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4 Test method
4.
Some test procedures specified by the test method may lead to dangerous situations
4.
Unless otherwise specified, only reagents confirmed to be analytically pure and grade 3 water specified in GB/T6682 are used in the analysis
The standard titration solutions, standard solutions for impurity determination, preparations and products used in the test methods are prepared in accordance with GB/T601, GB/T602, and GB/T603 unless other requirements are specified
4.
4.
The sample uses formic acid as auxiliary solvent, glacial acetic acid as solvent, crystal violet as indicator, and titration with perchloric acid standard titration solution.
4.
4.
4.
4.
4.
4.
4.
4.
4.
3.
4 Result calculation
The mass fraction w 1 of glycine , expressed in %, calculated according to formula (1):
Where:
V 1 —The value of the volume of the perchloric acid standard titration solution (4.
3.
2.
3) consumed by the sample, in milliliters (mL);
V 2 ——The value of the volume of the perchloric acid standard titration solution (4.
3.
2.
3) consumed in the blank test, in milliliter (mL);
c — The exact value of the concentration of perchloric acid standard titration solution, the unit is moles per liter (mol/L);
m——the value of the mass of the sample, the unit is grams (g);
M — The value of the molar mass of glycine , in grams per mole (g/mol) (M=75.
07)
.
Take the arithmetic mean of the two parallel determination results as the determination result, and the absolute difference between the two parallel determination results shall not exceed 0.
3%
.
4.
4 Determination of chloride content
4.
4.
1 Method summary
The sample uses potassium chromate as an indicator and is titrated with a silver nitrate standard titration solution to calculate the chloride content in the sample
.
4.
4.
2 Reagents
4.
4.
2.
1 Silver nitrate standard titration solution: c(AgNO 3 )=0.
05 mol/L;
4.
4.
2.
2 Potassium chromate solution: 100g/L, weigh 10g potassium chromate , accurate to 0.
01g, dissolve it in a small amount of water containing 1 drop of sodium hydroxide solution (100g/L), and dilute to 100mL
.
4.
4.
3 Analysis steps
4.
4.
3.
1 Weigh about 1g laboratory sample as the test material, accurate to 0.
0002g, place it in a 250mL conical flask, add 50mL water to dissolve, add 7 drops of potassium chromate solution, and titrate with silver nitrate standard titration solution to brick red For the end
.
4.
4.
3.
2 At the same time of measurement, perform a blank test with the same amount of reagent solution without adding samples according to the same steps as the measurement
.
4.
4.
4 Result calculation
The mass fraction w 2 of chloride (calculated as Cl) , the value is expressed in %, calculated according to formula (2):
Where:
V 1 —The value of the volume of the standard silver nitrate titration solution (4.
4.
2.
1) consumed by the sample, in milliliters (mL);
V 2 —The value of the volume of the silver nitrate standard titration solution (4.
4.
2.
1) consumed in the blank test, in milliliter (mL);
c— The exact value of the concentration of silver nitrate standard titration solution, in moles per liter (mol/L);
m—the value of the mass of the sample, in grams (g);
M—The value of the molar mass of chlorine, in grams per mole (g/mol) (M=35.
45)
.
Take the arithmetic average of the two parallel determination results as the determination result, and the absolute difference between the two parallel determination results shall not exceed 0.
03%
.
4.
5 Determination of loss on drying
4.
5.
1 Analysis steps
Weigh about 1g laboratory sample as a sample, accurate to 0.
0002g, and place it in a weighing bottle that has been dried at (105±2)℃ to a constant mass, and spread it into a layer with a thickness of less than 5mm.
) Dried at ℃ for 3h, placed in a desiccator to cool for 30min, and weighed
.
Keep the dried substance A for the determination of the content of aminoacetic acid
.
4.
5.
2 Result calculation
The mass fraction of loss on drying w 3 , the value is expressed in %, calculated according to formula (3):
Where:
m—The value of the mass of the sample before drying, in grams (g);
m 1 —The value of the mass of the sample after drying, in grams (g)
.
Take the arithmetic average of the two parallel determination results as the determination result, and the absolute difference between the two parallel determination results shall not exceed 0.
05%
.
Related Links: Glycine (Glycine) for Industrial Use (1)