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APPLICATION NOTE

Strong Acid Digestion

SUMMARY

The application note summarizes the digestion of a range of certified reference materials by AMIS, Geostats, CDN Lab and OREAS using ColdBlock™ Digestion Pro Series Technology.

Instrument: ColdBlock Pro Series CBM sample digester, HF compatible liners, chiller, ICP-OES & ICP-MS
Published: January 2023
Digestion Time: 30 Minutes
Acid Used: Aqua Regia, HF & H3BO3
Average ColdBlock Recovery vs. CRM:
  • 100% Arsenic
  • 100% Copper
  • 102% Silver
 

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 Aqua Regia and 3mL HF was added
  4. Samples were digested at 80% power for 20 minutes
  5. 20mL of 4%v/vBoric acid was added
  6. Samples were digested again at 80% power for 10 minutes
  7. Samples were cooled and bulked to 50mL with 2% HNO3 + 5%HClv/v

DISCUSSION

    • All samples were digested in triplicate
    • The addition of Boric acid will help re-solubilize any insoluble fluorides and will help neutralize any remaining HF in solution
    • If Silver precipitates out of solution as AgCl, bulk up with

    >20% HClv/v

    • If the Sulfide content of your sample is >10 % – reverse the ratios of Aqua Regia and use 1:3, HCl:HNO3 – always add the Nitric acid first (reddish brown NO2 fumes might form)

Results

Results of ColdBlock’s Strong Acid Method vs CRMs certified value

Elements

AMIS CRMs

% Recoveries

CDN-LABS CRMs

% Recoveries

Geostats CRMs

% Recoveries

OREAS CRMs

% Recoveries

AMIS 0566

AMIS 0559

AMIS 0571

CDN- ME-1709

CDN- ME-1805

CDN- ME-1902

GBMS 304-4

GBM 909-15

OREAS 503C

OREAS 134b

OREAS 901

Ag

100%

116%

N/A

107%

104%

93%

96%

94%

103%

95%

107%

Al

97%

99%

101%

N/A

N/A

N/A

N/A

N/A

97%

95%

99%

As

99%

101%

97%

N/A

N/A

N/A

103%

N/A

99%

105%

95%

Ba

102%

108%

106%

N/A

N/A

N/A

N/A

N/A

115%

N/A

102%

Be

N/A

100%

107%

N/A

N/A

N/A

N/A

N/A

116%

N/A

94%

Bi

98%

117%

123%

N/A

N/A

N/A

N/A

N/A

104%

N/A

97%

Ca

97%

99%

100%

N/A

N/A

N/A

N/A

N/A

102%

94%

108%

Cd

112%

113%

100%

N/A

N/A

N/A

N/A

N/A

97%

100%

N/A

Ce

105%

102%

104%

N/A

N/A

N/A

N/A

N/A

98%

N/A

95%

Co

96%

97%

98%

N/A

N/A

N/A

103%

N/A

97%

96%

100%

Cr

N/A

103%

N/A

N/A

N/A

N/A

N/A

N/A

106%

N/A

110%

Cs

N/A

105%

101%

N/A

N/A

N/A

N/A

N/A

107%

N/A

107%

Cu

99%

101%

101%

100%

98%

102%

102%

98%

97%

99%

100%

Fe

97%

99%

99%

N/A

N/A

N/A

N/A

N/A

98%

98%

98%

Ga

96%

102%

101%

N/A

N/A

N/A

N/A

N/A

96%

N/A

96%

Hf

N/A

88%

113%

N/A

N/A

N/A

N/A

N/A

96%

N/A

96%

K

97%

96%

101%

N/A

N/A

N/A

N/A

N/A

98%

N/A

101%

La

112%

106%

109%

N/A

N/A

N/A

N/A

N/A

100%

N/A

97%

Li

N/A

96%

97%

N/A

N/A

N/A

N/A

N/A

101%

N/A

97%

Lu

N/A

100%

109%

N/A

N/A

N/A

N/A

N/A

96%

N/A

99%

Mg

100%

100%

103%

N/A

N/A

N/A

N/A

N/A

102%

100%

101%

Mn

100%

107%

102%

N/A

N/A

N/A

N/A

N/A

102%

N/A

101%

Na

105%

110%

100%

N/A

N/A

N/A

N/A

N/A

86%

N/A

90%

Results of ColdBlock’s Strong Acid Method vs CRMs certified value

Elements

AMIS CRMs

% Recoveries

CDN-LABS CRMs

% Recoveries

Geostats CRMs

% Recoveries

OREAS CRMs

% Recoveries

AMIS 0566

AMIS 0559

AMIS 0571

CDN- ME-1709

CDN- ME-1805

CDN- ME-1902

GBMS 304-4

GBM 909-15

OREAS 503C

OREAS 134b

OREAS 901

Ni

N/A

95%

104%

N/A

N/A

N/A

106%

102%

106%

N/A

98%

Pb

98%

106%

109%

112%

100%

104%

118%

102%

98%

102%

98%

Rb

107%

96%

95%

N/A

N/A

N/A

N/A

N/A

96%

N/A

101%

Sb

106%

106%

106%

N/A

N/A

N/A

N/A

N/A

109%

98%

98%

Sc

N/A

105%

88%

N/A

N/A

N/A

N/A

N/A

106%

N/A

109%

Se

N/A

97%

N/A

N/A

N/A

N/A

N/A

N/A

92%

N/A

N/A

Sn

N/A

88%

88%

N/A

N/A

N/A

N/A

N/A

79%

N/A

87%

Sr

99%

94%

94%

N/A

N/A

N/A

N/A

N/A

96%

N/A

96%

Te

100%

97%

N/A

N/A

N/A

N/A

N/A

N/A

127%

N/A

124%

Th

99%

114%

117%

N/A

N/A

N/A

N/A

N/A

98%

N/A

100%

Tl

N/A

96%

122%

N/A

N/A

N/A

N/A

N/A

107%

N/A

107%

Tm

115%

117%

100%

N/A

N/A

N/A

N/A

N/A

99%

N/A

N/A

U

104%

103%

104%

N/A

N/A

N/A

N/A

N/A

110%

N/A

100%

V

98%

108%

91%

N/A

N/A

N/A

N/A

N/A

101%

N/A

99%

Y

98%

87%

94%

N/A

N/A

N/A

N/A

N/A

92%

N/A

96%

Yb

N/A

133%

118%

N/A

N/A

N/A

N/A

N/A

98%

N/A

98%

Zn

99%

98%

101%

103%

101%

103%

99%

100%

104%

98%

104%

Zr

N/A

92%

88%

N/A

N/A

N/A

N/A

N/A

85%

N/A

99%

Click here to download the Application Note in PDF format.

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ColdBlock Technologies Inc.
4551 Zimmerman Ave
Niagara Falls, ON L2E 3M5
info@coldblock.ca.