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Method for measuring bromine content in organic photoelectric material based on oxygen bomb combustion method

An organic photoelectric material and oxygen bomb combustion technology, applied in the field of detection, can solve the problems of affecting the detection limit of bromide ions, interfering with the detection of bromide ions, and difficult to meet the needs of bromide ion determination, etc.

Inactive Publication Date: 2020-07-07
GUANGDONG AGLAIA OPTOELECTRONICS MATERIALS
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Problems solved by technology

Ion chromatography at the test end is the preferred method for anion analysis, which has the advantages of rapidity and good selectivity. However, most organic optoelectronic materials contain nitrogen elements, which will produce nitrite ions after oxygen bomb combustion, and nitrite ions interfere with bromide ions. The detection limit of bromide ions is affected, and it is difficult to meet the needs of the determination of trace bromide ions in organic photoelectric materials.

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  • Method for measuring bromine content in organic photoelectric material based on oxygen bomb combustion method
  • Method for measuring bromine content in organic photoelectric material based on oxygen bomb combustion method
  • Method for measuring bromine content in organic photoelectric material based on oxygen bomb combustion method

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Embodiment 1

[0046] The first step: sample pretreatment:

[0047] 1. Use 4.5mM Na in the oxygen bomb when the oxygen bomb is out of service 2 CO 3 and 0.8mM NaHCO 3 Soaking, after pouring the soaking solution before use, use 10 times the volume of ultra-pure water to rinse the inner wall of the bomb to avoid environmental pollution of the oxygen bomb.

[0048] 2. Sample weighing: Weigh 0.5g of the sample (accurate to 0.0001g) into the sample cup of the oxygen bomb to promote the complete combustion of the sample, and wrap the sample with filter paper. The characteristics of the filter paper: bromide ion content ≤ 0.002mg / L.

[0049] 3. Install the ignition wire and sample: open the cover of the oxygen bomb, fix the sample cup containing the sample, fix the two ends of an ignition wire with a suitable length on the electrode column, and make it contact with the sample without touching the sample cup;

[0050] 4. Add absorption liquid:

[0051] 4.1 Preparation of absorption liquid: Na in...

Embodiment 2

[0073] Embodiment 2 method detection limit

[0074] Continuously use the same pretreatment method to conduct 7 blank tests, and the detection limit of the method is 0.25 mg / kg obtained by superimposing the blank level with 3 times the standard deviation, as shown in Table 2 below.

[0075] Table 2 7 test results of bromide ion blank content

[0076]

Embodiment 3

[0077] Embodiment 3 background blank stability verification

[0078] Monitor No. 1, No. 2, No. 3, and No. 4 oxygen bombs for three consecutive days and use the same sample pretreatment to conduct a blank test. The bromide ion blank value in Table 3 was obtained through the ICP-MS test, and the extremely poor result was 0.2-0.4ppb. It shows that the relative deviation of bromide ion content in different oxygen bombs is small, and it can be considered that there is no significant difference between different oxygen bombs, indicating that the background blank is stable. If the deviation of the blank test is greater than the detection limit (0.25mg / kg), that is, the absolute deviation of the blank is greater than 2.5ppb, it is necessary to re-use 4.5mM Na in the oxygen bomb 2 CO 3 and 0.8mM NaHCO 3 Soaking, after pouring the soaking solution before use, use 10 times the volume of ultra-pure water to rinse the inner wall of the bomb until the deviation of the blank test is less t...

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Abstract

The invention discloses a method for determining the bromine content in an organic photoelectric material based on an oxygen bomb combustion method, which uses a pretreatment mode of oxygen bomb combustion and combines a single quadrupole inductively coupled plasma mass spectrometer for detection, and comprises the following steps: 1, sample pretreatment: absorbing and fixing the volume after oxygen bomb combustion; 2, making a standard curve; 3, measuring the content of bromide ions in the sample; 4, calculating. The method is simple to operate, good in precision, high in sensitivity and capable of effectively detecting the content of trace bromine ions in the material.

Description

technical field [0001] The invention belongs to the technical field of detection, and in particular relates to a method for measuring bromide ion content in organic photoelectric materials based on an oxygen bomb combustion method. Background technique [0002] Organic electroluminescent materials have been one of the research hotspots in the field of optoelectronic information functional materials. After decades of development, breakthroughs have been made in organic electroluminescent materials, and the efficiency and lifespan of devices have been greatly improved. The improvement of the efficiency and life of the device is largely limited by the purity of the material. The improvement of the purity depends on multiple meticulous purification processes to reduce or even eliminate the impurities in the material, thereby improving the purity of the material. Multiple purifications mean increased material production costs, so it is particularly important to study the relatio...

Claims

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Application Information

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IPC IPC(8): G01N27/62G01N1/28G01N1/38G01N27/626
CPCG01N27/62G01N1/28G01N1/38
Inventor 潘统很陈景生徐炫宗戴雷蔡丽菲
Owner GUANGDONG AGLAIA OPTOELECTRONICS MATERIALS
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