CN101750465B - Method for determining calcium sulfite hemihydrate in desulfurized gypsum - Google Patents
Method for determining calcium sulfite hemihydrate in desulfurized gypsum Download PDFInfo
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- CN101750465B CN101750465B CN2008102402653A CN200810240265A CN101750465B CN 101750465 B CN101750465 B CN 101750465B CN 2008102402653 A CN2008102402653 A CN 2008102402653A CN 200810240265 A CN200810240265 A CN 200810240265A CN 101750465 B CN101750465 B CN 101750465B
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- calcium sulfite
- sulfite hemihydrate
- desulfurized gypsum
- reactor
- desulfurated plaster
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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: the dilute 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 the desulfurized gypsum can accurately determine the low content of calcium sulfite hemihydrate in the desulfurized gypsum.
Description
Technical field
The present invention relates to the mensuration of the calcium sulfite hemihydrate of the analytical approach of calcium sulfite hemihydrate in a kind of desulfurated plaster, particularly low content.
Background technology
The acceleration of in building material industry, using along with domestic desulfurated plaster; People begin to pay attention to the mensuration of impurity content in the desulfurated plaster, at present domestic more common be to adopt the instructions of technological associations " German large power plant operator " analytical approach in (being called for short VGB).Mainly there are following two shortcomings in the analytical approach of VGB calcium sulfite hemihydrate: a) when calcium sulfite hemihydrate content is very low in the desulfurated plaster, for example be lower than at 5% o'clock, the VGB analytical approach can't accurately be measured its content; B) used the concentrated sulphuric acid in the VGB analytic process, be unfavorable for that general lab technician carries out safe operation and factory safety management with strong oxidizing property and severe corrosive.
Summary of the invention
The technical matters that the present invention will solve provides determining calcium sulfite hemihydrate in a kind of desulfurated plaster, detects the content of calcium sulfite hemihydrate under can the situation that calcium sulfite hemihydrate content is very low in desulfurated plaster exactly.
In order to address the above problem, the invention provides that determining calcium sulfite hemihydrate comprises the steps: in a kind of desulfurated plaster
Step 1: an amount of desulfurated plaster to be measured is packed in the quartzy distillation cascade, and splash into an amount of phosphoric acid, then quartz ampoule is packed in the reactor;
Step 2: setting the reactor heating-up temperature is 100～200 ℃, and the reaction time is 6～20min;
Step 3: the startup reactor, feed purifying air of removal sour gas simultaneously the sulphuric dioxide that produces is discharged, controlling the flow that purifies air is 50～300ml/min.The sulphuric dioxide of discharging is used hydrogen peroxide oxidation, generates dilute sulfuric acid;
Step 4: through alkaline solution titration dilute sulfuric acid, thus the content of calcium sulfite hemihydrate in definite desulfurated plaster.
Preferably, said alkaline solution is a NaOH.
Preferably, said reactor can adopt distillation apparatus.
The present invention is through the stable control of reactor; Utilize boiling point than the calcium sulfite hemihydrate in the higher acid decomposed by phosphoric acid desulfurated plaster and generate sulphuric dioxide simultaneously; And purifying air the sulphuric dioxide discharge that produces of sour gas removed in feeding; Utilize oxydol that the oxidizing sulfur dioxide that generates is generated dilute sulfuric acid again; Carry out acid base titration through alkaline solution (for example NaOH) more at last, and count through PH and to control titration end-point, calcium sulfite hemihydrate is lower than 5% o'clock content in the desulfurated plaster thereby can measure exactly.In addition, the present invention has avoided using the concentrated sulphuric acid with strong oxidizing property and severe corrosive, greatly facilitates general lab technician and carries out safe operation and factory safety management.
Specific embodiment
Embodiment 1
Concrete operations step of the present invention is exemplified below:
(theoretical content of calcium sulfite hemihydrate is: 0.06564%) place in the quartzy distillation cascade to take by weighing desulfurated plaster sample about 0.1～1g; Toward the interior above phosphoric acid of the pure level of analysis that drips 3～10ml of quartz ampoule; (for example quartzy distillation cascade pack into TR Thermal Reactor then; Can be distillation apparatus); And with cleaner air package (fundamental purpose is to remove airborne sour gas, avoids producing deviation) the quartzy distillation cascade import of connection, the reactor outlet pipe inserts the absorber of the oxydol of 1: 1 ratio that fills 20～50ml.The impermeability of inspection pipeline starts reactor, and temperature is 100～200 ℃ on the controlling reactor table, and the reaction time is 6～20min, and the flow that purifies air is 50～300ml/min.Question response fully after, with the sodium hydroxide solution drop reaction product of demarcating 0.01 good～0.1N, through PH meter control pH value be 7.0 o'clock be titration end-point.Confirm the content of calcium sulfite hemihydrate in the desulfurated plaster at last with the sodium hydroxide solution volume number that consumes.
