FIELD FIELD PORTABLE PORTABLE FOR MINE FOR MINE WASTE AND RED MUD POLLUTED WASTE AND RED MUD POLLUTED FOR MINE FOR MINE WASTE AND RED MUD POLLUTED WASTE AND RED MUD POLLUTED
..
Mária Tolnera, Mónika Molnára, Emese Vágób, Viktória FeiglBudapest University of Technology and Economics
Department of Applied Biotechnology and Food Department of Chemical and Environmental Process Department of Chemical and Environmental Process
Budapest, Hungary Phone: +36-14632347; e-mail: [email protected],
IntroductionIntroductionIntroductionIntroduction
Fast, efficient and reliablein situ and/or on site metalanalysescharacterization and monitoring of soil contamination. This studyprovidesNi, Pb andZn concentrationsof a seriesof samplesmeasuredbothNi, Pb andZn concentrationsof a seriesof samplesmeasuredbothfluorescence Analyser (FP-XRF) and by traditional analyticalmethodsatomic emission spectroscopy (ICP-AES).We determined the toxic metal concentration of mine waste andcontaminatedsoil. Theeffectof moisturecontent,particlesizedistributioncontaminatedsoil. Theeffectof moisturecontent,particlesizedistributiontime were evaluated.
Analysed samplesAnalysed samplesFourdifferentsampleswereanalysedandcomparedversusthemeasuringtimeFourdifferentsampleswereanalysedandcomparedversusthemeasuringtime�MS is a metal polluted soil sample from the toxic metal pollutedareaofmaterial from mine waste and country rock was delivered downstream bythe�MW (mine waste material) derives from mine waste heaps left over in th�RMS is a red mud polluted soil sample from the Marcal river catchment,following the accidental spill of bauxite processing residue (red mud) inAjka�RM is a red mud sample taken following the accidental spillof bauxiteprocessing
Sample preparationSample preparation�Simplified sample preparation procedure Soil and waste samples�Simplified sample preparation procedure Soil and waste sampleswerecollected and air dried. Large rocks, organic matters such as leaves,twigs, grass or debris were removed. 10 g samplewas placed into theX-ray sample cup without grinding and sieving.�Thorough sample preparation procedure Samples werecollectedand
ResultsResultsAs error vs. moisture content pollutedagricultural soil (MS)
�Thorough sample preparation procedure Samples werecollectedandair dried. Large rocks, organic matters or debris were removed, ground,andsieved (2-mm sieve) (Hungarian Standard 21470- 50:2006).
ResultsResults
10
15
20
25
ppm
agricultural soil (MS)
45 sec
90 sec
135 sec
Effect of soil moisture contentmeasured concentrationanddensity of samples andtheincreasethephotoelectric
0
5
10
0 5% 10% 15% 20% 25%
Moisture content
135 sec
180 sec
225 sec
Location=RMSAs concentration vs. moisture content
increasethephotoelectricEffect of measurement timein error values. In thecasetrends were similar for allof
Location=RMSScatterplot of As Error against measurement time-sec
10
15
As
Err
or
(pp
m)
110
130
150
ppm
As concentration vs. moisture contentpolluted agricultural soil (MS)
45 sec
90 sec
45 90 135 180 225
measurement time - sec
5
10
As
Err
or
(pp
m)
50
70
90
0 5% 10% 15% 20% 25%
ppm
Moisture content
135 sec
180 sec
225 sec
40
50
60
ppm
Zn error - polluted agricultural soil(MS)
dry
Location=RMSScatterplot of Pb Error against measurement time-sec
15
Pb
Err
or
(pp
m)
0
10
20
30
45 90 135 180 225
ppm
sec
5%
10%
15%
20%
25%
45 90 135 180 225
5
10
Pb
Err
or
(pp
m)
1500
Zn concentration - pollutedagricultural soil (MS)
secmeasurement time - sec
Location=RMSScatterplot of Zn Error against measurement time-sec
20
25
Zn
Err
or
(pp
m)
0
500
1000
45 90 135 180 225
ppm
dry
5%
10%
15%
20%
25%5
10
15
Zn
Err
or
(pp
m)
ConclusionConclusion
45 90 135 180 225
sec
Fig. 1. As and Zn concentrations, As and Zn errors of
metal polluted agricultural soil against moisture content.
45 90 135 180 225
measurement time - sec
5
Fig. 2. As error, Pb error and Zn error of red mud
polluted soil against measurement time
ConclusionConclusionFP-XRF can be a rapid and appropriate analytical support toanalyzeanalysis of multiple elements saves time and money overtraditional,Howeverour preliminarystudydemonstratedthat the effectsof differentHoweverour preliminarystudydemonstratedthat the effectsof differentshould be investigated and corrected, because soil moisture andmeasurementXRF analysis.This study shows that one of the most important sources of errorvariablesoil moisturecontent. Drying of all soilsmaybeanacceptable
The financial support of Hungarian Research & Development Program (TECH_09-A4-2009-
variablesoil moisturecontent. Drying of all soilsmaybeanacceptablewater contents. Our experimental results confirmed theimportanceas ICP-AES.
