-
Categories
-
Pharmaceutical Intermediates
-
Active Pharmaceutical Ingredients
-
Food Additives
- Industrial Coatings
- Agrochemicals
- Dyes and Pigments
- Surfactant
- Flavors and Fragrances
- Chemical Reagents
- Catalyst and Auxiliary
- Natural Products
- Inorganic Chemistry
-
Organic Chemistry
-
Biochemical Engineering
- Analytical Chemistry
- Cosmetic Ingredient
-
Pharmaceutical Intermediates
Promotion
ECHEMI Mall
Wholesale
Weekly Price
Exhibition
News
-
Trade Service
5.
5.
The pentaerythritol and impurity components in the sample react with the silylation reagent to generate the corresponding silylated derivatives
5.
5.
5.
5.
5.
5.
5.
5.
5.
5.
5.
5.
The chromatographic column and chromatographic operating conditions recommended by this standard are shown in Table 2
The chromatographic column should be aged before first use
.
In the case of a carrier gas (N 2 ) flow rate of 10 mmL/min, the initial column temperature is kept at 120°C for 2 hours
.
Then the temperature was raised to 260°C for 2h, and then to 290°C for 12h
.
Table 2 Recommended chromatographic column and chromatographic operating conditions
5.
3.
2.
5 Analysis steps
Debug the instrument according to the chromatographic operating conditions listed in Table 2 to make the instrument stable
.
Weigh 5.
1 mg (5-6) mg of the prepared sample, place it in a 2mL sample bottle, add 0.
1mL N,N-dimethylformamide, 0.
05mL N,O-(trimethylsilyl ) Trifluoroacetamide, cover the bottle stopper and shake well, and heat it in an oven at (70-80)°C for 10 minutes to obtain the prepared silanized derivative
.
Use a 10uL glass syringe to draw 1uL for analysis or use an autosampler to inject
.
Quantify by area naturalization method
.
5.
3.
2.
6 Result calculation
The mass fraction w 2 of pentaerythritol , the value is expressed in %, calculated according to formula (2):
Where:
A—the area of the chromatographic peak of pentaerythritol silylated derivative;
A i —the area of the chromatographic peak of a silanized derivative of a component;
w 5 —5.
5 The mass fraction of the measured loss on drying, and the value is expressed in %
.
Take the arithmetic average of the two parallel determination results as the determination result
.
The absolute difference between the two parallel determination results is not more than 0.
20%
.
Related Links: Pentaerythritol for Industrial Use (2)