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Chiou C. T., Porter P. E., and Schmedding D. W., (1983), „Partition equilibria of non-ionic organic compounds between soil organic matter and water“.
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Vowles P. D., and Mantoura R. F. C, (1987), „Sediment-water partition coefficient and HPLC retention factors of aromatic hydrocarbons“.
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Eaton, et al.), p. 78-115, ASTM STP 707, Philadelphia.
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Chiou C.T., Peters L.J., and Freed V.H., (1979) ‘A physical concept of soil-water equilibria for non-ionic organic compounds’.
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Science, Vol. 206, pp. 831 – 832.3
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Karickhoff S.W., (1981), ‘Semi-empirical estimation of sorption of hydrophobic pollutants on natural sediments and soils’.
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Relation solubilité — reactivité.
Relation solubilité-reactivité“.
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Testing scheme
Schéma testu
Set up of a suitable analytical method
Výber vhodnej analytickej metódy Predbežná štúdia
Available?
Kinetika desorpcie
No further test
Desorpčná izoterma
Prerequisite
Vhodná metóda?
Preliminary study
Žiaden ďalší test
2 Soils
2 vzorky pôdy
Determination of equilibrium time
Stanovenie času dosiahnutia rovnováhy
Check for adsorption on the vessel surface
Kontrola adsorpcie na povrchu nádoby
If mass balance < 90%, test substance is unstable in the time scale of the test. The test test can continue by analysing both phases (soil and aqueous solution). 5 Soils
Kd*(mpô da/V0) > 0,3 (priama metóda, meranie obidvoch fáz)
Kd*(msoi/V0) > 0.3 (indirect method : measurement of solution depletion)
Ak rovnovážna hmotnosť je < 90 %, testovaná látka je nestabilná v časovom rozsahu testu. Test môže pokračovať po analýze obidvoch fáz (pôda a vodný roztok) Ak je to vhodné
INFLUENCE OF ACCURACY OF ANALYTICAL METHOD AND CONCENTRATION CHANGE ON ACCURACY OF ADSORPTION RESULTS
VPLYV PRESNOSTI ANALYTICKEJ METÓDY A KONCENTRAČNÝCH ZMIEN NA PRESNOSŤ VÝSLEDKOV ADSORPCIE
From the following table (84) it becomes obvious that when the difference between the initial mass (m0 = 110 μg) and equilibrium mass (maq
Z nasledujúcej tabuľky (8.4) vyplýva, že rozdiel medzi počiatočnou hmotnosťou (m0 = 110 μg) a rovnovážnou hmotnosťou (maq
= 100 μg) of the test substance in the solution is very small, an error of 5 % in the measurement of equilibrium concentration results in an error of 50 % in the calculation of the mass of the substance adsorbed in soil (ms
= 100 μg) testovanej látky v roztoku je veľmi malý, 5 % odchýlka pri meraní výsledkov rovnovážnej hmotnosti sa prejaví 50 % odchýlkou vo výpočte hmotnosti látky absorbovanej v pôde (ms
and of 52,4 % in the calculation of the Kd.
)a 52,4 % vo výpočte Kd.
Amount of soil
Množstvo pôdy
Volume of solution
Objem roztoku
FOR A = 9 %
PRE A = 9 %
= 110 μg or C0 = 1,100 μg/cm3
= 110 μg alebo C0=1,100 μg/cm3
true value
skutočná hodnota
FOR A = 55 %
PRE A = 55 %
m0= 110 μg or C0 = 1,100 μg/cm3
m0= 110 μg alebo C0=1,100μg/cm3
FOR A = 99 %
PRE A = 99 %
mass of the test substance in the soil phase at equilibrium, μg;
hmotnosť testovanej látky v pôde v rovnovážnom stave, μg;
mass of the test substance in the aqueous phase at equilibrium, μg;
hmotnosť látky v roztoku v čase adsorpčnej rovnováhy, μg;
content of the test substance in the soil phase at equilibrium, μg g-1;
obsah testovanej látky v pôdnej faze v rovnovážnom stave, μg g-1:
mass concentration of the test substance in the aqueous phase at equilibrium, μg cm-3;
hmotnostná koncentrácia testovanej látky vo vodnej fáze v rovnovážnom stave, μg cm-3
R analytical error in the determination of the maq
R analytlická odchýlka pri stanovení maq
R‡ calculated error due to the analytical error R.
