APPLICATION NOTE

Skimmed Milk Powder – ERM-BD150

SUMMARY

The application note summarizes the digestion of ERM-BD150, a skimmed milk powder Certified Reference Material using ColdBlock Digestion Pro Series Technology.

Instrument:

ColdBlock CBM sample digester, chiller, Quartz Vessels , ICP-MS

Published:March 2023
Digestion Time:20 Minutes
Acid Used:HNO3 & H2O2
Average ColdBlock Recovery vs. CRM:
  • 102% Cadmium

  • 104% Mercury

  • 98% Selenium

METHODOLOGY

  1. Chiller temperature was set to -5°C
  2. 0.5g of each sample was weighed and placed into a quartz ColdBlock Digestion vessel
  3. 15mL of Nitric acid was added
  4. Sample was digested at 70% power for 15 minutes
  5. 2mL of 30% v/vHydrogen Peroxide was added
  6. Samples were digested again at 70% power for 5 minutes
  7. Samples were cooled and bulked to 40mL using 2% HNO3 + 5% HCl v/v

DISCUSSION

  • The samples were clear at the end of the digestion
  • Samples were analyzed by ICP-MS

Figure 1 ERM-BD150 after bulk up

ERM-BD150; Skimmed Milk Powder; European Commission, Joint Research Centre, Directorate F – Health, Consumers and Reference Materials Retieseweg 111 B-2440 Geel, Belgium

Results

ERM BD-150 – Skimmed Milk Powder

Method:

0.25g

15mL HNO3 -Digest at 70% power for 15 minutes, add 2mL H2O2 and digest again at 70% power for 5 minutes

 

Element

Certified Value (ppm)

 

+/–

95% Confidence Limits

 

Sample A

 

Sample B

 

Sample C

 

Average (ppm)

 

Stdev

 

% RSD

 

%

Recovery

Low

High

Ca

13900

800

13100

14700

13522

13349

13656

13509

126

0.9%

97%

K

17000

700

16300

17700

17285

17372

17703

17453

180

1.0%

103%

Mg

1260

100

1160

1360

1231

1230

1244

1235

7

0.5%

98%

Na

4180

190

3990

4370

4104

4092

4164

4120

31

0.8%

99%

P

11000

600

10400

11600

11433

11593

11007

11344

247

2.2%

103%

Cd

0.0114

0.0029

0.0085

0.0143

0.0116

0.0118

0.0116

0.0117

0.0001

0.8%

102%

Cu

1.08

0.06

1.02

1.14

1.11

1.07

1.05

1.07

0.02

1.9%

99%

Fe

4.6

0.5

4.1

5.1

4.6

4.4

4.6

4.5

0.1

2.1%

98%

Hg

0.06

0.007

0.053

0.067

0.07

0.06

0.06

0.063

0.003

4.6%

104%

Mn

0.289

0.018

0.271

0.307

0.265

0.334

0.284

0.294

0.03

9.9%

102%

Pb

0.019

0.004

0.015

0.023

0.027

0.024

0.021

0.024

0.002

10.2%

126%

Se

0.188

0.014

0.174

0.202

0.207

0.172

0.173

0.184

0.016

8.8%

98%

Zn

44.8

2

42.8

46.8

46.4

44.7

46.8

46.0

0.9

2.0%

103%

Click here to download the Application Note in PDF format.

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