Montana I Soil, NIST 2710a

APPLICATION NOTE

SUMMARY

The application note summarizes the digestion of NIST 2710a, a Montana soil standard reference material using ColdBlock Digestion Pro Series Technology.

Instrument:	ColdBlock CBM, 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:	97% Arsenic 98% Cadmium 100% 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

16 samples of NIST 2710a after bulk up to 50mL

Results

Montana I Soil, NIST 2710a
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	Reference Value* EPA 3050b	ColdBlock Average (ppm) n=16	ColdBlock Stdev	ColdBlock % RSD	ColdBlock % Recovery vs EPA Method
Ag (ppm)	36	37	0.90	2.4%	103%
Al (ppm)	13220	14414	366	2.5%	109%
As (ppm)	1568	1524	33	2.2%	97%
Ba (ppm)	504	540	14.1	2.6%	107%
Be (ppm)	0.56	0.55	0.03	5.5%	98%
Ca (ppm)	1876	1887	84	4.5%	101%
Cd (ppm)	11.2	11	0.28	2.5%	98%
Co (ppm)	4.23	4.37	0.36	8.2%	103%
Cu (ppm)	3252	3388	80	2.4%	104%
Fe (ppm)	35687	36200	847	2.3%	101%
K (ppm)	4829	4914	116	2.4%	102%
Mg (ppm)	3811	3671	77	2.1%	96%
Mn (ppm)	1652	1665	37	2.2%	101%
Mo (ppm)	7.38	7.66	0.35	4.6%	104%
Na (ppm)	621	635	42	6.6%	102%
Ni (ppm)	6	7	0.4	5.7%	117%
Pb (ppm)	5092	5074	101	2.0%	100%
Se (ppm)	1.0	1.1	0.09	8.2%	110%
Sb (ppm)	10.1	29.1	3.41	11.7%	288%
Tl (ppm)	0.72	0.9	0.06	6.7%	125%
V (ppm)	46	48	1.4	2.9%	104%
Zn (ppm)	3852	3834	77	2.0%	100%

Click here to download the Application Note in PDF format.

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