CN104280368A - Method for efficiently and accurately detecting main content of industrial magnesium oxide - Google Patents
Method for efficiently and accurately detecting main content of industrial magnesium oxide Download PDFInfo
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- CN104280368A CN104280368A CN201310528430.6A CN201310528430A CN104280368A CN 104280368 A CN104280368 A CN 104280368A CN 201310528430 A CN201310528430 A CN 201310528430A CN 104280368 A CN104280368 A CN 104280368A
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Abstract
The invention provides a method for efficiently and accurately detecting the main content of industrial magnesium oxide. The method comprises the following steps: melting to-be-detected industrial magnesium oxide in a platinum crucible at high temperature by using analytically pure lithium tetraborate as a solvent to prepare sample wafers required by a luminoscope to serve as samples to be detected, melting a series of standard samples by using analytically pure lithium tetraborate as the solvent and adding high-grade pure magnesium oxide before detection, creating a standard work curve and finally detecting the samples to be detected with the work curve to analyze the content of magnesium oxide in the samples to be detected. The method has the beneficial effects that the standard samples and the samples to be detected are molten by utilizing analytically pure lithium tetraborate and are detected by utilizing the characteristics that the luminoscope is stable and fast in detection; the whole detection process of one sample comprises the steps of sample melting (automatic) and detection (with an instrument) and takes time within 25 minutes, so that human errors during chemical titration can be eliminated, the labor force can be also liberated and the technology content can be increased; by using analytically pure lithium tetraborate as the solvent, the molten samples are uniform and stable and the detection results are authentic and reliable; the elements in analytically pure lithium tetraborate are light elements and the method is almost free from matrix interference, so that the reliability of the detection results is higher than that in traditional methods.
Description
Technical field
The present invention relates to a kind of physico-chemical analysis method of industrial oxidation magnesium component, particularly a kind of method that is efficient, quick, the accurately main content of detection industrial magnesium oxide.
Background technology
Now research shows: industrial magnesium oxide is the main raw material(s) of common glass production, and autoxidation magnesium is exactly the principal ingredient of glass, greatly about 0-15%.Therefore the main content of its industrial magnesium oxide is to starting material accurate feed proportioning, seem particularly important, especially in TFT glass substrate is produced, magnesian content directly affects the quality of glass substrate, thus accurately, the main content that detects fast industrial magnesium oxide plays critical effect to control glass substrate steady quality.
Industrial magnesium oxide uses that commonplace method has EDTA compleximetry, ICP subtracts assorted method at present.But these methods have respective drawback.
Shortcoming as EDTA compleximetry: shelter a small amount of ferric iron, trivalent aluminium and divalent manganesetion with triethanolamine, when PH is 10, make indicator with eriochrome black T, with triethanolamine disodium standard titration solution titration content of calcium and magnesium, therefrom deduct calcium content, calculate content of magnesia.Take about 5g sample (being accurate to 0.0002g), be placed in 250mL beaker, use a small amount of water-wet, cover surface plate, add hydrochloric acid solution (about 42mL) and sample is dissolved, boil 3 ~ 5min, filter with middling speed quantitative filter paper while hot, to without after chlorion (checking with liquor argenti nitratis ophthalmicus) cooling, filtrate and washing lotion are moved in 500mL volumetric flask in the lump with hot wash, add water to scale, shake up and obtain testing liquid A.Testing liquid A is used for the mensuration of magnesium oxide, calcium oxide, iron and sulphates content.Retain residue and filter paper, for the mensuration of hydrochloric acid insoluble substance.Pipette more than 25.00ml and dissolve the solution of 5g sample constant volume to 250mL volumetric flask, be placed in 250mL volumetric flask, add water to scale, shake up, pipette 25.00mL, this testing liquid, be placed in 250mL conical flask, add 50mL water, 5mL triethanolamine solution, l0mL buffer solution and 0.lg chromium black T indicator, be titrated to solution with disodium ethylene diamine tetraacetate standard titration solution and become pure blue from aubergine; The mensuration of calcium oxide content: shelter a small amount of ferric iron, trivalent aluminium and bivalent manganese plasma with triethanolamine, when pH is 12.5, take calcium carboxylate as indicator, spent glycol pacifies this sodium acetate standard titration solution titration of calcium ions.Step: pipette more than 50.00mL and dissolve the solution of 5g sample constant volume to 250mL volumetric flask, be placed in 250ml conical flask, add 30mL water, 5mL triethanolamine solution, sodium hydroxide solution is dripped under shake, when solution just becomes muddiness, add people 0.1g calcium carboxylate indicator continuation dropping sodium hydroxide solution and become claret to testing liquid from blueness, excessive 0.5mL.Be titrated to solution with disodium ethylene diamine tetraacetate standard titration solution and become pure blue from claret.Visible process comparatively complexity, complex operation, time longer, a lot of step easily produces error, analyzes comparatively difficulty for fast, accurately detecting a new hand.
