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Schéma zkoušky
Testing scheme
Návrh vhodné analytické metody Předběžná studie
Set up of a suitable analytical method
Adsorpční kinetika
Available?
Desorpční isothermy
No further test
Je realizovatelná?
Prerequisite
Zkouška se nerealizuje
Preliminary study
2 půdy
2 Soils
Stanovení rovnovážného času
Determination of equilibrium time
Ověření adsorpce na povrchu nádoby
Check for adsorption on the vessel surface
Ověření stálosti hmotnostní bilance Je dosaženo rovnovážného plató? Ano Ano Ne 5 půd
Check for the stability by means of parental mass balance
Kd*(mpůda/V0) > 0,3 (nepřímou metodou: měřením úbytku v roztoku)
Tier 1 Equilibrium plateau is achieved? Yes Adsorption kinetics Tier 2
Kd*(mpůda/V0) > 0.1 (přímou metodou: měřením obou fází)
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
Je-li hmotnostní bilance < 90 %, je zkušební látka po dobu zkoušky nestálá. Zkouška může pokračovat analýzou obou fází (půda a vodný roztok) podle potřeby
Kd*(msoi/V0) > 0.3 (indirect method : measurement of solution depletion)
Stupeň 2
Kd*(msoi/V0) > 0.1 (direct method : measurement of both phases)
Stupeň 1
as appropriate
Stupeň 3
Tier 3 Adsorption isotherms
VLIV SPRÁVNOSTI ANALYTICKÉ METODY A ZMĚNY KONCENTRACE NA SPRÁVNOST VÝSLEDKŮ ADSORPČNÍ STUDIE
INFLUENCE OF ACCURACY OF ANALYTICAL METHOD AND CONCENTRATION CHANGE ON ACCURACY OF ADSORPTION RESULTS
Z následující tabulky (84) je zřejmé, že je-li rozdíl mezi počáteční hmotností zkoušené látky (m0 = 110 μg) a její rovnovážnou hmotností v roztoku (maq
From the following table (84) it becomes obvious that when the difference between the initial mass (m0 = 110 μg) and equilibrium mass (maq
=100 µg) velmi malý, je důsledkem 5 % chyby měření rovnovážné koncentrace 50 % chyba ve výpočtu hmotnosti zkoušené látky adsorbované v půdě (mp
= 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
a 52,4 % chyba ve výpočtu Kd.
and of 52,4 % in the calculation of the Kd.
Hmotnost půdy
Amount of soil
Objem roztoku
Volume of solution
PRO A = 9 %
FOR A = 9 %
= 110 μg nebo C0 = 1,100 μg/cm3
= 110 μg or C0 = 1,100 μg/cm3
skutečná hodnota
true value
PRO A = 55 %
FOR A = 55 %
m0= 110 μg nebo C0 = 1,100 μg/cm3
m0= 110 μg or C0 = 1,100 μg/cm3
PRO A = 99 %
FOR A = 99 %
mpůda
msoil .
, Kd=mp
Kd=ms
hmotnost zkoušené látky v půdě při rovnováze, μg;
mass of the test substance in the soil phase at equilibrium, μg;
hmotnost zkoušené látky ve vodné fázi při rovnováze, μg;
mass of the test substance in the aqueous phase at equilibrium, μg;
množství zkoušené látky v půdě při rovnováze, μg g-1;
content of the test substance in the soil phase at equilibrium, μg g-1;
množství zkoušené látky ve vodné fázi při rovnováze, μg cm-3;
mass concentration of the test substance in the aqueous phase at equilibrium, μg cm-3;
R analytická chyba stanovení maq
R analytical error in the determination of the maq
R‡ vypočtená chyba způsobená analytickou chybou R.
R‡ calculated error due to the analytical error R.
