APPLICATION NOTE

Metals in Soil – ERA 540

SUMMARY

The application note summarizes the digestion of ERA 540, a Metals in Soil certified reference material using ColdBlock Digestion Pro Series Technology.

Instrument:

ColdBlock CBM, chiller, ICP-OES, ICP-MS (with CRC technology)

Published:March 2025
Digestion Time:45 Minutes
Acid Used:HNO3, HCl & H2O2
Average ColdBlock Recovery vs. CRM:
  • 95% Antimony
  • 100% Mercury
  • 102% Silver

METHODOLOGY

  1. Chiller temperature was set to -5°C
  2. 0.5g of each sample was weighed and placed into a ColdBlock Digestion vessel
  3. 10mL of 1:1 HNO3 + 5mL 1:1 HCl were added, and the samples were digested at 70% power for 5 minutes
  4. 10mL HNO3 was added and digested again at 60% power for 20 minutes (repeat this step if fuming continues)
  5. 3mL of 30% H2O2 was added slowly, and digested again at 60% for 10 minutes
  6. 5mL HCl was added and digested at 60% power for 10 minutes
  7. Samples were cooled and bulked to 50mL using ultrapure water

DISCUSSION

  • This method yielded data comparable to EPA 3050B standards in just 45 minutes
  • The addition of HCl in the final step of the digestion helps keep certain elements such as antimony and silver solubilized
  • This method is not appropriate for standard ICP-MS instruments that are not equipped with Collision/Reaction Cell technology

15 samples of ERA 540 after bulk up to 50mL

Results

ERA #540 Metals in Soil (lot:D125-540)

Method:

0.5g Add 10mL 1:1 HNO3 + 5mL 1:1 HCl, digest at 70% for 5 minutes, then add 10mL HNO3 and digest at 60% for 20 minutes (repeat this step if fuming continues) Add 3mL of 30% H2O2, slowly and digest again @ 60% for 10 minutes, then add 5mL HCl and digest again @ 60% for 10 minutes. Cool and bulk to 50mL with ultrapure water

Element

*Reference Value (mg/kg) n=5

ColdBlock Average (mg/kg) n=16

ColdBlock Stdev

ColdBlock
% RSD

ColdBlock % Recovery vs SW-846 3050B

Aluminum

7165

7236

549.4

7.6%

101%

Antimony

129

123

9.66

7.9%

95%

Arsenic

139

152

5.52

3.6%

110%

Barium

196

208

19.6

9.4%

106%

Beryllium

223

245

31.7

13.0%

110%

Cadmium

181

194

14.6

7.6%

107%

Calcium

4421

4323

307.5

7.1%

98%

Chromium

136

131

8.08

6.2%

96%

Cobalt

129

137

10.1

7.3%

107%

Copper

235

259

21.8

8.4%

111%

Iron

6782

7012

353.2

5.0%

103%

Lead

89

100

6.2

6.2%

113%

Magnesium

1809

2033

92.67

4.6%

112%

Manganese

245

254

20.9

8.2%

103%

Mercury

27

27

1.9

7.1%

100%

Molybdenum

94

97

5.2

5.3%

102%

Nickel

154

163

11.5

7.0%

106%

Potassium

2069

2198

158.0

7.2%

106%

Selenium

129

136

7.54

5.5%

105%

Silver

54

55

2.7

4.8%

102%

Sodium

271

290

26.6

9.2%

107%

Thallium

166

179

14.0

7.8%

108%

Vanadium

139

135

8.09

6.0%

97%

Zinc

336

340

18.7

5.5%

101%

Click here to download the Application Note in PDF format.

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