CN103592280A - Rapid measurement method for content of CaCO3 in limestone flour by using fluorescence calcium-iron analyzer - Google Patents

Rapid measurement method for content of CaCO3 in limestone flour by using fluorescence calcium-iron analyzer Download PDF

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CN103592280A
CN103592280A CN201310627675.4A CN201310627675A CN103592280A CN 103592280 A CN103592280 A CN 103592280A CN 201310627675 A CN201310627675 A CN 201310627675A CN 103592280 A CN103592280 A CN 103592280A
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content
caco
agstone
analyser
fluorescence
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张文梅
王真香
刘志勇
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DATANG TAIYUAN CO-GENERATION POWER PLANT
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DATANG TAIYUAN CO-GENERATION POWER PLANT
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Abstract

The invention provides a rapid measurement method for the content of CaCO3 in limestone flour by using a fluorescence calcium-iron analyzer. The method is characterized by comprising the following steps: detection of sample content: a step of detecting the content of CaCO3 in a limestone flour sample by using an EDTA complexometric titration method; counting and measurement with the analyzer: a step of tabletting the limestone flour sample and then subjecting the tabletted limestone flour sample to counting and measurement on the fluorescence calcium-iron analyzer; establishment of a standard curve: a step of drafting the standard curve according to a relationship between the contents of CaCO3 and fluorescence counts detected by the fluorescence calcium-iron analyzer; and measurement of the content of CaCO3: a step of placing limestone flour in a wafer machine to prepare a wafer, putting the wafer in the fluorescence calcium-iron analyzer and allowing the content of CaCO3 to be automatically displayed. The method has the advantages of a fast analysis speed, accurate measurement results, simple operation, a few operation steps, low workload, no discharge of waste gas, waste water and industrial residue, accordance with environmental protection and safety requirements, etc.

