Anal Bioanal Chem (2002) 372 : 360–365
DOI 10.1007/s00216-001-1172-z
O R I G I N A L PA P E R
Vivien F. Taylor · Andrew Toms · Henry P. Longerich
Acid digestion of geological and environmental samples
using open-vessel focused microwave digestion
Received: 10 July 2001 / Revised: 10 September 2001 / Accepted: 8 October 2001 / Published online: 18 December 2001
© Springer-Verlag 2001
Abstract The application of open vessel focused mi-
crowave acid digestion is described for the preparation of
geological and environmental samples for analysis using
inductively coupled plasma-mass spectrometry (ICP-MS).
The method is compared to conventional closed-vessel
high pressure methods which are limited in the use of HF
to break down silicates. Open-vessel acid digestion more
conveniently enables the use of HF to remove Si from
geological and plant samples as volatile SiF4, as well as
evaporation-to-dryness and sequential acid addition dur-
ing the procedure. Rock reference materials (G-2 granite,
MRG-1 gabbros, SY-2 syenite, JA-1 andesite, and JB-2
and SRM-688 basalts) and plant reference materials (BCR
and IAEA lichens, peach leaves, apple leaves, Durham
wheat flour, and pine needles) were digested with results
comparable to conventional hotplate digestion. The mi-
crowave digestion method gave poor results for granitic
samples containing refractory minerals, however fusion
was the preferred method of preparation for these sam-
ples. Sample preparation time was reduced from several
days, using conventional hotplate digestion method, to
one hour per sample using our microwave method.
Keywords Digestion · Geological samples ·
Environmental samples · Microwave digestion ·
Open-vessel
Introduction
Acid digestion of solid geological and environmental
samples is a useful technique for achieving low back-
Electronic supplementary material to this paper can be obtained
by using the Springer Link server located at http://dx.doi.org/
10.1007/s00216-001-1172-z
V.F. Taylor · A. Toms · H.P. Longerich (✉)
Department of Earth Sciences
and Centre for Earth Resources Research,
Memorial University of Newfoundland,
St. John’s, NF A1B 3X5, Canada
e-mail: henry@sparky2.esd.mun.ca
grounds in ICP-MS analysis, compared to fusion methods
also commonly used for solid samples. When using acid
digestion, the resulting solution has a lower content of to-
tal dissolved solids compared to methods using fluxing
agents [1]. High purity acids are also more economical
and easier to obtain than high purity fluxing agents.
Open-vessel focused microwave digestion signifi-
cantly increases the efficiency of acid digestion and has
overcome several limitations of conventional closed-ves-
sel microwaves. Open-vessel microwave digestions of or-
ganic and carbonate samples, which produce large vol-
umes of gases on digestion, can be carried out avoiding
the safety concerns of forming high pressure bombs and
sample loss caused by effervescence when opening closed-
vessels. Large samples of organic material can be digested
using the open-vessel microwave, minimizing the time-
consuming steps of drying and grinding [2]. Automated
evaporation-to-dryness is not possible with closed-vessel
systems, but can be accomplished in an open-vessel by at-
taching a pump to evacuate the fumes while the container
is heated.
Acid addition can also be automated with the open-
vessel microwave, allowing the use of procedures with
multiple heating and evaporation steps. Recent studies
have used the open-vessel microwaves for plant digestion,
eliminating the need for ashing prior to digestion [3], and
enables the use of strong oxidant acids with HF [4]. A fo-
cused microwave has also been used for online HCl di-
gestion of slurries of oxide materials [5]. Open-vessel
mineralization of industrial waste and sediment certified
materials was compared to alkaline fusion methods and
high pressure digestion for the determination of 10 ele-
ments by inductively coupled plasma-optical emission
spectrometry (ICP-OES) and each method was shown to
have advantages and disadvantages depending on the
sample matrix [6].
