96 Organic compounds in soils, sediments & sludges
for all compounds in the two soils studied varied from 81 to 106% with a relative standard deviation between 2 and 9%. The limit of detection in the conditions assayed was at least 0.01 µg/g for all compounds. The developed procedure
was applied by the analysis of real soil samples, obtained after tomato harvest,
from 18 commercial fields in Spain, and residue levels of Pendimethalin (0.018–
0.650 µg/g) Endosulfan–I (0.011–0.032 µg/g), Endosulfan-II (0.014–0.178 µg) and
Endosulfan-sulfate (0.010–0.135 µg/g) was found.
Cox et al [271] studied the factors influencing the sorption and dissipation of
Imidacloprid in soil.
The effect of organic amendments on Imidacloprid sorption and dissipation in soil
was investigated. A sandy soil was treated at a rate of 10% w/w with three organic
amendments: one liquid (Liquid Fertiormont, LF) and two solid (Solid Fertiormont, SF
and Alperujo, A). Sorption was measured using a batch equilibration method, Dissipation studies in the dark were performed by incubating pesticide-treated soils at moisture
content of −0.33 KPa and 20 ± 2
◦ C for 28 days, whereas imidacloprid photolysis studies in soils were performed by irradiation of treated soils at water holding capacity in
a Suntest apparatus with a xenon lamp for 32 h. In both cases, soils were sampled
periodically and extracted for their Imidacloprid content. Solid Fentiormont SF and
Alperuyo A increased Imidacloprid sorption by soils, Whereas similar adsorption was
observed in soil amended with Fertiormont LF Imidacloprid half-lives obtained from
incubation studies in the dark remained unaffected upon amendment, where Fertiormont OA decreased the photolysis rate of Imidacloprid in soils. However, no relation
was observed between increase in sorption and decrease in the photodegradation rate
of Imidacloprid.
Liu et al [272] studied the dissipation rate of Myclobutanil fungicide in soil using
gas chromatography ion trap. MS spectrometry. Detection limits were 0.6 µg kg
−1 and
recoveries were in the range 3% to 19.7% at several spiking levels. The half lines in
Myclobutinil in soil was about 11 days.
The analysis of insecticide/herbicide mixtures in soil has been reviewed by various
workers. The determination of miscellaneous agrichemicals is shown in Table 3.6.
3.10 MULTI INSECTICIDE/HERBICIDE MIXTURES
Gas chromatography
Cotterill et al [277] has developed a procedure, discussed below, in which the herbicides
are extracted from soil with saturates calcium hydroxide solution. After clean-up the
residues are ethylated using iodoethane and tetrabutylammonium hydrogen sulphate
as counter ion. Liquid-liquid partition and the use of a macroreticular resin column
were compared as clean-up steps and the reaction conditions for optimum yield of
ethyl ester were evaluated.
The herbicides are estimated in the extract by electron capture gas chromatography. These clean-up methods used are capable of giving good results at the 1 µg g
−1
level.
Recoveries in excess of 80% were achieved for 2, 4-D, Dicamba, 3, 6dichloropicolinic acid, Dichloroprop, Picloram, 2, 4, 5-T Fenoprop, 2, 3, 6-TBA,
Bromoxynil and Ioxynil.
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