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APPLICATION NOTE

Industrial Sludge – NIST 2782

SUMMARY

The application note summarizes the digestion of NIST 2782, an Industrial Sludge standard 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:
  • 109% Arsenic
  • 103% Cadmium
  • 102% Antimony

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

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 NIST 2782 after bulk up to 50mL

Results

Industrial Sludge, NIST 2782

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

Arsenic

144

157

3.19

2.2%

109%

Aluminum

1468

1503

41.12

2.8%

102%

Antimony

2.07

2.12

0.420

20%

102%

Barium

136

153

2.14

1.6%

113%

Cadmium

2.14

2.20

0.112

5.3%

103%

Calcium

4544

4624

169.6

3.7%

102%

Chromium

65.4

69.4

1.46

2.2%

106%

Cobalt

52.2

53.5

1.86

3.6%

103%

Copper

2288

2511

66.06

2.9%

110%

Iron

247576

258116

7041

2.8%

104%

Lead

491

553

5.69

1.2%

113%

Magnesium

468

482

23.8

5.1%

103%

Manganese

243

264

8.64

3.6%

109%

Mercury

1.22

1.27

0.0509

4.2%

104%

Molybdenum

5.39

5.95

0.374

6.9%

110%

Nickel

95.54

106.2

4.65

4.9%

111%

Potassium

88

97

6.1

7.0%

111%

Silver

26.98

28.47

3.212

11.9%

106%

Sodium

2539

2637

75.98

3.0%

104%

Vanadium

10.7

14.4

0.678

6.3%

135%

Zinc

1143

1129

46.91

4.1%

99%

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.