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Determinación de Fe III y/o Fe total en Aguas Potables y Naturales por Medio de Extracción en Fase SólidaPapic Morales, Jorge 11 1900 (has links)
Seminario de Título entregado a la Universidad de Chile en cumplimiento parcial de los requisitos para optar al Título de Químico Ambiental / Iron (Fe) is a transition metal usually found in potable water at low concentrations, whose concentration limit is 0.3 mg / L according to NCh 409, and due to its common use mainly in pipelines and industries, it must be constantly monitored, in order to keep its concentration under the limits and guarantee the welfare of people.
The aim of this work is to promote an easy method to identify and extract Fe from potable and natural waters through solid phase extraction. This was done both for acid and basic mediums. 0.4 mL of sulfosalicylic acid (SSA) at 2.5% w/v was used as a ligand, adding 3 mL of a monochloroacetic acid buffer for the samples in acid medium and 3 mL of concentrated NH3 (12,66 M) for samples in basic medium and form a complex, either Fe(III)-SSA or Fetotal-SSA, in 100 mL total solution. Then, an anion exchange solid resin was added, called AG 2-x8 from BIORAD, in order to preconcentrate the complex. Previous studies were conducted without the addition of resin to observe the formation of the complex and study its characteristics. The quantification limits were 0.56 ppm and 0.28 ppm, which are very high or too close to the concentration limit of Fe allowed in potable water, that is, 0.3 ppm (NCh 409). Solid phase studies were carried out in order to decrease the quantification limits of the method. Then the chemical variables involved in obtaining the complex were optimized, such as the amount of SSA, anionic resin, buffer and total volume. Thus obtaining the adequate amounts for each analyte, mentioned above. The extraction of the Fe-ASS complex was possible for both media. However, in a basic medium it requires much higher Fe concentrations for its formation and presented a constant turbidity in the form of a colloidal compound of gray tone mainly referred so the procedure was more thoroughly studied in acid medium. The Fe(III)-SSA complex presented good linearity throughout the measurement range with an DL of 7.32 x 10-3 ppm and an QL of 0.024 ppm achieving a good sensitivity and a recovery percentage of 99.7%. Only SO4-2 presented interference in the sample with a tolerance limit of only 100 ppm. The standard addition method was effective to eliminate this interference by treating the entire matrix in the same way throughout the measurement range. Potable water samples were taken from different sources, such as, from the Analytic Chemistry Laboratory (Ñuñoa), Quinta Normal and from a construction zone adjacent of the the Faculty of Sciences of the University of Chile. Fe is generally found at concentrations below the norm (23.38 ppb and 172 ppb), but is sensitive to climatic factors (522 ppb after a very rainy day) and construction places with little waste treatment (342.3 ppb), so it must be constantly monitored. Solid phase extraction is a simple, fast and efficient method and has a wide range of applications for different compounds or chemical substances.
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