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APPLICATION NOTE

AMIS 0656 – Spodumene Concentrate, Brazil

SUMMARY

The application note summarizes the digestion of AMIS 0656, a Spodumene Concentrate Certified Reference Material using ColdBlockDigestion Pro Series Technology.

Instrument:ColdBlock CBM sample digester, chiller, HF compatible liners, ICP-MS & ICP-OES
Published:June 2023
Digestion Time:30 Minutes
Acid Used:Aqua Regia, HF & H3BO3
Average ColdBlock Recovery vs. CRM:

  • 100% Lithium

  • 105% Tantalum

  • 91% Niobium

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METHODOLOGY

  1. Chiller temperature was set to -5°C
  2. 0.25g of each sample was weighed and placed into a ColdBlock™ Digestion vessel
  3. 20 mL of Aqua Regia + 4mL HF was added
  4. Sample was digested at 80% power for 20 minutes
  5. 20mL of 4%w/v Boric acid was added
  6. Samples were digested again at 80% power for 10 minutes
  7. Samples were cooled and bulked to 50mL using 2% HNO3 + 0.5% HClv/v

DISCUSSION

  • The addition of Boric acid will help re-solubilize any insoluble fluorides and will help neutralize any remaining HF in solution
  • Samples appeared mostly clear at the end of the digestion; a minor amount of material settled on the bottom of the tube after bulk up

This material was made using ore sourced from the Volta Grande mine in Minas Gerais state, Brazil.

AMIS0656; Spodumene Concentrate, Brazil; AMIS matrix Reference Materials; A Division of Torre Analytical Services; Gauteng, South Africa (May, 2019)

Results

AMIS 0656 – Spodumene Concentrate, Brazil

Method:

0.25g

20mL Aqua Regia + 4mL HF, 80% 20 minutes – add 20mL 4%w/v Boric acid, 80% 10 minutes

Element

Certified Value (ppm)

+/-

95% Confidence Limits

Sample A

Sample B

Sample C

Average (ppm)

Stdev

% RSD

% Recovery

Low

High

*Ag

0.1

N/A

N/A

N/A

0.10

0.09

0.08

0.1

0.01

12.67%

91%

*Al

120702.9

N/A

N/A

N/A

131690

129711

126140

129180.3

2812.9

2.18%

107%

As

2

1

1

3

2.0

2.0

2.0

2

0.03

1.60%

100%

Ba

17

2

15

19

18

18

18

18

0.3

1.74%

105%

Be

273

45

228

318

268.7

248.9

254.9

258

10.2

3.94%

94%

Bi

2

0.5

1.5

2.5

3.40

3.20

3.50

3

0.2

4.54%

168%

*Ca

7713.6

N/A

N/A

N/A

7577

7866

7005

7482.5

438.1

5.86%

97%

*Cd

0.3

N/A

N/A

N/A

0.3

0.3

0.4

0.3

0.01

1.68%

114%

*Ce

4.3

N/A

N/A

N/A

5.4

5.4

5.3

5.4

0.1

1.08%

125%

Co

3

0.5

2.5

3.5

3.17

3.18

3.03

3

0.1

2.68%

104%

*Cr

99.9

N/A

N/A

N/A

128.0

127.4

124.0

126.5

2.1

1.69%

127%

Cs

86

23

63

109

94.06

96.63

95.44

95

1.3

1.35%

111%

Cu

25

6

19

31

28.2

25.6

23.9

26

2.2

8.40%

104%

*Fe

8769.6

N/A

N/A

N/A

9349

9129

9034

9170.5

161.6

1.76%

105%

Ga

140

9

131

149

147

148

146

147

1.2

0.81%

105%

Hf

7

2

5

9

7

7

7

7.1

0.4

5.95%

102%

K

3262

326

2936

3588

3274

3208

3262

3248

34.9

1.08%

100%

*La

1.7

N/A

N/A

N/A

1.9

2.0

1.9

1.9

0.1

3.13%

113%

Li

29400

2900

26500

32300

29894

29635

28784

29438

580.5

1.97%

100%

*Mg

384.7

N/A

N/A

N/A

583.4

569.7

572.2

575.1

7.3

1.27%

149%

Mn

1006

102

904

1108

1078

1046

1039

1055

20.8

1.97%

105%

Mo

1

0.1

0.9

1.1

1.35

1.23

1.27

1

0.1

4.76%

128%

Na

3879

246

3633

4125

4051

3918

3879

3949

89.8

2.27%

102%

Nb

26

5

21

31

24.38

22.94

23.88

24

0.7

3.08%

91%

Ni

16

5

11

21

17

17

19

18

0.9

5.21%

109%

P

1427

189

1238

1616

1624

1517

1507

1550

64.9

4.19%

109%

Pb

24

4

20

28

26.7

27.3

27.7

27

0.5

1.75%

113%

*Rb

838.7

N/A

N/A

N/A

993.2

988.2

978.4

986.6

7.5

0.76%

118%

**Si

297200

N/A

N/A

N/A

273608

265714

267564

268962

4128.6

1.54%

90%

Sb

4

0.6

3.4

4.6

4.14

4.00

4.04

4

0.1

1.78%

102%

*Sn

156.5

N/A

N/A

N/A

153.3

143.2

150.3

148.9

5.2

3.50%

95%

AMIS 0656 – Spodumene Concentrate, Brazil

Method:

0.25g

20mL Aqua Regia + 4mL HF, 80% 20 minutes – add 20mL 4% w/v Boric acid, 80% 10 minutes

Element

Certified Value (ppm)

+/-

95% Confidence Limits

Sample A

Sample B

Sample C

Average (ppm)

Stdev

% RSD

% Recovery

Low

High

*Sr

22.5

N/A

N/A

N/A

22.8

23.3

22.4

22.8

0.5

2.06%

102%

Ta

187

35

152

222

191.81

199.61

198.87

197

4.3

2.19%

105%

*Th

3.7

N/A

N/A

N/A

4.87

4.36

4.3

4.5

0.3

6.94%

122%

Ti

305

20

285

325

295

294

282

290

7.1

2.46%

95%

Tl

7

0.7

6.3

7.7

7.92

8.02

8.06

8

0.1

0.90%

114%

*U

2.8

N/A

N/A

N/A

5.02

5.07

5.19

5.1

0.1

1.72%

182%

V

8

0.9

7.1

8.9

7.2

7.0

6.8

7

0.2

2.44%

87%

W

1

0.4

0.6

1.4

1.4

1.4

1.4

1

0.0

1.89%

140%

*Y

6.7

N/A

N/A

N/A

10.36

10.08

9.67

10

0.3

3.46%

150%

Zn

58

6

52

64

60

58

58

59

1.0

1.69%

101%

Zr

32

8

24

40

34.84

33.19

34.08

34

0.8

2.43%

106%

* Represents uncertified elements
**Represents elements certified by Peroxide Fusion (no 4-acid data available)

Click here to download the Application Note in PDF format.

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