CN106769300B - The effective measuring method of aluminium and activated silica in a kind of gibbsitic bauxite - Google Patents
The effective measuring method of aluminium and activated silica in a kind of gibbsitic bauxite Download PDFInfo
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- CN106769300B CN106769300B CN201611144854.2A CN201611144854A CN106769300B CN 106769300 B CN106769300 B CN 106769300B CN 201611144854 A CN201611144854 A CN 201611144854A CN 106769300 B CN106769300 B CN 106769300B
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
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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
- G01N21/71—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light thermally excited
- G01N21/73—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light thermally excited using plasma burners or torches
Abstract
The present invention relates to the measuring methods of aluminium and activated silica effective in a kind of gibbsitic bauxite, the following steps are included: weighing the counteracting tank that sample is put into airtight microwave digestion instrument, sodium hydroxide solution is added to be cleared up, digestion solution is transferred to after the completion of resolution in the beaker for filling hydrochloric acid, heat slightly boiled dissolution hydrated aluminum silicate therein, solution is transferred to volumetric flask constant volume after cooling, it mixes, 10 mL of draw solution is in 100 mL volumetric flasks after clarification, 10 mL, 6 mol/L HCl is added, constant volume is diluted with distilled water, it mixes, measure the content of Aluminum and activated silica simultaneously with inductively coupled plasma atomic emission spectrometry, the content of effective aluminium is calculated by the content of Aluminum and activated silica, calculation formula: effective aluminium (%)=Aluminum (%)-k activated silica (%) , the content of effective aluminium and Aluminum is with Al2O3Meter, the content of activated silica is with SiO2Meter, for the value range of k between 0.90 to 1.10, best value is 1.006.Method simplicity provided by the invention rapidly and efficiently, can be widely applied to the exploration assessment to gibbsitic bauxite, and have directive significance to the adjustment of production technology.
Description
Technical field
The invention belongs to aluminium effective in chemical analysis detection technique field more particularly to a kind of gibbsitic bauxite and
The measuring method of activated silica.
Background technique
As increasingly scarcity, the gibbsitic bauxite of domestic bauxite resource are increasingly taken seriously.In three water
It is effective aluminium and activated silica that two important indicators whether it has economic value are measured in aluminum stone type bauxite, and effective aluminium refers to
Under alumina producing Bayer process process conditions, the content for the net aluminium oxide that can be extracted from ore, activated silica refers to
Under alumina producing Bayer process process conditions, the content of the compound for the silicon that can be chemically reacted with caustic alkali.
The measurement of effective aluminium and activated silica generallys use Austrian Anton Paar company and is published in gibbsitic bauxite
The method of periodical " rock and mineral testing " the 2nd phase of volume 26 in 2007 is added NaOH solution using microwave dissolver and disappears to sample
Digestion solution is diluted to 500 mL with water and mixed, 10 mL is taken to be surveyed with inductively coupled plasma atomic emission spectrometry by Xie Hou
The content of fixed effective aluminium, is then added in the surplus solution of 10 mL HCl to 500 mL dilutions, mixes, and acidification makes precipitating
Sodium aluminosilicate re-dissolves, and takes the content of a small amount of solution inductance coupled plasma-atomic emission spectrographic determination activated silica.
In this way, the measurement of effective aluminium and activated silica cannot carry out simultaneously, cannot play inductively coupled plasma body atom hair
The advantage of multiple element can be measured simultaneously by penetrating spectroscopic methodology, and to overcome above-mentioned deficiency, this patent in gibbsitic bauxite to having
The measuring method of effect aluminium and activated silica is studied.
