Microcoulomb analysis method for chlorinity high-temperature burning of organic phosphate fire-resistant oil and device thereof

Abstract

The invention belongs to a microcoulomb analysis method for the chlorinity high-temperature burning of organic phosphate fire-resistant oil and a device thereof, belonging to the field of power analysis chemistry and solving the defects of complicated operation steps, long time consumption, unobvious titration end point, poor accuracy and repetitiveness and high cost existing in the prior art. The device comprises a high-temperature furnace and a burning tube inserted in the high-temperature furnace; the burning tube is provided with an oxygen interface, a nitrogen interface and a sample inlet and comprises a gasifying section and a burning section, one end of the burning tube is connected with a sample inlet device, and the other end is connected with an electrolytic bath. The device adopts heating, gasifying and electrolytic analysis methods to obtain the chlorinity of a sample. The invention has simple and convenient operation and rapid analysis speed and adopts a microcoulomb method to analyze titration and judge the end point so as to be more accurate than the prior oxygen bomb method by visual inspection and manual measurement, have good test repetitiveness, avoid using toxic chemical reagents and improve the safety.

Description

【Technical field】 [0001] The invention belongs to the field of power analysis chemistry, in particular to a high-temperature combustion microcoulomb analysis method and a device thereof for phosphate ester anti-fuel oil chlorine content. 【Background technique】 [0002] Due to its excellent flame retardant performance (generally, the self-ignition point is higher than 535°C), the phosphate ester anti-fuel is widely used in the electro-hydraulic speed control system of the thermal power generation unit. Chlorine content in phosphate ester anti-fuel is an important chemical indicator. Excessive chlorine content will cause corrosion and jamming of the servo valve of the speed control system, resulting in serious accidents. The chlorine content of new oil should not exceed 50mg / kg , The chlorine content of operating oil is required to be no more than 100mg / kg, so it is necessary to analyze the chlorine content of phosphate ester fuel oil. [0003] There are generally two methods...

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Problems solved by technology

The operation steps of the oxygen bomb method are complicated and time-consuming, the titration end point is not obvious, the accuracy and repeatability are poor, and the titrant mercury nitrate is a toxic reagent, which has adverse effects on testers and the environment

[0005] X-ray spectroscopy is a quantitative analysis using the characteristic x-ray intensity of chlorine atoms. It is divided into two types: x-ray energy dispersive spectroscopy and x-ray wavelength dispersive spectroscopy. The detection limit of the former is generally higher, generally tens of mg / kg, not suitable for analyzing the chlorine content of phosphate ester fuel oil; the latter can reach a lower detection limit, generally several mg / kg, but the instruments used are very expensive and the test cost is high, which is difficult for general laboratories to meet Test Conditions

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