Method for detecting iron ions in chlorohydrocarbon
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A detection method, iron ion technology, applied in the field of chemical analysis and detection, can solve problems such as complex operation, environmental pollution, poisonous and harmful, and achieve the effect of improving detection efficiency and simple operation
Pending Publication Date: 2020-08-25
常州新东化工发展有限公司
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[0003] Iron ion content is an important central control index in the synthesis process of chloropropene. Usually, the traditional iron ion detection methods mainly include o-phenanthroline spectrophotometry, ICP-OES elemental analysis, atomic absorption spectrometry, etc. However, these iron ion The detection method is mainly suitable for aqueous solution systems, and the detection of iron ions in organic matter must be pre-treated
The commonly used pretreatment methods mainly include microwave digestion method, evaporation method, and roasting method. These treatment methods not only pollute the environment, but also complicate the operation, and will produce toxic and harmful gases during the operation, which do not meet the requirements of safety and environmental protection; Ions are relatively easy to lose, which affects the accuracy of the detection results
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Embodiment 1
[0027] Step 1. Draw a standard curve:
[0028] Place the standard sample with iron ion concentration of 0.01g / L in six 50ml volumetric flasks according to Table 1, see Table 1 for details:
[0029] Table 1
[0030]
[0031]
[0032] Get 1 milliliter sample and analyze by GB320-2006 iron ion detection method, and the measured results are as shown in Table 2:
[0035] Draw a standard curve with the iron content as the abscissa and the corresponding absorbance as the ordinate, and the measurement results are linearly fitted. The results are as follows: figure 1 As shown, by performing a linear fit on the measured results, the degree of fit R 2 is 0.9999, indicating that the iron content detection method of the present invention is accurate and reliable.
[0036] Step 2...
Embodiment 2
[0041] Step 1, drawing a standard curve, is consistent with Example 1, and will not be repeated here.
[0042] Step 2. Prepare the sample to be tested:
[0043] Prepare a 1,1,1,3-tetrachloropropane sample with an iron content of 150ppm, place the 1,1,1,3-tetrachloropropane sample in a 50ml volumetric flask, add methanol with a purity of 99.9% to volume Shake well, wherein the 1,1,1,3-tetrachloropropane sample accounts for 30% of the mass ratio of the organic solvent mixture; follow the sample preparation steps to make a blank sample control.
[0044] Step 3, the determination of iron ions in the sample to be tested:
[0045] According to the iron ion detection method in GB320-2006, the diluted sample to be tested prepared in step 2 was measured at a wavelength of 510nm by an ultraviolet spectrophotometer for the absorbance of the solution, and the iron content was calculated to be 147.4ppm according to the standard curve.
[0046] In the present invention, an appropriate amo...
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Abstract
The invention provides a method for detecting iron ions in chlorohydrocarbon. The method specifically comprises the following steps: drawing a standard curve; putting a proper amount of chlorohydrocarbon sample to be detected into a volumetric flask, adding a proper amount of organic solvent, and fully shaking up for later use, wherein the organic solvent can be dissolved in water and also can bedissolved in chlorohydrocarbon; and determining the absorbance of the diluted sample to be detected by using an ultraviolet spectrophotometer, and calculating the content of iron ions in the sample tobe detected according to the standard curve. According to the method, the solvent is added into the chlorohydrocarbon sample to be detected for dilution, water and oil phases can be fully dissolved with each other in the analysis process, and the phenomenon that the absorbance of the solution is influenced by an emulsification phenomenon is avoided; the iron ion detection result is high in accuracy, the problem that a traditional phenanthroline spectrophotometric method for determining iron ions is only suitable for an aqueous solution system is solved, a sample to be detected does not need to be pretreated, and the operation process does not influence a human body or the environment; the method is reasonable in design and easy to operate, the determination accuracy of the iron ions is 97% or above through verification, and the method is suitable for popularization.
Description
Technical field: [0001] The invention belongs to the technical field of chemical analysis and detection, in particular to a method for detecting iron ions in chlorinated hydrocarbons. Background technique: [0002] Chlorinated hydrocarbons include chlorinated alkanes, chlorinated alkenes, etc. Among them, 1,1,3-trichloropropene and 1,1,2,3-tetrachloropropene in chlorinated propenes are synthetic new environmentally friendly refrigerants2,3, An important intermediate of 3,3-tetrafluoropropene (HFO-1234yf). With the emergence of ozone depletion and global warming, HFO-1234yf, a new environmentally friendly refrigerant, will gradually replace CFCs and HCFCs. [0003] Iron ion content is an important central control index in the synthesis process of chloropropene. Usually, the traditional iron ion detection methods mainly include o-phenanthroline spectrophotometry, ICP-OES elemental analysis, atomic absorption spectrometry, etc. However, these iron ion The detection method is ...
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