As ICP subtracts the shortcoming of assorted method: containing tens kinds of even more impurity in industrial magnesium oxide, and impurity exists in a variety of forms, such as have with sulfate, oxide, chloride etc. form, all can not detect and accurately can not judge that element with which kind of compound form exists, therefore when deducting with Impure forms, can cause certain deviation, result is often higher.
Summary of the invention
The technical problem to be solved in the present invention is to provide efficiently, accurately detect the method for the main content of industrial magnesium oxide, analyzes pure lithium tetraborate and founds standard model and testing sample as solvent, and luminoscope detects to be analyzed, simple to operate, analyzes fast; Overcome the shortcoming that in prior art, detection time is long, deviation is larger.
For solving the problems of the technologies described above, the technical solution used in the present invention is:
Efficient, accurately to detect the main content of an industrial magnesium oxide method, comprises the following steps:
A, top grade pure zirconia magnesium is carried out calcination, then lowers the temperature, cools, be placed on measuring cup middle cover lid, stand-by;
The standard working curve of B, drafting content of magnesia:
The top grade pure zirconia magnesium taking steps A gained using as solute, analyze pure lithium tetraborate and found series standard sample as solvent and utilize the fluorescence intensity level corresponding to this series standard sample of luminoscope record, then be horizontal ordinate with magnesium oxide percentage composition, take fluorescence intensity as ordinate drawing standard working curve;
The determination of C, the main content of industrial magnesium oxide to be measured:
Industrial magnesium oxide to be measured is dried, be solute with industrial magnesium oxide to be measured, analyze pure lithium tetraborate and found testing sample as solvent, utilize luminoscope to detect the fluorescence intensity level of testing sample, and then search magnesian percentage composition corresponding to this fluorescence intensity level from the standard working curve that step B sets up.
In steps A, top grade pure zirconia magnesium is placed in the platinum crucible of lid lid, put into the muffle furnace calcination 0.5-1.5 hour being warming up to 700-800 DEG C, then take out cooling 3-5min, proceed in exsiccator, then be transferred to after cooling 10-20min measuring cup inner cap upper bottle cover wait for found series standard sample.
The scope of design of the magnesium oxide percentage composition of the standard working curve in step B is 98.5-99.99%.
In step B, C before adding the pure lithium tetraborate of solvent analysis, in the solute taken, first add quantitative supplementary lithium tetraborate to make the quality sum of solute and supplementary lithium tetraborate and to analyze pure lithium tetraborate mass ratio for 6:0.2 ~ 6:0.6.
Top grade pure zirconia magnesium, supplementary lithium tetraborate in step B and analyze pure lithium tetraborate and all weigh in platinum crucible, weighing precision is 0.0001g, again above-mentioned three kinds of materials are fully mixed with sticking plaster in platinum crucible, then drip the iodate ammonia solution that 5 ~ 8 concentration are 10 ~ 20%, in 1100-1150 DEG C of sample-melting stove, found standard model.
Industrial magnesium oxide to be measured in step C, supplementary lithium tetraborate, analyze pure lithium tetraborate and all with in platinum crucible weigh, weighing precision is 0.0001g, again above-mentioned three kinds of materials are fully mixed with sticking plaster in platinum crucible, then drip the iodate ammonia solution that 5 ~ 8 concentration are 10 ~ 20%, in 1100-1150 DEG C of sample-melting stove, found testing sample.
The purity of described supplementary lithium tetraborate is that analysis is pure.
In step C, the bake out temperature of industrial magnesium oxide to be measured is 100-110 DEG C, and drying time is 1.5-2.5 hour.
The present invention utilizes the pure lithium tetraborate of analysis to found standard specimen and testing sample, utilizes luminoscope to detect stable feature fast and detects.Such one side improves detection efficiency, and standard model can retain for a long time, when working curve drifts about, can correct.Detection time, comparatively classic method was high for credible result degree simultaneously generally within 2min.
