Di Luzio Marco

D’Agostino Giancarlo

Ghestem J. P.

Hubau A.

Noireaux J.

Oster C.

Touze S.

English

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12 August 2023ISTITUTO NAZIONALE DI RICERCA METROLOGICARepository IstituzionaleImproving valuable metals recycling: best digestion method for retrieving Technology Critical Elements /Noireaux, J.; Oster, C.; Hubau, A.; Touze, S.; DI LUZIO, Marco; D’Agostino, Giancarlo; Ghestem, J. P.. -(2023).OriginalImproving valuable metals recycling: best digestion method for retrieving TechnologyCritical ElementsPublisher:PublishedDOI:Terms of use:Publisher copyright(Article begins on next page)This article is made available under terms and conditions as specified in the corresponding bibliographicdescription in the repositoryAvailability:This version is available at: 11696/75999 since: 2023-02-22T14:21:37ZImproving valuable metals recycling : best digestion method for retrieving Technology Critical ElementsJ. Noireaux*1, C. Oster1, A. Hubau2, S. Touze2, M. Di Luzio3, G. D’Agostino3, J-P Ghestem2, 1 Department Environment and climate change, LNE, 75015, Paris, France2 , BRGM, 45060 Orléans, France3Unit of Radiochemistry and Spectroscopy, INRIM, Pavia 27100, ItalyINTRODUCTION METROLOGICAL TRACEABILITY FOR CHEMICAL ANALYSISMETROCYCLE EU PROJECT           metrocycle.euINAA INSTRUMENTAL NEUTRON ACTIVATION ANALYSISDIGESTION METHODS FOR ICP-MSWHAT’S NEXT?PRINTED CIRCUIT BOARD (PCB)• Technology Critical Elements (TCE) are at supply risk in the EUand are of high economic importance for the EU shift towardsrenewable energy and Green Deal strategy• Measuring the TCE potential of electrical wastes is a first step inthe development of TCE recycling and knowledge of its fluxesand loss to the environment• One main objective of MetroCycleEU project is to develop acertified reference material (CRM) for TCE in electrical wastes• As a first step, the sample digestion is being optimised for ICP-MS analysis with the help of INAA on a crushed Printed CircuitBoard (PCB) sample• Compare the digestion for all 14 TCE elements• Same study with LED and LiB• Assigment of reference value to the RM, includinghomogeneity determination and uncertaintycalucation• Use of the RM for LA-ICPMS calibration• Use of the RM for XRF calibrationThis project 20IND01 MetroCycleEU has received funding from the EMPIR programmeco-financed by the Participating States and from the European Union’s Horizon 2020 research and innovation programme.National Metrology Institute (NMI)BIPM CCQMTesting laboratorySI UNIT Pure CRM and Matrix CRMSI traceableChemical analysisPrimarymethodsRoutine methodsCRM is a reference material (RM) characterized by a metrologically valid procedure […], accompanied by a RM certificate that provides the value of the specified property, its associated uncertainty, and a statement of metrological traceabilityPressed pellets Stackedsample/StandardsSpectra acquired at different source‐detector distances (200, 100, 60, 20 mm from end‐cap)400 kg of PCB4 Successive steps of shredding and millingCo, Ga, Ge, In, Ta, Nd, Pr, Dy, Gd, La, Au, Pt, Pd, Rh, Li)SI-traceablemethods for TCE analysis in electricalwastesCertifiedreferencematerial3 candidate CRMPCB, LED, LiBInter-laboratorycomparisonICPMS, XRFGuidance for TCE analysisCalcination 600°C Acids/flux MethodA No HNO3+HCl+H2O2 microwave 240°CB NoHF+H2O2+HNO3+HCl and H3BO3microwave 240°CC Yes HNO3+HCl+H2O2 microwave 240°CD YesHF+H2O2+HNO3+HCl and H3BO3microwave 240°CE Yes Na2O2 Alkali fusion0102030405060708090Li Pd La AuMass concentration (mg/kg) A B C D E INAA050100150200250300350Tan.dICP-MS ANALYSISElement XR (ThermoFisher ) ElementIsotope measuredResolutionLi 6, 7 MRPd 104, 105 HRLa 139 HRAu 197 HRTa 181 HR• For Pd, La and Au, all digestions are equivalentwithin uncertainty• For Li, the calcination step is required• For Ta, the digestion requires HF in the acidmixture • La, Au and Ta concentrations obtained with INAA are in agreement with the data from ICP-MSEuropean Winter Conference on Plasma SpectrochemistryLjubljana, Slovenia, January 29th – February 3rd, 2023<200µm Sample ready for chemical analysis

Improving valuable metals recycling: best digestion method for retrieving Technology Critical Elements

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Improving valuable metals recycling: best digestion method for retrieving Technology Critical Elements

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