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4 Test method
The reagents used in the test methods of this standard refer to analytical reagents unless other requirements are indicated; the experimental water should meet the requirements of Grade 3 water in GB6682
The standard solutions, preparations and products required in the test are prepared according to the methods specified in GB601 and GB603 unless other regulations are specified
4.
4.
Measure 10.
4.
The difference between the two parallel determination results is not more than 0.
4.
4.
Carry out according to the method specified in 2.
4.
The difference between the two parallel measurement results is not more than 0.
4.
4.
4.
4.
4.
3.
1.
3 Sodium hydroxide standard titration solution: c(NaOH)=0.
1mol/L;
4.
3.
2 Analysis steps
Weigh 10g of the sample (accurate to 0.
1g), put it into a 250mL Erlenmeyer flask, add 100ml of absolute ethanol , add 2 to 3 drops of phenolphthalein indicator solution, mix well and titrate with sodium hydroxide standard titration solution to a reddish end point , And do a blank test at the same time
.
4.
3.
3 Result calculation
The mass percentage of acidity (calculated as HC1) x 1 is calculated according to formula (1):
In the formula: 0.
03646— the mass of hydrochloric acid in grams equivalent to 1.
00mL sodium hydroxide standard titration solution [e(NaOH)=1.
000mol/L] ;
c— The concentration of sodium hydroxide standard titration solution (4.
3.
1.
3), mol/L;
V— The volume of the standard titration solution of sodium hydroxide consumed by the sample , mL;
V 1 —The volume of the sodium hydroxide standard titration solution consumed in the blank test , mL;
m—the mass of the sample, g
.
4.
3.
4 Allowance
The difference between the two parallel determination results is not more than 0.
005%, and the arithmetic mean is the determination result
.
4.
4 Determination of non-volatile matter
4.
4.
1 Test device
The test device is shown in Figure 1:
4.
4.
1.
1 Tubular electric furnace: equipped with a temperature regulator that can be adjusted within the range of 100 to 400°C
.
4.
4.
1.
2 Quartz tube: tube length 450mm, outer diameter 25mm, wall thickness 2mm
.
4.
4.
1.
3 Sample boat: made of hard glass or quartz, with a volume of about 3 mL
.
The dimensions should be such that the boat can be put into the quartz tube freely, and a small hole is left at one end of the boat so that the sample boat can be taken out of the furnace with a hook
.
4.
4.
2 Analysis steps
Add 1.
0~1.
2g sample (accurate to 0.
1g) into the sample boat that has been cleaned and dried to a constant weight, and then carefully put it into a quartz tube preheated to 182±2℃, with 600mL/min Nitrogen was introduced at a flow rate of, and the tail gas was introduced into an absorption bottle containing sodium hydroxide alcohol solution for bubbling absorption for 15 minutes.
The sample boat was taken out and placed in a desiccator to cool for 45 minutes, and then weighed (accurate to 0.
0002g)
.
4.
4.
3 Result calculation
The mass percentage of non-volatile matter X 2 is calculated according to formula (2):
In the formula: X 2 — non-volatile content, %;
m 1 —The mass of the residue after volatilization, g;
m—the mass of the sample, g
.
4.
4.
4 Allowance
The difference between the two parallel determination results is not more than 0.
02%, and the arithmetic mean is the determination result
.
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