Detection method for ethlenethiourea in plastic products
A detection method and technology of ethyl thiourea, applied in the detection field of ethylene thiourea, can solve the problems of low accuracy of quantitative analysis and long detection time, and achieve the effect of good linear relationship and high accuracy
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Embodiment 1
[0059] 1. Pretreatment of samples
[0060] S1: Take a sample from the clean part of the plastic sample, cut it into pieces below 2mm×2mm×2mm, weigh 1g±0.1g (accurate to 0.1mg) of the sample into a 60ml glass reaction bottle, add 10ml of methanol, extract for 1h, repeat the above Operate once, combine the extracts twice, mix well, concentrate with a rotary evaporator to a small amount, then slowly blow nitrogen to dryness, then use methanol to make the volume to 1ml, and finally filter the sample through a 0.45um microporous membrane, Obtain the sample to be tested.
[0061] S2: Accurately weigh 0.01015g of ethylene thiourea standard product with a 100,000 graded analytical balance, add it to a 10ml volumetric flask, dissolve it in methanol to make a standard stock solution of 1000mg / L, and then dilute it step by step to 0.01 mg / L, 0.02mg / L, 0.05 mg / L, 0.1 mg / L, 0.2 mg / L, 0.5 mg / L, 1 mg / L standard working solutions.
[0062] 2. The sample to be tested and the standard working...
Embodiment 2
[0090] Example 2: Detection limit determination
[0091] Figure 4 It is the diode array diagram and the mass spectrogram of the 0.01mg / L ethylenethiourea standard substance that is the concentration of embodiment 2 of the present invention;
[0092] The standard samples with different concentrations were detected and analyzed by Figure 4 It can be concluded that the detection limit (3 times the signal-to-noise ratio) of ethylenethiourea can reach 0.01mg / L. The limit for each compound in the REACH regulation is 1000 mg / kg. It can be seen that this method can fully meet the restriction requirements of the REACH regulation for ethylene thiourea.
Embodiment 3
[0093] Example 3: Precision experiment
[0094] According to the detection method provided by the present invention, the standard sample of ethylene thiourea with an intermediate concentration point of 0.1 mg / L is taken and measured continuously for 7 times, and the relative standard deviation is less than 4%, and the precision is good. The results are shown in Table 3.
[0095] Table 3 Precision test of ethylene thiourea
[0096] test count Ethylenethiourea 1 0.096 2 0.094 3 0.090 4 0.088 5 0.093 6 0.092 7 0.099 average value 0.093 Relative deviation 0.0037 relative standard deviation / % 3.94
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