Anal. Chem.

2001, 73, 1515-1520

High-Temperature, Microwave-Assisted UV
Digestion: A Promising Sample Preparation
Technique for Trace Element Analysis
Dieter Florian and Gu
1 nter Knapp*

Institute for Analytical Chemistry, Micro- and Radiochemistry, Graz University of Technology,
Technikerstrasse 4, A-8010 Graz, Austria

A novel, microwave-assisted, high-temperature UV digestion procedure was developed for the accelerated decomposition of interfering dissolved organic carbon (DOC)
prior to trace element analysis of liquid samples such as,
industrial/municipal wastewater, groundwater, and surface water, body fluids, infusions, beverages, and sewage.
The technique is based on a closed, pressurized, microwave digestion device. UV irradiation is generated by
immersed electrodeless Cd discharge lamps (228 nm)
operated by the microwave field in the oven cavity. To
enhance excitation efficiency an antenna was fixed on top
of the microwave lamp. The established immersion system
enables maximum reaction temperatures up to 250-280
C, resulting in a tremendous increase of mineralization
efficiency. Compared to open UV digestion devices, decomposition time is reduced by a factor of 5 and the
maximum initial concentration of DOC can be raised by
at least a factor of 50. The systems performance on a realtype sample was evaluated for the mineralization of
skimmed milk (IRMM, CRM 151) and subsequent determination of trace elements using standard spectroscopic techniques. Recovery for Cd (109%), Cu (112%),
Fe (99%), and Pb (96%) showed good agreement with the
95% confidence interval of the certified values.
Trace analytical measurement techniques suffer from a significant decrease in detection power by matrix constituents. The
potentially very low detection limits (LODs) can only be achieved
when concentrations of dissolved inorganic and organic matrix
compounds are kept to a minimum.1 Especially, the presence of
dissolved organic carbon (DOC) may cause severe interferences
for trace element determination by, for example, DPASV,2-4
ICPMS,1,5,6 and AAS.2,7,8 Thus, complete oxidation of organic matrix
* Corresponding author: (fax) ++43/316/8738304; (e-mail) knapp@
analytchem.tu-graz.ac.at.
(1) Krachler, M.; Radner, H.; Irgolic, K. Fresenius J. Anal. Chem. 1996, 355,
120.
(2) Golimowski J.; Golimowska K. Anal. Chim. Acta 1996, 325, 111-133.
(3) Kolb M.; Rach P.; Schafer J.; Wild A. Fresenius J. Anal. Chem. 1992, 342,
341-349.
(4) Wu
rfels M.; Jackwerth E.; Stoppler M. Anal. Chim. Acta 1989, 226 (1),
31-41.
(5) Begerov J., Turfeld M., Duneman L. J. Anal. At. Spectrom. 1996, 11, 913916.
(6) Begerov J.; Turfeld M.; Duneman L. J. Anal. At. Spectrom. 1997, 12, 10951098.
10.1021/ac001180y CCC: $20.00
Published on Web 03/02/2001

