The inductively coupled plasma optical emission spectrometer Agilent 5110 ICP-OES (Agilent, USA) was used in As, B, Ca, K, Mg, Na, P, S, and Si determination. A synchronous vertical dual view (SVDV) of the plasma was accomplished with dichroic spectral combiner (DSC) technology which allows the axial and radial view to be analyzed simultaneously. Common instrumental conditions were applied: radio frequency (RF) power 1.2 kW, nebulizer gas flow 0.7 L min−1, auxiliary gas flow 1.0 L min−1, plasma gas flow 12.0 L min−1, charge coupled device (CCD) temperature − 40 °C, viewing height for radial plasma observation 8 mm, accusation time 5 s, 3 replicates. The content of S for selected samples was checked with a FLASH 2000 analyzer (Thermo Scientific) with FPD detector. Traceability was verified using the standard addition methods, and recoveries at the level of 80–120% were found as satisfactory. General characteristics of fundamental analytical data are present in supplementary data (Table S1 ).
Flash 2000 analyzer
Manufactured by Thermo Fisher Scientific
Sourced in United States
The FLASH 2000 analyzer is a high-performance elemental analyzer designed for the determination of carbon, hydrogen, nitrogen, sulfur, and oxygen in a wide range of organic and inorganic materials. The instrument utilizes the principle of flash combustion to provide rapid and accurate analysis of these elements.
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Lab products found in correlation
Sigma probe, by Thermo Fisher Scientific (2 mentions)
Agilent 5110 icp oes, by Agilent Technologies (1 mentions)
Agilent 5100 icp oes, by Agilent Technologies (1 mentions)
Jem 2100f microscope, by JEOL (1 mentions)
Vnmrs 600 spectrometer, by Agilent Technologies (1 mentions)
Nanonova 230, by Thermo Fisher Scientific (1 mentions)
Spectrum 100, by PerkinElmer (1 mentions)
Atomic force microscope, by Veeco (1 mentions)
Axis hsi, by Shimadzu (1 mentions)
Jem 2100f, by JEOL (1 mentions)
Jem 1010, by JEOL (1 mentions)
Tristar 3000, by Micromeritics (1 mentions)
Hi9835, by Hanna Instruments (1 mentions)
Icap 7000 plus series, by Thermo Fisher Scientific (1 mentions)
Ir prestige 21 spectrometer, by Shimadzu (1 mentions)
Evolution 60 spectrophotometer, by Thermo Fisher Scientific (1 mentions)
Jes fa200 spectrometer, by JEOL (1 mentions)
Drp 110, by Metrohm (1 mentions)
Multimode 8, by Bruker (1 mentions)
Asap 2020, by Micromeritics (1 mentions)
9 protocols using flash 2000 analyzer
1
Elemental Analysis Using ICP-OES
2
Elemental Analysis of Plant Samples
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The inductively coupled plasma optical emission spectrometer Agilent 5100 ICP-OES (Agilent, USA) was also applied for B, calcium (Ca), magnesium (Mg), K, sodium (Na), and Si determination. Additionally, phosphorus (P) and sulfur (S) were analyzed according to Cernusak et al. (2010 (link)) and Melo et al. (2009 (link)). The content of total S was confirmed in selected plant samples with a FLASH 2000 analyzer (Thermo Scientific) with an FPD detector. A synchronous vertical dual view (SVDV) of the plasma was accomplished with dichroic spectral combiner (DSC) technology which allows the axial and radial view to be analyzed simultaneously. The common instrumental conditions were the same as for total As analysis. The wavelengths (nm) were 249.772, 422.673, 766.491, 279.553, 589.592, 253.561, 180.669, and 288.158 for B, Ca, K, Mg, Na, P, S, and Si, respectively.
The detection limits were determined as 3-sigma criteria and were at the level of 0.03, 0.03, 0.03, 0.01, 0.03, 0.03, 0.04, and 0.06 mg kg−1 DW for B, Ca, K, Mg, Na, P, S, and Si, respectively. Traceability was checked using the standard addition methods and recoveries at the level 80–120% were found as acceptable. The characteristics of the results obtained for all six elements are presented in Supplementary data (TablesS1 –S4 ).