Description

A kind of fluorescence calcium iron analyser Fast Measurement agstone CaCO 3the method of content
Technical field
The present invention relates to chemical analysis technology field, refer to especially a kind of fluorescence calcium iron analyser Fast Measurement agstone CaCO that utilizes 3the method of content.
Background technology
In recent years, along with domestic socioeconomic development and progress, living standards of the people are improved day by day, and society has also reached unprecedented degree to the attention of environment; For power plant construction, flue gas desulfur device has become the ingredient that power plant can not vacancy, and the wet sulfur removal technology of limestone-gypsum is most widely used general, the most ripe desulfur technology of current power plant.
Agstone-gypsum wet sulfur removal technology adopts agstone as desulfurization absorbent, because the quality of agstone directly affects desulfuration efficiency, so the per car agstone of the quite strict ，Dui Ru of the check of agstone factory is sampled and analyzes.The standard that requires of agstone quality is: CaCO 3content > 90%; Fineness (325 order) > 90%.
At present, power plant mainly adopts the carry out quality restriction of EDTA compleximetry to agstone.
EDTA complexometry ratio juris is by agstone sample heating for dissolving with hydrochloric acid, when pH value > 12.5, magnesium ion generates after magnesium hydrate precipitate, take calcon-carboxylic acid as indicator, with the titration of EDTA standard solution, terminal colour becomes blueness from claret.Iron, aluminium disturb and can adopt triethanolamine to shelter.
Test apparatus and reagent: analytical balance (0.1mg), 50mL buret, 250mL triangular flask, concentrated hydrochloric acid (analyzing pure), triethanolamine (1+1), potassium hydroxide (200gL -1), calcon-carboxylic acid (1%NaCl), C (EDTA) standard solution (0.1molL -1).
Assay method is to take agstone sample 0.2g(to be accurate to 0.1mg), be placed in 250mL triangular flask, add demineralized water to 100mL, add 3mL concentrated hydrochloric acid, heating boils that to make volume be 50mL, is cooled to room temperature, adds (1+1) triethanolamine 2mL, 200gL -1potassium hydroxide 30mL(pH value is 12.7-13.2), add 0.1g calcon-carboxylic acid, use 0.1molL -1c(EDTA) standard solution titration, color is terminal from the purplish red blueness that becomes.
Computing formula:
Figure BDA0000425764450000021
In formula: m---the quality of agstone sample, g;
C eDTA---the concentration of EDTA standard solution, molL -1;
V eDTA---consume the volume of EDTA standard solution, mL;
100.09---the molal weight of calcium carbonate, gmol -1.
Adopt EDTA compleximetry to carry out CaCO to agstone 3content analysis, has following shortcoming:
(1) check length consuming time, each sample determination approximately needs 30min, inefficiency;
(2), because operating personnel's skill level is different, easily there is larger accidental error in assay;
(3) complicated operation, operation steps are many;
(4) dosing kind is many, and workload is large, often can not complete the examination of agstone on time;
(5) test drug consumption is large, need to often prepare medicines;
(6), easily there is personal injury in test contact strong acid and strong base;
(7) sample duplicate detection had both increased workload, again length consuming time;
(8) use chemical reagent, produce the three wastes, need to process and could discharge etc.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of method of fluorescence calcium iron analyser Fast Measurement agstone CaCO3 content, the problems such as inefficiency, accidental error that existing assay method exists are large to solve, complicated operation.
The embodiment of the present invention provides a kind of fluorescence calcium iron analyser Fast Measurement agstone CaCO 3the method of content, comprises the steps:
Detect sample size, by EDTA compleximetry, detect the CaCO of agstone sample 3content;
Analyser count measurement, carries out after compressing tablet agstone sample, on fluorescence calcium iron analyser, carries out count measurement;
Criterion curve, according to CaCO 3relation between the fluorescence counting that content and fluorescence calcium iron analyser detect, production standard curve;
Measure CaCO 3content, is placed on cooked flake wrapping machine by a certain amount of agstone and makes pie, puts into fluorescence calcium iron analyser, automatically shows CaCO 3content.
Wherein, in described Criterion curve, by CaCO 3the fluorescence counting that content and fluorescence calcium iron analyser detect utilizes one-variable linear regression, obtains standard working curve: y=kx+b.
Wherein, described step detects in sample size, and described agstone sample is selected one group 10, by EDTA compleximetry, does respectively CaCO three times 3analyze, using the average of three data as CaCO 3accurate content value, records the CaCO of one group of 10 sample 3content.
Wherein, the extreme difference of described three data is in 0.25% error range.
Wherein, described each sample CaCO 3content data spacing is 0.2-1.0%.
The beneficial effect of technique scheme of the present invention is as follows:
In such scheme, adopt fluorescence calcium iron analysis-e/or determining power plant desulfurization agstone CaCO 3content, has the analytic sample advantage such as more accurate sooner, specific as follows:
(1) analysis speed is fast, and the time of analyzing a sample is only 3min, can greatly increase work efficiency;
(2) measurement result is accurate, is not easy to produce accidental error, and relative standard deviation is less than 0.25%;
(3) simple to operate, operation steps is few, only has weighing, compressing tablet, mensuration three steps;
(4) do not need to add any medicament, do not use chemical reagent, do not need to prepare medicines;
(5) workload is low, the checking and accepting that 1 testing crew can complete independently agstone;
(6) mensuration process does not contact strong acid and strong base, safe and reliable;
(7) do not destroy sample, sample can duplicate detection;
(8) need not any chemical reagent, three-waste free discharge, meets Environmental Safety requirement.
Accompanying drawing explanation
Fig. 1 is embodiment of the present invention fluorescence calcium iron analyser Fast Measurement agstone CaCO 3the schematic flow sheet of the method for content.
Embodiment
For making the technical problem to be solved in the present invention, technical scheme and advantage clearer, be described in detail below in conjunction with the accompanying drawings and the specific embodiments.
As shown in Figure 1, embodiments of the invention provide a kind of fluorescence calcium iron analyser Fast Measurement agstone CaCO 3the method of content, comprises the steps:
(1) detect sample size;
By EDTA compleximetry, detect the CaCO of agstone sample 3content;
Be specially: select one group of 10 agstone sample, by EDTA compleximetry, do respectively CaCO three times 3analyze, using the average of three data as CaCO 3accurate content value, the extreme difference of described three data is in 0.25% error range; Record the CaCO of one group of 10 sample 3content, described each sample CaCO 3content data spacing is 0.2-1.0%.
(2) analyser count measurement;
Agstone sample is carried out after compressing tablet, on fluorescence calcium iron analyser, carry out count measurement.
(3) Criterion curve;
According to CaCO 3relation between the fluorescence counting that content and fluorescence calcium iron analyser detect, production standard curve;
Be specially: by CaCO 3the fluorescence counting that content and fluorescence calcium iron analyser detect utilizes one-variable linear regression, obtains standard working curve: y=kx+b.
(4) measure CaCO 3content;
A certain amount of agstone is placed on to cooked flake wrapping machine and makes pie, put into fluorescence calcium iron analyser, automatically show CaCO 3content.
In such scheme, adopt fluorescence calcium iron analysis-e/or determining power plant desulfurization agstone CaCO 3content, has the analytic sample advantage such as more accurate sooner; By to EDTA compleximetry and fluorescence calcium iron analysis-e/or determining agstone CaCO 3content data is analyzed, and the relative average debiation of two kinds of methods is all less than 0.20%, and relative standard deviation is all less than 0.25%, and distinct methods result error, between 0.15-0.25%, meets the error range of permission.
Its advantage is specific as follows:
(1) analysis speed is fast, and the time of analyzing a sample is only 3min, can greatly increase work efficiency;
(2) measurement result is accurate, is not easy to produce accidental error, and relative standard deviation is less than 0.25%;
(3) simple to operate, operation steps is few, only has weighing, compressing tablet, mensuration three steps;
(4) do not need to add any medicament, do not use chemical reagent, do not need to prepare medicines;
(5) workload is low, the checking and accepting that 1 testing crew can complete independently agstone;
(6) mensuration process does not contact strong acid and strong base, safe and reliable;
(7) do not destroy sample, sample can duplicate detection;
(8) need not any chemical reagent, three-waste free discharge, meets Environmental Safety requirement.
The above is the preferred embodiment of the present invention; it should be pointed out that for those skilled in the art, do not departing under the prerequisite of principle of the present invention; can also make some improvements and modifications, these improvements and modifications also should be considered as protection scope of the present invention.

