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0 The
photoinitiator is a key component of UV-cured coatings and play a decisive role in the sensitivity of photo-cured coating systems, which is related to the storage stability of the formulation system and the conversion efficiency of low polymers and active thinners from liquid to solid polymer membranes and the quality of film forming, so their dosage must be effectively controlled. At present, there are a wide variety of light triggers on the market, different manufacturers of its similar varieties of purity, which brings a certain pressure to the use of units of raw material testing, the traditional gas chromatography test substance purity, it is difficult to be suitable for vaporization temperature of light triggers (too high vaporization temperature may lead to the decomposition of light triggers), and liquid chromatography can make up for such deficiencies. This method is used in the current market more commonly used typical varieties of light trigger xylene, light trigger 1173, light trigger 819, T PO, parabens were measured, the quantitative results are fully in line with the quality control requirements
China
.
1 Test Section
1.1 Main instrument equipment and reagents
Efficient Liquid Chromatography Waters 1525 Pump, 2487 UVDetector, Column NUCLEODUR C18 Isis 250mm×4.6 mm, 5 sm. Xybenzene, 2,4,6-MDRY (dibenzene oxide, commonly known as T P O), 2-hydroxy-2-methyl-1-benzene-1-acetone (light trigger) 1173), benzene-based double (2,4,6-triamylphenyl) oxidation (light trigger 819), parabens, all of which are pure analysis;
1.2 chromatography conditions
flow phase: A (acetylene), B (pure water), detection wavelength 299 n m; sample volume 20 μL; gradient wash-out, see Table 1.
Flow phase gradient wash-out table
1.3 sample pre-treatment
called wet sample paint sample 1.5 g placed in a 50 m L capacity bottle, dissolved with acetylene, diluted fixed capacity, oscillation, full shake, with 0.45 μ L syringe filter membrane filtration, sample 20 μ L, collect data and use the corresponding parts of the standard quantitative curve. Taking into account the particularity of the sample, all of the above preparation processes need to be carried out in a light-absorbing environment.
2 Results and discussion
2.1 standard curve preparation
respectively accurately named a variety of analytical pure light trigger samples, dissolved with acetylene, add acetylene to the scale, and dilute into different concentrations of standard solution Under the chromatography conditions of 1.2, the linear range and detection limit are obtained, as shown in Table 2;
The equations of the various standard material curves
2.2 repetitive tests
take a standard solution of 2.1 and take 5 consecutive samples according to the chromatography conditions mentioned above, and measure the relative standard deviation of the peak area and retention time of each light trigger, as shown in Table 3, Figure 3.
5 kinds of light trigger standard solution repeat sample overlapping map
standard solution repeat sample accuracy
2.3 recovery rate test
add a certain amount of photoinstigation agent 1173, benzoyl toluene, xybenzene, T P O, photoinstrogen 819 control, according to 1.3 sample treatment, in 1.2 chromatography conditions. The recovery rate of 5 light triggers was more than 99.98% after 7 repeated measurements, and the deviation from standard
was 0.32% to 0.43%, as seen in Table 4.
recovery rate and relative standard deviation of
5 light triggers (n-7)
2.4 sample analysis
accurately called the appropriate amount of samples, according to 1.3 sample treatment, in 1.2 chromatography conditions, see Table 5.The test results of
5 kinds of light triggers
3 conclusion
above the test results show that the H P L C method is used to determine the content of light triggers in U V curing coatings, which is simple and accurate, especially for liquid samples.