CN112730365A - Metallurgical lime calcium oxide analysis method - Google Patents
Metallurgical lime calcium oxide analysis method Download PDFInfo
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- CN112730365A CN112730365A CN202011589322.6A CN202011589322A CN112730365A CN 112730365 A CN112730365 A CN 112730365A CN 202011589322 A CN202011589322 A CN 202011589322A CN 112730365 A CN112730365 A CN 112730365A
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- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 title claims abstract description 44
- 239000000292 calcium oxide Substances 0.000 title claims abstract description 33
- 235000008733 Citrus aurantifolia Nutrition 0.000 title claims abstract description 29
- 235000011941 Tilia x europaea Nutrition 0.000 title claims abstract description 29
- 239000004571 lime Substances 0.000 title claims abstract description 29
- 238000004458 analytical method Methods 0.000 title claims abstract description 22
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 title claims abstract description 20
- 238000000034 method Methods 0.000 claims abstract description 26
- 238000001304 sample melting Methods 0.000 claims abstract description 16
- 230000000694 effects Effects 0.000 claims abstract description 13
- 238000001514 detection method Methods 0.000 claims abstract description 12
- AMXOYNBUYSYVKV-UHFFFAOYSA-M lithium bromide Chemical compound [Li+].[Br-] AMXOYNBUYSYVKV-UHFFFAOYSA-M 0.000 claims abstract description 11
- 239000000126 substance Substances 0.000 claims abstract description 11
- 230000004907 flux Effects 0.000 claims abstract description 8
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 7
- 238000002474 experimental method Methods 0.000 claims abstract description 5
- AMUJFVCOMQMFIE-UHFFFAOYSA-N dilithium boric acid hydrogen borate Chemical compound [Li+].[Li+].OB(O)O.OB(O)O.OB(O)O.OB([O-])[O-] AMUJFVCOMQMFIE-UHFFFAOYSA-N 0.000 claims abstract description 4
- 230000003203 everyday effect Effects 0.000 claims abstract description 4
- 238000012544 monitoring process Methods 0.000 claims abstract description 3
- 238000007689 inspection Methods 0.000 claims description 5
- 238000005303 weighing Methods 0.000 claims description 4
- 235000012255 calcium oxide Nutrition 0.000 description 26
- 235000012431 wafers Nutrition 0.000 description 4
- 238000005457 optimization Methods 0.000 description 3
- 235000019738 Limestone Nutrition 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- PSHMSSXLYVAENJ-UHFFFAOYSA-N dilithium;[oxido(oxoboranyloxy)boranyl]oxy-oxoboranyloxyborinate Chemical compound [Li+].[Li+].O=BOB([O-])OB([O-])OB=O PSHMSSXLYVAENJ-UHFFFAOYSA-N 0.000 description 2
- 239000010459 dolomite Substances 0.000 description 2
- 229910000514 dolomite Inorganic materials 0.000 description 2
- 238000001506 fluorescence spectroscopy Methods 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 239000006028 limestone Substances 0.000 description 2
- HZRMTWQRDMYLNW-UHFFFAOYSA-N lithium metaborate Chemical compound [Li+].[O-]B=O HZRMTWQRDMYLNW-UHFFFAOYSA-N 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 230000003595 spectral effect Effects 0.000 description 2
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000002354 daily effect Effects 0.000 description 1
- 238000007405 data analysis Methods 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 239000000156 glass melt Substances 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- 235000010755 mineral Nutrition 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 230000008092 positive effect Effects 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 239000013589 supplement Substances 0.000 description 1
- 238000004876 x-ray fluorescence Methods 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
- G01N21/64—Fluorescence; Phosphorescence
- G01N21/6402—Atomic fluorescence; Laser induced fluorescence
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- Health & Medical Sciences (AREA)
- Physics & Mathematics (AREA)
- Analytical Chemistry (AREA)
- Nuclear Medicine, Radiotherapy & Molecular Imaging (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Optics & Photonics (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Analysing Materials By The Use Of Radiation (AREA)
- Investigating, Analyzing Materials By Fluorescence Or Luminescence (AREA)
Abstract
The invention discloses a method for analyzing calcium oxide in metallurgical lime, which belongs to the technical field of metallurgical lime and comprises the following steps: firstly, sample melting conditions are optimized, and the quality of a fuse piece is improved; the following conditions were obtained by several experiments: selecting anhydrous lithium tetraborate-lithium metaborate as a flux, lithium bromide as a release agent, and swinging for 13-14 min; secondly, controlling the temperature of the fluorescence chamber; controlling the temperature of the fluorescence chamber to be 25 +/-1 ℃, monitoring the temperature and the humidity of the fluorescence chamber in real time, continuously measuring the same sample for 10 times, and measuring the same sample by 4 time periods every day; thirdly, making a standard sample by self, and reestablishing a curve; selecting 12 in-plant samples with the CaO content range of 48% -92%, comparing data of each sample by a chemical method for 3 times, and if the data deviation is within an allowable range, establishing a fluorescence curve meeting the requirement of a detection analysis range by using an optimized sample melting condition fuse link by taking an average value as a standard value; and fourthly, effect checking.