The content of the calcium sulfite hemihydrate of the desulfurated plaster sample that detects through above-mentioned steps is: 0.06694, with the absolute deviation of theoretical value be+0.0013, relative deviation is+1.97%, so testing result is very accurate.
Embodiment 2
Concrete operations step of the present invention is exemplified below:
(theoretical content of calcium sulfite hemihydrate is: 0.10860%) place in the quartzy distillation cascade to take by weighing desulfurated plaster sample about 0.1～1g; Toward the interior above phosphoric acid of the pure level of analysis that drips 3～10ml of quartz ampoule; Then with the quartzy distillation cascade TR Thermal Reactor of packing into; And with cleaner air package (fundamental purpose is to remove airborne sour gas, avoids producing deviation) the quartzy distillation cascade import of connection, the reactor outlet pipe inserts the absorber of the oxydol of 1: 1 ratio that fills 20～50ml.The impermeability of inspection pipeline starts reactor, and temperature is 100～200 ℃ on the controlling reactor table, and the reaction time is 6～20min, and the flow that purifies air is 50～300ml/min.Question response fully after, with the sodium hydroxide solution drop reaction product of demarcating 0.01 good～0.1N, through PH meter control pH value be 7.0 o'clock be titration end-point.Confirm the content of calcium sulfite hemihydrate in the desulfurated plaster at last with the sodium hydroxide solution volume number that consumes.
The content of the calcium sulfite hemihydrate of the desulfurated plaster sample that detects through above-mentioned steps is: 0.10949, with the absolute deviation of theoretical value be+0.00088, relative deviation is+0.81%, so testing result is very accurate.
Embodiment 3
Concrete operations step of the present invention is exemplified below:
(theoretical content of calcium sulfite hemihydrate is: 0.23990%) place in the quartzy distillation cascade to take by weighing desulfurated plaster sample about 0.1～1g; Toward the interior above phosphoric acid of the pure level of analysis that drips 3～10ml of quartz ampoule; Then with the quartzy distillation cascade TR Thermal Reactor of packing into; And with cleaner air package (fundamental purpose is to remove airborne sour gas, avoids producing deviation) the quartzy distillation cascade import of connection, the reactor outlet pipe inserts the absorber of the oxydol of 1: 1 ratio that fills 20～50ml.The impermeability of inspection pipeline starts reactor, and temperature is 100～200 ℃ on the controlling reactor table, and the reaction time is 6～20min, and the flow that purifies air is 50～300ml/min.Question response fully after, with the sodium hydroxide solution drop reaction product of demarcating 0.01 good～0.1N, through PH meter control pH value be 7.0 o'clock be titration end-point.Confirm the content of calcium sulfite hemihydrate in the desulfurated plaster at last with the sodium hydroxide solution volume number that consumes.
The content of the calcium sulfite hemihydrate of the desulfurated plaster sample that detects through above-mentioned steps is: 0.24190, with the absolute deviation of theoretical value be+0.00200, relative deviation is+0.83%, so testing result is very accurate.
Embodiment 4
Concrete operations step of the present invention is exemplified below:
(theoretical content of calcium sulfite hemihydrate is: 0.67650%) place in the quartzy distillation cascade to take by weighing desulfurated plaster sample about 0.1～1g; Toward the interior above phosphoric acid of the pure level of analysis that drips 3～10ml of quartz ampoule; Then with the quartzy distillation cascade TR Thermal Reactor of packing into; And with cleaner air package (fundamental purpose is to remove airborne sour gas, avoids producing deviation) the quartzy distillation cascade import of connection, the reactor outlet pipe inserts the absorber of the oxydol of 1: 1 ratio that fills 20～50ml.The impermeability of inspection pipeline starts reactor, and temperature is 100～200 ℃ on the controlling reactor table, and the reaction time is 6～20min, and the flow that purifies air is 50～300ml/min.Question response fully after, with the sodium hydroxide solution drop reaction product of demarcating 0.01 good～0.1N, through PH meter control pH value be 7.0 o'clock be titration end-point.Confirm the content of calcium sulfite hemihydrate in the desulfurated plaster at last with the sodium hydroxide solution volume number that consumes.
The content of the calcium sulfite hemihydrate of the desulfurated plaster sample that detects through above-mentioned steps is: 0.66977, with the absolute deviation of theoretical value be-0.00673, relative deviation is-0.99%, so testing result is very accurate.
