Organic peroxide is a substance widely used as a chemical intermediate, catalyst, and initiator. Among them, di-tert-butyl peroxide is the most commonly used dialkyl peroxide and is often used as a synthetic resin initiator, photopolymerization sensitizer, rubber vulcanizing agent, and diesel ignition promoter.
Di-tert-butyl peroxide is often obtained by the reaction of tert butanol, sulfuric acid, and hydrogen peroxide. This article briefly introduces the detection method of di-tert-butyl peroxide:
A-Di-tert-butyl peroxide iodometry:
1) Add 20mL of acetic acid to a 250mL iodine bottle, bubble with rapidly passing carbon dioxide for 2 minutes, then stopper the bottle and store it for analysis;
2) Accurately weigh the sample containing 3-4 meq of reactive oxygen species with an accuracy of 0.1mg and transfer it to an iodine bottle;
3) Add 5mL of saturated NaI solution prepared on site, tighten the stopper, rotate the iodine bottle, add a few milliliters of water to the bottle, add 1mL of concentrated hydrochloric acid, and then partially immerse the iodine bottle in a water bath maintained at 60 ℃ for 1 hour;
4) Remove the iodine bottle from the water bath and cool it to room temperature;
5) Add 60mL of deoxygenated water and titrate with 0.1meq/mL (N) Na2S2O3 solution until the color of the solution turns light yellow. Then add 1-2 mL of starch solution and continue titrating until the blue color suddenly disappears. Record the milliliters of titration solution required for titration;
6) Subtract the milliliters of titrant consumed during blank titration and calculate the analytical value of the sample.
B-Di-tert-butyl peroxide chromatography
1) Instruments and materials
a) Gas chromatograph: FID detector;
b) Gas chromatography data workstation N2000;
c) Chromatographic column: quartz capillary column, model: OV-1, specification: 30m × 0.25mm × zero point three μ M;
d) Syringe 1 μ L.
2) Reference operating conditions for gas chromatographs
a) Keep the initial temperature at 50 ℃ for 4 minutes;
b) Heating rate 10 ℃/min;
c) Final temperature 150 ℃, maintained for 10 minutes;
d) Vaporization at 180 ℃;
e) Detection at 180 ℃;
f) Carrier gas: Nitrogen gas.
3) Measurement steps
Using a micro injector (1 μ L) Extract standard sample 0.2 μ Inject L into the chromatography, record the peak time, and then inject the sample under the same conditions. The peak area corresponding to the corresponding time is the content, calculated using the area normalization method.https://www.kz-opchem.com/organic-peroxides/dtbp-cas-110-05-4-di-tert-butyl-peroxide.html