.5 M hydrochloric acid to decompose the mineral fraction. Afterwards the residue was rinsed to neutral pH, acidified and kept in 80 °C for 12 hours in an acidic solution (pH = 3). The obtained supernatant was centrifuged, filtered, put in a glass vial and dried in an oven at 75 °C. The subsample of collagen was subjected to graphite preparation with an AGE-3 system equipped with VarioMicro (Elementar) elemental analyser and automated graphitization unit39 (link),40 (link). The 14C concentrations in graphite produced from our samples, Oxalic Acid II standards and coal blanks were measured in DirectAMS laboratory, Bothell, USA41 (link),42 (link). Radiocarbon dates were calibrated using the OxCal v. 4.2 software43 (link) and IntCal13 calibration curve44 (link). Hereafter the ages are provided as cal BP, i.e. calibrated age in years before AD 1950.
7
Quantifying Radioactive Carbon Levels
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[14C]levels were quantified as described previously.32 In brief, the tin foil cups were combusted on an elemental analyzer (Vario Micro; Elementar, Langenselbold, Germany). Generated carbon dioxide (CO2) was transferred to a home‐built gas interface, composed of a zeolite trap and syringe.32 CO2 was adsorbed to the trap on the interface; and after heating of the trap, the CO2 was transferred to a vacuum syringe using helium. A final CO2/helium mixture of 6% was directed to the AMS ion source, at a pressure of 1 bar and a flow of 60 µL/minute. A 1‐MV Tandetron AMS (High Voltage Engineering Europe B.V., Amersfoort, The Netherlands)33 was used. To determine the true amount of radioactivity in each fraction, the measured [14C]/[12C] ratios were multiplied by the corresponding total carbon measurement of the elemental analyzer.
8
Single-Crystal Structure Determination
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All chemicals and solvents were of
A.R. grade and HPLC grade and were used without further purification.
Single-crystal diffraction data were collected at 295 K on an Agilent
Xcalibur Eos diffractometer with graphite monochromatized Mo-Kα
(λ = 0.71073 Å) radiation in ω-scan mode. Elemental
analyses were carried out on a Vario MICRO from Elementar Analysensysteme
GmbH. Powder X-ray diffraction (PXRD) patterns were collected at 293
K on a Bruker D8 diffractometer (Cu Kα, λ = 1.54059 Å).
A.R. grade and HPLC grade and were used without further purification.
Single-crystal diffraction data were collected at 295 K on an Agilent
Xcalibur Eos diffractometer with graphite monochromatized Mo-Kα
(λ = 0.71073 Å) radiation in ω-scan mode. Elemental
analyses were carried out on a Vario MICRO from Elementar Analysensysteme
GmbH. Powder X-ray diffraction (PXRD) patterns were collected at 293
K on a Bruker D8 diffractometer (Cu Kα, λ = 1.54059 Å).
9
Purification and Characterization of Biochar-Derived Fulvic Acid
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BFA used in the experiments was supplied by a certain company in China, the content of C, H, O, N, S and ash was 46.32%, 3.26%, 45.12%, 1.26%, 3.58%, 0.46% using Elementar Analysensysteme GmbH (vario MICRO, ELEMENTAR, Hanau, Hessen, GER), and the micropollutant of Cu, Pb, Cr was not detected using ICP-AES (iCAP6500, Thermo, Waltham, MA, USA). The raw material fulvic acid needed to be further purified before the experiment began, due to some insoluble impurities, soluble amino acids, carbohydrates, etc. All other chemicals used in the experiments were of analytical purity and used without any further purification.
The acid-insoluble humin and humic acid were removed by base-dissolving acidification method. The water-soluble impurities, such as amino acids and polysaccharides, were removed by ethanol. BFA content was determined by potassium dichromic oxidation, as well as the COOH groups of it measured by calcium acetate method.
The acid-insoluble humin and humic acid were removed by base-dissolving acidification method. The water-soluble impurities, such as amino acids and polysaccharides, were removed by ethanol. BFA content was determined by potassium dichromic oxidation, as well as the COOH groups of it measured by calcium acetate method.
10
Comprehensive Microplastics Characterization
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The prepared microplastics were characterized by attenuated total reflectance (ATR)-Fourier transform spectroscopy (FTIR) (FT/ IR-4100 Jasco Inc., Tokyo, Japan), scanning electron photomicrography (SEM) (S-4800 Hitachi, Tokyo, Japan), N 2 -BET methods using a surface area and porosimetry analyzer (Nova 3200e, Quantachrome Instruments, Boynton Beach, FL) for identification of the component polymers, surface micro-morphology, specific surface area and pore volume of the particles, respectively. The carbon contents of the microplastic particles were analyzed using an elemental analyzer (Vario Micro, Elementar Analysensysteme GmbH, Lagenselbold, Germany). The point of zero charge (PZC) was measured using potentiometric titration (ZDJ-4A, Inesa Instruments, Shanghai, China).
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