Description
Technical Field
The invention belongs to the technical field of metallurgical lime, and particularly relates to a method for analyzing calcium oxide in metallurgical lime.
Background
The metallurgical lime CaO analysis method comprises a chemical method and an instrumental analysis method, the chemical method has complicated analysis steps and low analysis efficiency, at present, an X fluorescence fuse analysis method is mainly adopted, the analysis efficiency of the method is dozens of times or even hundreds of times of that of the chemical method, but the re-inspection rate of the laboratory metallurgical lime analysis is high at present, and because the metallurgical lime is easy to absorb moisture, a commercial metallurgical lime standard sample does not exist at present, an X fluorescence working curve of the metallurgical lime calcium oxide is established by limestone and dolomite standard substances, the calcium oxide content of the limestone and dolomite standard sample is 55.34% at most, the actually purchased metallurgical lime calcium oxide content is 79% -92%, the data difference is large, and the data stability and the accuracy are low when the curve is used for detecting the calcium oxide content of the metallurgical lime. The accuracy of the calcium oxide of the metallurgical lime plays a crucial role in sintering production, the content of the calcium oxide is related to the settlement of samples entering a factory, and the inaccurate data can influence the benefits of companies and clients. Therefore, the problems of the accuracy and the stability of the content of the calcium oxide in the metallurgical lime are urgently needed to be solved.
Disclosure of Invention
The method takes the daily sample as a self-made standard sample, reestablishes the X fluorescence curve suitable for the metallurgical lime, supplements the data blank between 79 and 92 percent of CaO content on the curve, eliminates the unstable factors in the detection process, and improves the stability and the accuracy of the detection data of the calcium oxide in the metallurgical lime.
The invention aims to provide a method for analyzing calcium oxide in metallurgical lime, which comprises the following steps:
step one, optimizing sample melting conditions and improving quality of a fuse piece; the method specifically comprises the following steps:
the following conditions were obtained by several experiments: selecting anhydrous lithium tetraborate-lithium metaborate as a flux, lithium bromide as a release agent, and swinging for 13-14 min;
step two, controlling the temperature of the fluorescence chamber; the method specifically comprises the following steps:
controlling the temperature of the fluorescence chamber to be 25 +/-1 ℃, monitoring the temperature and the humidity of the fluorescence chamber in real time, continuously measuring the same sample for 10 times, and measuring the same sample by 4 time periods every day;
step three, self-making a standard sample and reestablishing a curve; the method specifically comprises the following steps:
selecting 12 in-plant samples with the CaO content range of 48% -92%, comparing data of each sample by a chemical method for 3 times, and if the data deviation is within an allowable range, establishing a fluorescence curve meeting the requirement of a detection analysis range by using an optimized sample melting condition fuse link by taking an average value as a standard value;
step four, effect inspection;
weighing 10 samples of the same sample at the same time, analyzing, measuring a range difference value, and if the range difference value is within an allowable error range, the data fluctuation is small, the data is stable, and the experimental requirements are met;
counting the average value of the rechecking rate of three months, and comparing the average value with the rechecking rate of the previous period;
and 3 samples with different calcium oxide contents are selected to be respectively subjected to fluorescence and chemical analysis and sent to an external inspection, and if the difference values of the three groups of data are within an allowable error, the newly-established fluorescence curve data are accurate.
Preferably, the rocking time is 13 min.
Preferably, the rocking time is 14 min.
