提出了一种间接测定黄磷尾气中磷单质的方法——磷单质质量浓度等于总磷质量浓度减去磷化氢和五氧化二磷的质量浓度。尾气中总磷的测定采用喹钼柠酮容量法,五氧化二磷的测定采用抗坏血酸还原-钼蓝分光光度法,磷化氢的测定采用火焰光度气相色谱法。结果表明,总磷测定方法的加标回收率为98.33%-101.24%,测定结果的相对标准偏差(RSD)为0.29%;五氧化二磷测定方法的加标回收率为96.81%-101.21%,测定结果的RSD为0.87%。尾气中总磷的质量浓度为1 038.384 4 mg/m3,五氧化二磷和磷化氢的质量浓度分别为0.022 1 mg/m3和686.1 mg/m3,因此,尾气中单质磷的质量浓度为352.262 3 mg/m3。
This paper presents an indirect method to determine the 'yellow phosphorus in the yellow phosphorus tail-gas-- the contents of which were taken as the total phosphorus amount minus that of the phosphorus pentoxide and phosphine. We have adopted the sample connection of the yellow phosphorus exhaust gas installed in the tail vent pipe of the yellow phosphorus electric furnace under the lateral branch. When we were sampling of the yellow phosphorus when sampiing, we have also sampled the exhaust, an impurity, and other sorts of samples of the same category. Then, what we have done is to ensure the stability of the working conditions of the electric furnace, the sufficient airflow and the composition of the exhaust so as to indicate the data on different impurities with the subtraction operations going on as shown above. First of all, it is necessary to determine the contents of the total phosphorus with the method of stationary source emission through the total gaseous phosphorus--quimociac volumetric analysis. Then, it would be possible to assay the phosphorus pentox- ide in the way of ambient air-determination of the phosphorus pentox- ide and the molybdenum blue to the deoxidize spectrophotometric. And, finally, we have managed to use the spectro-photometric method to assay the contents of phosphine. Besides, in order to verify the reliability and accuracy of the assaying methods of the total phos- phorus and phosphorus pentoxide, we have done three groups of stan- dard addition recovery rate experiments, which are characteristic with high precision and accuracy. The results of our experiments demon- strate that the recovery rates of the total phosphorus with the method we have proposed are within the range of 98.33%- 101.24% with their relative standard deviation (RSD)being 0.29%, and that of phosphorus pentoxide is in the range of 96.81%- 101.21%, with the RSD being 0.87 % . The concentrations of the total phosphorus were 1 038. 384 4 mg/m3, and those of phosphorus pentoxide and phosphine account for 0.0