2001 American Chemical Society

constituents of biological samples is strongly recommended to

achieve accurate and reproducible analysis results.1,2,4,9
Digestion of organic samples routinely is carried out in closed,
pressurized devices, either microwave or conventionally heated,
applying concentrated mineral acids. A major drawback of this
digestion procedure is the introduction of relatively high background levels due to acid impurities. Even at the highest degree
of purity commercially available and after additional subboiling
distillation, the blank level of acids remains too high for certain
ultratrace determinations.5,6 Furthermore, wet decomposition
procedures lead to high acid concentrations in the resulting
digestion solution, which are not tolerated by many analytical
methods, especially by ICPMS, and thus have to be evaporated
or diluted prior to analysis.
The photochemical process of UV oxidation represents a
promising alternative for the decomposition of DOC in liquid
samples.2 Only minimum amounts of reagents are required
compared to conventional acid digestion procedures. Hence, a
potential source of contamination is eliminated. Furthermore,
sample dilution is avoided after digestion, resulting in an improvement of the detection limit. Therefore, especially ultratrace
determinations in the field of environmental analysis benefit from
this contamination-free digestion technique.5,6,10 Typical UV digestion equipment, fundamentals of the degradation mechanism, and
common fields of application were reviewed, comprehensively.2
So far, the majority of applications in trace element analysis were
performed using so-called batch devices. These open systems
work at atmospheric pressure and suffer from certain drawbacks
such as limited reaction temperature (65-90 C) to prevent loss
of volatile analytes and solvent evaporation, limited initial concentration of organic compounds, extended degradation time up
to several hours for a matrix of 100-300 mg L-1 C, and decreasing
decomposition rates for samples of high turbidity (e.g., heavily
polluted wastewater).
In general, reaction temperature turned out to be the key
parameter for UV mineralization. In fact, this phenomenon was
observed for the decomposition of vanillic acid as a model
substance for polyphenolic compounds in wastewater even within
(7) Bauer K. H.; Gehron M.; Wiskamp V. Poster at Tagung der Fachgruppe
Wasserchemie, Lindau, Germany, 1997.
(8) Schwedt G.; Petri J. Labor Praxis 1992, (Dec), 12-23.
(9) Mingorance, M. D.; Perez-Vazquez, M. L.; Lachica, M. J. Anal. At. Spectrom.
1993, 8, 853.

Analytical Chemistry, Vol. 73, No. 7, April 1, 2001 1515

a temperature range of 10-40 C.11 Other authors reported

considerable acceleration for the degradation of stable aromatic
systems when temperature was increased from 65 to 90 C.3 To
contribute to the advancement in UV mineralization technology,
now the main concern should be focused on the acceleration of
the photodegradation process and its application to sample
matrixes containing high DOC levels. Hence, the average decomposition temperature has to be increased considerably. This can
be achieved easily by application of a closed, pressurized, digestion
device. This way, reaction temperature is raised far above the
solutions boiling point without risking solvent evaporation or loss
of volatile elements. By applying a microwave-assisted device,
additional acceleration of the reaction rate by microwaves can be
observed. At present, this effect is under investigation since it is
assumed that microwave fields induce higher levels of chemical
and physical activity.12 Further improvement of chemical reactivity
was discussed recently for a combined microwave/UV process
due to simultaneous irradiation by ultraviolet (causing excitation
of valence electrons) and microwave (causing molecular rotation
and polarization) energy.13,14 However, the effects observed during
so-called microwave photochemistry are not investigated by now,
since this is definitely a new field of chemistry.
In this paper, a novel high-temperature microwave-assisted UV
mineralization procedure, using a commercially available pressurized digestion device, is described.15This procedure combines
the benefits of microwave digestion with those observed for UV
mineralization. The systems performance was evaluated for the
mineralization of model substances and of skimmed milk (certified
reference material CRM 151, IRMM) with subsequent determination of trace elements.
EXPERIMENTAL SECTION
Reagents. Nitric acid (69.5%), potassium hydrogen phthalate
(C8H5KO4) pro analysis reagent grade, and hydrogen peroxide
(30%). Suprapur reagent grade, were obtained from Merck
(Darmstadt, Germany). Nitric acid was purified in-house by
subboiling distillation using a quartz still. Standard solutions for
Cd, Cu, Fe, Pb, and Sc were prepared from 1000 mg L-1 (2%
HNO3) standard solutions (SPEX Plasma Standard, SPEX,
Metuchen, NJ). For cleaning purposes, detergent Decon90 was
obtained from Zinser Analytik GmbH (Frankfurt, Germany). The
certified reference material CRM 151 (skimmed milk) was
obtained from the European Commission Joint Research Center,
Institute for Reference Materials and Measurements (IRMM)
(B-2440 Geel, Belgium). Solutions were made up with distilled,
deionized (18.2 M cm-1) water (Barnstead Nanopure, Dubuque,
IA). For the production of UV lamps, Hg, Cd, and Zn, pro analysis
reagent grade, were obtained from Merck. Additional purification
(10) Krachler, M.; Alimonti, A.; Petrucci, F. J. Anal. At. Spectrom. 1998, 13,
701-705.
(11) Benitez F. J.; Heredia J. B.; Acero J. L. Toxicol. Environ. Chem. 1996, 56
(1-4), 199-210.
(12) Fanslow G. E. Mater. Res. Soc. Symp. Proc. 1991, 189, 43-48 (Microwave
Process. Mater. 2).
(13) Chemat S.; Aouabed A.; Bartels P. V.; Esveld D. C.; Chemat F. J. Microwave
Power Electromagnetic Energy 1999, 34, 55-59.
(14) Cirkva V.; Hajek M. Microwave photochemistry in organic synthesis. In
Proceeding of the Conference of Microwave and High Frequency Heating,
Fermo, Italy, 1997; pp 153-154.
(15) Zischka M.; Kettisch P.; Schalk A.; Knapp G. Fresenius J. Anal. Chem. 1998,
361, 90-95.