The beneficial effect adopting technique scheme to produce is: (1) the present invention utilizes the pure lithium tetraborate of analysis to found standard specimen and testing sample, utilize luminoscope to detect stable feature fast to detect, a whole process of sample is molten sample (automatically carrying out), detects (instrument detection), time is within 25min, chemistry titration can be got rid of and think the error caused, liberate labour simultaneously, increase technology content.(2) with analyzing pure lithium tetraborate as solvent, found sample stable homogeneous, testing result is true and reliable; (3) analyzing pure lithium tetraborate element is all light element, does not almost have Matrix effects, and testing result confidence level comparatively classic method is high.
Accompanying drawing explanation
Fig. 1 is standard working curve.
Embodiment
Be described in detail with an embodiment below.
Efficient, accurately to detect the main content of an industrial magnesium oxide method, comprises the following steps:
A, top grade pure zirconia magnesium is carried out calcination, then lowers the temperature, cools, be placed on measuring cup middle cover lid, stand-by.
Get the pure calcium carbonate of 5-10g top grade and to be placed in the platinum crucible that cleans up calcination 1h at 700-800 DEG C, take out cooling 3-5min, put into exsiccator cooling 10-20min, proceed to measuring cup inner cap lid stand-by;
The standard working curve of B, drafting content of magnesia:
The top grade pure zirconia magnesium taking steps A gained using as solute, analyze pure lithium tetraborate and found series standard sample as solvent and utilize the fluorescence intensity level corresponding to this series standard sample of luminoscope record, then be horizontal ordinate with magnesium oxide percentage composition, take fluorescence intensity as ordinate drawing standard working curve.
The scope of design of the magnesium oxide percentage composition of standard working curve is 98.5-99.99%, specifically see table 1, can include the percentage composition of the main content of industrial magnesium oxide to be measured.
Table 1 content of magnesia
| Standard specimen | 1# | 2# | 3# | 4# | 5# | 6# |
| Magnesium oxide percentage composition/% | 98.5 | 99.0 | 99.2 | 99.4 | 99.6 | 99.99 |
Calculate the quality of top grade pure zirconia magnesium needed for standard model, if the mass deficiency 0.2g of top grade pure zirconia magnesium, then add supplementary lithium tetraborate and meet 0.2g to make it.Then with (supplementary lithium tetraborate+top grade pure zirconia magnesium): the ratio analyzing pure lithium tetraborate=0.2:6 adds the pure lithium tetraborate of solvent analysis and founds series standard sample.During concrete operations, the purity of the lithium tetraborate supplemented is also pure for analyzing.Specifically can see table 2.
Top grade pure zirconia magnesium needed for table 2 standard specimen and analyze pure lithium tetraborate quality
| Standard specimen | 1# | 2# | 3# | 4# | 5# | 6# |
| Magnesia amount/the g of top grade pure zirconia | 0.1970 | 0.198 | 0.1984 | 0.1988 | 0.1992 | 0.2000 |
| Supplementary lithium tetraborate/g | 0.0030 | 0.002 | 0.0016 | 0.0012 | 0.0008 | 0.0000 |
| Analyze pure lithium tetraborate gross mass/g | 6.0030 | 6.002 | 6.0016 | 6.0012 | 6.0008 | 6.0000 |
| The amount of the ammonium iodide of 20% | 6 | 6 | 6 | 6 | 6 | 6 |
The standard working curve set up, specifically can see Fig. 1.
The determination of C, the main content of industrial magnesium oxide to be measured:
Industrial magnesium oxide to be measured is dried, be solute with industrial magnesium oxide to be measured, analyze pure lithium tetraborate and found testing sample as solvent, utilize luminoscope to detect the fluorescence intensity level of testing sample, and then search magnesian percentage composition corresponding to this fluorescence intensity level from the standard working curve that step B sets up.
First industrial magnesium oxide to be measured dries 2h at 100-110 DEG C in measuring cup, and founds consistent the carrying out of standard specimen and found testing sample, and detect sample, quantitative testing result can see table 3.
Table 3 is testing result quantitatively
Sample recovery rate.Adopt sample using standard samples recovery to carry out the accuracy of evaluation method, the results are shown in Table 4.As can be seen from Table 4, recovery of standard addition, between 99.96% ~ 100.05%, illustrates that the accuracy of the method is very high.
The magnesian recovery of standard addition of table 4
| Sample | Magnesium oxide background values/% | Magnesium oxide addition/% | Magnesium oxide measured value/% | The recovery/% |
| 1# | 99 | 0.2 | 99.21 | 100.01 |
| 2# | 99.2 | 0.2 | 99.45 | 100.05 |
| 3# | 99.4 | 0.2 | 99.56 | 99.96 |
| 4# | 99.6 | 0.2 | 99.76 | 99.96 |
About the precision of method.Carry out 11 parallel analysiss to same sample, the relative deviation of magnesium oxide composition is 1.42%.
