CN104215541A - Method for high efficiently and precisely measuring contents of high purity alumina and impurities - Google Patents
Method for high efficiently and precisely measuring contents of high purity alumina and impurities Download PDFInfo
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- CN104215541A CN104215541A CN201310378780.9A CN201310378780A CN104215541A CN 104215541 A CN104215541 A CN 104215541A CN 201310378780 A CN201310378780 A CN 201310378780A CN 104215541 A CN104215541 A CN 104215541A
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- aluminium oxide
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Abstract
The invention discloses a method for high efficiently and precisely measuring the contents of high purity alumina and impurities. The method comprises the following steps: step A, precisely weighing an alumina sample, recording the alumina weight as m1g, adding the weighed alumina into guaranteed reagent (GR) concentrated hydrochloric acid, fully impregnating the alumina, filtering to obtain a filtrate and a filter cake; step B, measuring the contents of impurities in alumina by carrying out ICP-OES detection on the filtrate obtained in the step A; step C, fully burning the filter cake obtained in the step A and the filter paper at a temperature of 800 to 1000 DEG C, precisely weighing the ash to obtain the ash weight recorded as m2g, and finally calculating the content of alumina according to the difference between the m1g and m2g. The alumina detection and impurity detection are separated, thus the relative deviation is small, the concentrated hydrochloric acid can dissolve almost all impurities, and the detection result is real and reliable. Basically no matrix interference exists during the detection process, the credibility of the detection result is higher than that of conventional methods, the operation is simple, and the analysis is quick.
Description
Technical field
The present invention relates to a kind of physico-chemical analysis method of aluminium oxide, particularly a kind of efficient, accurately detection high purity aluminium oxide content and impurity content method.
Background technology
Now research show: a variety of heavy metal has very large negative effect to glass substrate performance and production equipment, and part heavy metal and nonmetal environmental pollution very large.And these heavy metals very major part be introduce from the raw materials for production of glass substrate, wherein aluminium oxide is as a kind of important source material of glass substrate, its weight percentage is about 15 ~ 25%, even high purity aluminium oxide, wherein still containing some heavy metal element, therefore strengthen particularly important to the quality control of glass substrate to the detection analysis of the main content of aluminium oxide and impurity component content.
The fusing point of aluminium oxide is high, is insoluble to any acid solution, and in the detection of its impurity component, sample handling processes is quite difficult.The commonplace method of current use has x ray fluorescence spectrometry, chemical titration, spectrophotometer method, soda fusion method, boric acid and starch to make mixed flux fusion method.But these methods have respective drawback.
Shortcoming as soda fusion method: (1), owing to have employed NaOH and sodium carbonate as solvent, therefore after sample preparation, gained solution can not be used for the content measuring sodium, and the content of glass substrate industry to sodium requires effective control.Therefore this method has certain limitation.(2) because the impurity content in sample is natively lower, use comparatively complicated plurality of reagents in sample handling processes, also can bring the severe jamming of matrix, cause ICP testing result unreliable.
Shortcoming as boric acid and starch mixed flux fusion method: sample needs with mixed solvent in 1100 DEG C of melting 30min, then remove frit with boiling water leaching, with dissolving with hydrochloric acid frit, refilter.This process is loaded down with trivial details, and analysis efficiency is low, easily bring the loss of composition in sample, and power cost is high.
The testing result deviation of x ray fluorescence spectrometry is larger; And chemical titration, spectrophotometer method need to carry out a large amount of sample pretreatments, the processing time is long, the most important thing is that testing result deviation is larger.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of efficient, accurately detection high purity aluminium oxide content and impurity content method, the method of employing dipping, filtration, calcination is by main for aluminium oxide composition and impurity component separate detection, more traditional detection method is accurate, and the impurity component of 100-0.1PPM in aluminium oxide can be analyzed, simple to operate, analyze fast; To overcome in prior art that detection time is long, deviation is comparatively large, the lossy shortcoming of sample composition.
