An accurate and sensitive analytical strategy for the determination of palladium in aqueous samples: slotted quartz tube flame atomic absorption spectrometry with switchable liquid–liquid microextraction after preconcentration using a Schiff base ligand

  • Merve Fırat
  • Emine Gülhan BakırdereEmail author


This study presents a green analytical method for palladium determination by slotted quartz tube flame atomic absorption spectrometry (SQT-FAAS) following switchable liquid–liquid microextraction (SLLME). Efficient extraction of palladium was facilitated by complexation with a Schiff base ligand, synthesized specifically for this study. A three-stage thorough optimization procedure was carried out to boost the absorbance output of palladium. Complex formation was the first stage, and parameters evaluated included buffer solution pH and amount, concentration of ligand, and mixing period. The amount of switchable solvent and concentration and amount of sodium hydroxide and acid amount were optimized in the second stage. Optimization of sample and fuel flow rates and SQT parameters completed the third stage of optimization, and all optimum parameters were used to determine analytical performance of the method. The method had a broad linear dynamic range, and the calibration plots showed good linearity with R2 values greater than 0.9991. The limits of detection and quantification of the SLLME-SQT-FAAS method were 15 and 50 μg/L, respectively. The precision of the method, expressed as percent relative standard deviation, was below 9.0% for all measurements. Spiked recovery results performed for a palladium electroplating bath solution gave poor results when quantified against aqueous calibration standards. Matrix matching was therefore used to improve recovery results which ranged between 97 and 105% for four different spike concentrations.


Palladium FAAS Switchable liquid–liquid microextraction Slotted quartz tube Schiff base 


Compliance with ethical standards

Conflict of interest

The authors declare that they have no conflict of interest.