Conventional hotplate acid digestions are widely used
in geoanalysis but they nevertheless remain a major limit-
ing factor of analytical efficiency. Microwave digestion of
geological materials has not been widely reported, as
closed-vessel procedures limit the use of HF, which is

used to break down silicates. Open-vessel digestion of ge-
ological samples allows the use of HF to remove the Si as
volatile SiF4, further lowering the total dissolved solids in
the final digest and thus minimizing matrix and memory
effects in ICP-MS instrumentation. The removal of HF
also eliminates the need for sample introduction systems
that are HF resistant, or the addition of large quantities of
boric acid to complex the fluoride. Digestion using HF
can also be necessary in biological samples to break down
siliceous structures in plants [4].
Acid digestion of geologic samples is very successful
when applied to fine grained mafic samples, but digestion
is often incomplete when applied to coarse grained granitic
rocks, especially those containing significant quantities of
zircons (especially zircons which are large grained, young,
and contain low concentrations of U). This report com-
pares an open-vessel focused microwave acid digestion
with a conventional hotplate digestion of six rock refer-
ence materials (G-2 granite, MRG-1 gabbro, SY-2 syen-
ite, JA-1 andesite, JB-2 basalt and NIST SRM-688
basalt), six plant reference materials (BCR CRM-482
lichen, IAEA-336 lichen, NIST SRM-1547 peach leaves,
NIST SRM-1515 apple leaves, NIST SRM-8436 Durham
wheat flour, and NIST SRM-1575 pine needles), and two
“difficult to digest” granodiorite samples. Due to the pos-
sible occurrence of incomplete digestion for some sam-
ples, it was important to monitor the completeness of di-
gestion. For the granodiorite samples, the results obtained
by ICP-MS using digestion methods were compared with
those obtained using an XRF solid sample pressed-pellet
method [7], especially for the elements Rb, Sr, Y, Zr, and
Nb.
The procedure for open-vessel microwave digestion is
closely modeled on a current hotplate digestion method
used in the Department of Earth Sciences at Memorial
University, but reduces the digestion time from days to an
hour. There is potential to automate the entire microwave
procedure after the samples are weighed, including acid
addition and evaporation-to-dryness, and a 16 flask au-
tosampler could be attached and programmed [8].
Experimental
Reagents and labware
All water was distilled and deionised (Barnstead NanoPure II).
Concentrated nitric acid (Fisher Brand ACS.) was diluted to
8 mol L–1 and distilled in a Teflon two-bottle sub-boiling still
(Berhof America). Concentrated hydrofluoric acid (FisherBrand
ACS 49% v/v) was also distilled in a Teflon two-bottle still [9].
Oxalic (BDH ACS) and boric (Anachemia ACS) acids were ob-
tained in powdered crystalline forms and were used without further
purification. Three solutions were prepared: 1) 0.22 mol L–1 oxalic
acid, 2) 0.45 mol L–1 boric acid, 3) 0.45 mol L–1 boric acid solution
and 0.11 mol L–1HF. Digested samples were transferred to Corning
Snap Seal No.1730 vials for final dilution.
