APPLICATION NOTE

Lead Concentrate – OREAS-353

SUMMARY

This application note is for the digestion of OREAS-353, a Lead Concentrate.

Instrument:

ColdBlock CB15S sample digester technology, chiller, ICP-OES, ICP-MS

Published:August 2022
Digestion Time:20 Minutes
Acid Used:Reverse Aqua Regia
Average ColdBlock Recovery vs. CRM:
  • 91% Silver

  • 97% Lead

  • 99% Zinc

METHODOLOGY

  1. Chiller temperature was set to -5°C
  2. 0.25g of OREAS 353 was weighed and placed into a ColdBlock Digestion vessel
  3. 20mL of Reverse Aqua Regia was added (HNO3 is added first, followed by the HCl) (For elements requiring HF, 20mL Reverse Aqua Regia + 3mL HF was added) (Optional step if using HF: Add 20mL of 4%v/v Boric acid and digest another 10 minutes to re-solubilize any insoluble fluorides precipitating out and neutralize any remaining HF)
  1. Sample was digested at 80% power for 20 minutes
  2. Sample was cooled and bulked to 50mL using 2% HNO3v/v

DISCUSSION

  • Upon addition of HNO3, the evolution of reddish brown (N02) fumes occurred
  • After 20 minutes, the samples are dark yellow in color
  • Hydrofluoric acid can be added for a “near” total digestion to improve recoveries of certain elements (see table 2 for improved recoveries of Al, Co, Fe, Mg, Mn & Sb)
  • Boric acid can also be added to re-solubilize any insoluble fluorides and help neutralize any remaining HF)
  • For improved silver recoveries bulk up using a solution of >20% HClv/v

OREAS 353 is a certified reference material (CRM) prepared from a Pb-Ag concentrate sample sourced from South32 Ltd’s Cannington mine plant. The stratabound, metasediment hosted (Broken Hill Type) deposit is located ~200 kms south-east of Mount Isa in north- west Queensland, Australia.

Results

Table 1: Results of Reverse Aqua Regia digestion

Elements

Expected Value

ColdBlock Value 1

ColdBlock Value 2

Average

% RSD

% Recovery

Ag (ppm)

2184

1987

1969

1978

0.5%

91%

Al (ppm)

2040

794

640

717

10.7%

35%

Ca (ppm)

2360

2411

2291

2351

2.6%

100%

Cd (ppm)

205

198

206

202

2.0%

99%

Co (ppm)

48.8

36.8

50.0

43.4

15.2%

89%

Cu (ppm)

3120

2774

2790

2782

0.3%

89%

Fe (wt.%)

5.35

4.81

4.81

4.81

0.0%

90%

Mg (wt.%)

0.685

0.205

0.206

0.206

0.2%

30%

Mn (wt.%)

0.184

0.147

0.147

0.147

0.0%

80%

Pb (wt.%)

61.26

57.89

60.6

59.25

2.3%

97%

S (wt.%)

15.13

13.66

14.33

14.00

2.4%

92%

Sb (ppm)

1746

606

932

769

21.2%

44%

Zn (wt.%)

4.14

4.12

4.07

4.10

0.6%

99%

Table 2 Results of adding HF, showing improved recoveries of Al, Co, Fe, Mg, Mn, Sb

Elements

Expected Value

ColdBlock Value 1

ColdBlock Value 2

Average

% RSD

% Recovery

AI (ppm)

2040

2049

1677

1863

0.1%

91%

Co (ppm)

48.8

49.1

51.6

50.4

2.5%

103%

Fe (wt.%)

5.35

5.26

4.87

5.07

0.3%

95%

Mg (wt.%)

0.685

0.681

0.650

0.666

2.3%

97%

Mn (wt.%)

0.184

0.181

0.184

0.183

0.8%

99%

Sb (ppm)

1746

1738

1676

1707

1.8%

98%

Click here to download the Application Note in PDF format.

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