Summary of the invention
The present invention is based on the needs using Bayer process processing gibbsitic bauxite production alumina technology and to existing
Have analysis method supplements perfect and effective aluminium and activated silica in the gibbsitic bauxite of proposition measuring method.Using visiing
When ear method handles bauxite into alumina, due to after the silicon dissolution in gibbsitic bauxite in siliceous mineral and in solution
Sodium aluminate reaction generate hydrated aluminum silicate enter red mud, the reactive silica of 1kg in gibbsitic bauxite
The aluminium oxide for just having 1kg is reacted, but the hydrated aluminum silicate precipitating formed can be by dissolving with hydrochloric acid, therefore digestion solution passes through
The content of Aluminum and activated silica can be measured using inductively coupled plasma atomic emission spectrometry simultaneously after acidification, and can be through
The content that effective aluminium is calculated is crossed, calculation formula: effective aluminium (%)=Aluminum (%)-k activated silica (%), effective aluminium and dissolution
The content of aluminium is with Al2O3Meter, the content of activated silica is with SiO2Meter, the value range of k are best value between 0.90 to 1.10
It is 1.006.
The purpose of the present invention is what is be achieved through the following technical solutions.
A kind of the step of effective measuring method of aluminium and activated silica in gibbsitic bauxite, continuous mode, successively wraps
It includes:
(1) counteracting tank that 0.5000 g sample is put into airtight microwave digestion instrument is weighed, 10.0 mL, 90 g/L NaOH is added
Solution shakes up, and is packed into resolution instrument, inputs heating curve, 30 min are cleared up at 145 DEG C;
(2) digestion solution is transferred in the 250 mL beakers for filling 100.0 mL, 0.6 mol/L HCl, heats slightly boiled 5 min
Hydrated aluminum silicate therein is dissolved, solution is transferred to 250 mL volumetric flasks after cooling, constant volume is diluted with distilled water, mixes, it is clear
10 mL, 6 mol/L HCl is added in 100 mL volumetric flasks in 10 mL of draw solution after clear, dilutes constant volume with distilled water, mixes
It is even;
(3) Al is used when measuring2O3Standard curve series is 0,20,100,200ug/ml, SiO2Standard curve series be 0,
2,10,50ug/ml measure the content of Aluminum and activated silica using inductively coupled plasma atomic emission spectrometry simultaneously;
(4) content of effectively aluminium is calculated by the content of Aluminum and the content of activated silica, calculation formula: effective aluminium
The content of (%)=Aluminum (%)-k activated silica (%), effective aluminium and Aluminum is with Al2O3Meter, the content of activated silica is with SiO2Meter,
The value range of k is between 0.90 to 1.10, and best value is 1.006.
The measuring method of effective aluminium and activated silica in a kind of gibbsitic bauxite of the present invention, it is characterised in that measurement has
The process for imitating the content of aluminium and activated silica is that the content of effective aluminium is obtained by calculation, calculation formula: effective aluminium (%)=Aluminum
The content of (%)-k activated silica (%), effective aluminium and Aluminum is with Al2O3Meter, the content of activated silica is with SiO2Meter, the value model of k
It encloses between 0.90 to 1.10, best value is 1.006.
The content of effective aluminium and activated silica in energy Accurate Determining gibbsitic bauxite of the present invention, the method are easy quickly
Efficiently, it can be widely applied to the exploration assessment to gibbsitic bauxite, while there is guidance meaning to the adjustment of production technology
Justice.
Specific embodiment
The effective measuring method of aluminium and activated silica in a kind of gibbsitic bauxite, process is to weigh sample to be put into
The counteracting tank of airtight microwave digestion instrument is added NaOH solution, shakes up, and is packed into resolution instrument, is cleared up, digestion solution is transferred to and is filled
In the beaker of HCl, slightly boiled dissolution hydrated aluminum silicate therein is heated, solution is transferred to volumetric flask constant volume after cooling, is mixed, it is clear
10 mL, 6 mol/L HCl is added in 100 mL volumetric flasks in 10 mL of draw solution after clear, dilutes constant volume with distilled water, mixes
It is even, measure the content of Aluminum and activated silica simultaneously with inductively coupled plasma atomic emission spectrometry, and by calculating
The content of effective aluminium out, calculation formula: effective aluminium (%)=Aluminum (%)-k activated silica (%), the content of effective aluminium and Aluminum
With Al2O3Meter, the content of activated silica is with SiO2Meter, the value range of k are between 0.90 to 1.10, and best value is 1.006.
