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Calcium base desulfurater primary and secondary content and impurity element simultaneous determination method

A technology of impurity elements and desulfurizers, applied in the field of simultaneous determination of primary and secondary quantities of calcium-based desulfurizers and impurity elements, can solve the problems of increased consumption of absorbents and increased transportation costs

Active Publication Date: 2010-10-20
STATE GRID HEBEI ELECTRIC POWER RES INST +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The major elements in the desulfurizer should reach a certain content. If the content is too low, it will cause some problems in operation, resulting in increased consumption of absorbent and increased transportation costs.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Accurately weigh 0.05000 g (accurate to 0.0001 g) of a dry calcium-based desulfurizer analysis sample that has passed through a 200-mesh analytical sieve, and place it in a dry and clean microwave digestion inner tube. Add 2ml of concentrated hydrochloric acid and 4ml of concentrated nitric acid along the tube wall respectively (note: when adding acid to the inner tube, flush the solid sample on the tube wall into the bottom as much as possible to ensure that there is no solid sample on the tube wall, so as not to cause local overheating), Shake well and let sit for 10 minutes.

[0034] The three-step microwave digestion control conditions were set as follows: the microwave power gradient rise time was 10 minutes, the microwave power holding time was 30 minutes, and the cooling time was 30 minutes. Set other microwave digestion conditions as digestion power 800W, maximum control pressure of digestion tank as 60bar, maximum control temperature of digestion tube as 210°C,...

Embodiment 2

[0040] Accurately weigh 0.25000 g (accurate to 0.0001 g) of a dry calcium-based desulfurizer analysis sample that has passed through a 180-mesh analytical sieve, and place it in a dry and clean microwave digestion inner tube. Add 2ml of concentrated hydrochloric acid and 5ml of concentrated nitric acid along the tube wall respectively (note: when adding acid to the inner tube, flush the solid sample on the tube wall into the bottom as much as possible to ensure that there is no solid sample on the tube wall, so as not to cause local overheating), Shake well and let sit for 12 minutes.

[0041] The three-step microwave digestion control conditions were set as follows: the microwave power gradient rise time was 12 minutes, the microwave power holding time was 45 minutes, and the cooling time was 20 minutes. Set other microwave digestion conditions as digestion power 800W, maximum control pressure of digestion tank as 60bar, maximum control temperature of digestion tube as 210°C,...

Embodiment 3

[0047] Accurately weigh 0.20000 g (accurate to 0.0001 g) of a dry calcium-based desulfurizer analysis sample that has passed through a 190-mesh analytical sieve, and place it in a dry and clean microwave digestion inner tube. Add 2ml of concentrated hydrochloric acid and 6ml of concentrated nitric acid along the tube wall respectively (note: when adding acid to the inner tube, flush the solid sample on the tube wall into the bottom as much as possible to ensure that there is no solid sample on the tube wall, so as not to cause local overheating), Shake well and let sit for 15 minutes.

[0048] The control conditions of the three-step microwave digestion were set as follows: the microwave power gradient rising time was 15 minutes, the microwave power holding time was 40 minutes, and the cooling time was 15 minutes. Set other microwave digestion conditions as digestion power 800W, maximum control pressure of digestion tank as 60bar, maximum control temperature of digestion tube ...

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Abstract

The invention relates to a calcium base desulfurater primary and secondary content and impurity elements simultaneous determination method, including the following steps: a calcium base desulfurater analysis sample is quantitatively weighed by a 180-200 mesh analysis sieve, a multi-step microwave digestion method is adopted for carrying out high temperature high pressure mixed acid microwave digestion on the quantitative calcium base desulfurater analysis sample, wherein the mixed acid is 2ml concentrated hydrochloric acid and 4-6ml concentrated nitric acid and the microwave digestion includes three steps, the sample after digestion is transferred for constant volume to prepare analysis solution, namely 2% dilute nitric acid is used for transferring the solution in the digestion inner pipe into a 25-50ml volumetric flask for constant volume to scale; and full spectrum direct-reading plasma emission spectrometer is used for accurately determining contents of multiple elements in the analysis solution. The invention not only can fast and accurately determine primary and secondary content and content of multiple elements in the calcium base desulfurater but also is applicable to determination of multiple elements in grout during desulfuration.

Description

technical field [0001] The invention relates to a method for simultaneously determining the primary and secondary quantities and impurity elements of a calcium-based desulfurizer. technical background [0002] In recent years, with the continuous increase of national environmental protection efforts, the flue gas desulfurization technology of thermal power plants has developed rapidly. At present, more than 90% of my country's flue gas desulfurization technology uses calcium-based desulfurizers. The quality of the calcium-based desulfurizer will not only directly affect the desulfurization effect, but also have various effects on the desulfurization process equipment and processes. Most of the operation failures that often occur in the desulfurization system are related to the quality of the desulfurizer. affect the stability of the system. At present, there is no uniform standard for the element content of calcium-based desulfurizers in China, and the types, qualities and...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N21/73G01N1/44G01N1/28
Inventor 石景燕武玉霞
Owner STATE GRID HEBEI ELECTRIC POWER RES INST
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