For solving the problems of the technologies described above, the technical solution used in the present invention is:
Efficient, accurately to detect a high purity aluminium oxide content and impurity content method, comprises the following steps:
A, by the m of correct amount
1g aluminium oxide, through the pure concentrated hydrochloric acid heating of top grade fully dipping, then filters, obtains filtrate and filter cake respectively;
B, by the filtrate described in steps A with ICP-OES detect analyze impurity content in alumina;
C, by the filter cake described in steps A together with filter paper at 800-1000 DEG C after abundant calcination, correct amount, be designated as m
2g, according to the difference of twice weighing, calculates the content of aluminium oxide.
Preferably, in platinum crucible, aluminium oxide flooded in steps A and on resistance furnace, heat micro-10-20 minute that boils, stirring with platinum rod simultaneously.
First select 180nm ~ 800nm scope to carry out qualitative scanning in step B, then carry out quantitative test according to the result preparing standard solution of qualitative scanning.
In step C, filter cake is placed in the platinum crucible of constant weight together with filter paper, then in muffle furnace in 900 ~ 1100 DEG C of calcination 30 ~ 40min, after being cooled to constant weight, precise.
The present invention utilizes aluminium oxide to be insoluble in concentrated hydrochloric acid, and the impurity component in aluminium oxide almost all dissolves in concentrated hydrochloric acid after heating, thus main composition aluminium oxide and its impurity component is separated, and reaches the object simultaneously detected respectively.Such one side improves detection efficiency, and filtrate is detected with ICP-OES calibration curve method and analyzed on the other hand, and do not have Matrix effects, treat that test sample only needs one, credible result degree comparatively classic method is high.
The beneficial effect adopting technique scheme to produce is: main for aluminium oxide composition separates with impurity component and detects by (1) the present invention, therefore the sample size weighed is larger, generally 1.0 ~ 5.0g can be reached, be 5 ~ 25 times of traditional detection method sample weighing (0.2g), the relative deviation detected like this is just much smaller; (2) can dissolve most impurity component with salt acid dip, testing result is true and reliable; (3) filtrate is detected with ICP-OES calibration curve method and is analyzed, and do not have Matrix effects, treat that test sample only needs one, save the pre-treatment time, testing result confidence level comparatively classic method is high.
Embodiment
Be described in detail with an embodiment below.
Efficient, accurately to detect a high purity aluminium oxide content and impurity content method, comprises the following steps:
Steps A, by the m of correct amount
1g aluminium oxide, through the pure concentrated hydrochloric acid heating of top grade fully dipping, then filters, obtains filtrate and filter cake respectively.
First the alumina sample will fetched, carries out division, takes out about 10g, is placed in the weighing disk that cleans up, puts into the baking oven being warmed up to 110 DEG C, dries 2h, then takes out and be cooled to room temperature in exsiccator.
Then, accurately take the aluminium oxide 1.0g(of having dried with ten thousand/balance and be accurate to 0.0001g) be placed in and clean in advance and in the platinum crucible of drying, and in platinum crucible, add the dense pure hydrochloric acid of 30mL top grade, again platinum crucible is placed in little fire heating 1h on resistance furnace, frequently fully stirs with platinum rod and reach abundant dipping.
Finally take off platinum crucible, be cooled to room temperature.Clean funnel, 100mL glass beaker, be placed in by funnel on filtration stand, beaker is placed in below funnel, and filter paper is close to inner wall of hopper and is placed in funnel, filters (being undertaken by " three low three lean on " principle when filtering) under the drainage of platinum rod.Use 5-20%(mass ratio after filtering) the pure watery hydrochloric acid of top grade clean platinum crucible three times and be all transferred in funnel; Finally use the pure watery hydrochloric acid flush cake (aluminium oxide) of the top grade of a small amount of 5-20% three times again, filter completely, obtain filtrate and filter cake.
B, by the filtrate described in steps A with ICP-OES detect analyze impurity content in alumina.
