APPLICATION NOTE

Base Metals by Aqua Regia

SUMMARY

This application note summarizes the digestion of base metals by aqua regia in various certified reference materials using ColdBlock Digestion Technology.

Instrument:

ColdBlock CB15, chiller, ICP-OES, ICP-MS

Published:

May 2024

Digestion Time:15 Minutes
Acid Used:Aqua Regia
Average ColdBlock Recovery vs. CRM:
  • 99% Copper
  • 102% Nickel
  • 100% Zinc

METHODOLOGY

  1. Chiller temperature was set to -5°C
  2. 0.5g of each sample were weighed and placed into ColdBlock Digestion vessels
  3. 16 mL of Aqua Regia (AR) or reverse Aqua Regia (rAR) was added (reverse Aqua Regia was used for high sulphide samples)
  4. Samples were digested at 60% power for 15 minutes
  5. Samples were cooled and bulked to 50 mL using 15% HCl v/v

DISCUSSION

  • For samples with a Sulphide content >10%, it is recommended to invert the ratios of Aqua Regia (3:1 – HNO3:HCl), add HNO3 slowly and allow the samples to react before adding HCl (reaction can be vigorous and deep brown/red fumes will be generated (see table 1 for summary of sample types and methods used)

Results

Table 1 – Summary of sample types

CRM ID

TYPE

Sample Weight

Method

AMIS 0619

Copper Concentrate, Black Mountain, Northern Cape, South Africa

0.5

rAR

AMIS 0566

Copper Concentrate, Philippines

0.5

rAR

GBM318-6

Geochem Base Metal

0.5

AR

OREAS 504b

Porphyry Copper-Gold-Molybdenum

0.5

AR

OREAS 990

Copper-Gold Concentrate

0.5

rAR

OREAS 134b

Zn-Pb-Ag Ore

0.5

rAR

AMIS 0619 – Copper Concentrate, Black Mountain, Northern Cape, South Africa

Method:

0.5g

Slowly add 12mL HNO3 and 4mL HCl, digest at 60% power for 15 minutes.

Cool, and bulk to 50mL with 15%HCl v/v

Element

Certified Value

95% Confidence Limits

Sample A

Sample B

Sample C

Average (ppm)

Stdev

% RSD

%

Recovery

Low

High

Co (ppm)

476

438

514

411

408

476

432

31.4

7.3%

91%

Cu (%)

25.14

23.14

27.14

25.5

24.9

25.1

25

0.2

1.0%

100%

Fe (%)

34.22

31.22

37.22

33.7

33.7

34.0

34

0.1

0.4%

99%

Mo (ppm)

1098

975

1221

1040

1030

1050.0

1040

8.2

0.8%

95%

Ni (ppm)

330

294

366

313

306

308

309

2.9

1.0%

94%

Pb (%)

2.72

2.52

2.92

2.59

2.60

2.61

2.60

0.01

0.3%

96%

Zn (%)

1.24

1.17

1.31

1.22

1.25

1.22

1.23

0.01

1.1%

99%

GBM318-6 – Geochem Base Metal

Method:

0.5g

Slowly add 4mL HNO3 and 12mL HCl, digest at 60% power for 15 minutes.

Cool, and bulk to 50mL with 15%HCl v/v

Element

Certified Value

95% Confidence Limits

Sample A

Sample B

Sample C

Average (ppm)

Stdev

% RSD

%

Recovery

Low

High

Co (ppm)

49

47.5

50.5

46

47

48

47

0.8

1.7%

96%

Cu (ppm)

2423

2399.4

2446.6

2520

2610

2520

2550

42

1.7%

105%

Ni (ppm)

762

749

775

860

862

869

864

3.9

0.4%

113%

Pb (ppm)

10

9.3

10.7

14

9

10

11

2.3

20.3%

112%

Zn (ppm)

130

122.3

137.7

134

130

131

132

1.7

1.3%

101%

OREAS 504b – Porphyry Copper-Gold-Molybdenum

Method:

0.5g

Slowly add 4mL HNO3 and 12mL HCl, digest at 60% power for 15 minutes.

Cool, and bulk to 50mL with 15% HCl v/v

Element

Certified Value

95% Confidence Limits

Sample A

Sample B

Sample C

Average (ppm)

Stdev

% RSD

%

Recovery

Low

High

Co (ppm)

18.7

18.1

19.4

19

19

19

18.9

0.05

0.2%

101%

Cu (%)

1.1

1.09

1.11

1.06

1.05

1.06

1.1

0.005

0.4%

96%

Fe (%)

6.71

6.51

6.91

6.57

6.63

6.58

6.59

0.03

0.4%

98%

Ni (ppm)

30

29.1

31

29

30

30

30

0.2

0.6%

99%

Mo (ppm)

476

467

485

459

457

459

458

0.9

0.2%

96%

Pb (ppm)

26.2

25.1

27.3

25.2

28.2

24.8

26.1

1.5

5.8%

99%

Zn (ppm)

96

94

99

86

90

82

86

3.3

3.8%

90%

OREAS 990 – Copper-Gold Concentrate

Method:

0.5g

Slowly add 12mL HNO3 and 4mL HCl, digest at 60% power for 15 minutes.

Cool, and bulk to 50mL with 15% HCl v/v

Element

Certified Value

95% Confidence Limits

Sample A

Sample B

Sample C

Average (ppm)

Stdev

% RSD

%

Recovery

Low

High

Cu (%)

16.99

16.72

17.25

16.6

16.6

15.5

16.21

0.5

3.2%

95%

Fe (%)

20.07

19.38

20.77

19.0

18.7

18.9

18.87

0.1

0.7%

94%

Ni (ppm)

93

87

100

96

94

96

95

0.9

1.0%

103%

Mo (ppm)

116

108

125

116

116

120

117

1.9

1.6%

101%

Pb (%)

8.62

8.51

8.73

8.28

8.07

8.61

8.32

0.2

2.7%

97%

Zn (%)

13.43

13.1

13.75

13.69

13.48

13.49

13.55

0.1

0.7%

101%

OREAS 134b – Zn-Pb-Ag Ore

Method:

0.5g

Slowly add 12mL HNO3 and 4mL HCl, digest at 60% power for 15 minutes.

Cool, and bulk to 50mL with 15% HCl v/v

Element

Certified Value

95% Confidence Limits

Sample A

Sample B

Sample C

Average (ppm)

Stdev

% RSD

%

Recovery

Low

High

Co (ppm)

104

92

116

95

96

94

95

0.8

0.9%

91%

Cu (ppm)

1337

1284

1391

1290

1300

1300

1297

4.7

0.4%

97%

Fe (%)

12.25

11.71

12.8

11.7

11.6

11.8

11.7

0.08

0.7%

96%

Pb (%)

13.31

12.85

13.78

13.1

12.9

13.1

13.03

0.1

0.7%

98%

Zn (%)

17.7

17.04

18.36

17.7

17.9

18.1

17.9

0.2

0.9%

101%

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