1516

Analytical Chemistry, Vol. 73, No. 7, April 1, 2001

was performed by distillation when transferred into the quartz

bulb. Rare gases Ar, Kr, and Xe, 5.0 purity, were obtained from
AGA Gas GmbH & Co KG (Hamburg, Germany).
Instrumentation. A Multiwave pressurized microwave digestion device, equipped with 50-mL quartz vessels, were obtained
from Anton Paar GmbH (Graz, Austria) and Perkin-Elmer (Norwalk, CT). A Cd low-pressure discharge microwave lamp (MWL)
was developed in cooperation with Gesellschaft fur lichttechnische
Erzeugnisse mbH (G.L.E., Berlin, Germany). It was made from
quartz glass,: type, Ilmasil; PN thickness, 1.0 mm; filler elements,
1 mg of Cd + 4 mbar Ar; bulb dimensions, 30 mm hight, 15 mm
width, antenna length 35 mm. The emission domain in the UV
region is located at 228 nm. The radiation intensity of the MWL
during the digestion procedure depends on the microwave energy
absorbed and varies from less than 1 W to more than 10 W. The
actual microwave power input is regulated automatically by the
Multiwave to maintain the preselected digestion temperature and
is dependent on sample type and amount as well as on the number
of digestion vessels employed. A Shimadzu TOC-5050 total organic
carbon analyzer (Shimadzu GmbH Europe, Duisburg, Germany)
was used for the determination of the remaining organic carbon
content. ICP-AES (Optima 3000XL, Perkin-Elmer, Norwalk, CT)
and GFAAS (AAnalyst 800, Perkin-Elmer, Norwalk, CT) were
employed for element determination.
Digestion Technique. A 7-mL aliquot of sample solution, 1
mL of H2O2, and 50 L of HNO3 were mixed in the quartz vessel
and digested by means of the Multiwave at 72 bar reaction
pressure. The microwave energy is reduced automatically when
the reaction pressure in one of the vessels exceeds the limit of
72 bar. The preadjusted parameters at the Multiwave were as
follows: microwave power, 1000 W; digestion time, 30 min with
cooling fan at level 1; cooling time, 15 min with cooling fan at
level 3.
Sample Preparation. UV mineralization of skimmed milk was
performed for five samples and one blank simultaneously. An
aliquot of 75 ( 2 mg of powder was transferred to each digestion
vessel already containing an UV source. The powder was
suspended in 7 mL of H2O (initial DOC concentration, 4000 mg
L-1 C) and acidified with 50 L of HNO3 + 50 L of HCl.
Immediately before sealing the vessel, 1 mL of H2O2 was added.
Vessels were sealed and heated by following the established
microwave program. Upon finishing the digestion step, each vessel
was carefully opened in a fume hood at ambient temperature to
release the reaction pressure. The resulting sample solution was
transferred quantitatively into a 10-mL polyethylene (PE) tube.
The certified reference material was not oven-dried prior to
digestion to prevent loss of volatile compounds and possible
contamination. The element concentrations measured were based
on dry weight after correcting for moisture content determined
from separate subsamples dried in an oven at 105 C for 24 h.
Cleaning. Each quartz vessel and its corresponding quartz
lamp were treated like a unit to avoid any contamination of the
UV source. Vessels and lamps were soaked in 5% Decon90 for 48
h followed by careful rinsing with distilled, deionized water. After
this treatment, a pressure-controlled digestion was performed with
3 mL of HNO3 for a period of 20 min followed by careful rinsing
with distilled, deionized water.

