A kind of determination method of oxalic dihydrazide purity
A technique for measuring oxalohydrazide and its method, which is applied in the field of chemical analysis, can solve problems such as the absence of a method for measuring the purity of oxalyldihydrazine, which affects the accuracy of test results, and achieve the goal of improving accuracy and stability and avoiding impurities Interfering and improving the effect of separation
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Embodiment 1
[0045] The C18 chromatographic short column used in this example was purchased from Philomon Corporation of the United States, the model is ACE C-18, the length of the chromatographic column is 50 mm, the inner diameter is 4.6 mm, the particle size of the filler is 2.5 μm, and the Hilic chromatographic column is purchased from Agilent Corporation of the United States, The model is Agilent poroshell 120 Hillic chromatographic column with a length of 150mm, an inner diameter of 4.6mm and a particle size of 2.7μm;
[0046] Step 1, prepare the test sample: Weigh seven parts of oxalic dihydrazide, the weighing samples are respectively 0.0208g, 0.0509g, 0.0401g, 0.0355g, 0.0907g, 0.01079g and 0.0080g, dissolve in ultrapure water for 30min , after the sample solution is all clear and transparent, let it stand to constant volume. The solution to be tested is formed, and its concentration is 4.16×10 -4 g / mL, 1.08×10 -4 g / mL, 8.02×10 -4 g / mL, 7.10×10 -4 g / mL, 1.83×10 -3 g / mL, 2.16×...
Embodiment 2
[0051] The C18 chromatographic column used in this example was purchased from Agilent in the United States, the model is Agilent poroshell120 EC C-18, the column length is 50 mm, the inner diameter is 4.6 mm, the particle size of the filler is 2.7 μm, and the Hilic chromatographic column is purchased from Agilent in the United States, model It is an Agilent poroshell 120 Hillic chromatographic column with a length of 150 mm, an inner diameter of 4.6 mm and a particle size of 2.7 μm.
[0052] Step 1, prepare the test sample: Weigh seven parts of oxalic dihydrazide, the weighing samples are respectively 0.0208g, 0.0509g, 0.0401g, 0.0355g, 0.0907g, 0.01079g and 0.0080g, dissolve in ultrapure water for 30min , after the sample solution is all clear and transparent, let it stand to constant volume. The solution to be tested is formed, and its concentration is 4.16×10 -4 g / mL, 1.08×10 -4 g / mL, 8.02×10 -4 g / mL, 7.10×10 -4 g / mL, 1.83×10 -3 g / mL, 2.16×10 -4 g / mL and 1.6×10 -4 g / ...
Embodiment 3
[0057] The C18 chromatographic short column used in this example was purchased from Philomon Corporation of the United States, the model is ACE C-18, the length of the chromatographic column is 50 mm, the inner diameter is 4.6 mm, and the particle size of the filler is 2.7 μm; the Hilic chromatographic column is purchased from Agilent Corporation of the United States, The model is an Agilent poroshell 120 Hillic chromatographic column with a length of 150 mm, an inner diameter of 4.6 mm, and a particle size of 2.7 μm; the oxalic dihydrazide standard sample was purchased from Sigma Company in the United States, and the purity was marked as 97.36% in the manual.
[0058] Step 1, prepare a test sample: Weigh oxalic dihydrazide with a sample weight of 0.0220 g, dissolve it in ultrapure water for 30 minutes, and after the sample solution is all clear and transparent, let it stand to constant volume. The solution to be tested is formed with a concentration of 4.40g×10 -4 / mL, filter...
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