Microwave system
A PROLABO MicroDigest 301 system (Rhone-Poulenc, France),
consisting of a microwave heating/digesting unit and a control
361
unit, was used. A vacuum pump (KNF Neuberger Inc., Model UN
726.1.2FTP) was used to aid in the removal of volatile compo-
nents. Microwave sample vessels were machined in-house from
virgin Teflon PTFE. Hotplate vessels were Savillex 15 mL Teflon
screw cap jars. Microwave and hotplate vessels were cleaned by
heating for 2 days in 4 mol L–1 HNO3, then 2 days in 4 mol L–1
HCl, and were finally rinsed and heated in water for 12 h prior to
being dried in a flow of HEPA filtered air. Samples were weighed
into vessels and placed into the cavity of the microwave module,
where the lower few cm of the vessel were exposed to the micro-
waves, while the upper part of the vessel remained outside the mi-
crowave cavity at ambient temperature. Microwave power could
be regulated from 20 to 200 W, with energy delivered to the sam-
ple solution through a wave guide. A condenser top was screwed
on to the vessel and decreased loss through evaporation; it con-
tained a small opening through which acids could be added or the
vessel could be evacuated during drying steps [10]. During opera-
tion, the vessel, with condenser top attached, was placed in the
cavity of the microwave module and an evaporator head was
moved into place above the vessel. For refluxing steps, the evapo-
rator head sat about 2 cm above the top of the vessel, and for evap-
oration it was manually lowered and fitted into the top of the con-
denser, where it formed a seal. This evaporator head was attached
by a Teflon tube to the vacuum pump unit, which is a two piston
pump which rapidly draws air in through the tube attached to the
evaporator head, and out through an exhaust tube which feeds into
a fume hood. The pump lining and the tubes attached to it were
made from Teflon, which has a high resistance to digestion fumes
containing HF. When the evaporator head was in place, samples
could be evaporated-to-dryness during heating. A programmable
control unit was attached to the microwave module to operate the
heating stages of the digestion procedure. Programs are stored as a
series of steps in which the microwave power and time were spec-
ified. With the addition of a 3 pump dispenser, the program could
also control the addition of reagents. The system could be com-
pletely automated by the addition of a robotic arm to raise and
lower the condenser head between refluxing and condensing steps.
A sixteen vessel autosampler is also available for the microwave
unit which would allow multiple samples to be run unattended.
Procedure
Both digestion methods used were based reported procedures [11],
except that quantities of both sample and acid were doubled in the
microwave procedure (keeping sample to acid proportions the
same), because of the large sample chamber where the microwaves
are focused at the bottom of the vessel. In the first step of the di-
gestion, the oxidizing acid HNO3 and HF were used. A subsequent
evaporation with H3BO3 and HNO3 then complexes and removes
any residual HF. The addition of H3BO3 aids in the prevention of
the formation of insoluble fluorides, especially with Mg and Al,
which can otherwise remove trace elements from the solution.
Two further evaporations with HNO3 complete the oxidation of the
elements in solution and dissolve most metallic elements as solu-
ble nitrates [10]. In the final step, the digested sample is dissolved
with HNO3, then the HF-H3BO3 solution and oxalic acid solution
are added, and the sample solution is diluted by weight with water.
The low concentration of HF in the solution complexes elements
as their stable fluorides, and boric acid then serves to complex ex-
cess residual fluorine, producing a solution buffered in fluoride.
Oxalates form stable soluble complexes especially with Fe, which
at high concentrations can become insoluble in solution unless HCl
is added.
Development of the microwave method was closely modeled
on the hotplate method, keeping the same reflux/evaporation cy-
cles. Refluxing was achieved at 10% delivered power (20 W) and
evaporation was achieved at 65% power (130 W), while the use of
higher power was found to cause damage to the microwave vessel.
In the development of a method for open-vessel digestion of waste
samples [11], it was reported that the heating power and heating
time were found to have an insignificant effect on Hg recovery,
362
whereas procedures with multiple heating steps were found to im-
prove Hg recovery compared to a single step procedure.
Hotplate procedure [12]
Approximately 0.1 g of each sample was weighed into a clean
Teflon screw cap jar, and 2 mL of 8 mol L–1 HNO3 and 1 mL of
concentrated HF were added to each jar. The jars were then cov-
ered and heated overnight on a hotplate at 80–100 °C. If samples
were not dissolved, they were heated for an additional day. The jar
covers were then removed and rinsed into the jar with 8 mol L–1
HNO3, and the solutions were then evaporated to dryness at
80–100 °C. Jars were cooled and another 2 mL of 8 mol L–1 HNO3
and 1 mL of HF were added to each jar, and the solutions were
then heated for 4–5 days, then evaporated to dryness as before. To
each jar, 2 mL of 8 mol L–1 HNO3 and 1 mL of 0.45 mol L–1 boric
acid were added, and the solutions were evaporated to dryness on
the hotplate. Two more cycles of adding 2 mL of 8 mol L–1 HNO3
followed by evaporation-to-dryness were completed. Finally, 2 mL
of 8 mol L–1 HNO3 were added to each sample and the jars were
covered and warmed until all the residue had completely dis-
solved. Samples were then transferred to clean, weighed, Corning
Snap Seal No.1730 vials, and jars and covers were rinsed into the
vials with water. To each vial, 1.3 mL of 0.22 mol L–1 oxalic acid,
0.67 mL of 0.45 mol L–1 boric/0.11 mol L–1 HF solution, and wa-
ter were added to afford solutions with a final weight of approxi-
mately 60 g.
