Method for rapidly determining sulfur species in solid-phase mineral by using infrared-programmed heating oxidation combination method

A temperature-programmed, rapid measurement technology, applied in the field of analysis and detection, can solve the problems of complex processing, high equipment cost, expensive cost, etc., and achieve the effects of high test accuracy, simple operation and cost reduction.

Active Publication Date: 2020-10-27
GUIZHOU INST OF TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, these methods have their own limitations. For example, the traditional chemical method is cumbersome and time-consuming, and the XPS and XANES methods require expensive instruments and high costs.
In recent years, temperature-programmed reduction (TPR) or temperature-programmed oxidation (TPO) combined with mass spectrometry (MS) and electrochemical techniques have also emerged to measure sulfur-containing gases (mainly H2) released from coal during pyrolysis. 2 S or SO 2 ) escape curve to deduce the content of different sulfur species in coal, but due to the complex sample pretreatment and high equipment cost of this method, it is difficult to achieve rapid determination of sulfur species in solid-phase minerals

Method used

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  • Method for rapidly determining sulfur species in solid-phase mineral by using infrared-programmed heating oxidation combination method
  • Method for rapidly determining sulfur species in solid-phase mineral by using infrared-programmed heating oxidation combination method
  • Method for rapidly determining sulfur species in solid-phase mineral by using infrared-programmed heating oxidation combination method

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Experimental program
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Effect test

Embodiment 1

[0058] Such as figure 1 As shown, the method for rapidly determining sulfur species in solid-phase minerals by infrared-programmed temperature oxidation combined method comprises the following steps:

[0059] (1) Crush phosphate rock (produced in Kaiyang, Guizhou), grind, sieve, and dry in an oven at 80°C to obtain 200-mesh phosphate rock powder. Weigh 1573.8 mg of 200-mesh phosphate rock with a precision balance (accuracy greater than 1 / 10,000). Put the phosphate rock powder into the ceramic boat after roasting at 1200°C for 8 hours;

[0060] (2) Put the ceramic boat containing phosphate rock powder into the constant temperature zone of the tube furnace, and set the temperature rise program from 20°C to 1050°C at a rate of 10°C / min, turn on the infrared carbon and sulfur analyzer, and turn on the computer control software, input the weighed sample mass (1573.8mg), sampling time (6180s) and other parameters, open the carrier gas O 2 (purity>99.5%), set the flow rate to 1.8L / ...

Embodiment 2

[0062] The method for quickly determining sulfur species in solid-phase minerals by infrared-programmed temperature oxidation combined method comprises the following steps:

[0063] (1) Crush phosphate rock (produced in Weng'an, Guizhou), grind, sieve, and dry in an oven at 80°C to obtain 200-mesh phosphate rock powder, and weigh 1165.5 mg of 200-mesh phosphate rock with a precision balance (accuracy greater than 1 / 10,000). Put the phosphate rock powder into the ceramic boat after roasting at 1200°C for 8 hours;

[0064] (2) Put the sample into the constant temperature zone of the tube furnace, and set the temperature rise program from 20°C to 1050°C at a rate of 10°C / min, turn on the infrared carbon and sulfur analyzer, turn on the computer control software, and input the weighing The sample quality (1165.5mg), sampling time (6180s) and other parameters, open the carrier gas O 2 (purity>99.5%), set the flow rate to 1.8L / min; start sampling after the baseline of the infrared ...

Embodiment 3

[0066] The method for quickly determining sulfur species in solid-phase minerals by infrared-programmed temperature oxidation combined method comprises the following steps:

[0067] (1) Pulverize gas coal (Chongqing Yongchuan Coal Mine), grind, sieve, and dry in an oven at 80°C to obtain 80-mesh phosphate rock powder, and weigh 62.34 mg of 80-mesh phosphate rock powder with a precision balance (accuracy greater than 1 / 10,000). Put the phosphate rock powder into the ceramic boat after roasting at 1200°C for 8 hours,

[0068] (2) Put the sample into the constant temperature zone of the tube furnace, and set the temperature rise program from 20°C to 1050°C at a rate of 10°C / min, turn on the infrared carbon and sulfur analyzer, turn on the computer control software, and input the weighing The sample quality (62.34mg), sampling time (6180s) and other parameters, open the carrier gas O 2 (purity>99.5%), the flow rate is set to 1.8L / min; after the infrared carbon and sulfur analyzer...

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Abstract

The invention discloses a method for rapidly determining sulfur species in a solid-phase mineral by utilizing an infrared-programmed heating oxidation combination method. The method comprises the following steps of: (1) calibrating an infrared detector and establishing a standard curve by taking silver sulfide as a calibration standard sample; (2) establishing a sulfur species qualitative database; (3) detecting sulfur species in a to-be-detected solid-phase mineral sample. The step (3) specifically comprises the following steps that: (a) solid-phase mineral powder is put into a roasted container, the container filled with the solid-phase mineral powder is put into a constant-temperature area of a tubular furnace, and the final temperature and heating rate of the constant-temperature areaof the tubular furnace are set; (b) an infrared carbon and sulfur analyzer is turned on, computer control software is started, technical parameters are input, carrier gas oxygen is opened, sampling isstarted after the baseline of the infrared carbon and sulfur analyzer is stable, meanwhile, the constant-temperature area of the tube furnace starts to be heated, after the software of the infrared carbon and sulfur analyzer automatically records a sulfur dioxide escape curve, a sulfur quality curve is derived, and sulfur species in the solid-phase mineral are analyzed. According to the method, O2 is adopted to oxidize or pyrolyze the sulfur species in the solid-phase mineral, and SO2 formed by oxidation or pyrolysis is monitored on line through the infrared carbon and sulfur analyzer.

Description

technical field [0001] The invention relates to the technical field of analysis and detection, in particular to a method for rapidly determining sulfur species in solid-phase minerals by using an infrared-programmed temperature-rising oxidation method. Background technique [0002] As we all know, sulfur is a harmful element in many fields, such as the field of environmental protection. At high temperatures, sulfur is easily oxidized to form SO 2 , SO 2 Further react with water vapor in the atmosphere to form acid rain; in the field of catalysis, sulfur and SO 2 Sulfur species such as sulfur can easily cause catalyst poisoning; in the field of coal chemical industry, when coal is gasified, the sulfur in the gas not only easily poisons the catalyst, but also corrodes equipment. In the process industry, the processing of solid-phase minerals often needs to consider the sulfur species contained in it and their content. However, until now it is still necessary to fully underst...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N1/44G01N21/3504
CPCG01N1/44G01N21/3504
Inventor 唐石云唐安江郭俊江刘浪
Owner GUIZHOU INST OF TECH
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