CN110006736A - The method that ICP-AES quickly measures Main elements aluminum oxide, silica and chromic oxide content in high alumina refractories containing chromium - Google Patents
The method that ICP-AES quickly measures Main elements aluminum oxide, silica and chromic oxide content in high alumina refractories containing chromium Download PDFInfo
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 59
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 title claims abstract description 47
- 239000011651 chromium Substances 0.000 title claims abstract description 31
- 239000000377 silicon dioxide Substances 0.000 title claims abstract description 30
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 title claims abstract description 29
- 229910052804 chromium Inorganic materials 0.000 title claims abstract description 28
- 238000000034 method Methods 0.000 title claims abstract description 25
- 239000011819 refractory material Substances 0.000 title claims abstract description 22
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 title claims abstract description 16
- WGLPBDUCMAPZCE-UHFFFAOYSA-N Trioxochromium Chemical compound O=[Cr](=O)=O WGLPBDUCMAPZCE-UHFFFAOYSA-N 0.000 title claims abstract description 15
- 238000002354 inductively-coupled plasma atomic emission spectroscopy Methods 0.000 title claims description 12
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 33
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 24
- QDOXWKRWXJOMAK-UHFFFAOYSA-N dichromium trioxide Chemical compound O=[Cr]O[Cr]=O QDOXWKRWXJOMAK-UHFFFAOYSA-N 0.000 claims abstract description 22
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 14
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 14
- 238000004458 analytical method Methods 0.000 claims abstract description 11
- 230000029087 digestion Effects 0.000 claims abstract description 6
- 239000002253 acid Substances 0.000 claims abstract description 5
- 239000000243 solution Substances 0.000 claims description 21
- 229910021642 ultra pure water Inorganic materials 0.000 claims description 20
- 239000012498 ultrapure water Substances 0.000 claims description 20
- 229910052782 aluminium Inorganic materials 0.000 claims description 19
- 239000004411 aluminium Substances 0.000 claims description 18
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 18
- 239000007788 liquid Substances 0.000 claims description 14
- 229910052710 silicon Inorganic materials 0.000 claims description 14
- 239000012086 standard solution Substances 0.000 claims description 14
- 230000003647 oxidation Effects 0.000 claims description 13
- 238000007254 oxidation reaction Methods 0.000 claims description 13
- 239000010703 silicon Substances 0.000 claims description 12
- 239000000463 material Substances 0.000 claims description 10
- 239000003153 chemical reaction reagent Substances 0.000 claims description 9
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 8
- 239000007789 gas Substances 0.000 claims description 8
- 238000009616 inductively coupled plasma Methods 0.000 claims description 8
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 7
- 239000003518 caustics Substances 0.000 claims description 7
- 238000010790 dilution Methods 0.000 claims description 7
- 239000012895 dilution Substances 0.000 claims description 7
- 150000001844 chromium Chemical class 0.000 claims description 5
- 238000006243 chemical reaction Methods 0.000 claims description 4
- 230000003595 spectral effect Effects 0.000 claims description 4
- 239000012490 blank solution Substances 0.000 claims description 3
- 239000006199 nebulizer Substances 0.000 claims description 3
- 239000011550 stock solution Substances 0.000 claims description 3
- 238000005303 weighing Methods 0.000 claims description 3
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 2
- 230000014759 maintenance of location Effects 0.000 claims description 2
- 150000003839 salts Chemical class 0.000 claims description 2
- 229910052708 sodium Inorganic materials 0.000 claims description 2
- 239000011734 sodium Substances 0.000 claims description 2
- 230000006641 stabilisation Effects 0.000 claims description 2
- 238000011105 stabilization Methods 0.000 claims description 2
- 239000001301 oxygen Substances 0.000 claims 1
- 229910052760 oxygen Inorganic materials 0.000 claims 1
- 238000001514 detection method Methods 0.000 abstract description 14
- 238000012360 testing method Methods 0.000 abstract description 9
- 239000003795 chemical substances by application Substances 0.000 abstract description 4
- 238000000120 microwave digestion Methods 0.000 abstract description 3
- 238000009614 chemical analysis method Methods 0.000 abstract description 2
- 230000008878 coupling Effects 0.000 abstract description 2
- 238000010168 coupling process Methods 0.000 abstract description 2
- 238000005859 coupling reaction Methods 0.000 abstract description 2