METODY ODHADU KD
ESTIMATION TECHNIQUES FOR KD
Metody odhadu umožňují předpovědět Kd na základě korelací například s hodnotami Pow (12, 39, 63–68), s údaji o rozpustnosti ve vodě (12, 19, 21, 39, 68–73) nebo s údaji o polaritě získanými při použití HPLC s obrácenou fází (74–76).
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).
Jak je ukázáno v tabulkách 1 a 2, vypočtou se z takových rovnic hodnoty Kou nebo Kom a poté nepřímo hodnoty Kd z rovnic:
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:
Koncepce těchto korelací je založena na dvou předpokladech: 1) adsorpci látky nejvíce ovlivňuje organický materiál v půdě a 2) interakce jsou převážně nepolární.
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.
V důsledku toho tyto korelace: 1) nejsou použitelné pro polární látky (nebo jsou použitelné jen do určité míry) a 2) nejsou použitelné v případech, kdy je obsah organického materiálu v půdě velmi malý (12).
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).
Kromě toho, ačkoli byla zjištěna uspokojivá korelace mezi Pov a a adsorpcí (19), nelze totéž říci o vztahu mezi rozpustností ve vodě a rozsahem adsorpce (19, 21); dosud si tyto studie protiřečí.
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.
Některé příklady korelace mezi adsorpčním koeficientem a rozdělovacím koeficientem mezi oktanol a vodu a rovněž rozpustností ve vodě jsou uvedeny v tabulkách 1 a 2.
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.
Příklady korelací mezi adsorpčním distribučním koeficientem a rozdělovacím koeficientem mezi oktanol a vodu; další příklady jsou uvedeny v literatuře (12, 68)
Examples of correlations between the adsorption distribution coefficient and the octanol-water partition coefficient; for further examples (12) (68).
Korelace
Correlations
Substituované močoviny
Substituted ureas
log Kom = 0,69 + 0,52 log Po/v
log Kom = 0,69 + 0,52 log Pow
Chlorované aromatické
Aromatic chlorinated
log Kou = -0,779 + 0,904 log Po/v
log Koc = -0,779 + 0,904 log Pow
Různé pesticidy
Various pesticides
log Kom = 4,4 + 0,72 log Po/v
log Kom = 4,4 + 0,72 log Pow
Aromatické uhlovodíky
Aromatic hydrocarbons
log Kou = -2,53 + 1,15 log Po/v
log Koc = -2,53 + 1,15 log Pow
Příklady korelací mezi adsorpčním distribučním koeficientem a rozpustností ve vodě; další příklady jsou uvedeny v literatuře (68, 69)
Examples of correlations between the adsorption distribution coefficient and water solubility; for further examples see (68) (69).
Sloučeniny
Compounds
log Kom = 3,8 – 0,561 log Sv
log Kom = 3,8 - 0,561 log Sw
Chlorované alifatické a aromatické látky
Aliphatic, aromatic chlorinated substances
log Kom = (4,040 ± 0,038) – (0,557 ± 0,012) log Sv
log Kom = (4,040 +/- 0,038) - (0,557 +/- 0,012) log Sw
1-Naftol
α-naphtol
log Kou = 4,273 – 0,686 log Sv log Sw
logKoc = 4,273 - 0,686 log Sw
Cyklické, alifaticko-aromatické látky
Cyclic, aliphatic aromatic substances
log Kou = -1,405 – 0,921 log Sv-0,00953 (mp-25)
logKoc = -1,405 - 0,921 log Sw-0,00953 (mp-25)
Různé sloučeniny
Various compounds
log Kom = 2,75 – 0,45 log Sv
log Kom = 2,75 - 0,45 log Sw
VÝPOČTY PRO URČENÍ PODMÍNEK CENTRIFUGACE
CALCULATIONS FOR DEFINING THE CENTRIFUGATION CONDITIONS
Centrifugační doba se za předpokladu, že jsou částice kulové, vypočte podle této rovnice:
The centrifugation time is given by the following formula, assuming spherical particles:
-ρvod
ρaq
lnRb
ln Rb