Académique Documents
Professionnel Documents
Culture Documents
GB5413.24-2010
Preface
4.11.3 The determination of the end point for the titration: according to the titration
records (4.11.2), Based on measured E and V calculate E, V, first
derivative and second derivative , then fill into the table.
Table 1 The records for the titration of the sodium chloride standard solution by using the
standard silver nitrate titration solution
V E Ea Vb First Second
c
derivative derivative d
( E/ V)
In this formula:
V1—the volume of the standard silver nitrate titration solution at the end point of the
titration, mL;
Va—the volume of the standard silver nitrate titration solution at time point a, mL;
a—the value of second derivative before it changes into zero;
b—the value of second derivative after it changes into zero;
V—the value between a and b, mL.
Example:
It is found in the table that the maximal first derivative is 850, then second derivative
should be between 650 and -350 when second derivative is zero, therefore, a=650,
b=-350, Va=4.8 mL, V=0.10 mL
That is to say, the consumption of the standard silver nitrate titration solution at the end
4.11.4 The determination of the concentration of the standard silver nitrate solution:
In this formula:
C2- the accurate concentration of the standard silver nitrate solution, mol/L;
C1—the accurate concentration of the standard sodium chloride solution, mol/L;
V1—the volume of the standard silver nitrate titration solution that is consumed at the end
point of the titration, mL.
5. Instruments and equipments
5.1 pH meter: the precision ±0.1;
5.2 Glass electrode
5.2 Silver electrode
5.4 Electromagnetic stirrer;
5.5 Burette
5.6 Balance: precision 0.1mg, 1mg
6. Operation procedures
6.1 The preparation of the sample solution
Into 250 ml conical flask , Weigh about 20 g sample (accurate to 0.001 g) add 100 mL
hot water of 70 and heat to boiling for 15 min, with stirred. Cool to room
temperature, then add 4 mL precipitant I (4.8.1) and 4 mL precipitant II (4.8.2) in order.
Each addition, mix well. Stand for 30 min. Transfer to a 200 mL volumetric flask and
make up to the mark. Well mix and filter with filter paper, the first part of filter should
be discarded.
In this formula:
35.5—the mass of chlorine that is equal to that in 1.00 mL standard silver nitrate
titration solution [c(AgNO3)=1.000 mol/L], mg;
V2—the volume of the standard silver nitrate titration solution that is consumed during
the titration of the sample, mL;
f—the dilution factor;
m1—the mass of the sample, g;
c2—the accurate concentration of the standard silver nitrate titration solution, mol/L.
8. The precision
The difference between the two parallel measurements on the same sample should
be no more than 0.2 g for every 100 g sample.
Method 2 Precipitation titration
9. Principles
Organic acids are used to precipitate the protein in the sample and silver nitrate is
used to titrate the chloride ion in the sample and produce silver chloride precipitation.
Excessive silver nitrate will react with the potassium chromate indicator and changes
the solution into orange, it is the end point for the titration. The chlorine content is
calculated according to the consumption of the silver nitrate solution.
0.1×10
c= (4)
V
In which,
c- the concentration of silver nitrate, mol/L
V- the volume of silver nitrate, ml
0.1- the concentration of sodium chloride standard solution, mol/L
10- volume of the sodium chloride standard solution, ml
10.11 Phenolphthalein ethanol indicator: 10 g/L: dissolve 1g Phenolphthalein into
95% ethanol
11 Instruments and equipments
11.1 balance: nearest to 0.1mg
11.2 Volumetric flask, 100 mL
11.3 Conical flask, 125 mL
11.4 Brown burette, 10 mL
12 Operation procedures
12.1 into small flask, weigh 10 g homogenate sample (nearest to 0.1 mg), add 50 mL
water to dissolve the sample, transfer to a 100 mL volumetric flask, add10 mL
trichloracetic acid solution (10.5) , mix well and make up to the mark, stand for about 1 min
then filter.
12.2 Piptte10 mL filtrate into 125 mL conical flask , add three drops of Phenolphthalein
indicator (10.11) ,adjusted to slightly red with sodium hydroxide solution (10.6) and then
adjusted backward with nitric acid solution (10.7) until the red color has just disappeared.
Add another 10 drops of potassium chromate solution (10.8) then the solution is titrated
with silver nitrate solution (10.4) to orange and the color can not disappear within 1 minute,
and thus it is the end point for the titration, a piece of yellow paper is placed at the bottom
of the conical flask during the titration and thus the end point can be easily distinguished.
The blank experiment should be carried out at the same time.
V 5 100
X 2 = (V 3 − V 4) × C 3 × 35.5 × × (5)
V 6 m2
In this formula:
X2- content of chlorine in the samples, mg/100g
V3—the volume of the silver nitrate solution that is consumed for the titration of the
sample solution, mL;
V4—the volume of the silver nitrate solution that is consumed by the blank solution, mL;
C3—the concentration of the silver nitrate solution, mol/L;
V5—the volume of the sample solution, mL;
V6—the volume of the filtrate that is taken, mL;
m2—the mass of the sample, g.
The result is the mean of two repeat measurement results. Report results to two digital.
8. The precision
The absolute difference between the two results of repeat measurements should be less
then 5% of the mean.