R‡ vypočítaná odchýlka spôsobená analytickou chybou R.
ESTIMATION TECHNIQUES FOR KD
TECHNIKA ODHADU Kd
Estimation techniques permit prediction of Kd based on correlations with, for example, Pow values (12)(39)(63-68), water solubility data (12)(19)(21)(39)(68-73), or polarity data derived by application of HPLC on reversed phase (74-76).
Technika odhadu umožňuje predpoklad Kd na základe korelácie, napr. s hodnotami Pow (12), (39), (63 – 68), s údajmi o rozpustnosti vo vode (12), (19), (21), (39), (68 – 73) alebo s údajmi o polarite získanými uplatnením HPLC na obrátených fázach (74 – 76).
As shown in Tables 1 and 2, is the Koc or Kom that are calculated from these equations and then, indirectly, the Kd from the equations:
Ako je vidieť z tabuliek 1 a 2, hodnoty Koc a Kom sa vypočítavajú podľa týchto rovníc a potom nepriamo, Kd podľa týchto rovníc:
The concept of these correlations is based on two assumptions: (1) it is the organic matter of the soil that mainly influences the adsorption of a substance; and (2) the interactions involved are mainly non-polar.
Podstata týchto korelácií je založená na dvoch predpokladoch: (1) na organickej podstate pôdy, hlavne jej vplyvoch na adsorpciu látky a (2) na interakciách, hlavne medzi nepolárnymi látkami.
As a result, these correlations: (1) are not, or are only to some extent, applicable to polar substances, and (2) are not applicable in cases where the organic matter content of the soil is very small (12).
Výsledkom týchto korelácií je: (1) nie sú alebo sú iba do istej miery aplikovateľné na polárne látky a (2) sú neaplikovateľné v prípadoch, kde obsah organickej látky v pôde je veľmi malý (12).
In addition, although satisfactory correlations have been found between Pow and adsorption (19), the same cannot be said for the relationship between water solubility and extent of adsorption (19)(21); so far the studies are very contradictory.
Okrem toho, hoci medzi Pow a adsorpciou (19) bola zistená uspokojivá súvzťažnosť, to isté sa nedá tvrdiť o vzťahu medzi rozpustnosťou vo vode a rozpätím adsorpcie (19), (21); keďže sú štúdie ohľadom tejto témy veľmi protichodné.
Some examples of correlations between the adsorption coefficient and the octanol-water partition coefficient, as well as water solubility are given in Tables 1 and 2, respectively.
V tabuľkách 1 a 2 sú uvedené niektoré príklady korelácií medzi adsorpčným koeficientom a rozdeľovacím koeficientom pre oktanol-voda, ako aj rozpustnosť vo vode.
Examples of correlations between the adsorption distribution coefficient and the octanol-water partition coefficient; for further examples (12) (68).
Príklady korelácií medzi adsorpčným koeficientom a rozdeľovacím koeficientom pre oktanol-voda, ďalšie príklady pozri (12) (68).
Correlations
Korelácie
Substituted ureas
Substituované močoviny
Aromatic chlorinated
Chlórované aromáty
Various pesticides
Rôzne prípravky na ochranu rastlín
Aromatic hydrocarbons
Aromatické uhľovodíky
Examples of correlations between the adsorption distribution coefficient and water solubility; for further examples see (68) (69).
Príklady korelácií medzi adsorpčným rozdeľovacím koeficientom a rozpustnosťou vo vode; ďalšie príklady pozri (68) (69).
