Distributor login
Contact us

APPLICATION NOTE

Lead Concentrate, CPb-3

SUMMARY

The application note summarizes the digestion of CPb-3, a lead concentrate certified reference material using ColdBlock Digestion Pro Series Technology.

Instrument: ColdBlock CBM Pro-Series, chiller, HF liners, ICP-OES
Published: May 2025
Digestion Time: 30 Minutes
Acid Used: HNO3, HCl, HF & H3BO3
Average ColdBlock Recovery vs. CRM:
  • 100% antimony
  • 102% lead
  • 100% zinc

METHODOLOGY

  1. Set the chiller temperature to -5°C.
  2. Weigh 0.25 g of each sample and transfer into a ColdBlock Digestion vessel with liner
  3. Add 20 mL of reverse aqua regia (add HNO3 first, followed by HCl) and 3 mL of HF to each vessel.
  4. Digest samples at 80% power for 20 minutes.
  5. Add 20 mL of 4% boric acid (w/v) to each sample.
  6. Digest samples again at 80% power for 10 minutes.
  7. Cool the samples and adjust the volume to 50 mL with DI water

DISCUSSION

  • The addition of boric acid aids in the re-solubilization of insoluble fluorides and neutralizes residual hydrofluoric acid (HF). This step is crucial for sample dissolution and minimizing analyte loss during digestion.
  • Following the digestion process, the samples were visibly clear – indicating that the sample matrix had dissolved.
    A trace amount of material settled on the bottom of the tube – see figure 1

Figure 1- CPb-3 after bulking-up to 50mL

Results

CPb-3, Lead Concentrate

Method:

0.25g – Add 20mL reverse aqua regia + 3mL HF and digest at 80% power for 20 minutes. Add 20mL of 4% boric acid
w/v and digest again at 80% power for 10 minutes. Let cool, and adjust the volume to 50mL with DI water

Element

CPb-3
Certified Values

ColdBlock Average
n=5

ColdBlock
Stdev +/–

ColdBlock
RSD

ColdBlock Recovery vs Certified Value

Al (%)

0.203

0.200

0.005

2.5%

99%

Ca (%)

0.059

0.053

0.003

5.7%

90%

Cd (%)

0.0652

0.0653

0.002

3.1%

100%

Co (µg/g)

13.6

13.7

1.4

10.2%

101%

Cr (%)

0.0102

0.0104

0.0002

1.9%

102%

Cu (%)

0.240

0.245

0.004

1.6%

102%

Fe (%)

8.45

8.51

0.08

0.9%

101%

Mg (%)

0.1062

0.1

0.0024

2.3%

100%

Pb (%)

58.53

59.02

0.39

0.7%

101%

S (%)

17.03

17.93

0.21

1.2%

105%

Sb (%)

0.5800

0.5778

0.008

1.4%

100%

Zn (%)

5.96

5.98

0.04

0.7%

100%

The material for CPb-3 was donated by a North American refinery.
CCRMP CanmetMINING NRCan (2020). Certificate of Analysis for CPb-3, Lead Concentrate https://natural-resources.canada.ca/

Click here to download the Application Note in PDF format.

Join our monthly e-newsletter for expert tips, updates, and exclusive content delivered straight to your inbox.

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