Abstract：In order to realize the accurate determination of fluorine content in solid waste, an analysis method of fluorine content in solid waste by ion selective electrode was established after melting the sample with sodium hydroxide. L9(34) orthogonal tests were performed on four factors, including the temperature of alkali fusion, the time of alkali fusion, the composition of alkali fusing agent, and the dosage of alkali fusing agent. The results showed that the influence degree of 4 factors on the alkali fusion process was presented as below: the temperature of alkali fusion > the time of alkali fusion > the dosage of alkali fusing agent > the composition of alkali fusing agent. Through the intuitive analysis and computational analysis of orthogonal test results, two kinds of optimized alkali fusion were obtained. The electroplating waste slags except for waste flux with high fluorine content and hard texture were selected as the test objects to further compare two optimized conditions. It was found that the following conditions were applicable for the solid waste samples: 3.0 g of NaOH was covered on sample surface followed by constant temperature fusion in a muffle at 600 ℃ for 30 min. Then, a screen test was performed on total ionic strength adjustment buffer (TISAB) solution using Al3+ which had the strongest interference. The results revealed that sodium citrate had a stronger masking capacity than 1,2-cyclohexanediamine tetraacetic acid (CDTA) or Tiron. Furthermore, the combination use of sodium citrate and citric acid was superior to the use of single sodium citrate. Therefore, the combination of sodium citrate and citric acid was used as TISAB in experiments. The linear range of method was 0.10-10.0 mg/L with correlation coefficient of 0.999 9. The limit of detection was 0.02 g/kg, and the limit of quantification was 0.08 g/kg. The contents of fluoride in household waste, sewage sludge, electroplating sludge, solid waste fly ash, and waste flux were determined according to the experimental method. The relative standard deviations (RSD, n=7) of determination results were between 2.3% and 8.3%. The spiked recoveries were between 85% and 105%. The electroplating sludge, solid waste fly ash and waste flux with relatively high content of fluoride were determined by online combustion-ion chromatography. It was found that the measurement results of two methods were consistent.
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