Black Mass

APPLICATION NOTE

SUMMARY

The application note summarizes the digestion of large sample sizes of active material concentrate, NMC cathode material and shredded lithium-ion batteries using ColdBlock Digestion Pro Series Technology.

Instrument:	ColdBlock CBL sample digester, chiller, ICP-OES
Published:	October 2024
Digestion Time:	25 Minutes
Acid Used:	Reverse Aqua Regia
Average ColdBlock Recovery vs. CRM:	100% Cobalt 100% Lithium 99% Nickel

METHODOLOGY

Chiller temperature was set to -5°C
0.20g of each sample was weighed and placed into a ColdBlock Digestion vessel
45mL HNO₃ was slowly added (5mL at a time)
Wait 5 minutes
10mL of 5%v/v antifoaming solution was added
15mL of HCl was slowly added (3mL at a time)
Sample was digested at 60% power for 10 minutes
Pause digestion for 5 minutes (optional step: if sample is rising up the tube, add more anti-foaming solution)
Digest again at 60% power for an additional 10 minutes
Samples were cooled and bulked to 100 mL using 2% HNO3 v/v

DISCUSSION

Black mass can be very reactive, use caution when adding acid
If sample continues to rise up the test tube after adding additional anti-foaming solution, consider decreasing the sample size
After the digestion is complete, samples will most likely be black
Prior to analysis, samples were allowed to settle Filtering is also an option.

Active Material Concentrates after bulk-up to 100mL

Results

Active Material Concentrate A
Analyte	Digestion/ Fusion Results (%)	ColdBlock 1 (%)	ColdBlock 2 (%)	Average	St. Dev	% RSD	% Recovery
Co	2.67	2.73	2.79	2.76	0.0424	1.5	103
Li	7.04	7.29	7.29	7.29	0.0003	0.004	104
Mn	0.003	0.003	0.003	0.003	0.0001	2.3	102
Ni	57	56	57	57	0.30	0.5	99

Active Material Concentrate B
Analyte	Digestion/ Fusion Results (%)	ColdBlock 1 (%)	ColdBlock 2 (%)	Average	St. Dev	% RSD	% Recovery
Co	13.6	13.5	13.1	13.3	0.283	2.1	98
Li	3.60	3.62	3.56	3.59	0.0424	1.2	100
Mn	6.21	6.32	6.35	6.34	0.0212	0.3	102
Ni	11.4	11.6	11.4	11.5	0.14	1.2	101

NMC Cathode
Analyte	Digestion/ Fusion Results (%)	ColdBlock 1 (%)	ColdBlock 2 (%)	Average	St. Dev	% RSD	% Recovery
Co	12.6	12.9	12.4	12.7	0.354	2.8	100
Li	3.43	3.35	3.27	3.31	0.0566	1.7	97
Mn	8.62	8.22	7.99	8.11	0.163	2.0	94
Ni	11.2	10.8	11.1	11.0	0.212	1.9	98

Shredded Lithium-Ion Batteries
Analyte	Digestion/ Fusion Results (%)	ColdBlock 1 (%)	ColdBlock 2 (%)	Average	St. Dev	% RSD	% Recovery
Co	5.97	5.86	5.88	5.87	0.014	0.2	98
Li	6.06	5.96	5.91	5.94	0.035	0.6	98
Mn	4.40	4.30	4.22	4.26	0.057	1.3	97
Ni	40.9	39.9	39.8	39.9	0.071	0.2	97

Click here to download the Application Note in PDF format.

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ColdBlock Technologies Inc.
4551 Zimmerman Ave
Niagara Falls, ON L2E 3M5
info@coldblock.ca.