Compounds
Látky
Aliphatic, aromatic chlorinated substances
Alifatické, aromatické chlórované látky
α-naphtol
α-naftol
Cyclic, aliphatic aromatic substances
Cyklické, alifatické aromatické látky
Various compounds
Rôzne zlúčeniny
log Kom = 2,75 - 0,45 log Sw
log Kom= 2,75 – 0,45 log Sw
CALCULATIONS FOR DEFINING THE CENTRIFUGATION CONDITIONS
VÝPOČTY NA DEFINOVANIE PODMIENOK ODSTREĎOVANIA
The centrifugation time is given by the following formula, assuming spherical particles:
Čas odstreďovania je stanovený nasledujúcim vzorcom za predpokladu, že častice majú sférický tvar:
For simplification purposes, all parameters are described in non-SI units (g, cm).
Na zjednodušenie sú všetky parametre popísané v jednotkách SI (g, cm).
ω = rotational speed (=2 π rpm/60), rad s-1
ω rýchlosť rotácie (=2 π rpm/60), rad s1;
rpm = revolutions per minute
rpm počet otáčok za minútu;
η = viscosity of solution, g s-1 cm-1
η viskozita roztoku, g s-1 cm-1;
= particle radius, cm
polomer častice, cm;
= soil density, g cm-3
hustota pôdy (merná hmotnosť), g cm-3;
= solution density, g cm-3
hustota roztoku (merná hmotnosť), g cm-3;
= distance from the centre of centrifuge rotor to top of solution in centrifuge tube, cm
vzdialenosť od stredu rotora odstredivky po vrchol roztoku v odstred'ovacej skúmavke, cm;
= distance from the centre of centrifuge rotor to bottom in centrifuge tube, cm
vzdialenosť od stredu rotora odstredivky po spodok roztoku v odstred'ovacej skúmavke, cm;
= length of the soil/solution mixture in the centrifuge tube, cm.
výška stĺpca zmesi pôdy a roztoku v odstred'ovacej skúmavke, cm.
In general practice, double the calculated times is used to ensure complete separation.
V bežnej praxi sa používa dvojnásobok vypočítaného času odstreďovania, aby sa zaistila úplná separácia.
The equation (1) can be simplified further if we consider the viscosity (η) and the density (ρaq) of the solution as equal to the viscosity and density of water at 25 oC; thus, η = 8,95 × 10-3 g s-1 cm-1 and ρaq = 1,0 g. cm-3.
Rovnica (1) sa dá ďalej zjednodušiť, ak budeme považovať dynamickú viskozitu (η) a hustotu [mernú hmotnosť] (ρaq) roztoku za rovnú dynamickej viskozite a hustote vody pri 25 oC, teda η = 8,95 × 10-3 g.s-1 cm-1 a ρaq = 1,0 g. cm-3.
Then, the centrifugation time is given by the equation (2):
Potom je čas odstreďovania daný rovnicou (2):
From the equation (2) it becomes apparent that two parameters are important in defining the centrifugation condition, i.e. time (t) and speed (rpm), in order to achieve separation of particles with a specific size (in our case 0,1 μm radius): (1) the density of the soil and (2) the length of the mixture in the centrifuge tube (Rb-Rt), i.e. the distance which a soil particle covers from the top of the solution to the bottom of the tube; obviously, for a fixed volume the length of the mixture in the tube will depend on the square of the radius of the tube.
Z rovnice (2) je zrejmé, že nasledujúce dva parametre sú dôležité na definovanie podmienok odstreďovania, t. j. čas t) a rýchlosť (rpm), aby sa dosiahla separácia častíc so špecifickou veľkosťou (v našom prípade priemer častíc 0,1 μm): merná hmotnosť pôdy a (2) výška stĺpca zmesi v odstreďovacej skúmavke (Rb – Rt), t. j. vzdialenosť, ktorú častica pôdy pokrýva od vrcholu roztoku po spodok skúmavky; je zrejmé, že pre stály objem bude výška stĺpca v skúmavke závisieť od štvorca polomeru skúmavky.
Fig. 1 presents variations in the centrifugation time (t) versus centrifugation speed (rpm) for different soil densities (ρs) (Fig.1a) and different lengths of the mixture in the centrifuge tubes (Fig.2a).