Microwave procedure
Approximately 0.2 g of powdered sample was weighed into a di-
gestion vessel, a condenser head was then attached and the vessel
was placed in the digester (Fig. 1). During heating stages, the up-
per portion of the flask, which was outside of the actual digester,
remained at ambient temperature, so that it acted as a reflux con-
denser to minimize sample loss. The heating and evaporation steps
of the procedure were automated, and acids were added manually
by pipette, although a pump dispensing system is available which
can be attached to the microwave unit and also be programmed to
dispense specified volumes of up to three different solutions. In
this work, the suction head was lowered manually for the evapora-
tion steps and then raised for refluxing. To more fully automate the
digestion process a robotic arm could to be added to the system to
raise and lower the suction head.
To the sample vessel were added 4 mL of 8 mol L–1 HNO3 and
2 mL of concentrated HF, and the solution was refluxed for 15 min
at 10% microwave power (20 W), with the evaporator head raised.
The evaporator head was then lowered, and the solution was
heated for 5 min at 65% power (130 W). The acid addition, reflux-
ing, and evaporation steps were then repeated once. Another 4 mL
Fig. 1 Schematic of microwave vessel, condenser top, and evapo-
rator head
of 8 mol L–1 HNO3, and 2 mL of 0.45 mol L–1 H3BO3 were added
to the sample vessel, and the solution was evaporated at 65%
power for 5 min. To the vessel, 4 mL of 8 mol L–1 HNO3 was
added, and the solution was evaporated for 5 min at 65% power.
This step was repeated once, then 4 mL of 8 mol L–1 HNO3 was
added and the solution was refluxed at 10% power for 4 min, to
dissolve all the sample residues. The sample solution was trans-
ferred to a clean, weighed, labeled vial, and 5.4 mL of 0.22 mol L–1
oxalic acid and 2.67 mL of the boric/HF solution were added. The
solution was then made up to a final weight of 120 g with water.
Inductively coupled plasma-mass spectrometer (ICP-MS)
All the ICP-MS data acquired for this study was obtained using a
Hewlett-Packard 4500 Series inductively coupled plasma mass
spectrometer.
Trace procedure
Samples were analyzed by two routine methods in use at the
Memorial University. The “Trace” package determined the iso-
topes 7Li, 85Rb, 86Sr, 89Y, 90Zr, 93Nb, 133Cs, 137Ba, 139La, 140Ce,
141Pr, 145Nd, 147Sm, 151Eu, 160Gd, 159Tb, 163Dy, 165Ho, 167Er, 169Tm,
173Yb, 175Lu, 177Hf, 181Ta, 205Tl, 206Pb, 207Pb, 208Pb, 209Bi, 232Th, and
238U. The Trace package uses a combination of external calibra-
tion, surrogate calibration, standard addition, and an internal stan-
dard for data reduction. The standard addition spike contained Li,
Sr, Zr, Cs, Ba, La, Pr, Nd, Sm, Er, Tm, Tl, Bi, and U. Into each
“spiked” tube was weighed 0.5 g of sample solution, 5.0 g of spike
and 4.5 g of 0.2 mol L–1 HNO3. Into each “unspiked” tube was
weighed 0.5 g sample solution and 9.5 g of 0.2 mol L–1 HNO3. An
internal standard solution of indium (In) was mixed on line using
the sample peristaltic pump using flow rates of 0.3 g min–1 sample
and 0.015 g min–1 In spike. This produced a solution which
reached the nebulizer having a concentration of approximately
0.08 g sample per kg solution. The samples and standards were
first background-corrected by subtracting the mean of all calibra-
tion blanks in the run (0.2 mol L–1 HNO3). Interference corrections
for the oxides of Ba, Pr, Nd, Sm, Eu, Gd, Tb, Dy, and Ho were ap-
plied to the analytes Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu, and Hf.
