Separation and preconcentration of platinum-group metals from spent autocatalysts solutions using a hetero-polymeric S, N-containing sorbent and determination by high-resolution continuum source graphite furnace atomic absorption spectrometry

•Digestion of spent ceramic-based autocatalysts by two methods: autoclave decomposition in mixture of acids HCl:HNO3 (3:1) and high-temperature melting with K2S2O7.•Use of heterochain polymer S, N-containing sorbent is the optimal way to separate from matrix elements and concentrate Pt, Pd and Rh.•Limits of determination achieved by HR CS GFAAS were 1.1·10−5 wt% for Pt, 6.9·10−5 wt% for Pd, and 8.3·10−5 wt% for Rh.•The combined method for the determination of Pt, Pd and Rh in spent ceramic-based autocatalysts was developed using high resolution electro-thermal atomic absorption spectrometry with a continuum spectrum source (HR CS GFAAS).•The analytes were determined with a relative error less than 5%.

This paper describes the potential of high-resolution continuum source graphite furnace atomic absorption spectrometry for determination of Pt, Pd and Rh after separation and concentration by original in-house developed heterochain polymer S, N-containing sorbent. The methods of sample preparation of spent ceramic-based autocatalysts were considered, two of which were used: autoclave decomposition in mixture of acids HCl:HNO3 (3:1) and high-temperature melting with K2S2O7. Both methods anyway limit the direct determination of analytes by HR CS GFAAS. Using the first method it is an incomplete digestion of spent autocatalysts samples, since the precipitate is Si, and the rhodium metal dissolves with difficulty and partially passes into solution. In contrast to the first method, the second method allow to completely transfer analytes into solution, however, the background signal produced by the chemical composition of the flux, overlaps the analytical zone.It was found, that Pt, Pd and Rh contained in the spent ceramic automotive catalysts could be effectively separated and concentrated by heterochain polymer S, N-containing sorbent, which has high sorption capacity, selectivity and resistant to dilute acids. The chosen HR CS GFAAS analysis conditions enable us to determine Pt, Pd and Rh with good metrological characteristics. The concentrations of Pt, Pd and Rh in two samples of automobile exhaust catalysts were found in range of 0.00015–0.00050; 0.170–0.189; 0.0180–0.0210 wt%, respectively. The relative standard deviation obtained by HR CS GFAAS was not more than 5%. Limits of detection by HR CS GFAAS achieved were 6.2·10−6 wt% for Pt, 1.8·10−6 wt% for Pd, and 3.4·10−6 wt% for Rh. Limits of determination achieved by HR CS GFAAS were 1.1·10−5 wt% for Pt, 6.9·10−5 wt% for Pd, and 8.3·10−5 wt% for Rh.To control the accuracy of PGM in sorption concentrates by HR CS GFAAS method, it was appropriate to conduct an inter-method comparative experiment. The researches on the application of atomic-emission spectroscopy method with inductively coupled plasma as a comparative method were conducted. In addition, the trueness control of the obtained results is confirmed by added-found method.

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