Analysis. Determination of the remaining DOC was carried

out with a matrix solution containing 0.5 vol % HNO3. A linear
calibration with up to three DOC standards was prepared. For
calibration, C8H5KO4 was used as the standard compound.
Calibration standards ranging from 0 to 200 mg L-1 were prepared
daily by diluting a 1000 mg L-1 stock solution. Samples were
diluted according to the calibrated range. Trace element determination was carried out with a matrix solution containing 0.5
vol % HNO3. For AAS measurements, the instrument manufacturers recommended temperature programs were applied; linear
calibration with up to four element standards were prepared as
follows: Cd, 0-5 g L-1; Cu, 0-20 g L-1; and Pb, 0-40 g L-1.
Fe was determined by ICP-OES. Linear calibration ranged from
0 to 1000 g L-1, Sc was used as an internal standard (1000 g
L-1). Samples were diluted according to the calibrated range. All
calibrations were verified by measuring control standards periodically.
RESULTS AND DISCUSSION
Description of the High-Temperature UV Digestion Device. In contrast to an open batch device equipped with one
electrically driven UV source situated in the center surrounded
by symmetrically distributed sample holders,2 the presented UV
digestion device establishes a multiple immersion system using
special, microwave-boosted, electrodeless discharge lamps. Single
UV sources are directly immersed into the sample solution inside
of the individual digestion vessels. Lamp operation is initiated and
maintained by the oscillating microwave field distributed within
the oven cavity. Immersed UV lamps simply behave like inert
quartz bulbs, which continuously emitting UV irradiation. Consequently, this system does not require a separate power supply
for the operation of the UV sources. Furthermore, pressurized
vessels do no require a separate cooling device to prevent sample
evaporation. Here, the microwave device automatically controls
reaction temperature and pressure.15 In Figure 1 a schematic is
given of the quartz pressure reaction vessel with the polyetheretherketone (PEEK) vessel jacket containing a MWL. The quartz
vessel with the MWL and the appearance of the microwaveboosted plasma discharge is shown in Figure 2. The maximum
number of samples treated simultaneously during one digestion
run depends on the employed rotor system (vessel holding
device). In this project, the number was limited to six vessels per
run (Figure 3); however a new rotor generation is already available
offering space for 12 vessels.
Development of a Microwave-Boosted UV Source. The
application of an electrodeless discharge lamp (EDL) located
directly inside the closed digestion vessel is the only possibility
to generate UV radiation inside a high-pressure, microwaveassisted digestion device. However, operation of a standard EDL
is seriously impaired inside the applied kitchenlike microwave
cavity. First, the observed electromagnetic field is of low homogeneity, since generated microwave energy is simply transferred
by two waveguides into the oven cavity and is distributed by
multiple reflections. Second, the amount of microwave-absorbing
material (e.g., sample solution, number of digestion vessels, rotor
system) and its orientation in the cavity additionally affect the
electric field strength. Consequently, the electromagnetic field
established inside such a cavity is by far less homogeneous and
of lower electric field strength compared to standard microwave-

Figure 1. Schematic of a high-pressure digestion vessel with MWL:

a, plug; b, safety disk; c, seal; d, screw cap; e, microwave radiation,
h1; f, PEEK vessel jacket; g, quartz pressure reaction vessel; h,
electrodeless UV source; i, UV radiation, h2; j, vessel base plate; k,
air flow.

