Fast Determination of the Sulfur Species in Solid Phase Systems by a Tpo-Ir Method

Abstract

Qualitative and quantitative assessment of total sulfur and sulfur species in solid phase is necessarily important for development of effective desulfurization methods, reduction of environmental pollution, and prevention of catalyst poisoned. In this work, TPO-IR (Temperature Programmed Oxidation- Infrared) method was used for rapid determination of sulfur species in solid minerals. The high purity of Ag2S was used as the calibration materials at the fixed temperature of 1100 °C, and the TPO experimental runs were performed on the solid minerals of phosphorite and coal. The results show that pyrite sulfur with Tmax of 426 °C, and two thiophene sulfurs with Tmax of 450 °C and 481 °C were found in Kaiyang phosphorite by fitting the TPO-IR curves; while pyrite sulfur with Tmax of 432 °C, complex sulfide with Tmax of 679 °C and sulfate sulfur with Tmax of 939 °C were found in Weng’an phosphorite. For Gas coal, the TPO-IR curves of sulfur release can be deconvoluted into seven individual curves, while that of Anthracite deconvoluted into four individual curves. In conclusion, the TPO-IR method has many advantages for determination of sulfur species in solid phase systems, such as less sample consumption, simple pretreatment, convenient operation and low cost, etc.

Application of Temperature Programmed Oxidation-Infrared Technique in the Analysis of Sulfur Occurrence and Genesis in Phosphate Rock

“…First, the infrared detector is calibrated, and the standard material used is Ag 2 S with a purity of 99.995%, which is detected at a fixed high temperature of 950 °C (as the red path). e corresponding calibration curve is shown in previous works [27], and the standard deviation is about 1.94%. en, the characteristic temperature was collected in the temperature-programmed detection mode, and the TPO-IR database of sulfur species with known structures was established (as the green path).…”

“…In the TPO-IR process, 99.5% pure O 2 with a flow rate of 1.80 L/ min was used as the carrier gas and oxidizing agent. e TPO device was designed by our group, and the IR detector was the GCS-80 SO 2 tubular infrared carbon and sulfur analyzer developed by Sichuan Science Instruments Co., Ltd. A detailed description of the device is given in reference [27].…”

“…By comparison, the TPO-IR technique has more advantages in the detection of sulfur species in solid minerals, such as fast analysis speed, low sample consumption, high accuracy, low interference, and high detection limit. In previous works, the TPO-IR technique has been used to analyze sulfur in coal and phosphate rock at low-temperature areas (<1000 °C) [27]. In this work, we improved the upper limit of the detection temperature range and increased the exploration of sulfur species in the high-temperature areas (>1000 °C) of phosphate rock.…”