Dispersive Solid–Liquid Microextraction Based on the Poly(HDDA)/Graphene Sorbent Followed by ICP-MS for the Determination of Rare Earth Elements in Coal Fly Ash Leachate
Authors
Slavković-Beškoski, LatinkaIgnjatović, Ljubiša
Bolognesi, Guido
Maksin, Danijela
Savić, Aleksandra
Vladisavljević, Goran
Onjia, Antonije
Article (Published version)
Metadata
Show full item recordAbstract
A dispersive solid-phase microextraction (DSPME) sorbent consisting of poly(1,6-hexanedi-ol diacrylate)-based polymer microspheres, with embedded graphene microparticles (poly(HDDA)/g-raphene), was synthesized by microfluidic emulsification/photopolymerization and characterized by optical microscopy and X-ray fluorescence spectrometry. This sorbent was applied for simple, fast, and sensitive vortex-assisted DSPME of rare earth elements (RREs) in coal fly ash (CFA) leachate, prior to their quantification by inductively coupled plasma mass spectrometry (ICP-MS). Among nine DSPME variables, the Plackett–Burman screening design (PBD), followed by the central composite optimization design (CCD) using the Derringer desirability function (D), identified the eluent type as the most influencing DSPME variable. The optimum conditions with maximum D (0.65) for the chelating agent di-(2-ethylhexyl) phosphoric acid (D2EHPA) amount, the sorbent amount, the eluting solvent, the extraction temperature..., the centrifuge speed, the vortexing time, the elution time, the centrifugation time, and pH, were set to 60 µL, 30 mg, 2 M HNO3, 25◦ C, 6000 rpm, 1 min, 1 min, 5 min, and 4.2, respectively. Analytical validation of the DSPME method for 16 REEs (Sc, Y, La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu) in CFA leachate samples estimated the detection limits at the low ppt level, the recovery range 43–112%, and relative standard deviation within ± 22%. This method was applied to a water extraction procedure (EP) and acetic acid toxicity characteristic leaching procedure (TCLP) for leachate of CFA, from five different coal-fired thermoelectric power plants. The most abundant REEs in leachate (20 ÷ 1 solid-to-liquid ratio) are Ce, Y, and La, which were found in the range of 22–194 ng/L, 35–105 ng/L, 48–95 ng/L, and 9.6–51 µg/L, 7.3–22 µg/L, 2.4–17 µg/L, for EP and TCLP leachate, respectively. The least present REE in TCLP leachate was Lu (42–125 ng/L), which was not detected in EP leachate.
Keywords:
alkali-acid leaching / coal-fired power plant / Derringer desirability / DSPME / Plackett–Burman / REEsSource:
Metals, 2022, 12, 5-Publisher:
- MDPI
Funding / projects:
- This research was supported by the Science Fund of the Republic of Serbia (Grant No. 7743343 SIW4SE).
DOI: 10.3390/met12050791
ISSN: 2075-4701
WoS: 00080265110000
Scopus: 2-s2.0-85129429603
Institution/Community
Tehnološko-metalurški fakultetTY - JOUR AU - Slavković-Beškoski, Latinka AU - Ignjatović, Ljubiša AU - Bolognesi, Guido AU - Maksin, Danijela AU - Savić, Aleksandra AU - Vladisavljević, Goran AU - Onjia, Antonije PY - 2022 UR - http://TechnoRep.tmf.bg.ac.rs/handle/123456789/5131 AB - A dispersive solid-phase microextraction (DSPME) sorbent consisting of poly(1,6-hexanedi-ol diacrylate)-based polymer microspheres, with embedded graphene microparticles (poly(HDDA)/g-raphene), was synthesized by microfluidic emulsification/photopolymerization and characterized by optical microscopy and X-ray fluorescence spectrometry. This sorbent was applied for simple, fast, and sensitive vortex-assisted DSPME of rare earth elements (RREs) in coal fly ash (CFA) leachate, prior to their quantification by inductively coupled plasma mass spectrometry (ICP-MS). Among nine DSPME variables, the Plackett–Burman screening design (PBD), followed by the central composite optimization design (CCD) using the Derringer desirability function (D), identified the eluent type as the most influencing DSPME variable. The optimum conditions with maximum D (0.65) for the chelating agent di-(2-ethylhexyl) phosphoric acid (D2EHPA) amount, the sorbent amount, the eluting solvent, the extraction temperature, the centrifuge speed, the vortexing time, the elution time, the centrifugation time, and pH, were set to 60 µL, 30 mg, 2 M HNO3, 25◦ C, 6000 rpm, 1 min, 1 min, 5 min, and 4.2, respectively. Analytical validation of the DSPME method for 16 REEs (Sc, Y, La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu) in CFA leachate samples estimated the detection limits