The detection limits were determined as 3-sigma criteria and were at the level of 0.03, 0.03, 0.03, 0.01, 0.03, 0.03, 0.04, and 0.06 mg kg−1 DW for B, Ca, K, Mg, Na, P, S, and Si, respectively. Traceability was checked using the standard addition methods and recoveries at the level 80–120% were found as acceptable. The characteristics of the results obtained for all six elements are presented in Supplementary data (Tables
3
Comprehensive Characterization of Novel Material
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Fourier transform infrared (FT-IR) spectra were obtained on a Spectrum 100 (Perkin-Elmer, USA) with a KBr pellet. Magic-angle spinning (MAS) nuclear magnetic resonance (NMR) spectra were measured at room temperature on an Agilent VNMRS 600 spectrometer. The thermogravimetric analysis (TGA) was carried out using a STA 8000 thermal analyzer at a heating rate of 10 °C min−1 under air and nitrogen atmosphere. Powder X-ray diffraction (PXRD) patterns were recorded using a High-Power X-Ray Diffractometer D/MAX 2500 V/PC (Cu-Kα radiation, 40 kV, 200 mA, λ = 1.54056 Å) (Rigaku Inc., Japan). Scanning electron microscope (SEM) measurements with Pt coated samples were obtained by a Field Emission Scanning Electron Microscope Nanonova 230 (FEI Inc., USA). X-ray photoelectron spectroscopy (XPS) was performed on an X-ray Photoelectron Spectrometer K-alpha (Thermo Fisher, UK). Elemental analysis (EA) data was obtained from a Flash 2000 Analyzer (Thermo Scientific Inc., USA). High-resolution transmission electron microscopy (HR-TEM) was conducted using a JEM-2100F microscope (JEOL inc., Japan) at an operating voltage of 200 keV. The samples were prepared by drop casting dispersed ethanol on a holey carbon TEM grid, and drying in an oven at 50 °C under vacuum.
4
Soil Nutrient Composition Analysis
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To determine Carbon/Nitrogen (C/N) ratios, reducing sugar and lipid levels, 200 g samples were dried in a 65 °C oven for 5 days, ground into a fine powder and sent to the Bromatology Laboratory (Ecosur) for analysis. Carbon and nitrogen levels were determined using a Flash 2000 Analyzer (Thermo Fischer Scientific, http://www.thermoscientific.com/ ). Reducing sugars were measured using the 3,5 dinitrosalicylic acid (DNS) method (Miller 1959 (link)), and total lipids were determined according to Williams (1984 ).
5
Multimodal Characterization of Nanomaterials
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TEM images and TEM-EDS images were obtained using a JEOL JEM-1010 and JEM-2100F, respectively. AFM images were obtained using a Veeco atomic force microscope. Raman spectroscopy measurements were carried out on a Dongwoo DM500i Raman spectrometer using green (514.5 nm) laser excitation. BET surface area and BJH pore size distributions were measured by using a Micromeritics Tristar 3000. XPS was carried out using a Kratos AXIS-HSi. Elemental analysis was performed using a Thermo Scientific Flash 2000 analyzer at NCIRF (National Center for Inter-university Research Facilities, Seoul National University, Korea).
6
Comprehensive Soil Characterization Protocol
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Particle size distribution of soil was determined using sieve methods according to [74 ]. Water holding capacity of soil was determined using the gravimetric method, hydraulic conductivity by Darcy’s law, and the soil porosity from the measured values of soil particle and bulk densities calculations [75 ]. Soil electrical conductivity (EC) was measured using HANNA (HI9835) EC meter in 1:2.5 soil/water extract, soil pH (1:2.5 DI water suspension) by Jenway 3505 pH/mV/Temperature Meter and the total carbonate content (expressed as CaCO3) using the gasometric determination following 6.0 M HCl application [76 ]. Water-soluble cations and anions (1:2.5 DI water extract) were determined using standard methods [76 ]: Na+ using a Sherwood, flame photometer (MODEL 360), Ca2+, Mg2+, and K+ using ICP-OES Thermo Scientific™ iCAP™ 7000 Plus Series, CO32− and HCO3− by titration with a standardized H2SO4 solution and Cl− by AgNO3 titration. Total organic elements concentration in soil (C, N, H, and S) was determined using dry combustion method by a Thermo Scientific Flash 2000 analyzer. Available concentrations of PTEs were determined using ICP-OES after extraction by diethylene tri-amine Penta acetic acid (DTPA).
7
Comprehensive Characterization of Metal Complexes
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Chemical analyses of carbon, nitrogen, and hydrogen were carried out in a Thermo Scientific Flash 2000 analyzer.
FT-IR spectra were obtained using KBr in the 4000 to 400 cm−1 region on a Shimadzu IR Prestige 21 spectrometer. UV–visible (UV–vis) spectra of aqueous solutions of the complexes were recorded on a Thermo Scientific Evolution 60 spectrophotometer in a 1 cm-path length quartz cells.