The invention has the advantages and positive effects that:
by adopting the technical scheme, the invention has the following technical effects:
by adopting the technical scheme, the stability and the accuracy of the analysis data of the CaO of the metallurgical lime are improved, the reinspection rate is greatly reduced (to be within 1%), the workload of staff is reduced, and the working efficiency is improved. Compared with a tabletting method, the technical scheme can eliminate the influence of the matrix effect, the mineral effect and the granularity effect of the sample on the analysis result, further eliminate unstable factors and ensure the accuracy and stability of data. The system can provide data timely and accurately, provide guidance and service for production, and simultaneously ensure the benefits of companies for the metallurgical lime materials entering the factory through accurate data analysis. In addition, the technical scheme can be well popularized, and similar materials such as quicklime powder and the like can be used for improving the accuracy of detection and analysis results by adopting the same method.
Description of the drawings:
FIG. 1 is a diagram of a glass melt before optimization;
FIG. 2 is a view of the optimized glass fuse;
FIG. 3 is a graph of the effect of different temperatures on the results of the analysis;
FIG. 4 is a diagram showing the results of analysis of 10 samples simultaneously weighed from the same sample;
FIG. 5 is a CaO standard curve;
Detailed Description
In order to further understand the contents, features and effects of the present invention, the following examples are given below for further explanation.
Please refer to fig. 1 to 5;
a method for analyzing calcium oxide in metallurgical lime comprises the following steps:
1. instrument and reagent selection
XF-2400X-ray fluorescence Spectroscopy (Shimadzu); an HNJC-L6D type full-automatic sample melting furnace (Luoyang Haina detection instrument Co., Ltd.); electronic balance model BSA224S (sartorius scientific instruments ltd); anhydrous lithium tetraborate (67%) + lithium metaborate (33%) mixed flux (luoyanghaina instrumentation, ltd); lithium bromide (shinny chemical research institute of Tianjin).
2. Experimental methods
Weighing 0.3000g of a metallurgical lime sample with certain content gradient CaO, 8.0000g of anhydrous lithium tetraborate (67%) + lithium metaborate (33%) mixed flux, uniformly mixing in a platinum crucible, dropwise adding 5-7 drops of 10% lithium bromide solution (release agent), pre-melting for 120 seconds, melting for 780 seconds (13 minutes), standing for 30 seconds in a full-automatic sample melting furnace at 1050 ℃, cooling, demolding to obtain a corresponding glass fuse piece, and establishing a working curve for analyzing the content of the metallurgical lime CaO by using an X-ray fluorescence spectrometer (measuring conditions are spectral line K alpha, spectral crystal J1-LiF, tube voltage 40kV and tube current 70 mA). The accuracy and stability of the analysis of the metallurgical lime CaO are improved by optimizing the conditions of the fuse pieces, the temperature of the fluorescent chamber, self-making a standard sample and establishing a working curve and the like.
(1) Optimize the sample melting condition and improve the quality of the melt sheet
The method comprehensively considers six conditions of sample weighing, flux, dilution ratio, release agent, sample melting temperature and time to find that the flux and swing time are not suitable during sample melting, so that a sample wafer is not well melted, the sample wafer is not uniform, the release agent demoulding effect is not good, the sample wafer is easy to generate cracks, bubbles and crescent sample wafers, the fluorescence data accuracy and stability are poor, the repeated sample melting work efficiency is low, and the detection result is directly influenced by the parameters.
3 sample melting conditions are optimized through multiple experiments, and the obtained optimal conditions are as follows: the anhydrous lithium tetraborate-lithium metaborate is used as a flux, lithium bromide (LiBr) is used as a release agent, the swing time is 13min (the swing 13min and 14min sample melting effect is the best, and the 13min is the best time in consideration of reducing the cost and improving the efficiency).
Table 1 is an effect table for optimizing the condition of molten sample
(2) Controlling the temperature of a phosphor chamber
The temperature rise of the fluorescence chamber can cause the detection result to be higher, the error of the measurement result is larger, and the detection error exceeds the allowable error when the temperature is 33 ℃, so the temperature fluctuation of the fluorescence chamber directly influences the accuracy of the detection result.
The temperature of the fluorescence chamber is controlled to be 25 +/-1 ℃, the temperature and the humidity of the fluorescence chamber are monitored in real time by a hygrothermograph, the same sample is continuously measured for 10 times and is measured in 4 time periods every day, the stability of the obtained two groups of data is good, and the out-of-tolerance phenomenon does not exist.
(3) Making standard sample and re-establishing curve
Selecting 12 incoming samples with CaO content ranging from 48% to 92%, comparing data of each sample by a chemical method for 3 times, and if the data deviation is within an allowable range, taking the average value as a standard value, and establishing a fluorescence curve meeting the requirement of a detection and analysis range by using an optimized sample melting condition fuse piece. The highest point of the curve before optimization only covers about 55.5%, and the highest point of the curve after optimization already covers about 92%.