- 230000001939 inductive effect Effects 0.000 abstract description 2
- 230000007613 environmental effect Effects 0.000 abstract 1
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 10
- 229910052593 corundum Inorganic materials 0.000 description 8
- 229910000831 Steel Inorganic materials 0.000 description 7
- 238000005259 measurement Methods 0.000 description 7
- 239000010959 steel Substances 0.000 description 7
- 239000011449 brick Substances 0.000 description 6
- 229910052681 coesite Inorganic materials 0.000 description 6
- 229910052906 cristobalite Inorganic materials 0.000 description 6
- 229910052682 stishovite Inorganic materials 0.000 description 6
- 229910052905 tridymite Inorganic materials 0.000 description 6
- 229910052697 platinum Inorganic materials 0.000 description 5
- 239000010431 corundum Substances 0.000 description 4
- 229910001845 yogo sapphire Inorganic materials 0.000 description 4
- 229910018125 Al-Si Inorganic materials 0.000 description 3
- 229910018520 Al—Si Inorganic materials 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 238000011088 calibration curve Methods 0.000 description 2
- 239000000112 cooling gas Substances 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 241000790917 Dioxys <bee> Species 0.000 description 1
- 229910003978 SiClx Inorganic materials 0.000 description 1
- 238000003723 Smelting Methods 0.000 description 1
- 150000008065 acid anhydrides Chemical class 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 description 1
- 239000004327 boric acid Substances 0.000 description 1
- ZCDOYSPFYFSLEW-UHFFFAOYSA-N chromate(2-) Chemical compound [O-][Cr]([O-])(=O)=O ZCDOYSPFYFSLEW-UHFFFAOYSA-N 0.000 description 1
- 238000004737 colorimetric analysis Methods 0.000 description 1
- 239000006184 cosolvent Substances 0.000 description 1
- 230000001351 cycling effect Effects 0.000 description 1
- 238000007865 diluting Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000003628 erosive effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000009970 fire resistant effect Effects 0.000 description 1
- 239000005357 flat glass Substances 0.000 description 1
- 238000001506 fluorescence spectroscopy Methods 0.000 description 1
- 238000013467 fragmentation Methods 0.000 description 1
- 238000006062 fragmentation reaction Methods 0.000 description 1
- 230000004927 fusion Effects 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 238000001095 inductively coupled plasma mass spectrometry Methods 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 238000002203 pretreatment Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000002133 sample digestion Methods 0.000 description 1
- 239000002893 slag Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 238000004846 x-ray emission Methods 0.000 description 1
Classifications
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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
- G01N1/30—Staining; Impregnating ; Fixation; Dehydration; Multistep processes for preparing samples of tissue, cell or nucleic acid material and the like for analysis
-
- 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
- G01N1/44—Sample treatment involving radiation, e.g. heat
-
- 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
-
- 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
- G01N2001/2893—Preparing calibration standards
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- Health & Medical Sciences (AREA)
- Physics & Mathematics (AREA)
- Life Sciences & Earth Sciences (AREA)
- Pathology (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- Engineering & Computer Science (AREA)
- Nuclear Medicine, Radiotherapy & Molecular Imaging (AREA)
- Plasma & Fusion (AREA)
- Biomedical Technology (AREA)
- Molecular Biology (AREA)
- Investigating, Analyzing Materials By Fluorescence Or Luminescence (AREA)
- Analysing Materials By The Use Of Radiation (AREA)
Abstract
The present invention relates to a kind of methods that ICP-AES quickly measures Main elements aluminum oxide, silica and chromic oxide content in high alumina refractories containing chromium, using sodium hydroxide solution+hydrochloric acid+nitric acid as Acid system after microwave digestion, digestion solution is diluted, the content of Main elements aluminum oxide, silica and chrome green in high alumina refractories containing chromium is determined with inductive coupling plasma emission spectrograph (ICP-AES).This method is quick to sample pretreating, and dissolved efficiency is high, using instrument detection high-content (up to 95%) Main elements, substitutes traditional chemical analysis method completely, the result provided is reliable and stable；Testing cost is lower；Agents useful for same safety and environmental protection rationally replaces manual operation using instrument analysis, improves work efficiency, have highly application value.
