4th EucheMs chemistry congress

Poster Session 2
s1152
chem. Listy 106, s257–s1425 (2012)
Poster session 2 - Analytical Chemistry
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exPeriMentAL deSiGn APPLied on
PyrohydroLytiC extrACtion of fLuorine
And ChLorine froM CoAL
i. SredoviC 1 , d. CoKeSA 2 , A. onJiA 2 ,
L. rAJAKoviC 3
1 Faculty of Agriculture, Chemistry and Biochemistry,
Belgrade-Zemun, Serbia
2 Vinca Institute, Chemical Dynamics, Belgrade, Serbia
3 Faculty of Technology and Metalurgy, Analytical Chemistry,
Belgrade, Serbia
This research has been focused on the determination of
fluorine and chlorine content in the lignite coal by applying a
experimental design approach. A pyrohydrolysis (Phy) apparatus
system was constructed, and the pyrohydrolytic parameters were
evaluated and optimized by two statistical methods:
Plackett-Burman (PB) design and response surface methodology
(RSM). Halogen content in the absorption solution was measured
by ion selective electrode (ISE) and by ion chromatography (IC).
Results of PB designed experiments indicated that the most
important parameters on Phy-ISE determination of fluorine in coal
were time, temperature and oxidation atmosphere, while the
Phy-IC determination of chlorine was strongly influenced by
absorption solution and temperature. These screening experiments
signified that during the pyrohydroytic extraction and within the
range of investigated parameters, in some degree the chlorine in
coal could volatilizied as molecular chlorine.
The RSM is a statistical modeling technique employed for
multiple regression analysis using the data obtained from designed
experiments. The statistical models applied were suitable for
predicting and optimizing of fluorine determination within the
range of variables used.
It was concluded that optimal conditions for Phy-ISE
determination of fluorine in coal were: 0.25 g of coal sample,
0.30 mL min-1 of oxygen flux, a temperature of 1100 °C, 15 min
of pyrohydrolysis and Na CO (2 mmol L 2 3 -1 ) as adsorption
solution. The limit of detection of the proposed method was
20 μg g-1 , with good recovery (95 %) and relative standard
deviation value less than 5 %. According to the applied
experimental design, the pyrohydrolytic extraction was unsuitable
for chlorine in coal determination.
4 th EucheMs chemistry congress
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effeCtS of Liquid MAnure AMendMent on
ACCuMuLAtion of heAvy MetALS in wheAt And
BArLey
S. StAniSiC 1 , L. iGnJAtoviC 1 , S. PoPov 2 ,
S. SKrivAnJ 3
1 Faculty of Physical Chemistry, Environmental Chemistry,
Belgrade, Serbia
2 Oenological Laboratory, Environmental Chemistry, Vrsac,
Serbia
3 Faculty of Chemistry, Environmental Chemistry, Belgrade,
Serbia
An experiment was carried out to evaluate uptake of heavy
metals by wheat and barley in the presence of liquid manure
amendment. Wheat and barley seedlings were grown on a filter
paper in a 12-cm diameter Petri dish. Additionally, wheat
seedlings were grown in pots containing unpolluted agricultural
soil. All the seedlings were irrigated three times per week with
prepared solutions: first solution with composition similar to rain
water, second solution containing Cd, Cu, Zn, Pb, Ni, Fe, Mn, Hg
and As, and the third solution of liquid manure containing the
same heavy metals as the second one. After 10 days the plants
were weighed and 1 g of plant tissue was prepared for ICP-OES
analysis by microwave digestion with mixture of HNO and H O .
3 2 2
The results have shown that the uptake of arsenic and mercury
was highest for both plants grown in Petri dish. Beside high
arsenic content, the pot grown wheat contained a high amounts
of iron and manganese, probably due to the adsorption of nickel,
cadmium, cooper and mercury on soil phases. On the other hand,
the wheat grown without soil had higher content of nickel,
cadmium and cooper, while the uptake of manganese and iron was
lowered. The lower uptake of all heavy metals was observed by
amendment of liquid manure, with exception of manganese in pot
grown wheat and mercury in all plants.
Keywords: analytical chemistry; environmental chemistry;
arsenic; mercury;
AUGUst 26–30, 2012, PrAGUE, cZEcH rEPUbLIc