Table 2 shows the CaO rating results of metallurgical lime
(4) Effect inspection
10 samples are simultaneously weighed for analysis on the same sample, the measurement range difference value is 0.34%, and within the allowable error range, the data fluctuation is small, the data are stable, and the experimental requirements are met.
After the sample melting condition is optimized, the fuse pieces are clean and thorough, cracks and bubbles do not exist, the crescent bending condition does not exist, the average value of the rechecking rate of three months is counted to be 0.87%, and the rechecking rate is far lower than that of the previous one (4.67%).
3 samples with different calcium oxide contents are selected to be respectively subjected to fluorescence and chemical analysis and compared with other laboratory data, and the average difference of the three groups of data is 0.1023% -0.1400%, which is within the allowable error (plus or minus 0.5%), so that the new fluorescence working curve is accurate in determination of the metallurgical lime calcium oxide data.
Table 3 shows the data comparison results
The above description is only for the preferred embodiment of the present invention, and is not intended to limit the present invention in any way, and all simple modifications, equivalent changes and modifications made to the above embodiment according to the technical spirit of the present invention are within the scope of the technical solution of the present invention.
Claims (3)
1. The method for analyzing the calcium oxide in the metallurgical lime is characterized by comprising the following steps of:
step one, optimizing sample melting conditions and improving quality of a fuse piece; the method specifically comprises the following steps:
the following conditions were obtained by several experiments: selecting anhydrous lithium tetraborate-lithium metaborate as a flux, lithium bromide as a release agent, and swinging for 13-14 min;
step two, controlling the temperature of the fluorescence chamber; the method specifically comprises the following steps:
controlling the temperature of the fluorescence chamber to be 25 +/-1 ℃, monitoring the temperature and the humidity of the fluorescence chamber in real time, continuously measuring the same sample for 10 times, and measuring the same sample by 4 time periods every day;
step three, self-making a standard sample and reestablishing a curve; the method specifically comprises the following steps:
selecting 12 in-plant samples with the CaO content range of 48% -92%, comparing data of each sample by a chemical method for 3 times, and if the data deviation is within an allowable range, establishing a fluorescence curve meeting the requirement of a detection analysis range by using an optimized sample melting condition fuse link by taking an average value as a standard value;
step four, effect inspection;
weighing 10 samples of the same sample at the same time, analyzing, measuring a range difference value, and if the range difference value is within an allowable error range, the data fluctuation is small, the data is stable, and the experimental requirements are met;
and (5) counting the average value of the rechecking rate of three months, and comparing the average value with the rechecking rate of the previous period.
2. The method of analyzing metallurgical lime calcium oxide according to claim 1, wherein the rocking time is 13 min.
3. The method of analyzing metallurgical lime calcium oxide according to claim 1, wherein the rocking time is 14 min.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104280368A (en) * | 2013-10-31 | 2015-01-14 | 东旭集团有限公司 | Method for efficiently and accurately detecting main content of industrial magnesium oxide |
| CN104280369A (en) * | 2013-10-31 | 2015-01-14 | 东旭集团有限公司 | Method for efficiently and accurately detecting main content of industrial calcium carbonate |
| CN106290438A (en) * | 2016-09-13 | 2017-01-04 | 中钢集团马鞍山矿山研究院有限公司 | A kind of X-ray fluorescence spectra fusion method measures the method for Calcium Fluoride Content in fluorite |
| CN111982951A (en) * | 2020-08-31 | 2020-11-24 | 广东韶钢松山股份有限公司 | Method for processing sample and determining element content |
-
2020
- 2020-12-29 CN CN202011589322.6A patent/CN112730365A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104280368A (en) * | 2013-10-31 | 2015-01-14 | 东旭集团有限公司 | Method for efficiently and accurately detecting main content of industrial magnesium oxide |
| CN104280369A (en) * | 2013-10-31 | 2015-01-14 | 东旭集团有限公司 | Method for efficiently and accurately detecting main content of industrial calcium carbonate |
| CN106290438A (en) * | 2016-09-13 | 2017-01-04 | 中钢集团马鞍山矿山研究院有限公司 | A kind of X-ray fluorescence spectra fusion method measures the method for Calcium Fluoride Content in fluorite |
| CN111982951A (en) * | 2020-08-31 | 2020-11-24 | 广东韶钢松山股份有限公司 | Method for processing sample and determining element content |
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