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26 protocols using multiwave go

1

Microwave-Assisted Elemental Analysis of EVOO and Pomace

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Plastic bottles containing 20 mL of EVOO were centrifuged at 3500 g for 5 min. In order to avoid any disturbance of the pomace precipitated on the bottom of the bottles, EVOO supernatant was carefully removed with a pipette using acid-cleaned tips. Extra virgin olive oil samples were weighed (0.5 g) and digested in a mixture of 5 mL HNO 3 (69% v/v Fluka TraceSELECT ® , Steinheim, Germany) and 1 mL of Milli-Q ® water in a microwave oven (Multiwave GO, Anton Paar, Graz, Austria, maximum power 850 W). A microwave-assisted heating program included 20 min of ramp time and 10 min of hold time at 180 °C.
Ten pomace samples (0.05 g) were digested in a mixture of 5 mL HNO 3 (69% v/v Fluka TraceSELECT ® , Steinheim, Germany) and 2 mL of Milli-Q ® water in a microwave oven (Multiwave GO, Anton Paar, Graz, Austria) with a heating program including 20 min of ramp time and 10 min of hold time at 160 °C. A risk of explosion during oil and pomace digestion limited the mass of sample and necessitated the use of a Multiwave GO microwave that is suitable for highly reactive samples.
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2

Extracting Phycocyanin from Dried Cake

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0.1 g of dried phycocyanin cake was mixed with 10 ml of solvent in a pressure vessel HVT50 (Multiwave GO, Anton Paar GmbH, Graz, Austria). Three vessels were loaded into a microwave digestion system (Multiwave GO, Anton Paar GmbH, Graz, Austria). Each run consisted of a 5 min heating ramp, kept at the target temperature for the desired amount of time and finally cooled down to 40 ºC during 15 min. The reaction was stopped by submerging the flask in an ice bath for 15 min. The reaction mixture was filtered and the resulting deep blue solution was analysed. The dry mater content in the solution determined as described in section 2.2.1.
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3

Microwave-Assisted Wet Digestion Protocol

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One gram of each sample was weighed using laboratory scale balance (ME4002, Mettler Toledo, USA) in a Teflon tube (HVT50, Anton Paar, Austria). Four milliliters of nitric acid (HNO3) at 65% reagent quality (Sigma-Aldrich, Germany) and 2 mL of hydrogen peroxide (H2O2) (Sigma-Aldrich, Germany) were then added. Samples were subjected to a wet microwave digestion process (Multiwave Go, Anton Paar, Austria) (Table 3) [22 (link)]. The digestion process lasted for 1 h. Once the samples had been digested, they were placed in 10-mL volumetric flasks, made up to the mark with Milli-Q quality distilled water, and transferred to hermetic containers for measurement (in triplicate). The proportion was 1:10 (w/v).

Instrumental microwave conditions for wet digestion of samples

NoRamp (min)Temperature (°C)Time (min)
115′00″505′00″
25′00″604′00″
35′00″703′00″
43′00″902′00″
520′00″18010′00″

Microwave processing power, 850 W; limit temperature, 200 °C; cooling temperature, 50 °C

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4

Cannabis Concentrate Pretreatment for Metals Analysis

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Before metals analysis, cannabis
concentrate, flower, cartridge
pieces, filter paper, and dried organic solvent residues were digested
as follows: 0.2 to 0.5 g of sample was added to a vial with 4.0 mL
of concentrated nitric acid, 1.0 mL of hydrochloric acid, and 5.0
mL of water. The organic solvent impinger or tubing rinse samples
that consisted of the residue remaining after solvent removal were
digested with the same amount of acid and water but not weighed. All
digestions are based on the EPA method 305236 and were performed on an Anton Paar Multiwave GO with the following
parameters: a 12 min ramp to 80 °C, 12 min ramp to 130 °C,
12 min ramp to 185 °C, and maintained at 185 °C for 20 min.
After digestion, samples were diluted with RO water to a final acid
concentration of 2% HNO3 and 0.5% HCl, appropriate for ICP-MS analysis.
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5