at the low ppt level, the recovery range 43–112%, and relative standard deviation within ± 22%. This method was applied to a water extraction procedure (EP) and acetic acid toxicity characteristic leaching procedure (TCLP) for leachate of CFA, from five different coal-fired thermoelectric power plants. The most abundant REEs in leachate (20 ÷ 1 solid-to-liquid ratio) are Ce, Y, and La, which were found in the range of 22–194 ng/L, 35–105 ng/L, 48–95 ng/L, and 9.6–51 µg/L, 7.3–22 µg/L, 2.4–17 µg/L, for EP and TCLP leachate, respectively. The least present REE in TCLP leachate was Lu (42–125 ng/L), which was not detected in EP leachate. PB - MDPI T2 - Metals T1 - Dispersive Solid–Liquid Microextraction Based on the Poly(HDDA)/Graphene Sorbent Followed by ICP-MS for the Determination of Rare Earth Elements in Coal Fly Ash Leachate SP - 5 SP - 791 VL - 12 DO - 10.3390/met12050791 ER -
@article{ author = "Slavković-Beškoski, Latinka and Ignjatović, Ljubiša and Bolognesi, Guido and Maksin, Danijela and Savić, Aleksandra and Vladisavljević, Goran and Onjia, Antonije", year = "2022", abstract = "A dispersive solid-phase microextraction (DSPME) sorbent consisting of poly(1,6-hexanedi-ol diacrylate)-based polymer microspheres, with embedded graphene microparticles (poly(HDDA)/g-raphene), was synthesized by microfluidic emulsification/photopolymerization and characterized by optical microscopy and X-ray fluorescence spectrometry. This sorbent was applied for simple, fast, and sensitive vortex-assisted DSPME of rare earth elements (RREs) in coal fly ash (CFA) leachate, prior to their quantification by inductively coupled plasma mass spectrometry (ICP-MS). Among nine DSPME variables, the Plackett–Burman screening design (PBD), followed by the central composite optimization design (CCD) using the Derringer desirability function (D), identified the eluent type as the most influencing DSPME variable. The optimum conditions with maximum D (0.65) for the chelating agent di-(2-ethylhexyl) phosphoric acid (D2EHPA) amount, the sorbent amount, the eluting solvent, the extraction temperature, the centrifuge speed, the vortexing time, the elution time, the centrifugation time, and pH, were set to 60 µL, 30 mg, 2 M HNO3, 25◦ C, 6000 rpm, 1 min, 1 min, 5 min, and 4.2, respectively. Analytical validation of the DSPME method for 16 REEs (Sc, Y, La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu) in CFA leachate samples estimated the detection limits at the low ppt level, the recovery range 43–112%, and relative standard deviation within ± 22%. This method was applied to a water extraction procedure (EP) and acetic acid toxicity characteristic leaching procedure (TCLP) for leachate of CFA, from five different coal-fired thermoelectric power plants. The most abundant REEs in leachate (20 ÷ 1 solid-to-liquid ratio) are Ce, Y, and La, which were found in the range of 22–194 ng/L, 35–105 ng/L, 48–95 ng/L, and 9.6–51 µg/L, 7.3–22 µg/L, 2.4–17 µg/L, for EP and TCLP leachate, respectively. The least present REE in TCLP leachate was Lu (42–125 ng/L), which was not detected in EP leachate.", publisher = "MDPI", journal = "Metals", title = "Dispersive Solid–Liquid Microextraction Based on the Poly(HDDA)/Graphene Sorbent Followed by ICP-MS for the Determination of Rare Earth Elements in Coal Fly Ash Leachate", pages = "5-791", volume = "12", doi = "10.3390/met12050791" }
Slavković-Beškoski, L., Ignjatović, L., Bolognesi, G., Maksin, D., Savić, A., Vladisavljević, G.,& Onjia, A.. (2022). Dispersive Solid–Liquid Microextraction Based on the Poly(HDDA)/Graphene Sorbent Followed by ICP-MS for the Determination of Rare Earth Elements in Coal Fly Ash Leachate. in Metals MDPI., 12, 5. https://doi.org/10.3390/met12050791
Slavković-Beškoski L, Ignjatović L, Bolognesi G, Maksin D, Savić A, Vladisavljević G, Onjia A. Dispersive Solid–Liquid Microextraction Based on the Poly(HDDA)/Graphene Sorbent Followed by ICP-MS for the Determination of Rare Earth Elements in Coal Fly Ash Leachate. in Metals. 2022;12:5. doi:10.3390/met12050791 .
Slavković-Beškoski, Latinka, Ignjatović, Ljubiša, Bolognesi, Guido, Maksin, Danijela, Savić, Aleksandra, Vladisavljević, Goran, Onjia, Antonije, "Dispersive Solid–Liquid Microextraction Based on the Poly(HDDA)/Graphene Sorbent Followed by ICP-MS for the Determination of Rare Earth Elements in Coal Fly Ash Leachate" in Metals, 12 (2022):5, https://doi.org/10.3390/met12050791 . .