Search results for "Microwave digestion"

To incinerate or not? - Effects of incineration on the concentrations of heavy metals and leaching efficiency of post-precipitated sewage sludge (RAV…

2020

The major element and heavy metal concentrations of post-precipitated sewage sludge (PPS) and its ash residue (PPA) were determined using microwave digestion followed by inductively coupled plasma optical emission spectrometry (ICP-OES) and mass spectrometry (ICP-MS). To the best of our knowledge, this has not been previously done. In both PPS and PPA the heavy metal concentrations were clearly below the average concentrations than those encountered in sewage sludge in Europe. The leaching efficiency of the metal (Al/ Fe) used as a precipitation agent from post-precipitated sludge and its ash residue with phosphoric acid was also investigated with previously optimized leaching conditions. T…

The determination of trace element concentrations in fly ash samples using ultrasound-assisted digestion followed with inductively coupled plasma opt…

2009

Abstract A method of ultrasound-assisted digestion followed by inductively coupled plasma optical emission spectrometry (ICP-OES) used for the determination of trace element (chromium, copper, lead, nickel, vanadium and zinc) concentrations in fly ash samples was developed. All the measurements were performed in robust plasma conditions. Ultrasound-assisted digestion procedures using digestion solutions of aqua regia and hydrofluoric acid (HF) resulted in recovery rates of over 80% for all the analyte elements. Ultrasound-assisted two-step digestion with digestion solutions of 6 mL of HNO3 (Step 1) and 3 mL of HNO3 + 3 mL of HF (Step 2) resulted in recovery rates of over 92% for all the ana…

Optimization of selenium determination in human milk and whole blood by flow injection hydride atomic absorption spectrometry.

1998

abstract A flow injection hydride atomic absorption spectrometry (FI-HAAS) method was developed for determining selenium in human milk and whole blood after microwave digestion of the sample. The sample (2 mL human milk or 0.25 mL blood) was introduced into the microwave vessel with 1.5 mL HN03 and 0.25 mL H202 and 300 W (4 min) and 600 W (4 min) were applied. The digestion was completed by heating to 140 C (2-3 h). Se (VI) was reduced to Se (IV) with hydrochloric acid. The instrumental conditions for FI-HAAS (concentrations of reducing agent and carrier acid, flow rate of argon carrier gas, and sample volume injected) were optimized. The detection limit of the proposed method was 0.23 ng/m…

Determination of mineral and trace element concentrations in pine needles by ICP-OES: evaluation of different sample pre-treatment methods

2008

In the present study, the determination of mineral and trace elements (Al, B, Ca, Cu, Fe, K, Mg, Mn, Na, P and Zn) from pine needles using three sample pre-treatment methods followed by inductively coupled plasma optical emission spectrometry, was examined. Sample pre-treatment methods tested were microwave digestion, ultrasound-assisted digestion and dry ashing. The new ultrasound-assisted digestion method was optimised by the analysis of the standard reference material (SRM) 1575a (pine needles) sample. The speed of dry ashing method was significantly increased by ultrasound dissolution after ashing. All the ICP-OES measurements were performed in robust plasma conditions which were tested…

Procedures of Separation and Pre‐concentration for Molybdenum Determination Using Atomic Spectrometry—a Review

2004

Abstract The literature concerning the improvement of atomic and ionic procedures for molybdenum determination through separation and pre‐concentration were updated. Analytical procedures based on flame atomic absorption spectrometry (AAAS), electrothermal or graphite furnace atomic absorption spectrometry (GFAAS), inductively coupled plasma optical emission spectrometry (ICP‐OES), and inductively coupled plasma mass spectrometry were reviewed taking into consideration the preliminary steps, which can enhance the selectivity and sensitivity based on co‐precipitation, solvent extraction, and solid‐phase extraction. Both in‐batch and on‐line procedures were considered.

An ultrasound-assisted digestion method for the determination of toxic element concentrations in ash samples by inductively coupled plasma optical em…

2007

Abstract A method of ultrasound-assisted digestion followed by inductively coupled plasma optical emission spectrometry (ICP-OES) used for the determination of toxic element concentrations (arsenic, barium, cobalt, copper, lead, nickel, strontium, vanadium and zinc) in ash samples was developed. All the measurements were performed in robust plasma conditions which were tested by measuring the Mg(II) 280.270 nm/Mg(I) 285.213 nm line intensity ratios. The highest line intensity ratios were observed when a nebulizer gas flow of 0.6 L min−1, auxiliary gas flow of 0.2 L min−1 and plasma power of 1400 W were used for radially viewed plasma. The analysis of SRM 1633b showed that the ultrasound-ass…

Determination of chromium in foods by flame atomic absorption and inductively coupled plasma spectrometry

1989

Copper, iron and zinc determinations in human milk using FAAS with microwave digestion

2000

Abstract A method for determining copper, iron and zinc in human milk was optimized and validated. It includes microwave mineralization of the sample and measuring the elements by flame atomic absorption spectroscopy (FAAS). Only 2 ml of milk is needed, and the method is free of matrix interferences. The values obtained for the detection limits (0.07; 0.07; 0.11 μg/ml milk, for copper, iron and zinc) precision of the method, intra-assay (2.9; 5.2; 6.1%RSD for copper, iron and zinc) and accuracy, evaluated using recovery assays (98.8; 100.4; 95.9% for copper, iron and zinc) show that the method is useful for the purpose mentioned. Moreover, the method is rapid and simple, and the determinati…

Determination of mercury in dry-fish samples by microwave digestion and flow injection analysis system cold vapor atomic absorption spectrometry

1997

Abstract Flow injection analysis system cold vapor atomic absorption spectrometry (FIAS-CV-AAS) preceded by a wet digestion in a microwave oven, as a method for measuring mercury in fish was studied. The digestion process and conditions of the FIAS (carrier concentration: HCl 3% v v ; reducing agent: SnCl2 2% w v : filling and injection times: 8 and 25 min, respectively; and sample volumes) were optimized. The analytical parameters of the proposed method (detection limit = 7.7 ng/g; precision intraassay = 6.7%; interassay = 14.0%) demonstrates its adequacy and are similar to the ones (detection limit = 19.4 ng/g; precision intraassay = 11.2%; interassay = 15.9%) obtained using a conventiona…

Multi-element trace determinations in pure alkaline earth fluoride powders by high-resolution ICP-MS using wet-chemical sample preparation and laser …

2003

Four alternative analytical procedures for the determination of ten important trace impurities (Mg, Cr, Fe, Cu, Zn, Sr, Zr, Cd, Ba, and Pb) in pure alkaline earth fluoride powders were applied using high-resolution inductively coupled plasma mass spectrometry (ICP-MS). Two procedures are based on a wet-chemical microwave digestion with boric acid and quantification by the standard addition technique and isotope dilution mass spectrometry (IDMS), respectively. In addition, analyses are also performed by laser ablation as a direct solid sampling technique applying matrix-matched external calibration as well as isotope dilution of the powdered sample. For most elements good agreement between t…