detection
method of metaldehyde
Principle:
The impurity of metaldehyde product are acetaldehyde, trimeric acetaldehyde, water and stabilizing agent. Extract acetaldehyde and trimeric acetaldehyde in the product by alcohol, then detect the content of acetaldehyde and the content of trimeric acetaldehyde in the extract.
Method:
First, weigh up metaldehyde product range from 0.3g to 0.5g(be accurate
to0.0002g)and dump into a little glass flask that could be airproof, then add
one drop 0.1N NaOH solution and 20ml ethanol, and weigh it, then add 6µl
toluene as internal standard with micro injector, and weigh it, then oscillate
the flask in order to completely extract acetaldehyde, trimeric acetaldehyde.
chromato term:
chromato column:length 30 meters microcolumn
press the column ahead N2:0.04Mpa;
H2:0.03Mpa;Air:0.03Mpa
Vaporization
temperature:100℃;detector
temperature:220℃
Column temperature:
At first, maintain 60℃ for 5 mins ,then raise the temperature from 60℃ to 80℃, then raise the temperature from 80℃ to 200℃ at the speed 20℃/min and maintain 200℃ for 30mins.The setup of the column temperature may be adjusted in according to the fact
calculation:
the percent of acetaldehyde content
=( acetaldehyde peak area /internal standard peak area)×(internal
standard weigh/sample weigh)×2.08
the percent of trimeric acetaldehyde=( trimeric acetaldehyde peak area /internal standard peak area)×(internal standard weigh/sample weigh)×3.02
remark:2.08
and 3.02 are correction factors
The percent of metaldehyde content is that 100 percent minus the percent of acetaldehyde content minus the percent of trimeric acetaldehyde content minus the percent of stabilizing agent content
(metaldehyde)% =100 — (acetaldehyde)% — (trimeric acetaldehyde)% —0.2
remark: the percent of stabilizing agent content is 0.2%.