Supplementary material

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  1. Afzali, D., Jamshidi, R., Ghaseminezhad, S., & Afzali, Z. (2012). Preconcentration procedure trace amounts of palladium using modified multiwalled carbon nanotubes sorbent prior to flame atomic absorption spectrometry: 1st nano update. Arabian Journal of Chemistry, 5(4), 461–466. Scholar
  2. Ataman, O. Y. (2008). Vapor generation and atom traps: atomic absorption spectrometry at the ng/L level. Spectrochimica Acta Part B: Atomic Spectroscopy, 63(8), 825–834. Scholar
  3. Biparva, P., & Matin, A. A. (2012). Microextraction techniques as a sample preparation step for metal analysis. In Atomic absorption spectroscopy: InTech.Google Scholar
  4. Bodur, S., Erarpat, S., Selali Chormey, D., Büyükpınar, Ç., & Bakırdere, S. (2018). Determination of bismuth in bottled and mineral water samples at trace levels by T-shaped slotted quartz tube-atom trap-flame atomic absorption spectrometry. Analytical Letters, 1–10.
  5. Büyükpınar, Ç., Maltepe, E., Chormey, D. S., San, N., & Bakırdere, S. (2017). Determination of nickel in water and soil samples at trace levels using photochemical vapor generation-batch type ultrasonication assisted gas liquid separator-atomic absorption spectrometry. Microchemical Journal, 132, 167–171. Scholar
  6. Chormey, D. S., Büyükpınar, Ç., Turak, F., Komesli, O. T., & Bakırdere, S. (2017). Simultaneous determination of selected hormones, endocrine disruptor compounds, and pesticides in water medium at trace levels by GC-MS after dispersive liquid-liquid microextraction. [journal article]. Environmental Monitoring and Assessment, 189(6), 277. CrossRefGoogle Scholar
  7. Citak, D., & Tuzen, M. (2015). Ultrasonication ionic liquid-based dispersive liquid–liquid microextraction of palladium in water samples and determination of microsampler system-assisted FAAS. Desalination and Water Treatment, 53(10), 2686–2691. Scholar
  8. de Almeida Bezerra, M., Zezzi Arruda, M. A., & Costa Ferreira, S. L. (2005). Cloud point extraction as a procedure of separation and pre-concentration for metal determination using spectroanalytical techniques: a review. [review]. Applied Spectroscopy Reviews, 40(4), 269–299. CrossRefGoogle Scholar
  9. Erarpat, S., Özzeybek, G., Chormey, D. S., & Bakırdere, S. (2017). Determination of lead at trace levels in mussel and sea water samples using vortex assisted dispersive liquid-liquid microextraction-slotted quartz tube-flame atomic absorption spectrometry. Chemosphere, 189, 180–185. Scholar
  10. Firat, M., Bodur, S., Tisli, B., Ozlu, C., Chormey, D. S., Turak, F., et al. (2018). Vortex-assisted switchable liquid-liquid microextraction for the preconcentration of cadmium in environmental samples prior to its determination with flame atomic absorption spectrometry. Environmental Monitoring and Assessment, 190(7), 393. CrossRefGoogle Scholar
  11. Hasegawa, H., Barua, S., Wakabayashi, T., Mashio, A., Maki, T., Furusho, Y., & Rahman, I. M. M. (2018). Selective recovery of gold, palladium, or platinum from acidic waste solution. Microchemical Journal, 139, 174–180. Scholar
  12. Kasa, N. A., Chormey, D. S., Büyükpınar, Ç., Turak, F., Budak, T. B., & Bakırdere, S. (2017). Determination of cadmium at ultratrace levels by dispersive liquid-liquid microextraction and batch type hydride generation atomic absorption spectrometry. Microchemical Journal, 133, 144–148. Scholar
  13. Kaya, G., & Yaman, M. (2008). Online preconcentration for the determination of lead, cadmium and copper by slotted tube atom trap (STAT)-flame atomic absorption spectrometry. Talanta, 75(4), 1127–1133. Scholar
  14. Kokya, T. A., & Farhadi, K. (2009). Optimization of dispersive liquid–liquid microextraction for the selective determination of trace amounts of palladium by flame atomic absorption spectroscopy. Journal of Hazardous Materials, 169(1), 726–733. Scholar
  15. Łobiński, R., & Marczenko, Z. (1996). Separation and preconcentration. In S. G. Weber (Ed.), Comprehensive Analytical Chemistry (Vol. 30, pp. 17–43): Elsevier.Google Scholar
  16. Memon, Z. M., Yilmaz, E., & Soylak, M. (2017). Switchable solvent based green liquid phase microextraction method for cobalt in tobacco and food samples prior to flame atomic absorption spectrometric determination. Journal of Molecular Liquids, 229, 459–464. Scholar
  17. Nakajima, J., Ohno, M., Chikama, K., Seki, T., & Oguma, K. (2009). Determination of traces of palladium in stream sediment and auto catalyst by FI-ICP-OES using on-line separation and preconcentration with QuadraSil TA. Talanta, 79(4), 1050–1054. Scholar