In sum, the method for testing time of the present invention short (within 20min), precision is high, the recovery is higher, comparatively classic method efficiency is higher, credible result degree is high, has great importance to the quality control of the research of frit side and glass substrate.
Claims (8)
1. a method that is efficient, the accurately main content of detection industrial magnesium oxide, is characterized in that comprising the following steps:
A, top grade pure zirconia magnesium is carried out calcination, then lowers the temperature, cools, be placed on measuring cup middle cover lid, stand-by;
The standard working curve of B, drafting content of magnesia:
The top grade pure zirconia magnesium taking steps A gained using as solute, analyze pure lithium tetraborate and found series standard sample as solvent and utilize the fluorescence intensity level corresponding to this series standard sample of luminoscope record, then be horizontal ordinate with magnesium oxide percentage composition, take fluorescence intensity as ordinate drawing standard working curve;
The determination of C, the main content of industrial magnesium oxide to be measured:
Industrial magnesium oxide to be measured is dried, be solute with industrial magnesium oxide to be measured, analyze pure lithium tetraborate and found testing sample as solvent, utilize luminoscope to detect the fluorescence intensity level of testing sample, and then search magnesian percentage composition corresponding to this fluorescence intensity level from the standard working curve that step B sets up.
2. a kind of method that is efficient, the accurately main content of detection industrial magnesium oxide according to claim 1, it is characterized in that in steps A, top grade pure zirconia magnesium is placed in the platinum crucible of lid lid, put into the muffle furnace calcination 0.5-1.5 hour being warming up to 700-800 DEG C, then cooling 3-5min is taken out, proceed in exsiccator, then be transferred to after cooling 10-20min measuring cup inner cap upper bottle cover wait for found series standard sample.
3. a kind of method that is efficient, the accurately main content of detection industrial magnesium oxide according to claim 1, is characterized in that the scope of design of the magnesium oxide percentage composition of the standard working curve in step B is 98.5-99.99%.
4. a kind of method that is efficient, the accurately main content of detection industrial magnesium oxide according to claim 1, it is characterized in that in step B, C before adding the pure lithium tetraborate of solvent analysis, in the solute taken, first add quantitative supplementary lithium tetraborate to make the quality sum of solute and supplementary lithium tetraborate and to analyze pure lithium tetraborate mass ratio for 6:0.2 ~ 6:0.6.
5. a kind of method that is efficient, the accurately main content of detection industrial magnesium oxide according to claim 4, it is characterized in that top grade pure zirconia magnesium, supplementary lithium tetraborate in step B and analyze pure lithium tetraborate all weighing in platinum crucible, weighing precision is 0.0001g, again above-mentioned three kinds of materials are fully mixed with sticking plaster in platinum crucible, then drip the iodate ammonia solution that 5 ~ 8 concentration are 10 ~ 20%, in 1100-1150 DEG C of sample-melting stove, found standard model.
6. a kind of method that is efficient, the accurately main content of detection industrial magnesium oxide according to claim 4, it is characterized in that the industrial magnesium oxide to be measured in step C, supplementary lithium tetraborate, analyze pure lithium tetraborate and all with in platinum crucible weigh, weighing precision is 0.0001g, again above-mentioned three kinds of materials are fully mixed with sticking plaster in platinum crucible, then drip the iodate ammonia solution that 5 ~ 8 concentration are 10 ~ 20%, in 1100-1150 DEG C of sample-melting stove, found testing sample.
7. a kind of method that is efficient, the accurately main content of detection industrial magnesium oxide according to claim 4, is characterized in that the purity of described supplementary lithium tetraborate is that analysis is pure.
8. a kind of method that is efficient, the accurately main content of detection industrial magnesium oxide according to claim 1, it is characterized in that the bake out temperature of industrial magnesium oxide to be measured in step C is 100-110 DEG C, drying time is 1.5-2.5 hour.
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| CN108896428A (en) * | 2018-04-28 | 2018-11-27 | 中国建材检验认证集团股份有限公司 | A kind of measuring method of sample loss on ignition |
| CN111426635A (en) * | 2020-04-07 | 2020-07-17 | 陈海锋 | Method for detecting conversion rate of magnesium oxide to magnesium hydroxide |
| CN112730365A (en) * | 2020-12-29 | 2021-04-30 | 天津天钢联合特钢有限公司 | Metallurgical lime calcium oxide analysis method |
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Cited By (3)
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