Concrete operation step includes:
(1) counteracting tank that 0.5000 g sample is put into airtight microwave digestion instrument is weighed, 10.0 mL, 90 g/L NaOH is added
Solution shakes up, and is packed into resolution instrument, inputs heating curve, 30 min are cleared up at 145 DEG C;
(2) digestion solution is transferred in the 250 mL beakers for filling 100.0 mL, 0.6 mol/L HCl, heats slightly boiled 5 min
Hydrated aluminum silicate therein is dissolved, solution is transferred to 250 mL volumetric flasks after cooling, constant volume is diluted with distilled water, mixes, it is clear
10 mL, 6 mol/L HCl is added in 100 mL volumetric flasks in 10 mL of draw solution after clear, dilutes constant volume with distilled water, mixes
It is even;
(3) Al is used2O3Standard curve series is 0,20,100,200ug/ml, SiO2Standard curve series be 0,2,10,
50ug/ml measures the content of Aluminum and activated silica with inductively coupled plasma atomic emission spectrometry simultaneously;
(4) content of effectively aluminium is calculated by the content of Aluminum and the content of activated silica, calculation formula: effective aluminium
The content of (%)=Aluminum (%)-k activated silica (%), effective aluminium and Aluminum is with Al2O3Meter, the content of activated silica is with SiO2Meter,
The value of k is 1.006.
Claims (1)
1. the measuring method of effective aluminium and activated silica in a kind of gibbsitic bauxite, comprising the following steps:
(1) counteracting tank that 0.5000g sample is put into airtight microwave digestion instrument is weighed, 10.0mL90g/L NaOH solution is added, shakes
It is even, it is packed into resolution instrument, heating curve is inputted, clears up 30min at 145 DEG C;
(2) digestion solution is transferred in the 250mL beaker for filling 100.0mL0.6mol/L HCl, heats slightly boiled 5min dissolution wherein
Hydrated aluminum silicate, solution is transferred to 250mL volumetric flask constant volume after cooling, is mixed, draw solution 10mL is in 100mL after clarification
In volumetric flask, 10mL6mol/L HCl is added, dilutes constant volume with distilled water, mixes;
(3) Al is used2O3Standard curve series is 0,20,100,200ug/ml, SiO2Standard curve series is 0,2,10,50ug/
Ml measures the content of Aluminum and activated silica with inductively coupled plasma atomic emission spectrometry simultaneously;
(4) content of effectively aluminium is calculated by the content of Aluminum and the content of activated silica, calculation formula: effective aluminium (%)=
The content of Aluminum (%)-k activated silica (%), effective aluminium and Aluminum is with Al2O3Meter, the content of activated silica is with SiO2Meter, k
Value range be 0.90 to 1.10 between.
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CN108362685B (en) * | 2018-01-23 | 2020-10-20 | 中国航发北京航空材料研究院 | Analysis method for determining silicon element in high-purity aluminum |
CN111272737B (en) * | 2018-12-05 | 2023-05-30 | 核工业理化工程研究院 | Method for measuring percentage content of multiple elements in high-silicon aluminum alloy by microwave digestion-ICP-OES and application thereof |
CN109596547A (en) * | 2018-12-18 | 2019-04-09 | 中钢集团郑州金属制品研究院有限公司 | The spectroscopic methodology of oxide content in a kind of rapid and accurate determination cement |
CN112179973A (en) * | 2020-09-10 | 2021-01-05 | 河南省有色金属地质勘查总院 | Method for measuring content of effective rare earth elements in gibbsite |
CN113406022A (en) * | 2021-01-29 | 2021-09-17 | 郑州机械研究所有限公司 | Method for rapidly judging silicon content in alloy |
CN113447473A (en) * | 2021-06-28 | 2021-09-28 | 中蓝长化工程科技有限公司 | Method for detecting element content in silicate by microwave alkali digestion |
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Effective date of registration: 20200921 Address after: Group 22 and 23, Taohong village, Dongyuan Town, Qidong City, Nantong City, Jiangsu Province, 226000 Patentee after: Nantong pinglaide Energy Saving Technology Co., Ltd Address before: 467000, No. 12, building 8, welfare Street, Weidong East, Pingdingshan, Henan Patentee before: Ban Junsheng |
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