The filtrate of gained in steps A is settled in 100mL volumetric flask.Start ICP-OES main frame and cooling-water machine, open high-purity argon gas, instrument condition: RF power 1000W.Plasma (orifice) gas: 12 L min; Atomization gas: 0.8 L min; Assisted gas: 0L min; Argon gas sheath gas: 2 L min; Observed altitude 15 mm.Light plasma flame, after stable 10min, select the scope of scanning 180nm-800nm to carry out qualitative scanning, according to the qualitative impurity element components that scans and semiquantitative testing result (see table 1), formulate Sample series (see table 2); And set impurity element testing conditions (Element detection spectral line, RF power, assisted gas flow, integral time, atomization gas flow, pump speed, pump stabilization time), specifically see table 3.
The qualitative scanning result of table 1
Table 2 formulates standard series according to qualitative results
The instrument parameter of each element of table 3 is arranged
The quantitative result of blank rear various element deducted by table 4
The concentration conversion of each element is become the percentage composition of corresponding oxide, obtain the percentage composition of impurity in table 5.
The percentage composition of each impurity of table 5
C, by the filter cake described in steps A together with filter paper at 800-1000 DEG C after abundant calcination, correct amount, be designated as m
2g, according to the difference of twice weighing, calculates the content of aluminium oxide.
By the filter paper filtered, with the tweezers cleaned up, pinch filter paper edge aluminium oxide is wrapped completely, be placed in and clean, in the platinum crucible of pre-burn, be placed on resistance furnace, low temperature dry ashing, treat that ashing is complete, platinum crucible is placed in be warming up to 1000 DEG C muffle furnace in, calcination 30min; Then take out, be placed in exsiccator, to be cooled to room temperature, be placed in ten thousand/balance, weigh gross weight, total amount deducts the weight of platinum crucible, obtains the amount m of aluminium oxide
2for 0.9979g, the content calculating the aluminium oxide not being dissolved in concentrated hydrochloric acid is 99.69%; The content of adding the aluminium oxide being dissolved in concentrated hydrochloric acid is the total content of aluminium oxide: 99.69%+0.1115%=99.8115%.The temperature range of calcination is 800 ~ 1000 DEG C.
Do not detect that organism and other component contents are:
The main composition alumina content of 100%-99.8115%()-0.0863% (detecting impurity component content)=0.0122%(do not detect component content).
In order to verify method of the present invention, the method repeating steps A ~ step C processes again to the aluminium oxide in step C after dipping, calcination.Analysis result after deduction blank is in table 6.
The aluminium oxide of table 6 after dipping, calcination is again with the oxide content in filtrate after concentrated hydrochloric acid dipping
The result of table 6 illustrates, Impurities In Alumina composition is fully flooded by the pure concentrated hydrochloric acid of top grade, and ICP-OES detects analysis result and has higher confidence level.
About the problem of matrix effect.Essential element in high purity aluminium oxide sample is aluminium, and other compositions are trace or trace.The present invention, owing to being filtered with the form of aluminium oxide by most aluminium element, therefore matrix effect can be ignored.Experiment proves when aluminium content reaches 5mg/mL, and the mensuration of matrix to impurity element still has no significant effect.
About the problem of spectral line interference.Measure the elemental standards solution such as Fe, Si, Na, Ca (100 μm/mL) and hybrid standard working solution respectively, respective line strength is unchanged, illustrates that between impurity element, matrix is noiseless, without the need to adopting the coupling of standard solution.
About method detection limit.Preparing 1 part of blank solution, with above built standard solution, as treating that test sample carries out detection continuously and analyzes, calculating its standard deviation, with the detection limit of 3 times of each elements of standard deviation calculation, in table 7.
The detection limit of each element of table 7 the present invention (unit μm/mL)
Sample recovery of standard addition.Adopt sample using standard samples recovery to carry out the accuracy of evaluation method, the results are shown in Table 8.As can be seen from Table 8, recovery of standard addition, between 97.4% ~ 103.3%, illustrates that the accuracy of the method is very high.
