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Marine Geochemistry - Laboratory Methods

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Fluoride detection with Ion Selective Electrode
method Fluoride in seawater is detected using a ion selective electrode
 
electrode ORION F-combination electrode 96-09.
method ion selective electrode measurement. details
electrolyte INGOLD #9811 3M KCl, AgCl saturated
standard stock :Merck #19814, 1000 mg F/L
work standard 100 ppm F by dilution with pure water
buffer

TISAB III (Total Ionic Strength Adjustment Buffer):
dissolve 300 g Na-citrate x 2H2O 22g Titriplex IV (1,2 Cyclo-hexylen-dinitrilo-tetra-acidic acid) and 60 g NaCl in pure water and fill up to 1L

dilution solution NaF-free artificial seawater
calibration standards appropiate amounts of work standard are diluted with NaF-free artificial seawater. Add 10% TISAB (50 mL standard + 5 mL TISAB) (usually 0.5 and 5 ppm)
general conditions Ionic strength should be similar in all standards and samples. pH should be in the range of pH 5 - pH 8. Seawater Mg concentration considerably affects analysis and has to be compensated for by using either seawater background standards or standard addition. If calibrated with seawater background standards, direct measurement may be performed.
buffer dose 10% of sample volume
sample volume We work with sample volumes as low as 1.5 mL (+ 150 µL TISAB) if necessary. ORION combination electrodes have a flat membrane and a concentric diaphragm such that solution level of a few mm is sufficient
storage and conditioning

Store in 1000 ppm standard solution (without TISAB !)
Do not immerse into solutions containing TISAB for extended periods.
Do not store solutions containing fluoride ions in glass containers. Rinse all glassware immediately after use

tips + tricks

This electrode leaks electrolyte (on purpose) -> electrolyte level needs to be controlled frequently:electrolyte level should be 2.5 cm above solution level. The same setup may be used to measure fluoride in toothpaste

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