The elemental ion interference of 160Dy on 160Gd was also cor-
rected. Each of these interference corrections were determined
from the external standard solutions used and then normalized to
the UO+/U+ ratio in the calibration standards relative to that of the
spiked samples. Two external standard solutions were used for the
calibration of all elements, with the exception of Nb and Ta, which
were surrogated by Zr or Hf. A matrix correction factor was calcu-
lated from the ratio of the sensitivity determined by external cali-
bration to the sensitivity determined by using internal standardiza-
tion from each element in the spike. For elements not contained in
the spike, the matrix was corrected using mass interpolation of the
determined matrix factors. Drift was corrected using the signal
from the In internal standard.
Environmental/exploration procedure
The “environmental/exploration” package, determined 51V, 55Mn,
59Co, 60Ni, 66Zn, 107Ag, 111Cd, 118Sn, 121Sb, 125Te, 139La, 140Ce,
141Pr, 145Nd, 167Er, 169Tm, 175Lu, 208Pb, 209Bi, and 232Th. The di-
gested solutions containing geological materials were diluted,
0.2 g sample to 9.8 g 0.2 mol L–1 HNO3, for analysis by this pack-
age, giving a final solution reaching the nebulizer of approxi-
mately 0.035 g sample per kg solution. The biological reference
materials, which contained much lower concentrations of most el-
ements, as well as much lower total dissolved solids, were diluted,
2 g sample to 8 g 0.2 mol L–1 HNO3 to give a final dilution of
0.35 g sample kg–1. During analysis, as with the trace package, an
internal standard solution was pumped in online to the sample so-
lution before it reached the nebulizer; which in this case contained
Table 1 Detection limits and mean concentrations with standard deviations determined Reported values [13] for reference materials and XRF analysis of D-314 Granodiorite are
from triplicate analysis of two geological reference material (MRG-1 Gabbro and G-2 given for comparison. All concentrations are in mg kg–1
Granite) and a “problem” sample (D-314), prepared by microwave and hotplate digestion.

Det. MRG-1 G-2 D-314

Limit
Reported Microwave ± Hotplate ± Reported Microwave ± Hotplate ± XRF Microwave ± Hotplate ±
Li 0.1 4.2 4.0 0.3 4.0 0.3 36 31 0.1 34 3 5.4 1.8 8.0 0.2
Co 0.2 87 77.2 2.3 77.4 1.3 4.6 4.51 0.25 4.02 0.17 33 2 35 2
Ni 0.5 193 178 4 183 2 4.9 2.4 1.0 3.2 0.5 7 19.8 0.3 25.5 1.0
Zn 5.7 191 193 25 176 7 85 93 5 122 6 31 71 5 85 6
Rb 0.2 8.5 7.2 0.2 7.4 0.7 170 133 13 184 37 58.6 14.3 4.0 57.0 5.1
Sr 1.2 266 272 7 277 30 478 435 12 501 149 876.6 463 105 809 91
Y 0.005 14 11.9 0.3 12.2 1.1 11.4 6.7 0.5 8.7 2.3 15.3 6.9 3.1 16.0 2.3
Zr 0.14 108 95 3 98 9 300 39 4 68 8 158.2 74 16 112 20
Nb 0.003 20 22.4 0.4 23.6 1.3 13 12.1 0.2 14.1 1.4 10 9.1 0.1 9.8 1.1
Cd 0.045 0.168 0.181 0.006 0.152 0.011 0.025 ld ld ld ld 0.126 0.046 0.093 0.006
Cs 0.07 0.57 0.58 0.003 0.60 0.03 1.33 1.29 0.02 1.36 0.11 0.083 0.048 0.194 0.008
La 0.006 9.8 8.9 0.1 9.1 0.6 86 69.8 7.6 94.2 7.7 14.6 5.2 34.9 2.0
Sm 0.03 4.5 4.37 0.08 4.52 0.31 7.2 6.31 0.42 7.33 0.47 3.4 1.0 6.4 0.5
Eu 0.03 1.39 1.43 0.02 1.45 0.10 1.41 1.18 0.07 1.51 0.06 0.79 0.24 1.55 0.15
Tm 0.008 0.11 0.15 0.001 0.15 0.004 0.17 0.10 0.01 0.10 0.03 0.14 0.04 0.24 0.01