focusing antennas. Finally, the surrounding solution in the

immersion system caused serious shielding for the microwave,
thus impaired excitation efficiency of the EDL. To circumvent
these problems, the development of an appropriate metal antenna
was required to focus the microwave field into the EDL, thus to
enhance the electric field constant in the lamp environment. A
schematic of the established MWL is given in Figure 4.
The antenna was made of a molybdenum foil positioned on
top of the MWL, which was directly embedded into quartz to avoid
contact between the metal and the sample solution. A W wire
established the connection between the Mo foil and the discharge
volume (quartz bulb). Considering the physical fundamentals of
an alternating high-frequency radiation, maximum interaction
between the microwave field and the antenna was assumed for
an antenna length corresponding to 1/4 MW. In this case (MW )
0.1224 m), the theoretical length was calculated to 30.6 mm and,
thus, corresponded well with the obtained experimental result of
30 ( 3 mm for the optimum Mo foil length. Using this antenna
construction, MWL operation and thus UV generation was
maintained during the entire digestion run for a microwave power
level of PMW g 100 W delivered by the magnetron. This means
that the microwave energy distributed to the MWL is much lower.
Analytical Chemistry, Vol. 73, No. 7, April 1, 2001

1517

Table 1. Selection of MWL Prototypes

MWL type

system
emission domain
filler element
fill gas
% [DOC]remaining
( SD (n ) 3)
bulb dimensions
(height/width)

Hg

Cd

Zn

high-pressure
metal vapor
254 nm
1.5 mg
4 mbar Ar
1.1 ( 0.9

low-pressure
metal vapor
228 nm
0.5 mg
4 mbar Ar
(a) 0.13 ( 0.04
(b) 0.03 ( 0.02
(a) 30/15 mm
(b) 52/12 mm

low-pressure
metal vapor
213 nm (weak)
0.5 mg
4 mbar Ar
5.4 ( 0.3
30/15 mm

30/15 mm

Kr

Xe

gas discharge

gas discharge

<400 nm (weak)

<400 nm (weak)

4 mbar Kr
6.5 ( 0.7

4 mbar Xe
9.3 ( 0.8

30/15 mm

30/15 mm

Figure 2. Quartz pressure reaction vessel with MWL.

Figure 4. Schematic of a MWL.

Figure 3. Rotor system with digestion vessel and MWL.

Different lamp dimensions, filler elements, and fill gases were

investigated according to recommendations given in the literature.16 A selection of MWL prototypes is given in Table 1. The
performance of each prototype was evaluated by UV oxidation of
a 2500 mg L-1 C solution of C8H5KO4 following the given digestion
1518 Analytical Chemistry, Vol. 73, No. 7, April 1, 2001

procedure and subsequent determination of the remaining carbon.

The calculated value is expressed as percent remaining DOC of
the initial concentration. The lower the [DOC]remaining value, the
better is the obtained mineralization efficiency. Three different
metal vapor discharge systems and two rare gas discharge
systems are presented. First, a Hg metal vapor MWL was
developed. This system is operating significantly above the lowpressure range but does not establish a high-pressure discharge
either. This is demonstrated by the resulting line-rich emission
spectrum (Figure 5) showing common Hg resonance lines (e.g.,
Hg 254 nm) but no continuum located in the deep UV typical for
a high-pressure discharge. To the contrary, a low-pressure system
was established for Cd and Zn due to the lower volatility of these
(16) Sneddon J.; Browner R. F.; Keliher P. N.; Winefordner J. D.; Butcher D. J.;
Michel R. G. Prog. Anal. Spectrosc. 1989, 12, 369-402.

Table 2. Comparison of Open versus Closed UV

Mineralization

Figure 5. Emission spectrum of a Hg MWL.

