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4.
4.
4.
a.
b.
c.
4.
a.
b.
c.
4.
4.
Detector: hydrogen flame ionization detector, the lowest detection concentration is 0.
4.
a.
b.
c.
Filling method: plug the outlet end of the chromatographic column (connected to the detector) with a little glass wool, draw a vacuum from the outlet end, and fill it with about 20g of stationary phase under gentle vibration, fill it evenly and tightly, and then use a glass wool plug Good
.
d.
Aging of the chromatographic column: Put the filled column into the column box of the chromatograph.
After checking the air tightness, pass nitrogen and gradually increase the temperature to 210°C and age at 210°C for more than 8 hours until the baseline is stable
.
4.
7.
2.
3 Injector
Micro glass syringe
.
4.
7.
2.
4 Chromatographic data processor
Recorder or integrator
.
4.
7.
3 Analysis steps
4.
7.
3.
1 Adjust the instrument Adjust the instrument according to the following reference conditions
a.
Vaporization chamber temperature: 250~300℃;
b.
Testing room temperature: 250~300℃:
c.
Oven temperature: 180~200℃;
d.
Nitrogen flow rate: 25mL/min~30mL/min;
e.
Hydrogen flow rate: 25mL/min~30mL/min;
f.
Air flow rate: 400mL/min;
g.
Sample dilution: sample+solvent=1+5;
h.
Injection volume: 0.
02uL~0.
1uL
.
4.
7.
3.
2 Quantitative method
Modified area normalization method
.
4.
7.
3.
3 Test
Adjust the instrument according to the above reference conditions.
After the baseline is stable, use a micro glass syringe to inject the sample, and use the chromatogram recorder or integrator to process and calculate the data according to the corrected area normalization method
.
4.
7.
4 Calculation of analysis results
4.
7.
4.
1 Calculate according to formula (4) for each component X i (%):
In the formula: x i — the content of component i, when X i is Xc16 , it represents the purity of cetyl alcohol , and when X i is X RH , it represents the content of alkane;
A i —corresponding to the chromatographic peak area of component i;
f—The chromatographic peak quantitative correction factor corresponding to component i
.
4.
7.
4.
2 Quantitative correction factor: Measured with chromatographically pure known samples, calculated according to formula (5):
In the formula: f w -weight correction factor;
A i , W i , A s , W s -are the peak area and weight of the analyte and the known chromatographically pure standard, respectively
.
Take the arithmetic mean of the two parallel determination results as the determination result, and the difference between the two parallel determination results shall not exceed 0.
5%
.
Figure 2 C16 alcohol chromatogram