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Chemosphere, 16(1), p. 109-116.
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Testplan
Testing scheme
opsætning af en egnet analysemetode Indledende undersøgelse
Set up of a suitable analytical method
Adsorptionskinetik
Available?
Desorptionsisotermer
No further test
Til rådighed?
Prerequisite
Ingen yderligere test
Preliminary study
Bestemmelse af ligevægtstid
Check for the stability by means of parental mass balance
Kd*(msoil/V0) > 0,3 (indirekte metode: bestemmelse af svindet i opløsningen)
Kd*(msoi/V0) > 0.3 (indirect method : measurement of solution depletion)
Kd*(msoil/V0) > 0,1 (direkte metode: bestemmelse af begge faser) Er massebalancen < 90 %, er prøvestoffet ustabilt inden for testtiden.
Kd*(msoi/V0) > 0.1 (direct method : measurement of both phases)
Testen kan fortsættes ved, at man analyserer begge faser (jord og vandig opløsning) som passende Trin 2 Trin 1
as appropriate
Trin 3
Tier 3 Adsorption isotherms
BETYDNINGEN AF ANALYSEMETODENS NØJAGTIGHED OG KONCENTRATIONSÆNDRINGER FOR ADSORPTIONSRESULTATERNES NØJAGTIGHED
INFLUENCE OF ACCURACY OF ANALYTICAL METHOD AND CONCENTRATION CHANGE ON ACCURACY OF ADSORPTION RESULTS
Af følgende tabel (84) ses, at når der er meget lille forskel mellem prøvestoffets begyndelsesmasse (m0 =110 μg) og ligevægtsmasse (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) i opløsningen, vil en fejl på 5 % på ligevægtskoncentrationsmålingen føre til en fejl på 50 % på beregningen af den stofmængde, som er adsorberet på jorden (ms
= 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
og på 52,4 % på beregningen af Kd.
and of 52,4 % in the calculation of the Kd.
Mængde jord
Amount of soil
Opløsningens rumfang
Volume of solution
= 110 μg eller C0=1,100 μg/cm3
= 110 μg or C0 = 1,100 μg/cm3
sand værdi
true value
m0= 110 μg eller C0=1,100 μg/cm3
m0= 110 μg or C0 = 1,100 μg/cm3
masse af prøvestof i jordfasen ved ligevægt, μg
mass of the test substance in the soil phase at equilibrium, μg;
masse af prøvestof i vandfasen ved ligevægt, μg
mass of the test substance in the aqueous phase at equilibrium, μg;
indhold af prøvestof i jordfasen ved ligevægt, μg g-1
content of the test substance in the soil phase at equilibrium, μg g-1;
massekoncentration af prøvestoffet i vandig fase ved ligevægt, μg cm-3
mass concentration of the test substance in the aqueous phase at equilibrium, μg cm-3;
R analysefejl på bestemmelse af maq
R analytical error in the determination of the maq
R‡ beregnet fejl som følge af analysefejl R.
R‡ calculated error due to the analytical error R.
TEKNIKKER TIL SKØNSMÆSSIG BEREGNING AF Kd
ESTIMATION TECHNIQUES FOR KD
Ved hjælp af teknikker til skønsmæssig beregning kan størrelsen af Kd forudsiges på grundlag af korrelationer med f.eks. værdier af Pow (12)(39)(63-68), vandopløselighedsdata (12)(19)(21)(39)(68-73) eller polaritetsdata afledt ved brug af omvendt fase HPLC (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).
Som vist i tabel 1 og 2 beregnes Koc eller Kom og dermed indirekte Kd af ligningerne:
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:
Desuden gælder, at skønt der er fundet tilfredsstillende korrelation mellem Pow og adsorptionen (19), kan det samme ikke siges om forholdet mellem vandopløselighed og adsorptionsgrad (19)(21); undersøgelser heraf har hidtil givet meget modstridende resultater.
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.
Nogle eksempler på korrelationen mellem adsorptionskoefficient og oktanol-vand fordelingskoefficient samt vandopløselighed er givet henholdsvis i tabel 1 og 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.
Eksempler på korrelation mellem adsorptionsfordelingskoefficienten og oktanol-vand fordelingskoefficienten; flere eksempler er givet i (12) og (68)
Examples of correlations between the adsorption distribution coefficient and the octanol-water partition coefficient; for further examples (12) (68).
Korrelation
Correlations
Forfatter
Authors
Substituerede urinstoffer
Substituted ureas
Aromatiske klorerede
Aromatic chlorinated
Forskellige pesticider
Various pesticides
Aromatiske carbonhydrider
Aromatic hydrocarbons
log Koc = -2,53 + 1,15 log Pow.
log Koc = -2,53 + 1,15 log Pow
Eksempler på korrelationen mellem adsorptionsfordelingskoefficient og vandopløselighed; flere eksempler er givet i (68) og (69)
Examples of correlations between the adsorption distribution coefficient and water solubility; for further examples see (68) (69).
