Determination of Fluoride by Conductometric Titration - Analytical

Chem. , 1959, 31 (2), pp 283–286. DOI: 10.1021/ac60146a041. Publication Date: February 1959. ACS Legacy Archive. Cite this:Anal. Chem. 31, 2, 283-28...
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zero, the copper became niolteii in about 3 minutes, and the pressure bccame constant in 8 to 10 minutes. RESULTS AND DISCUSSION

Table I shows the variation of the results n i t h sample neight. The results indicate that the method is almost independent of sample weight. The slight deviation of the results w h m samples less than 2.5 grams were used is possiiil,~due to error in reading the nianonieter as the readings are ion, or to a different temperature gradient existing in the systeni nhen low pressures of gas are present, as the correction factor for the expansion of the gas may not be the samc a t all prcssures. The appxratus n a s calibrated a t gas prcwurcs equivalent to those n hich nould lie obtained from the saniplrs to be analyzed. Thc data contained in the first and third columns of Table I n prc’ fittcd by the method of least squares, assuming a rnoclcl of the form I’ = a bx, nhere Y is thc iiiicrogranie of oxygen recovered and z is the sample neight in grams. The brst estimates of the constants

+

Table

I. Variation of Results with

Table II.

Sample Weight

Sample Wt., Grams 0.76

Pressure, l l n i.

1.10

2.59 3.11 3 49 5 61

5 1

16 19 2.‘ :34

Oxygen,

‘;C

Sample

0.055 0.057

1 2

0 061 0 063 0.062

1

0.061

3

5 6

7 8

and 650, respectively, with 95% confidence intervals of -155