The recovery of standard addition of each element of table 8
About the precision of method.Carry out 11 parallel analysiss to same sample, the relative deviation of each element is in table 9.
The standard deviation of each element that table 9 is measured
In sum, method of testing matrix effect of the present invention is little, precision is high, the recovery is higher, detection limit is lower, and comparatively classic method efficiency is higher, credible result degree is high, has great importance to the quality control of glass substrate.
Claims (4)
1. efficient, accurately detection high purity aluminium oxide content and impurity content a method, is characterized in that comprising the following steps:
A, by the m of correct amount
1g aluminium oxide, through the pure concentrated hydrochloric acid heating of top grade fully dipping, then filters, obtains filtrate and filter cake respectively;
B, by the filtrate described in steps A with ICP-OES detect analyze impurity content in alumina;
C, by the filter cake described in steps A together with filter paper at 800-1000 DEG C after abundant calcination, correct amount, be designated as m
2g, according to the difference of twice weighing, calculates the content of aluminium oxide.
2. efficient, accurately detection high purity aluminium oxide content and impurity content method according to claim 1, it is characterized in that flooding aluminium oxide in platinum crucible in steps A and on resistance furnace, heating micro-10-20 minute that boils, stir with platinum rod simultaneously.
3. efficient, accurately detection high purity aluminium oxide content and impurity content method according to claim 1, it is characterized in that in step B, first selecting 180nm ~ 800nm scope to carry out qualitative scanning, then carry out quantitative test according to the result preparing standard solution of qualitative scanning.
4. efficient, accurately detection high purity aluminium oxide content and impurity content method according to claim 2, it is characterized in that the platinum crucible in step C, filter cake being placed in constant weight together with filter paper, then in muffle furnace in 900 ~ 1100 DEG C of calcination 30 ~ 40min, after being cooled to constant weight, precise.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106568643A (en) * | 2016-11-09 | 2017-04-19 | 芜湖东旭光电科技有限公司 | Method for measuring impurity content in aluminium oxide sample and method of sample pretreatment |
| CN113218811A (en) * | 2021-04-30 | 2021-08-06 | 哈尔滨工业大学 | Effectively detect TaSi2Method of purity |
| CN114354577A (en) * | 2021-10-13 | 2022-04-15 | 中国第一重型机械股份公司 | Quantitative analysis method and device for acid-insoluble aluminum in steel |
| CN114354577B (en) * | 2021-10-13 | 2024-05-03 | 中国第一重型机械股份公司 | Quantitative analysis method and device for acid insoluble aluminum in steel |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106568643A (en) * | 2016-11-09 | 2017-04-19 | 芜湖东旭光电科技有限公司 | Method for measuring impurity content in aluminium oxide sample and method of sample pretreatment |
| CN113218811A (en) * | 2021-04-30 | 2021-08-06 | 哈尔滨工业大学 | Effectively detect TaSi2Method of purity |
| CN113218811B (en) * | 2021-04-30 | 2022-08-05 | 哈尔滨工业大学 | Effectively detect TaSi 2 Method of purity |
| CN114354577A (en) * | 2021-10-13 | 2022-04-15 | 中国第一重型机械股份公司 | Quantitative analysis method and device for acid-insoluble aluminum in steel |
| CN114354577B (en) * | 2021-10-13 | 2024-05-03 | 中国第一重型机械股份公司 | Quantitative analysis method and device for acid insoluble aluminum in steel |
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Denomination of invention: Method for high efficiently and precisely measuring contents of high purity alumina and impurities Effective date of registration: 20200710 Granted publication date: 20160914 Pledgee: Beijing State Owned Financial Leasing Co., Ltd Pledgor: WUHU DONGXU OPTOELECTRONIC EQUIPMENT TECHNOLOGY Co.,Ltd. Registration number: Y2020990000735 |
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