  18. Panhwar, A. H., Kazi, T. G., Naeemullah, Afridi, H. I., Shah, F., Arain, M. B., et al. (2016). Evaluated the adverse effects of cadmium and aluminum via drinking water to kidney disease patients: application of a novel solid phase microextraction method. Environmental Toxicology and Pharmacology, 43, 242–247, doi:
  19. Pérez-Álvarez, E. P., Garcia, R., Barrulas, P., Dias, C., Cabrita, M. J., & Garde-Cerdán, T. (2019). Classification of wines according to several factors by ICP-MS multi-element analysis. Food Chemistry, 270, 273–280. Scholar
  20. Rojas, F. S., Ojeda, C. B., & Pavón, J. M. C. (2006). Automated on-line separation preconcentration system for palladium determination by graphite furnace atomic absorption spectrometry and its application to palladium determination in environmental and food samples. Talanta, 70(5), 979–983. Scholar
  21. Runge, J., Heringer, O. A., Ribeiro, J. S., & Biazati, L. B. (2019). Multi-element rice grains analysis by ICP OES and classification by processing types. Food Chemistry, 271, 419–424. Scholar
  22. Sakaguchi, R. L., & Powers, J. M. (2012). Restorative materials—metals. In R. L. Sakaguchi, & J. M. Powers (Eds.), Craig’s restorative dental materials (Thirteenth Edition) (pp. 199–251). Saint Louis: Mosby.Google Scholar
  23. Soylak, M., Khan, M., & Yilmaz, E. (2016). Switchable solvent based liquid phase microextraction of uranium in environmental samples: a green approach. Analytical Methods, 8(5), 979–986. CrossRefGoogle Scholar
  24. Tavallali, H., Yazdandoust, S., & Yazdandoust, M. (2010). Cloud point extraction for the preconcentration of silver and palladium in real samples and determination by atomic absorption spectrometry. CLEAN – Soil, Air, Water, 38(3), 242–247. Scholar
  25. Titretir, S., Kendüzler, E., Arslan, Y., Kula, İ., Bakırdere, S., & Ataman, O. Y. (2008). Determination of antimony by using tungsten trap atomic absorption spectrometry. Spectrochimica Acta Part B: Atomic Spectroscopy, 63(8), 875–879. Scholar
  26. Turan, N. B., Chormey, D. S., Büyükpınar, Ç., Engin, G. O., & Bakirdere, S. (2017). Quorum sensing: little talks for an effective bacterial coordination. TrAC Trends in Analytical Chemistry, 91, 1–11. Scholar
  27. Wysocka, I., & Vassileva, E. (2016). Determination of cadmium, copper, mercury, lead and zinc mass fractions in marine sediment by isotope dilution inductively coupled plasma mass spectrometry applied as a reference method. Microchemical Journal, 128, 198–207. Scholar
  28. Xia, L., Wu, Y., & Hu, B. (2007). Hollow-fiber liquid-phase microextraction prior to low-temperature electrothermal vaporization ICP-MS for trace element analysis in environmental and biological samples. Journal of Mass Spectrometry, 42(6), 803–810. Scholar
  29. Yu, H., Ai, X., Xu, K., Zheng, C., & Hou, X. (2016). UV-assisted Fenton digestion of rice for the determination of trace cadmium by hydride generation atomic fluorescence spectrometry. Analyst, 141(4), 1512–1518.CrossRefGoogle Scholar
  30. Yusop, R. M., Unciti-Broceta, A., Johansson, E. M. V., Sánchez-Martín, R. M., & Bradley, M. (2011). Palladium-mediated intracellular chemistry. [Article]. Nature Chemistry, 3, 239–243. Scholar
  31. Zaman, B. T., Bakırdere, E. G., Kasa, N. A., Deniz, S., Sel, S., Chormey, D. S., & Bakırdere, S. (2018). Development of an efficient and sensitive analytical method for the determination of copper at trace levels by slotted quartz tube atomic absorption spectrometry after vortex-assisted dispersive liquid-liquid microextraction in biota and water samples using a novel ligand. [journal article]. Environmental Monitoring and Assessment, 190(7), 437. CrossRefGoogle Scholar
  32. Zhang, N., Shen, K., Yang, X., Li, Z., Zhou, T., Zhang, Y., Sheng, Q., & Zheng, J. (2018). Simultaneous determination of arsenic, cadmium and lead in plant foods by ICP-MS combined with automated focused infrared ashing and cold trap. Food Chemistry, 264, 462–470. Scholar
  33. Zhou, J., Xu, S., Dong, X., Chen, Z., & Zhao, W. (2018). Near-infrared off-on fluorescent probe for fast and selective detection of palladium(II) in living cells. Journal of Photochemistry and Photobiology A: Chemistry, 355, 158–164. Scholar
  34. Zhou, S.-Y., Song, N., Liu, S.-X., Chen, D.-X., Jia, Q., & Yang, Y.-W. (2014). Separation and preconcentration of gold and palladium ions with a carboxylated pillar[5]arene derived sorbent prior to their determination by flow injection FAAS. [journal article]. Microchimica Acta, 181(13), 1551–1556. CrossRefGoogle Scholar

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© Springer Nature Switzerland AG 2019

Authors and Affiliations

  1. 1.Faculty of Art and Science, Chemistry DepartmentYıldız Technical UniversityIstanbulTurkey
  2. 2.Department of Science Education, Faculty of EducationYıldız Technical UniversityIstanbulTurkey

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