The present invention utilizes the stability of reactor control; Under suitable decomposition temperature condition, than the calcium sulfite hemihydrate in the higher acid decomposed by phosphoric acid desulfurated plaster, pass to suitable purifying air again with boiling point; The sulphuric dioxide that produces is discharged; The sulphuric dioxide that ejects is used hydrogen peroxide oxidation, generates dilute sulfuric acid (mensuration of the calcium sulfite hemihydrate of the content, particularly low content through confirming calcium sulfite hemihydrate in the desulfurated plaster with sodium hydroxide solution titration dilute sulfuric acid at last); Therefore avoided using the concentrated sulphuric acid, greatly facilitated general lab technician and carry out safe operation and factory safety management with strong oxidizing property and severe corrosive.In addition; Owing to carry out titration through sodium hydroxide solution at last, so the present invention utilized the characteristics of reactor control stabilization, and integrated use the analysis principle that absorbs of distillation-oxydol; Thereby realized the analytic process control stabilization, analysis result is test target relatively accurately.
Claims (3)
1. determining calcium sulfite hemihydrate in the desulfurated plaster is characterized in that, comprises the steps:
Step 1: desulfurated plaster to be measured is packed in the quartzy distillation cascade, splash into an amount of phosphoric acid, again with the quartz ampoule TR Thermal Reactor of packing into, and be heated to 100～200 ℃, reaction generates sulphuric dioxide, and the reaction time is 6～20min;
Step 2: pass to purifying air of an amount of removal sour gas the sulphuric dioxide that produces is discharged, the sulphuric dioxide of discharge is used hydrogen peroxide oxidation, generates dilute sulfuric acid;
Step 3: through alkaline solution titration dilute sulfuric acid, thus the content of calcium sulfite hemihydrate in definite desulfurated plaster.
2. the method for claim 1 is characterized in that, said alkaline solution is a NaOH.
3. the method for claim 1 is characterized in that, said TR Thermal Reactor is a distillation apparatus.
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| CN2008102402653A CN101750465B (en) | 2008-12-18 | 2008-12-18 | Method for determining calcium sulfite hemihydrate in desulfurized gypsum |
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| CN2008102402653A CN101750465B (en) | 2008-12-18 | 2008-12-18 | Method for determining calcium sulfite hemihydrate in desulfurized gypsum |
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| CN101750465A CN101750465A (en) | 2010-06-23 |
| CN101750465B true CN101750465B (en) | 2012-07-04 |
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Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103134736B (en) * | 2013-02-22 | 2014-12-31 | 江苏省沙钢钢铁研究院有限公司 | Method for accurately determining calcium-based desulfurization agent main component |
| CN107063916B (en) * | 2017-04-27 | 2019-10-25 | 中国大唐集团科学技术研究院有限公司华东分公司 | The detection method of gypsum particle content in a kind of desulfurization exiting flue gas |
| CN112816613A (en) * | 2019-11-15 | 2021-05-18 | 大唐环境产业集团股份有限公司 | Calcium sulfite online monitoring system and method |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6197200B1 (en) * | 1999-05-11 | 2001-03-06 | Eastroc Llc | Method of purifying flue gas waste slurries for use in gypsum production |
| CN2929713Y (en) * | 2006-07-26 | 2007-08-01 | 重庆大学 | Test device for detecting oxidation of sulfite |
| CN101091875A (en) * | 2007-04-24 | 2007-12-26 | 颜松林 | Method for recovering ammonia from by-product of ammonia process of desulfurization for boiler flue gas |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6197200B1 (en) * | 1999-05-11 | 2001-03-06 | Eastroc Llc | Method of purifying flue gas waste slurries for use in gypsum production |
| CN2929713Y (en) * | 2006-07-26 | 2007-08-01 | 重庆大学 | Test device for detecting oxidation of sulfite |
| CN101091875A (en) * | 2007-04-24 | 2007-12-26 | 颜松林 | Method for recovering ammonia from by-product of ammonia process of desulfurization for boiler flue gas |
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| CN101750465A (en) | 2010-06-23 |
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Application publication date: 20100623 Assignee: XINXIANG BEIXIN BUILDING MATERIAL CO.,LTD. Assignor: BEIJING NEW BUILDING MATERIALS PLC Contract record no.: 2017990000001 Denomination of invention: Method for determining calcium sulfite hemihydrate in desulfurized gypsum Granted publication date: 20120704 License type: Common License Record date: 20170106 |
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Effective date of registration: 20230320 Address after: 315600 Tuanjie Tang, Qiangjiao Town, Ninghai County, Ningbo City, Zhejiang Province Patentee after: BNBM NINGBO Co.,Ltd. Address before: 100037, Beijing, Haidian District, Three Mile Road, No. 11, China building materials building, 16 floor Patentee before: BEIJING NEW BUILDING MATERIALS PLC |
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