Iron (oxy)hydroxides play an important role in a variety of disciplines, among others, environmental and exploration geochemistry, mineralogy, geology and soil science. In selective leaching ...procedures, either for the removal of (oxy)hydroxide prior to clay minerals analysis or for the determination of metals in reducible soil/sediment fractions, it is very important to preserve the entire undissolved residue. Therefore, the objectives of the study were: (1) to fi nd the most effective reagent rinsing method which follow the dissolution of (oxy)hydroxides; and (2) to test if the content of Fe (oxi)hydroxides could be determined gravimetrically. The following reagent rinsing methods were tested: (1) centrifugation, (2) filtration, (3) dialysis. The analysis was conducted on the sample of red soil with 5.12% Fe2O3. The time needed for rinsing increased in this order: centrifugation < fi ltration < dialysis. The amount of gravimetrically determined dissolved reducible fraction upon rinsing varies signifi cantly depending on the methods and it is remarkably higher than the amount of Fe2O3 calculated from iron content determined by atomic absorption in leachate. The most effective reagent rinsing method which follows the dissolution of (oxy)hydroxides using dithionite-citrate-bicarbonate is dialysis. No loss of sample is the advantage of this method, but its disadvantage is time needed for its completion. Centrifugation is relatively rapid, but can lead to loss of the smaller particles. In this case the loss was unacceptably great. Filtration using filter paper is more time consuming than centrifugation and it showed the worst results. The conclusions are that: (1) the content of Fe (oxi)hydroxides cannot be determined gravimetrically upon selective leaching; (2) rinsing of reagents after Fe (oxi)hydroxide removal prior to clay mineral analysis should be carefully selected and performed; (3) centrifugation, accepted rinsing method in all sequential extraction sequences, can cause misleading results.
Iron (oxy)hydroxides play an important role in a variety of disciplines, among others, environmental and exploration geochemistry, mineralogy, geology and soil science. In selective leaching ...procedures, either for the removal of (oxy)hydroxide prior to clay minerals analysis or for the determination of metals in reducible soil/sediment fractions, it is very important to preserve the entire undissolved residue. Therefore, the objectives of the study were: (1) to find the most effective reagent rinsing method which follow the dissolution of (oxy)hydroxides; and (2) to test if the content of Fe (oxi) hydroxides could be determined gravimetrically. The following reagent rinsing methods were tested: (1) centrifugation, (2) filtration, (3) dialysis. The analysis was conducted on the sample of red soil with 5.12% Fe2O3. The time needed for rinsing increased in this order: centrifugation < filtration < dialysis. The amount of gravimetrically determined dissolved reducible fraction upon rinsing varies significantly depending on the methods and it is remarkably higher than the amount of Fe2O3 calculated from iron content determined by atomic absorption in leachate. The most effective reagent rinsing method which follows the dissolution of (oxy)hydroxides using dithionite-citrate-bicarbonate is dialysis. No loss of sample is the advantage of this method, but its disadvantage is time needed for its completion. Centrifugation is relatively rapid, but can lead to loss of the smaller particles. In this case the loss was unacceptably great. Filtration using filter paper is more time consuming than centrifugation and it showed the worst results. The conclusions are that: (1) the content of Fe (oxi)hydroxides cannot be determined gravimetrically upon selective leaching; (2) rinsing of reagents after Fe (oxi)hydroxide removal prior to clay mineral analysis should be carefully selected and performed; (3) centrifugation, accepted rinsing method in all sequential extraction sequences, can cause misleading results.
Željezovi (oksi)hidroksidi imaju važnu ulogu u različitim disciplinama, među ostalim u zaštiti okoliša, prospekciji rudnih ležišta, mineralogiji, geologiji i pedologiji. U postupcima selektivnoga ...otapanja, bilo da su namijenjeni uklanjanju (oksi)hidroksida prije analize minerala gline ili za određivanje metala u reducirajućoj frakciji tla/sedimenta, vrlo je važno sačuvati cijeli neotopljeni ostatak. Stoga su ciljevi ovoga rada bili: (1) odrediti najučinkovitiju metodu ispiranja reagensa nakon otapanja (oksi)hidroksida i (2) provjeriti može li se sadržaj željezova (oksi)hidroksida odrediti gravimetrijski. Testirane su sljedeće metode ispiranja: (1) centrifugiranje, (2) filtriranje, (3) dijaliza. Analiza je provedena na uzorku crvenice koji sadržava 5,12 % Fe2O3. Vrijeme potrebno za ispiranje povećava se ovim redoslijedom: centrifugiranje < filtriranje < dijaliza. Udio gravimetrijski određene otopljene frakcije znatno se razlikuje ovisno o odabranoj metodi ispiranja te je neusporedivo veći od udjela Fe2O3 određenoga mjerenjem željeza u ekstraktu nakon otapanja. Najučinkovitija metoda ispiranja ditionit-citrat-bikarbonata nakon otapanja (oksi)hidroksida jest dijaliza. Prednost je ove metode u tome što nema gubitka uzorka, a nedostatak je vrijeme potrebno za njezino provođenje. Centrifugiranje je relativno brza metoda, no može dovesti do gubitka sitnih čestica. U ovome istraživanju gubitak je bio neprihvatljivo velik. Filtriranje pomoću fi ltarskoga papira oduzima više vremena od centrifugiranja te je pokazalo najlošije rezultate. Na temelju rezultata možemo zaključiti: (1) sadržaj željezova (oksi)hidroksida ne može se odrediti gravimetrijski nakon selektivnoga otapanja; (2) način ispiranja reagensa nakon uklanjanja željezova (oksi)hidroksida pri pripremi uzoraka za analizu minerala glina treba biti pažljivo odabran i izveden; (3) centrifugiranje, uobičajena metoda ispiranja u svim postupcima sekvencijske ekstrakcijske analize, može dovesti do krivih rezultata.
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