Figure 6. Emission spectrum of a Cd MWL.

metals. Especially for Cd, the reaction temperature ranging from

250 to 280 C turned out to be perfectly suited for generation of
an ideal low-pressure discharge, since the heatup effect in the
immersion system resulted in a metal vapor pressure in the range
of 1.3 10-3-1.3 10-2 mbar (following the vapor pressure table
for Cd) and thus corresponded well with the recommended
value.16 In this case, only single resonance lines (e.g., Cd 228 nm)
were observed (Figure 6). The investigated rare gas discharge
systems of Kr and Xe require further optimization work. By now,
the emission domain is located in the visible and IR region;
however, emission in the range of < 200 nm (vacuum UV, VUV)
was reported recently for microwave-boosted systems.17,18 Production and appropriate spectral characterization of MWL prototypes
is described in detail elsewhere.19
High-Temperature, Microwave-Assisted UV Oxidation
versus Open-Vessel UV Mineralization. The presented UV
digestion device outmatched by far common, open batch devices
(Table 2). The rigorous conditions established with the closedvessel, microwave/UV decomposition system result in a significant
improvement for the UV mineralization process. First, enormous
acceleration is achieved for the light-induced degradation, and
second, access to complex samples matrixes containing a high
fraction of DOC is enabled. Beside the elevated reaction temperature and the enhancement in reactivity, several other advantages
(17) Ametepe J. D., Diggs J., Manos D. M., Kelly M. J. J. Appl. Phys. 1999, 85
(11), 7505-7510.
(18) He Z. A microwave-driven excimer lamp and its applications. Dissertation,
University of Missouri, Columbia, MO, 1996.
(19) Florian D. Development of a High-Temperature, Microwave-Assisted, UV
Digestion Device for Sample Preparation in Trace Element Analysis.
Dissertation, Technical University, Graz, Austria, 2000.

parameter

open system

closed system

temperature
pressure
maximum DOC
av digestion time
reagent addition
principle

65-90 C
atmospheric
100-300 mg L-1
up to several hours
continuous
batch type

250-280 C
72 bar
5000-7500 mg L-1
30 min
discontinuous
immersion type

arise from this system. The immersed UV source enables a high

efficiency of generated UV irradiation due to the 4 geometry.
The extremely short light pathway (maximum light pathway 5-10
mm) avoids severe reduction of UV irradiance and thus enables
mineralization of heavily polluted (high-turbidity) samples as well.
Following this degradation only induced by UV irradiation turned
out to be rather efficient as well. Furthermore, emission domain
for the Cd MWL ( ) 228 nm) was moved closer to VUV and,
thus, improved hydroxyl radical yield for the photoinduced H2O2 decay in comparison to standard Hg UV sources
( ) 254 nm).19 Since no interfering air atmosphere is present
between the UV source and the sample, the application of VUV
is possible if an appropriate light source is developed. Irradiation
with VUV considerably improves degradation yield.20 Beside the
increased energy transfer, this is mainly attributed to almost
quantitative absorption of the VUV by the aqueous medium and
dissolved gases, followed by the generation of radical species.21
In this case, no oxidant would be required to catalyze the
degradation process during UV mineralization, followed by almost
quantitative elimination of contamination introduced through
reagents.
Furthermore, a high-temperature device enables dissolution
of solid organic matrixes using diluted mineral acids and thus
opens the process of photochemical degradation to the mineralization of solid organic samples as well. This combined acid/UV
digestion is under investigation, but so far it appears that the
required amount of acid may be reduced dramatically, hence again
decreasing risk of contamination and causing less dilution after
digestion.
Finally, from the technical point of view, no separate power
supply is required for the operation of the UV lamps, no external
cooling device is required, and reaction temperature is controlled
and regulated by the microwave systems electronics. Consequently, quality control tools are introduced to the process of UV
mineralization, establishing a modern sample preparation technique. So far, the discontinuous reagent addition has turned out
to be the only disadvantage of this closed UV system. Continuous
addition of small amounts of the oxidant most likely results in
further acceleration of the microwave-assisted UV degradation
process.19,22 Furthermore, the total reagent amount required might
be decreased, reducing risk of contamination. Technical realization
of continuous reagent addition will be very critical, due to reagent
introduction into a pressurized reaction vessel and due to the
transport of a microwave-absorbing medium through the oven
cavity.
(20) Baum G.; Oppenlander T. Chemosphere 1995, 30 (9), 1781-1790.
(21) Jakob L.; Hashem T. M.; Bu
rki S.; Guindy M. N.; Braun A. M. J. Photochem.
Photobiol. Chem. 1993, 75, 97-103.
(22) Kroder H.; Bauer K. H.; Saur D. Vom Wasser 1994, 82, 269-279.

