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Anton Paar Microwavedigestion - ApplReport - Fly - Ash

1. Recovery of mercury and arsenic from fly ash samples using the Multiwave GO leaching system with a venting rotor was as complete as using a sealed high pressure vessel, demonstrating volatile elements can be completely recovered with venting. 2. Mercury, arsenic, and other element concentrations were measured in fly ash, bottom ash, and reference materials after leaching with Multiwave GO and compared to results from a sealed Multiwave 3000 system, showing nearly complete recoveries for all elements tested. 3. Leaching tests using the Multiwave GO system achieved full recovery of mercury and arsenic as well as other elements like cadmium, copper, nickel, lead, zinc, and others from a variety

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Absheen Zaman
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191 views2 pages

Anton Paar Microwavedigestion - ApplReport - Fly - Ash

1. Recovery of mercury and arsenic from fly ash samples using the Multiwave GO leaching system with a venting rotor was as complete as using a sealed high pressure vessel, demonstrating volatile elements can be completely recovered with venting. 2. Mercury, arsenic, and other element concentrations were measured in fly ash, bottom ash, and reference materials after leaching with Multiwave GO and compared to results from a sealed Multiwave 3000 system, showing nearly complete recoveries for all elements tested. 3. Leaching tests using the Multiwave GO system achieved full recovery of mercury and arsenic as well as other elements like cadmium, copper, nickel, lead, zinc, and others from a variety

Uploaded by

Absheen Zaman
Copyright
© © All Rights Reserved
We take content rights seriously. If you suspect this is your content, claim it here.
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Download as PDF, TXT or read online on Scribd
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Complete Recovery of Mercury, Arsenic and other Elements

from Fly Ash with Multiwave GO

Recovery of mercury from fly ash is as complete after leaching with Multiwave GO using
SMART VENT technology as it is in closed vessels without venting capabilities.
This report compares data for samples of fly ash, bottom ash and
a reference material "Fly Ash"BCR - 176R.

2 Instrumentation

Leachings used for this comparison were done with a


Multiwave GO with Rotor 12 HVT50 and a Multiwave
3000 with rotor 8 SXF100.
Mercury analysis was done with a PerkinElmer
FIMS400 mercury system, a specific mercury analyzer
that circumvents the problem often associated with
mercury determination by ICP-OES and ICP-MS.
Arsenic analysis was done with Zeeman-corrected
GF-AAS PerkinElmer 800 due to its lower level of
interferences as compared to ICP-MS.
Other elements were analyzed with ICP-MS Agilent
7500c.
1 Introduction 3 Experimental

Mercury and arsenic are difficult elements to be rou- 3.1 Samples


tinely determined in fly ashes because of the possible
losses as volatile elements. Evaluation of sample The samples used in this study were the BCR refer-
preparation methods, however, is hindered by the lack ence materials „Fly ash“ (BCR 176R) and „Basic Slag“
of reference materials certified for mercury. (BCR 382), which are both not certified for their mer-
For a vessel system using the SMART VENT technol- cury content. In addition also routine samples have
ogy it is important to prove that a potentially volatile been leached and compared, one fly ash with ex-
element as mercury can be completely recovered. pected higher mercury concentration and two samples
So the recoveries from acid leaching by Multiwave GO of ground ash with considerably lower concentration.
with a rotor 12HVT50 are compared with a Multiwave
1
3000 system equipped with a rotor 8SXF100 . This is
a completely sealed system that has, during its long
time availability, proven to recover mercury and arse-
nic completely.
Reliable leaching for mercury, arsenic and other envi-
ronmentally relevant elements can be achieved with
pressure activated venting vessels of rotor 12HVT50
with Multiwave GO in the same quality as with a her-
metically sealed high pressure vessel.

1
Experiments were carried out in collaboration with Anton Paar by
Figure 1: Multiwave GO
Umweltbundesamt GmbH, Vienna

C93IA010EN-B 1 www.anton-paar.com
3.2 Digestion Procedure Temperature Ramp Hold
Step
[°C] [min] [min]
About 500 mg of sample were directly weighed into 1 175 15 15
the HVT50 vessels with an analytical balance.
Table 2: Faster temperature program
The following acid mixture was added to the weighed
3.4 Complexation
samples:
HCl (37%, subboiled): 6 mL For ICP-OES/MS nebulizers made of quartz or glass-
HNO3 (68%, subboiled): 10 mL ware it is common to use saturated boric acid to com-
HF (40%, suprapur): 2 mL plex the excess of fluoride in solution. To each sample
22 ml saturated boric acid was added and the follow-
The vessels were closed and Rotor 12HVT50 was
ing method was executed.
loaded with samples and blanks. The rotor was placed
in the cavity.
3.3 Temperature Program Step
Temperature Ramp Hold
[°C] [min] [min]
The following digestion program was carried out. The 1 60 5 15
temperature input strategy was set to „Average“, Table 3: Complexation program
which uses the running average of the temperature of
all vessels for the control of the microwave energy.
The temperature limit was set to 190 °C. 3.5 Measuring the Samples

After the complexation step the residues were filtered


Step
Temperature Ramp Hold off, rinsed with DI water and made up to volume.
[°C] [min] [min]
1 130 15 5
4 Results
2 175 15 15
Table 1: Temperature program The table below shows the values after Multiwave GO
digestion for 3 everyday ash samples and 2 SRMs
This method was a very cautious one, accounting for and the %-recovery with respect to the values after
unknown and potentially highly reactive samples con- digestion in a Multiwave 3000 and - in brackets - the
taining significant amounts of organic residues. If the recoveries with respect to the certified values
reactivity of the samples is small, we suggest using
the following faster method.

Element Ground Ash 7528 Ground Ash 7523 Fly Ash 7525 SRM Fly Ash SRM Slag

recovery recovery recovery recovery recovery


mg/kg mg/kg mg/kg mg/kg mg/kg
% % % % %
Cd 2,2 101 3,4 101 49 100 236 99(104) 0,60 92
Cu 71 94 104 80 193 94 130 100 (89) 1.030 101 (98)
Ni 41 100 48 119 59 102 32 96 (87) 117 96 (100)
Pb 27 99 55 93 509 97 18 66 5.200 101 (105)
Zn 359 99 1.316 98 7.336 99 148 105 (105) 16.500 99 (98)
Hg 0,025 100 0,12 101 5 100 0,041 98 1,6 101
As 4,7 100 9,9 99 80 100 55 98 (98) - -
Table 4: Results

5 Conclusion
Contact Anton Paar GmbH
The leaching of fly ash samples in Multiwave GO re- Tel: +43 316 257-0
sulted in complete recoveries possibly volatile ele- asc@anton-paar.com | www.anton-paar.com
ments like mercury and arsenic, but also for all stud-
ied elements Cd, Cu, Ni, Pb, and Zn

C93IA010EN-B 2 www.anton-paar.com

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