eutech-instruments fluoride epoxy Manual Do Utilizador

Página de 22
Instruction Manual 
 
Fluoride Electrode
 
 
9
Prepare 2, 1, and 0.5 ppm fluoride standards by serial dilution of the 100 ppm fluoride standard. To 
each 50 ml of standard, add 50 ml of TISAB 1 or TISAB 2. Calibrate the meter as previously 
described by using the 2, 1, and 0.5 ppm standards. The calibration curve should be drawn on semi-
logarithmic 2-cycle graph paper or use an ion meter. 
 
Direct Measurement of Fluoride in Acid Solutions 
 
Hydrogen ion complexes a portion of the fluoride ion in solutions with a pH below 5, forming HF 
or HF
2
-1
, which cannot be detected by the electrodes. Adjustment to weakly acidic/weakly basic 
range before making the fluoride determination is necessary, but not with strongly basic solutions. 
The use of sodium acetate buffers the pH above 5 and helps fix the total ionic strength of standards 
and samples to the same level. 
 
1. 
Dissolve reagent grade sodium acetate (CH
3
COONa) in distilled water to prepare a 15% 
solution.  Prepare a sufficient quantity to dilute all standards and samples. 
 
2. 
Prepare a blank solution containing all components of the sample except fluoride. This 
solution will be used to prepare standards. 
 
3. 
Add fluoride to the blank solution to prepare standards in the concentration range of the 
unknown solutions. If using a standard pH/mV meter, prepare three standards and a 
calibration curve as previously described.  If an ion meter is used, only two standards are 
necessary. Add 9 parts of sodium acetate to each 1 part of standard. Fresh standards should 
be prepared every two weeks if the standard contains less than 10 ppm fluoride. 
 
4. 
Calibrate the electrodes as described in the section 
Electrode Slope Check
 
5. 
After diluting each unknown sample 10:1 with sodium acetate (as in 3 above), measure the 
mV potential and determine the fluoride concentration. 
 
 
Direct Measurement of Fluoride in Alkaline Solutions 
 
Hydroxide ions interfere with fluoride measurements in basic solutions with a low fluoride content. 
At a fluoride concentration less than 1.0X10
-4
M and at a pH of 9.5 or above, the electrode potential 
reading, caused by the concentration of both hydroxide and fluoride ions, is higher than it would be 
if fluoride alone were present. (See section entitled pH Effects.
        
Using a 4M buffered potassium acetate solution to adjust the pH to between 5 and 6 eliminates 
hydroxide ion error and raises the total ionic strength of both standards and samples to the same 
value. The fluoride ion concentration can be determined in the usual manner after both standards 
and samples are diluted 10:1 with the buffer solution. 
 
1. 
To prepare a 4M buffered potassium acetate solution, add one part of distilled water, 
slowly, to two parts of 6M acetic acid, CH
3
COOH, in a large beaker surrounded by a water 
bath.  Slowly add 50% KOH solution to the acetic acid mixture, with constant stirring, 
until a pH of 5 is reached. Prepare enough buffer to dilute all standards and samples 10:1.