Stoffer
Compounds
Alifatiske og aromatiske klorerede forbindelser
Aliphatic, aromatic chlorinated substances
a-naphtol
α-naphtol
log Koc = 4,273 - 0,686 log Sw
logKoc = 4,273 - 0,686 log Sw
Cykliske, alifatiske og aromatiske stoffer
Cyclic, aliphatic aromatic substances
log Koc = -1,405 - 0,921 log Sw - 0,00953 (mp-25)
logKoc = -1,405 - 0,921 log Sw-0,00953 (mp-25)
Forskellige forbindelser
Various compounds
BEREGNINGER TIL FASTLÆGGELSE AF CENTRIFUGERINGSBETINGELSER
CALCULATIONS FOR DEFINING THE CENTRIFUGATION CONDITIONS
Centrifugeringstiden er givet ved følgende formel, idet partiklerne forudsættes at være kugleformede:
The centrifugation time is given by the following formula, assuming spherical particles:
-ρaq
ρaq
For enkelhedens skyld er alle parametre angivet i ikke-SI-enheder (g, cm)
For simplification purposes, all parameters are described in non-SI units (g, cm).
ω rotationshastighed (=2 π rpm/60), rad s-1
ω = rotational speed (=2 π rpm/60), rad s-1
rp omdrejninger pr. minut
rpm = revolutions per minute
η opløsningens viskositet, g s-11 cm-1
η = viscosity of solution, g s-1 cm-1
partikelradius, cm
= particle radius, cm
massefylde af jord, g cm-3
= soil density, g cm-3
massefylde af opløsning, g cm-3
= solution density, g cm-3
afstand fra centrum af centrifugerotoren til overfladen af opløsningen i centrifugeglasset, cm
= distance from the centre of centrifuge rotor to top of solution in centrifuge tube, cm
afstand fra centrum af centrifugerotoren til bunden i centrifugeglasset, cm
= distance from the centre of centrifuge rotor to bottom in centrifuge tube, cm
længde af jord/opløsning-blandingen i centrifugeglasset, cm.
= length of the soil/solution mixture in the centrifuge tube, cm.
I praksis fordobler man sædvanligvis de beregnede tider for at sikre fuldstændig separation.
In general practice, double the calculated times is used to ensure complete separation.
Ligning 1 kan forenkles yderligere, hvis opløsningens viskositet (η) og massefylde (ρaq) sættes lig viskositeten og massefylden afvand ved 25 oC, η = 8,95 × 10-3 g s-1 cm-1 og ρaq = 1,0 g cm-3.
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.
Centrifugeringstiden er da givet ved ligning 2:
Then, the centrifugation time is given by the equation (2):
Af ligning 2 ses, at to parametre er vigtige ved fastlæggelse af centrifugeringsbetingelseme, nemlig tid (t) og hastighed (rpm), når man vil udskille partikler med en given størrelse (i vort tilfælde radius 0,1 μm): (1) jordens massefylde og (2) længden af blandingen i centrifugeglasset (Rb-Rt), dvs. den distance, som en jordpartikel tilbagelægger fra overfladen af opløsningen til glassets bund; for et givet rumfang er det klart, at længden af blandingen i røret bestemmes af kvadratet på rørets radius.
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.
Figur 1 viser sammenhængen mellem centrifugeringstiden (t) og centrifugeringshastigheden (rpm) for forskellige jordmassefylder (ps (Figur la) og forskellige længder af blandingen i centrifugeglassene (Figur 2a).
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).
Af figur la ses betydningen af jordens massefylde tydeligt; for en typisk centrifugeringshastighed på 3000 rpm er centrifugeringstiden ca.240 min for jord med massefylde 1,2 g cm men kun 50 min., når massefylden er 2,0 g cm Tilsvarende ses af figur 1b, at for en typisk centrifugeringshastighed på 3000 rpm er centrifugeringstiden ca. 50 min for en længde af blandingen på 10 cm men kun 7 min for en længde på 1 cm.
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.
Det er imidlertid vigtigt at finde et optimalt forhold mellem den centrifugering, som kræver mindst mulig længde, og den. som gør det let for eksperimentatoren at adskille faserne efter centrifugering.
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.
Ved fastlæggelse af forsøgsbetingelserne med henblik på adskillelse af fast og flydende fase er det desuden vigtigt at tage hensyn til eventuel tilstedeværelse af en tredje »pseudo«-fase, kolloiderne.
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.
Disse partikler, der er under 0,2 μm, kan i væsentlig grad påvirke hele absorptionsmekanismen for et stof i en jordsuspension.
These particles, with a size less than 0,2 μm, can have an important impact on the whole adsorption mechanism of a substance in a soil suspension. When centrifugation is performed as described above, colloids remain in the aqueous phase and are subjected to analysis together with the aqueous phase.
Når der centrifugeres som ovenfor beskrevet, forbliver kolloiderne i den vandige fase og bliver analyseret sammen med den vandige fase.
Thus, the information about their impact is lost.
Derfor går oplysningerne om deres indflydelse tabt.
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.
Hvis det laboratorium, som forestår undersøgelsen, har faciliteter til ultracentrifugering eller ultrafiltrering, kan adsorption/desorption af et stof i jord undersøges mere tilbundsgående, herunder stoffets adsorption på kolloiderne, I så tilfælde bør der anvendes ultracentrifugering ved 60000 rpm eller ultrafiltrering med en filterporøsitet på 100000 Dalton til at adskille de tre faser jord, kolloider og opløsning.
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.
Den forsøgsprotokol bør desuden ændres tilsvarende, således at alle tre faser analyseres for stoffet.
The test protocol should also be modified accordingly, in order all three phases to be subjected to substance analysis.
Figur 1a.
Fig. 1a.