Analytical Chemistry, Vol. 73, No. 7, April 1, 2001

1519

Safety Aspects. Process control mechanisms in terms of

continuous documentation of reaction temperature and pressure
and safety precautions are simply overtaken from the basic
microwave digestion device.15 MWL operation is allowed only
using standard high-pressure digestion vessels and corresponding
PEEK bombs. This way, no dangerous UV irradiation can get out
of the digestion device. For handling of the MWL, special care is
required as for other quartz glass equipment. In case of breakage,
the Cd-contaminated quartz bulb must be disposed as toxic waste.
Application to a Real-Type Sample Matrix. Optimization of
principle degradation parameters was carried out using organic
model compounds. Mineralization efficiency is dependent on
reaction temperature, digestion time, reagent concentration, acid
medium, and initial concentration of DOC; detailed documentation
is given elsewhere.19 Here, skimmed milk was chosen as a
representative sample for beverages containing a relatively high
organic fraction. The dissolved milk powder (IRMM, CRM 151)
resulted in a solution of very high turbidity. At the dilution factor
applied, the concentration of initial DOC was determined to be
4000 mg L-1 C. Within a mineralization time of 30 min, 99% of
the initial DOC was decomposed. No process optimization was
required, since a clear and colorless sample solution with only a
low fraction of remaining DOC was obtained. Recovery for Cd
(109%), Cu (112%), Fe (99%), and Pb (96%) showed good agreement with the 95% confidence interval of the certified value (Table
3). Since no trace element blank levels were determined, introduction of the UV lamps did not contaminate the digestion vessels. If
interferences would have been observed for the subsequent
analytical method caused by the remaining fraction of DOC,
mineralization efficiency will be improved first, by extending the
digestion time and, second, by reducing the amount of sample
(initial DOC) dissolved prior to the UV treatment.

1520 Analytical Chemistry, Vol. 73, No. 7, April 1, 2001

Table 3. Element Concentrations in Skimmed Milk

Cd
Pb
Cu
Fe

kg-1)

(g
(mg kg-1)
(mg kg-1)
(mg kg-1)

UV digestion (n ) 5)

certified value

110.0 ( 12
1.921 ( 0.045
5.86 ( 0.16
49.8 ( 0.9

101.0 ( 8.0
2.002 ( 0.026
5.23 ( 0.08
50.1 ( 1.3

CONCLUSION
A novel, high-temperature, microwave-assisted UV digestion
procedure was developed. This technique combines the benefits
of pressurized microwave digestion with those observed for UV
mineralization. This new technique significantly improved the
performance of the process of UV digestion. Now, UV mineralization meets the requirements to be a powerful alternative to
standard acid digestion for the decomposition of interfering
organic carbon in liquid samples such as industrial/municipal
wastewater, groundwater, and surface water, body fluids, infusions,
beverages, and sewage. The technique of UV oxidation is
especially dedicated to ultratrace analysis due to its extremely
low risk of contamination.
ACKNOWLEDGMENT
The authors thank Anton Paar GmbH (Graz, Austria) for
providing the digestion equipment and G.L.E. (Berlin, Germany)
for the support concerning the MWL development. This research
project has been supported by Grant P13582-CHE from Fonds
zur Forderung der wissenschaftlichen Forschung (FWF), Vienna,
Austria.
Received for review October 3, 2000. Accepted January
10, 2001.
AC001180Y