Claims (5)

1. a fluorescence calcium iron analyser Fast Measurement agstone CaCO 3the method of content, is characterized in that, comprises the steps:
Detect sample size, by EDTA compleximetry, detect the CaCO of agstone sample 3content;
Analyser count measurement, carries out after compressing tablet agstone sample, on fluorescence calcium iron analyser, carries out count measurement;
Criterion curve, according to CaCO 3relation between the fluorescence counting that content and fluorescence calcium iron analyser detect, production standard curve;
Measure CaCO 3content, is placed on cooked flake wrapping machine by a certain amount of agstone and makes pie, puts into fluorescence calcium iron analyser, automatically shows CaCO 3content.
2. fluorescence calcium iron analyser Fast Measurement agstone CaCO according to claim 1 3the method of content, is characterized in that, in described Criterion curve, by CaCO 3the fluorescence counting that content and fluorescence calcium iron analyser detect utilizes one-variable linear regression, obtains standard working curve: y=kx+b.
3. fluorescence calcium iron analyser Fast Measurement agstone CaCO according to claim 1 3the method of content, is characterized in that, described step detects in sample size, and described agstone sample is selected one group 10, by EDTA compleximetry, does respectively CaCO three times 3analyze, using the average of three data as CaCO 3accurate content value, records the CaCO of one group of 10 sample 3content.
4. fluorescence calcium iron analyser Fast Measurement agstone CaCO according to claim 3 3the method of content, the extreme difference of described three data is in 0.25% error range.
5. fluorescence calcium iron analyser Fast Measurement agstone CaCO according to claim 3 3the method of content, described each sample CaCO 3content data spacing is 0.2-1.0%.
CN201310627675.4A 2013-11-29 2013-11-29 Rapid measurement method for content of CaCO3 in limestone flour by using fluorescence calcium-iron analyzer Pending CN103592280A (en)

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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN2063870U (en) * 1988-01-11 1990-10-17 国家建筑材料工业局建筑材料科学研究院 Raw materials proportion auto-controlling system
CN2781362Y (en) * 2005-04-29 2006-05-17 上海爱斯特电子有限公司 Calcium iron analyser
CN101038259A (en) * 2006-03-14 2007-09-19 中电投远达环保工程有限公司 Method for measuring component of limestone CaCO3 and MgCO3.

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN2063870U (en) * 1988-01-11 1990-10-17 国家建筑材料工业局建筑材料科学研究院 Raw materials proportion auto-controlling system
CN2781362Y (en) * 2005-04-29 2006-05-17 上海爱斯特电子有限公司 Calcium iron analyser
CN101038259A (en) * 2006-03-14 2007-09-19 中电投远达环保工程有限公司 Method for measuring component of limestone CaCO3 and MgCO3.

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
屈国普 等: "一种适合于教学的X射线荧光钙铁分析仪", 《核技术》 *
李海波 刘国红: "X射线荧光光谱仪在水泥检测中的应用", 《山西科技》 *

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Application publication date: 20140219