Metals in Fly Ash – CRM019 Certified Reference Material

APPLICATION NOTE

Metals in Fly Ash – CRM019 Certified Reference Material

SUMMARY

The application note summarizes the digestion of Metals in Fly Ash, CRM019, a Certified Reference Material using ColdBlock Digestion CB15S Technology.

Instrument:	ColdBlock CB15S sample digester technology, chiller, ICP-OES, ICP-MS
Published:	August 2022
Digestion Time:	20 Minutes
Acid Used:	HNO₃ & HCl
Average ColdBlock Recovery vs. CRM:	106% Arsenic 97% Manganese 100% Lead

METHODOLOGY

Chiller temperature was set to -5 °C
0.5g of Fly Ash was weighed and placed into a ColdBlock™ Digestion vessel
12ml HNO3 was added, and mixed with sample
Sample was digested at 80% power for 10 minutes
4mL HCl was added, and sample was digested again at 80% power for 10 minutes

DISCUSSION

Upon addition of HNO3, the evolution of reddish brown (NO2) fumes occurred
The NO2 fumes subsided and turned white prior to the addition of HCl
After 20 minutes the samples are greenish brown, and a minor amount of solid material remains
Longer digestion times can be used to improve the recoveries of certain elements
Hydrofluoric acid can be added for a “near total” digestion

CRM019 after 20-minute digestion

Metals in Fly Ash, CRM019 is a Certified Reference Material used for QC verification and/or method development purposes. It was sourced from a wastewater treatment facility in the Western Unit.

Results

Trace Metals – Fly Ash 3
Method:	0.5g	12mL HNO3 – Digest at 80% for 600 seconds – Add 4mL HCl and digest again for 600 seconds. Bulk to 50mL with 2% HNO3
Element	Certified Value mg/kg (non-certified)	ColdBlock Sample A	ColdBlock Sample B	ColdBlock Sample C	ColdBlock Average (mg/kg)	Stdev	% RSD	% Recovery
Ag	7.35	7.96	8.04	7.3	7.8	0.04	0.5%	106%
As	77.2	80.9	82.1	81.7	82	0.6	0.7%	106%
Ca	(51900)	50962	50182	53225	51456	390	0.8%	99%
Cd	432	414	439	434	429	12.5	2.9%	99%
Co	(26)	24	23	23	23	0.5	2.1%	90%
Cr	55.2	55.1	59.3	54.2	56.2	2.1	3.7%	102%
Cu	279	280	288	284	284	4	1.4%	102%
Fe	(12690)	12473	11135	12581	12063	669	5.5%	95%
Mg	6310	6778	6543	6575	6632	117.5	1.8%	105%
Mn	(480)	456	448	488	464.0	4	0.9%	97%
Na	(50500)	50925	52257	51707	51630	666	1.3%	102%
Ni	22.2	24.3	22.8	25.4	24	0.75	3.1%	109%
Pb	4540	4515	4632	4525	4557	58.5	1.3%	100%
Se	4.11	4.14	4.25	3.7	4.0	0.055	1.4%	98%
V	28.9	29.8	30.2	30.4	30	0.2	0.7%	104%
Zn	22400	21139	21637	21459	21412	249	1.2%	96%

Click here to download the Application Note in PDF format.

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