Elemental Composition Analysis of Catalysts

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The
elemental composition of the catalysts was determined by ICP-OES using
an Agilent 5100 VDV instrument. Typically, 2–3 mg of the sample
was dissolved in 5 mL of aqua regia, followed by microwave digestion
at 175 °C for 30 min (Anton Paar, Multiwave GO). The resulting
solution was cooled down to room temperature and diluted to 25 mL
with deionized water. For the calibration of the instrument, a multielement
standard (multielement standard solution 5, Sigma-Aldrich) was used.
Each measurement was repeated three times, and the average values
are reported in Table S1.
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6

Sewage Sludge Elemental Analysis

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At the beginning and at the end of each experiment, an aliquot of digested sewage sludge was sampled to measure the total and dissolved elements' content. About 5 g of raw sample (total content) or 2 mL of supernatant (dissolved content), recovered after centrifugation at 3.000 g for 20 min, were digested with 6 mL of 69% HNO 3 and 3 mL of 37% HCl in a microwave oven (Multiwave GO, Anton Paar GmbH) at 180°C for 60 min.
Digested samples were further diluted with ultrapure water and analyzed by ICP-MS (Agilent 7700X) except for Fe which was analyzed by MP-AES (Agilent 4210). During the ICP-MS analysis, internal standards were added: 115 In for Al, As, Cd, Co, Cr, Cu, Fe, Mn, Mo, Ni, Se and 209 Bi for Pb. Blanks (i.e. ultrapure water adjusted to 2 % HNO 3 ) were analyzed every 10 samples.
Moreover, quality controls at 5 and 10 µg/L were added to check the performance of the analysis.
The recovery was equal or above 86% for each element among all analyses performed by ICP-MS or MP-AES.
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7

ICP-MS Analysis of Elemental Composition

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ICP-MS by an iCAP RQ (Thermo Scientific) was used to determine
the elemental composition of the samples. Prior to ICP analysis, the
samples were dissolved in a mixture of 6 mL of HCl, 2 mL of H2SO4, and 2 mL of HNO3 and subsequently
digested in a microwave (Multiwave GO, Anton Paar) at 180 °C
for 30 min. For the ICP measurement, the samples were further diluted
with ultrapure water (18.2 MΩ·cm).
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8

TXRF Analysis of Mineralized Samples

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All labware used for TXRF analysis was decontaminated in acid baths for 48 h before use. Freeze-dried samples (approximately 200 mg) were mineralized with HNO3 in Teflon reactors, following a microwave digestion process (Multiwave GO, Anton Paar GmbH., Graz, Austria) according to the EPA 3052 method [29 ]. After cooling, an internal standard (gallium) was added to each sample, and 5 μL of each sample was then applied to a siliconized quartz disk (BrukerNano, Berlin, Germany) and dried. Total reflection X-ray fluorescence spectroscopy was performed in a TXRF S2 PICOFOX (Bruker, Germany). Instrumental recalibration (gain correction, sensitivity analysis, and multi-elemental standards) and analytical blanks were used for quality control. The data were acquired using Spectra PICOFOX Software (version 7.8.20. Bruker, Berlin, Germany).
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9

Determining Sb Accumulation in T. natans

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To determine the Sb accumulation efficiency in different parts of T. natans, leaves, stems and roots were separated. Drying of harvested plant materials was carried out using standard protocol21 (link). The plant materials were digested with a mixture of HNO3 (69%) and H2O2 (30%) in microwave digestion system (Anton Paar Multiwave GO) at 105 °C for 30 min and then cooled for 3 min. Samples were diluted to a final volume of 12.5 mL with deionized water83 (link). The blank and certified reference material (SRM-1573a tomato leaves, NIST standard reference material, USA) were used for quality control. Sb concentrations in the digested samples were measured by ICP-OES (Optima 2100, Perkin Elmer) with detection limit 3 µg/L.
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10

Catalyst Digestion and ICP-MS Analysis

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Catalysts were first digested in a microwave digestion
system (Anton Paar, Multiwave GO) at 180 °C for 20 min in an
acid mixture containing cc. HNO3, cc. H2SO4, cc. HCl in a volume ratio of 2:2:6. Then, the solutions
were filtered and diluted to ca. 50 mL with ultrapure water. For the
ICP-MS measurement, a 20× dilution of each sample in 3% HNO3 was prepared. The measurements were performed with a ThermoScientific
iCAP RQ instrument.
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