Hf 0.02 3.76 3.93 0.19 3.98 0.26 7.9 0.87 0.11 5.37 1.59 1.89 0.42 2.87 0.54
Pb 0.76 10 5.34 0.90 4.70 0.34 31 29.1 0.8 31.6 0.8 17 15.4 1.1 16.1 0.8
Th 0.004 0.93 0.77 0.01 0.81 0.06 24.6 23.9 1.3 28.6 2.7 1.36 0.42 2.97 0.19
363
364
Sc, In, Re, and U. The same online dilution was used as before.
Data was reduced first by a background-correction, which was ap-
plied by subtracting the median calibration blank value for the run.
Interferences from Ca and Ti oxides were normalized to the
U+/UO+ ratio and subtracted from the signal for the elements Co,
Ni, and Zn. Matrix correction is calculated from the internal stan-
dard elements Sc, In, and Re, and mass interpolated or extrapo-
lated for each of the analytes. Three external standards containing
the analyte elements are used for calibration.
Results and discussion
Complete data tables containing detection limits and mean
concentrations and standard deviations for six geological
reference materials (Table S1), two “problem” samples
(Table S2), and six biological materials (Table S3), pre-
pared in triplicate by the microwave and hotplate diges-
tion method, are included as Electronic Supplementary
Material (http://dx.doi.org/10.1007/s00216-001-1172-z).
In the print-version, element concentrations determined
by each method are given for three geological materials
(MRG-1, G-2, and a “problem” sample, D-314) in Table 1.
All procedure blanks for the elements reported are lower
than detection limits. Reference values [13], are given
for reference materials G-2 (USGS), MRG-1 (CCRMP),
SY-2 (CCRMP), JA-1 (GSJ), JB-2 (GSJ), and SRM-688
(NIST) for comparison with the ICP-MS analysis. Ac-
ceptable agreement with the digestion methods is defined
as overlapping within one standard deviation of the mean
concentration, calculated from triplicate samples prepared
separately. Results of analysis from the two digestion
methods show agreement between determined concentra-
tions for the more easily dissolved reference materials
(MRG-1, SRM-688, JB-2, and SY-2), with the exception
of Ni in SY-2 and Cd in JB-2, which are unexplained.
A high standard deviation for the mean concentration of
Ni in JA-1 is possibly due to contamination of a sample.
Determined concentrations of the rare earth elements
show agreement with reference values for these samples.
The concentrations of Zr and Hf in G-2, a granite con-
taining zircons, were much lower than literature values,
clearly indicating incomplete digestion of the sample. The
elements Zr and Hf are contained in zircons, a mineral
which is difficult to dissolve with acid, although the ease
with which it can be digested depends on its degree of
metamictization and grain size. The microwave digestion
yields lower concentrations of these elements in solution,
as well as the elements Rb, Sr, and Y, and the rare earth el-
ements, suggesting this difficult to dissolve phase is
slightly better digested by the hotplate method. The an-
desite sample, JA-1, has a high value for the Hf concen-
tration from the hotplate digestion, possibly due to conta-
mination. Hotplate and microwave methods are otherwise
comparable, except for slight differences in the values for
Cd and Sn.