Conductivity measurements of 1 mM aqueous solutions of the complexes were performed in a Jenway Conductivity Meter 4310, at 25 °C.
EPR measurements of aqueous solutions at room temperature were carried out at X-band (9.5 GHz) using a JEOL JES-FA200 spectrometer and a cavity with 100 kHz field modulation. Other experimental parameters were optimized to maximize the signal-to-noise ratio and avoid spectra saturation.
Cyclic voltammetry studies were performed in 1 mM aqueous solutions of the complexes (2 ), (3 ), (4 ), and (5 ) in 0.1 M KCl, in a Dropsens µStat potentiostat (Metrohm) with a disposable carbon electrode (DRP-110, Metrohm). Potassium ferrocyanide was used as internal reference. Voltammograms were obtained at 0.05, 0.10, 0.150, and 200 mV/s to verify reversibility for the Cu(II)/Cu(I) process.
FT-IR spectra were obtained using KBr in the 4000 to 400 cm−1 region on a Shimadzu IR Prestige 21 spectrometer. UV–visible (UV–vis) spectra of aqueous solutions of the complexes were recorded on a Thermo Scientific Evolution 60 spectrophotometer in a 1 cm-path length quartz cells.
Conductivity measurements of 1 mM aqueous solutions of the complexes were performed in a Jenway Conductivity Meter 4310, at 25 °C.
EPR measurements of aqueous solutions at room temperature were carried out at X-band (9.5 GHz) using a JEOL JES-FA200 spectrometer and a cavity with 100 kHz field modulation. Other experimental parameters were optimized to maximize the signal-to-noise ratio and avoid spectra saturation.
Cyclic voltammetry studies were performed in 1 mM aqueous solutions of the complexes (
8
Characterization of 2D Zirconia Nanosheets
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Elemental analysis (C, H, and O) was performed using a FLASH 2000 analyzer (Thermo Fisher Scientific). Before elemental analysis, all samples were dried under vacuum at 323 K for 12 hours. XRD patterns were recorded using a Smartlab x-ray diffractometer (RIGAKU) equipped with a CuKα radiation source (λ = 1.5406 Å, 40 kV, 300 mA). C 1s and O 1s XPS measurements were carried out on a Sigma Probe instrument (Thermo Fisher Scientific VG) equipped with a microfocused monochromator x-ray source. CO2 adsorption isotherms were measured with an ASAP 2020 (Micromeritics) at 273 K. Before the measurement, all samples were degassed under vacuum at 473 K for 12 hours. The pore size distributions were calculated using the NLDFT method. TEM images were taken using a field emission TEM (JEM-2100F HR) operated at 200 kV after mounting the samples on a lacey carbon grid (LC300-Cu). SEM images were collected using an SU8230 (HITACHI) operating at 3 kV without metal coating. Raman spectra were recorded using a LabRAM ARAMIS with an Ar ion laser (514 nm). AFM images were collected in a tapping mode in air using a Multimode 8 (Bruker) equipped with a silicon cantilever and an RTESPA-150 tip. Before AFM investigation, a fresh silicon wafer was coated with a drop of diluted o-2DZTC NMP solution (0.01 mg ml−1) and then dried under vacuum at 298 K for 12 hours.
9
Dye Sorption Analysis of Goldenrod Biomass
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The following laboratory equipment was used in the study:
Laboratory grinder Microfine MF-2 (CONBEST, Kraków, Poland)—(for crushing the goldenrod biomass);
Water bath shaker type 357 (Elpin-Plus, Lubawa, Poland)—(for the modification/activation of goldenrod biomass with epichlorohydrin);
HI 110 pH meter (HANNA Instruments, Olsztyn, Poland)—(for the measurement and correction of the solutions’ pH);
Laboratory shaker SK-71 (JEIO TECH, Daejeon, Korea)—(for the process of sorption);
Multi-Channel Stirrer MS-53M (JEIO TECH, Daejeon, Korea)—for dye sorption analyses;
UV-3100 PC—UV/Visible spectrophotometer (VWR spectrophotometers, VWR International LLC., Mississauga, ON, Canada)—(for determining the concentration of dye in solutions);
FT/IR-4700LE FT-IR Spectrometer with a single reflection ATR attachment (JASCO International, Tokyo, Japan)—(for preparing the sorbent’s FTIR spectra);
FLASH 2000 analyzer (Thermo Scientific, Waltham, MA, USA)—(for elemental analysis, and for the measurement of carbon and nitrogen contents).
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