Contaminated Soil, SS-1

APPLICATION NOTE

SUMMARY

The application note summarizes the digestion of SS-1 a contaminated soil Certified Reference Material using ColdBlock Digestion Pro Series Technology.

Instrument:	ColdBlock CBM sample digester, chiller, ICP-OES, ICP-MS (with CRC technology)
Published:	December 2024
Digestion Time:	45 minutes
Acid Used:	HNO₃, HCl & H₂O2
Average ColdBlock Recovery vs. CRM:	99% Antimony 96% Silver 101% Lead

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METHODOLOGY

Chiller temperature was set to -5°C
0.5g of each sample was weighed and placed into a ColdBlock™ Digestion vessel
10mL of 1:1 HNO₃ + 5mL 1:1 HCl was added, and the samples were digested at 70% power for 5 minutes
10mL HNO₃ was added and digested again at 60% power for 20 minutes (repeat this step if fuming continues)
3mL of 30% H₂O₂ was added slowly, and digested again at 60% for 10 minutes
Add 5mL HCl and digest a final time at 60% power for 10 minutes
Samples were cooled and bulked to 50mL using ultrapure water

DISCUSSION

This method yielded data comparable to EPA 3050b standards (with improved recovery of antimony) in just 45
The addition of HCl in the final step of the digestion helps keep certain elements such as antimony and silver solubilized
This method is not appropriate for standard ICP-MS instruments that are not equipped with Collision/Reaction Cell technology, for more detailed information please contact ColdBlock at info@coldblock.ca

Contaminated Soil, SS-1 after bulk up to 50mL

Results

Contaminated Soil, SS-1
Method:	0.5g	10mL 1:1 HNO₃ + 5mL 1:1 HCl, digest at 70% for 5 minutes, then add 10mL HNO₃ and digest at 60% for 20 minutes (repeat this step if fuming continues) Add 3mL of 30% H₂O₂, slowly and digest again @ 60% for 10 minutes, then add 5mL HCl and digest again @ 60% for 10 minutes.Cool and bulk to 50mL with 2% HNO₃
Element	Certified Value	+/-	Sample A	Sample B	Sample C	Sample D	Sample E	Average (ppm)	Stdev	% RSD	% Recovery vs certified value
Ag	0.88	0.03	0.84	0.84	0.89	0.84	0.82	0.85	0.03	3.1%	96%
Al	12163	410	12077	12634	11519	11542	11985	11951	458	3.8%	98%
As	20.7	1	19.3	20.6	19.6	19.9	20.3	19.9	0.522	2.6%	96%
Ba	464	16	445	473	456	431	436	448	16.8	3.8%	97%
Be	0.48	0.05	0.49	0.46	0.47	0.48	0.49	0.48	0.013	2.7%	100%
Ca	50265	1213	49491	51721	47580	47290	49195	49055	1775	3.6%	98%
Cd	3.2	0.2	3.5	3.4	3.2	3.4	3.0	3.3	0.20	6.1%	103%
Co	12.9	0.4	12.8	13	12.4	12.1	12.9	12.6	0.38	3.0%	98%
Cr	103	5	98.1	103	101	97.5	98.8	100	2.28	2.3%	97%
Cu	403	10	399	427	384	370	385	393	21.6	5.5%	98%
Fe	72000	2273	69216	71857	67438	68507	68635	69131	1654	2.4%	96%
Hg	0.41	0.02	0.38	0.40	0.39	0.41	0.38	0.39	0.01	3.3%	96%
K	2232	150	2493	2576	2438	2523	2468	2500	53	2.1%	112%
Mg	9690	230	9275	9325	9206	9274	9547	9325	131	1.4%	96%
Mn	737	19	708	738	691	687	719	709	21	3.0%	96%
Mo	6.8	0.3	7.3	7.4	6.5	7.5	6.9	7.1	0.41	5.8%	105%
Na	650	64	637	641	582	593	615	614	26.1	4.3%	94%
Ni	59.2	1.3	59.8	62.1	59.2	56.5	57.1	58.9	2.24	3.8%	100%
Pb	764	15	764	794	784	753	767	772	16.4	2.1%	101%
Sb	5.5	1.1	5.6	5.2	6	5.3	5.2	5.5	0.34	6.3%	99%
Se	0.78	0.14	0.82	0.86	0.78	0.8	0.71	0.79	0.055	7.0%	102%
V	27.2	1.4	26.6	26.9	26.1	26.0	26.0	26.3	0.409	1.6%	97%
Zn	1114	37	1130	1179	1156	1095	1100	1132	36	3.2%	102%

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