Obr. 1 predstavuje variácie v čase odstreďovania t) verzus rýchlosť (rpm) pri rôznych hodnotách mernej hmotnosti pôdy (ps) (obr. la) a rôzne výšky stĺpcov zmesí v odstreďovacej skúmavke (obr. 2a).
From Fig.1a the influence of the soil density appears obvious; for example, for a classical centrifugation of 3000 rpm the centrifugation time is approximately 240 min for 1,2 g cm3 soil density, while it is only 50 min for 2,0 g cm3. Similarly, from Fig 1b, for a classical centrifugation of 3000 rpm the centrifugation time is approximately 50 min for a length of the mixture of 10 cm and only seven min for a length of 1 cm.
Z obr. la je vidieť, že vplyv mernej hmotnosti pôdy sa stáva očividným; napr. pri klasickom odstreďovaní pri 3000 otáčkach/min. je čas odstreďovania približne 240 min. pri mernej hmotnosti pôdy 1,2 g cm3, zatiaľ čo pri mernej hmotnosti pôdy rovnajúcej sa 2,0 g cm3 je to iba 50 min. Podobne (obr. lb) pri klasickom odstreďovaní pri 3000 otáčkach/min. je čas odstreďovania približne 50 min. pri výške stĺpca zmesi 10 cm a iba 7 min. pri výške stĺpca 1 cm.
However, it is important to find an optimal relation between centrifugation which requires the less length possible and easy handling for the experimenter in separating the phases after centrifugation.
Je však dôležité nájsť optimálny vzťah medzi odstreďovaním, ktoré vyžaduje najmenšiu možnú výšku stĺpca a ľahkou manipuláciou pre experimentátora pri oddeľovaní fáz po odstreďovaní.
Moreover, when defining the experimental conditions for the separation of soil/solution phases, it is important to consider the possible existence of a third ‘pseudo-phase’, the colloids.
Okrem toho, pri definovaní experimentálnych podmienok na separáciu fáz pôdy a roztoku je dôležité vziať do úvahy možnú existenciu tretej „pseudofázy“ koloidov.
Thus, the information about their impact is lost.
Takto sa stratí informácia o ich vplyve.
If the conducting laboratory has ultracentrifugation or ultrafiltration facilities, the adsorption/desorption of a substance in soil could be studied more in depth, including information on the adsorption of the substance on the colloids.
Ak má riadiace laboratórium veľkú odstredivku alebo možnosť ultrafiltrácie, adsorpcia/desorpcia látky vo vode sa dá preskúmať do väčšej hĺbky vrátane informácií o adsorpcii látky na koloidoch.
In this case, an ultracentrifugation at 60000 rpm/min or an ultrafiltration with filter porosity of 100000 Daltons should be applied in order to separate the three phases soil, colloids, solution.
V tomto prípade sa ultraodstredivka nastaví na 60000 otáčok/min alebo sa použije ultrafiltrácia s filtrom o porozite/veľkosť pórov/100000 daltonov, aby sa oddelili tri fázy – pôda, koloidy, roztok.
The test protocol should also be modified accordingly, in order all three phases to be subjected to substance analysis.
Podľa toho sa upraví aj protokol o výsledkoch testu, aby sa všetky tri fázy stali súčasťou analýzy.
Fig. 1a.
Obr. 1a
Variations of centrifugation time (t) versus centrifugation speed (rpm) for different soil densities (ρs).
Variácie času odstreďovania (t) verzus rýchlosť odstreďovania (rpm) na rôzne merné hmotnosti pôdy (ρs).
Rt = 10 cm, Rb - Rt = 10 cm, η = 8,95 × 10-3 g s-1 cm-1 and ρaq = 1,0 g. cm-3 at 25 oC.
Rt = 10 cm, Rb – Rt = 10 cm, η = 8,95 × 10-3 g s-1 cm-1a ρaq = 1,0 g.cm-3 pri 25 oC.
Fig. 1b.
Obr. 1b