The two “problem” samples, D-314 and D-316, were
digested in triplicate by both methods and were also ana-
lyzed using XRF. The samples are granoriodites from the
Wathaman Batholith in northern Saskatchewan. Samples
D-314 and D-316 contain 25% and 15% hornblende and
biotite, respectively, as well as >1% of the accessory min-
erals titanite, epidote, allanite, apatite, and zircon. The
presence of these accessory minerals, especially zircon, in
the samples makes them difficult to digest using acid. The
concentrations of the analytes in the samples digested by
the hotplate method are higher for most of the elements,
suggesting the hotplate method performs a more complete
digestion of all the minerals. The concentrations from the
hotplate digestion show better agreement with XRF val-
ues than do the results of the microwave digestion for the
elements Rb, Sr, Y, and Ba. The concentrations of Zr and
Ce are closer to the XRF values for the hotplate digestion
than the microwave procedure, but are still significantly
lower. The low concentrations of alkali and alkaline earth
elements (Rb, Sr, Cs, and Ba) in the samples digested by
the microwave method, compared to the hotplate method,
suggested there was incomplete digestion of the horn-
blende and biotite phases in the samples. These minerals
are micas that are sometimes difficult to breakdown by
acid digestion due to their flat, layered structure, and the
more incomplete digestion by the microwave method,
compared to the hotplate procedure, may be due to the fo-
cused microwaves being unable to reach the layered mi-
cas. The concentrations of Zr, Y, Hf, and the REEs were
significantly higher in the hotplate digested samples than
those digested in the microwave for both problem sam-
ples, suggesting the accessory minerals were also more
resistant to the microwave digestion.
Six biological reference materials prepared in triplicate
by the hotplate and microwave methods show satisfactory
agreement between the methods for most elements. Certi-
fied and recommended values from the distributing organ-
isation also showed agreement with determined concen-
trations.
Conclusions
A procedure was developed for the digestion of geologi-
cal and environmental materials using a semi-automated
open-vessel microwave apparatus, for subsequent analysis
using ICP-MS. Microwave digestion does have the advan-
tage of greatly reducing processing time, enabling start-to-
finish sample preparation in one hour, reduced from one
to two weeks required by the hotplate method. A further
advantage is the potential for complete automation of the
process, with an apparatus that has been designed for
“load it and leave” operation.
While this work did not show the anticipated ability to
digest samples with difficult to dissolve phases, such as
zircons, these samples are generally not suited for routine
acid dissolution methods. Satisfactory dissolution of re-
sistant phases were accomplished with a high pressure mi-
crowave [14], although the procedure is labour intensive
as samples were transferred to beakers and evaporated on
a hotplate after the microwave heating. The current prac-
tice in our laboratory for dissolving resistant mineral
phases is to use a sodium peroxide sinter method. As
these granitic materials have higher analyte concentra-

tions (especially the lanthanides), additional reagent con-
tamination from the flux is of less importance. A pre-
analysis using XRF is employed to select samples for
which acid digestion difficulties are expected, in which
case the sample owner is advised against using an acid di-
gestion.
Open-vessel microwave digestion appears to be a suit-
able and rapid alternative to conventional hotplate diges-
tion for mafic geological and environmental plant materi-
als. The addition of open microwave to elemental analysis
will advance the long neglected science of sample prepa-
ration.
Acknowledgements The authors acknowledge the large financial
support of the Natural Sciences and Engineering Research Council
of Canada (NSERC) which provided the equipment grant for the
purchase the microwave system. An NSERC research grant to
HPL contributed to this work. Thanks to Graduate Studies for
graduate student financial support to VFT. Special thanks to Don
Fillier of the university department of Technical Services who as-
sisted in the vacuum exhaust system which went through several
trials before an HF resistant system was put in place. Thanks to
Doug Bolger of Technical Services who fabricated the microwave
digestion vessels. Thanks to Mike Tubrett and Lakmali Hewa who
contributed to ICP-MS instrument maintenance and operation.
Thanks to T. MacHattie and G. Jenner for the two unknown sam-
ple materials.
365
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