Method for determining calcium sulfite hemihydrate in desulfurized gypsum

A technology of calcium sulfite hemihydrate and desulfurization gypsum is applied in the direction of chemical analysis by titration method, which can solve the problems of inability to accurately measure the content, unfavorable safety operation of laboratory technicians and safety management of factories, etc., and achieve convenient and safe operation and factory safety management. The effect of safety management

Active Publication Date: 2012-07-04
NINGBO BEIXIN BUILDING MATERIAL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The analysis method of VGB calcium sulfite hemihydrate mainly has the following two shortcomings: a) when the calcium sulfite hemihydrate content is very low in the desulfurized gypsum, for example, when it is lower than 5%, the VGB analysis method cannot accurately measure its content; b ) During the VGB analysis process, concentrated sulfuric acid with strong oxidizing and corrosive properties is used, which is not conducive to the safe operation of general analysts and factory safety management

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0013] Concrete operation steps of the present invention are exemplified as follows:

[0014] Weigh about 0.1-1g of desulfurized gypsum sample (theoretical content of calcium sulfite hemihydrate: 0.06564%) and place it in a quartz distillation tube, add 3-10ml of phosphoric acid above analytical grade into the quartz tube dropwise, and then put the quartz distillation tube Put it into a temperature-controlled reactor (for example, it can be a distillation apparatus), and connect the air purification device (the main purpose is to remove the acid gas in the air to avoid deviation) to the inlet of the quartz distillation tube, and insert the outlet tube of the reactor into a container containing 20~ 50ml absorber of 1:1 hydrogen peroxide. Check the airtightness of the pipeline, start the reactor, control the temperature on the surface of the reactor to 100-200°C, the reaction time to 6-20min, and the flow rate of the purified air to be 50-300ml / min. After the reaction is comple...

Embodiment 2

[0017] Concrete operation steps of the present invention are exemplified as follows:

[0018] Weigh about 0.1-1g of desulfurized gypsum sample (theoretical content of calcium sulfite hemihydrate: 0.10860%) and place it in a quartz distillation tube, add 3-10ml of phosphoric acid above analytical grade into the quartz tube dropwise, and then put the quartz distillation tube Put it into a temperature-controlled reactor, and connect the air purification device (the main purpose is to remove the acid gas in the air to avoid deviation) to the inlet of the quartz distillation tube, and insert the outlet tube of the reactor into 20-50ml of hydrogen peroxide at a ratio of 1:1 the absorber. Check the airtightness of the pipeline, start the reactor, control the temperature on the surface of the reactor to 100-200°C, the reaction time to 6-20min, and the flow rate of the purified air to be 50-300ml / min. After the reaction is complete, titrate the reaction product with a calibrated 0.01-...

Embodiment 3

[0021] Concrete operation steps of the present invention are exemplified as follows:

[0022] Weigh about 0.1-1g of desulfurized gypsum sample (theoretical content of calcium sulfite hemihydrate: 0.23990%) and place it in a quartz distillation tube, add 3-10ml of phosphoric acid above analytical grade into the quartz tube dropwise, and then put the quartz distillation tube Put it into a temperature-controlled reactor, and connect the air purification device (the main purpose is to remove the acid gas in the air to avoid deviation) to the inlet of the quartz distillation tube, and insert the outlet tube of the reactor into 20-50ml of hydrogen peroxide at a ratio of 1:1 the absorber. Check the airtightness of the pipeline, start the reactor, control the temperature on the surface of the reactor to 100-200°C, the reaction time to 6-20min, and the flow rate of the purified air to be 50-300ml / min. After the reaction is complete, titrate the reaction product with a calibrated 0.01-...

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Abstract

The invention provides a method for determining calcium sulfite hemihydrate in desulfurized gypsum, which comprises the following steps: step 1: an appropriate amount of desulfurized gypsum to be determined is put into a quartz distillation tube, an appropriate amount of phosphoric acid is dripped in, and then the quartz tube is put into a temperature control reactor; step 2: the heating temperature of the reactor is set to be 100 to 200 DEG C, and the reaction time is 6 to 20min; step 3: the reactor is started, and simultaneously the purified air with the acid gas removed is fed in to emit the produced sulfur dioxide, and the flow of the purified air is controlled to be 50 to 300ml / min. The emitted sulfur dioxide is oxidized by hydrogen peroxide to generate sulfuric acid; and step 4: thedilute sulphuric acid is titrated by lye so as to determine the content of the calcium sulfite hemihydrat in the desulfurized gypsum. The method for determining the calcium sulfite hemihydrate in thedesulfurized gypsum can accurately determine the low content of calcium sulfite hemihydrate in the desulfurized gypsum.

Description

technical field [0001] The invention relates to an analysis method for calcium sulfite hemihydrate in desulfurized gypsum, in particular to the determination of calcium sulfite hemihydrate with low content. Background technique [0002] With the acceleration of the application of desulfurized gypsum in the building materials industry in China, people began to pay attention to the determination of the impurity content in desulfurized gypsum. At present, the analysis method in the "Manual of the Technical Association of German Large Power Plant Operators" (VGB for short) is commonly used in China. . The analysis method of VGB calcium sulfite hemihydrate mainly has the following two shortcomings: a) when the calcium sulfite hemihydrate content is very low in the desulfurized gypsum, for example, when it is lower than 5%, the VGB analysis method cannot accurately measure its content; b ) During the VGB analysis process, concentrated sulfuric acid with strong oxidizing and corro...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N31/16
Inventor 周梦文冯菊莲杨青陈红霞
Owner NINGBO BEIXIN BUILDING MATERIAL
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