PORTABLE PORTABLE XRF XRF ANALYSER ANALYSER WASTE AND RED MUD POLLUTED WASTE AND RED MUD POLLUTED SOIL SOIL WASTE AND RED MUD POLLUTED WASTE AND RED MUD POLLUTED SOIL SOIL
..
Feigla, Orsolya Klebercza, Éva Ujaczkia and Katalin Gruiza
Budapest University of Technology and Economics,of Applied Biotechnology and Food Sciencea,
Department of Chemical and Environmental Process EngineeringbDepartment of Chemical and Environmental Process Engineeringb
Budapest, Hungary mail: [email protected], [email protected]
IntroductionIntroductionIntroductionIntroduction
analysesmethods are required for preliminary site assessment, forprovidesa comparative statistical evaluation of the As, Ba, Cu, Cr,
both by a ThermoScientific Niton XL3t 600S field portableX-rayboth by a ThermoScientific Niton XL3t 600S field portableX-raymethodsafter Aqua Regia digestion, using inductively coupled plasma
mine waste contaminated agricultural soil, red mud and red muddistributionandhomogeneityof soil samplesaswell asthemeasuringdistributionandhomogeneityof soil samplesaswell asthemeasuring
Analysed samplesAnalysed samplestime andmoisturecontent.time andmoisturecontent.
of Gyöngyösoroszi, Toka watershed (North-East Hungary). The erodedsolidtheToka creek reaching an agriculturalarea.
the forest at the foot of the Mátra hills inNorth-East Hungary.tchment,red mud flooded area in western Hungary the. The sample was taken
Ajka.processingresidue (red mud) in Ajka (Hungary).
Sample preparationSample preparation�Each sample was analysedafter wetting the soil at 6 different�Each sample was analysedafter wetting the soil at 6 differentmoisture contents (air dried and 5-25 w%).�To establish the effect of measurement time on precision andaccuracy all samples were measured for 45, 90, 180 and 225 secs (15,30, 45, 60, 75sec/filter).
ResultsResults
30, 45, 60, 75sec/filter).
ResultsResultscontent The increasingwater content resulted in exponential decrease inand recorded error for all elements. It is due to presumably the increasedthe replacement of air withwater in soil pores. Thisreplacement mayabsorption.absorption.
time Increasing measurement time inmost cases led to non-linear decreasecaseof Ag we didn’t found any measurement time-dependency. The observed
of investigated environmental samples.
Scatterplot of As Error against measurement time-sec Effect of sample preparation Results show that the sample-preparation had slight effect on the quality of XRF data. Measuredmetal concentrations in thoroughly prepared samples are usuallylower than following simplifiedpreparation .
225
AsMean Plot of Value (ppm) grouped by Moisture content %;
categorized by Preparation100
PbMean Plot of Value (ppm) grouped by Moisture content %;
categorized by Preparation400
Scatterplot of Pb Error against measurement time-sec
pp
m
80
90
Not- groundGround
pp
m
320
340
360
380
400
Not- groundGround
225 Fig.3. Effects of sample preparation in case of metal polluted agricultural soil
Moisture content %
5 10 15 20 25
70
Moisture content %
5 10 15 20 25280
300
320
Scatterplot of Zn Error against measurement time-secPb
Scatterplot of ppm against metal polluted soil parallels
600
700
NiScatterplot of ppm against metal polluted soil parallels
80
100
120
Fig.3. Effects of sample preparation in case of metal polluted agricultural soil
ICP-AES
1 2 3 4
300
400
500
pp
m
0
20
40
60
80
pp
m
ICP-AES
ConclusionConclusion
225
As error, Pb error and Zn error of red mud
1 2 3 4
Parallel No.
1 2 3 4
Parallel No.
0
Fig. 4. As and Pb concentration changes in parallel metal polluted soil samples compared with
results done by ICP-AES on Aqua Regia extracts
ConclusionConclusionanalyzeenvironmental samples in a timely fashion. The simultaneous
traditional,laboratory techniques.different samplepreparationmethodsandmeasurementconditionsdifferent samplepreparationmethodsandmeasurementconditions
measurementtime have a significant impact on the accuracy of FP-
in quantitative FP-XRF analysis of environmental samples is theacceptablealternativeto eliminatetheerrorsconnectedwith differentsoil
-0129, SOILUTIL project and NKFP-3/020/2005 MOKKA project) is greatly acknowledged.
acceptablealternativeto eliminatetheerrorsconnectedwith differentsoilimportanceof cross-validating the results with an alternative technique such
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