Description
Technical field
The invention belongs to spectral detection field, be specifically related to Main elements alchlor in a kind of measurement refractory material,
The method of silica, chromic oxide content.
Background technique
It is chrome corundum brick that high alumina refractories containing chromium is most representative, belongs to sial series refractory material.Pink fused alumina
Brick has the features such as high temperature resistant, high pressure, chemical erosion, in metallurgy, glass, petroleum using alumina chromia as primary raw material
Industrial and commercial bank's industry achieves good using effect.In steel industry application, material containing pink fused alumina is used than common corundum material
Service life extends one times or more, such as air brick of steel ladle；In nonferrous smelting industry in use, the wearability and anti-erosion of chrome corundum brick
Property is substantially better than other brick kinds.Aluminum oxide and chrome green are two most important fire resisting oxidations in material containing pink fused alumina
Object, the height of Main elements content can directly affect the quality of the property of materials chemistry containing pink fused alumina.Survey to Main elements content
Surely it can be used for evaluating chrome corundum brick quality quality.
The detection method of pink fused alumina is at present according to GB/T3044-2007 white fused alumina, pink fused alumina chemical analysis method, dioxy
SiClx and chrome green using colorimetric method, the content of aluminum oxide is calculated when impurity content is not more than 3% with minusing,
To three kinds of Main elements, measuring band carrys out significant limitation simultaneously.
In addition, Zibo Entry-Exit Inspection and Quarantine Bureau is using 7 kinds of impurity elements in ICP-MS detection white fused alumina, pink fused alumina, body
Reveal the superiority of instrument analysis detection microelement, but does not provide the detection method of Main elements.Northeast special steel group is big
Even special steel material tests Co., Ltd discloses the measurement of metallic aluminium and aluminum oxide in a kind of steel slag, this method measurement three
Using mixing cosolvent in high-temperature fusion in platinum crucible when Al 2 O, it is found through experiment that, when aluminum oxide content is up to
When 90% or more, continuous use 3 times or more can cause to corrode to platinum crucible, cause platinum to be lost, substantially increase testing cost.
The invention of aluminium oxide and silica is special in a kind of measurement Al-Si Refractory Materials of application number 201310703019.8
In benefit, using boric acid powder tabletting, aluminium oxide and silica contains in x-ray fluorescence spectrometry Al-Si Refractory Materials
Amount, but pressed powder grain dispersion is very big, causes accuracy in detection lower.Using melting film-making-X at Ji steel technical supervision
Ray fluorescence spectrometry measures Al-Si Refractory Materials, need to draw calibration curve using at least 30 kinds of standard samples, complicated for operation,
Heavy workload is detected, testing cost is high；And when the sample of aluminium containing graininess in sample powder, detection band is given in sheet glass easily fragmentation
Come difficult.
Currently, it is seldom using the report of the host element of high-content in instrument analysis pink fused alumina, it still uses and routinizes mostly
It learns analytic approach and detects Main elements.At present there has been no a kind of fast and convenient, testing cost is low, can also analyze High-Alumina containing chromium simultaneously
The method of host element aluminum oxide, silica and chrome green generates in refractory material.
Summary of the invention
The technical problem to be solved by the present invention is to provide Main elements in a kind of refractory material for the above-mentioned prior art
Measuring method while (content up to 95% or more) can avoid using platinum crucible, substantially reduced detection using micro-wave digestion sample
Cost directly measures Main elements using ICP spectrometer, by by cycling of elements be element oxide, immediately arrive at measured value,
It is simple and quick.
The present invention solves the above problems used technical solution are as follows: it is resistance to that a kind of ICP-AES quickly measures High-Alumina containing chromium
The method of Main elements aluminum oxide, silica and chromic oxide content, key step are as follows in fiery material:
(1) sample is accurately weighed, is placed in TFM counteracting tank, is put into HTC safety guard, is soaked with a small amount of ultrapure water, is added
Hydrochloric acid is added after reacting a period of time in caustic lye of soda, weak vibrations tank body, stands, is eventually adding nitric acid, gently shakes molten
Liquid runs out of portion gas, covers TFM lid and safety spring piece, tightens lid with torque spanner, is put into microwave cavity, connects
Upper temperature sensor, is put into microwave dissolver and is cleared up, and after clearing up EP (end of program), is cooled to 30 DEG C hereinafter, by digestion solution
It is transferred in volumetric flask, is settled to scale, shake up, stand, dilution is prepared into prepare liquid；
(2) standard solution working curve is prepared: according to the resolution dosage of sample, pipette the caustic lye of soda of equivalent, hydrochloric acid,
Nitric acid is used after ultrapure water constant volume in volumetric flask as reagent blank；Dilute silicon respectively with ultrapure water, chromium standard reserving solution waits for
With separately taking several identical volumetric flasks, sequentially add aluminium, silicon, chromium series standard solution, refer again to prepare liquid in step (1)
Extension rate pipette blank reagent solution and be separately added into several volumetric flasks, scale is diluted to ultrapure water, is mixed；
(3) ICP instrument is opened, after each index of instrument meets the requirements and stabilization of lighting a fire, is established according to the operating condition of ICP
The analysis method of sample optimizes the pressure of two pump folders, converts oxidation for single element mass fraction content in method foundation
Amount of substance fractional content, sequentially determining blank solution, mixed standard solution and prepare liquid, are divided in order with element oxide amount of substance
Number content is abscissa, and spectral intensity values are ordinate linear curve, can directly calculate High-Alumina containing chromium to be measured automatically
The content of aluminum oxide, silica and chrome green in refractory material.
The concentration of sodium hydroxide used is 2%-10%, and the volume by volume concentration of hydrochloric acid is 1:1~1:10, the volume ratio of nitric acid
Concentration is 1:1~1:10.
Specifically, for weighing 0.1g sample, it is accurate to 0.1mg, is placed in TFM counteracting tank, HTC safety guard is put into
In, it is soaked with a small amount of ultrapure water, addition 2mL caustic lye of soda, weak vibrations tank body, 10mL hydrochloric acid is added after 2-5min, stands
2-10min is eventually adding 5mL nitric acid, gently shakes solution, runs out of its portion gas, then covers tightly counteracting tank, is put into microwave
It is cleared up in resolution instrument；After clearing up EP (end of program), digestion solution is transferred to constant volume in 100mL volumetric flask, is made after 10 times of dilution
For at prepare liquid.
Preferably, micro-wave digestion program is specifically arranged in step (1): clearing up power 800W, pressure 800psi or more climbs
Time 10-3015min, retention time 20min or more, 200-220 DEG C of temperature.
Specifically, it is stand-by to 100 μ g/mL to dilute silicon, chromium standard reserving solution with ultrapure water respectively for step (2), separately takes 6
100mL volumetric flask sequentially adds aluminium, silicon, chromium series standard solution, then pipettes 10mL blank reagent solution and be separately added into 6
In 100mL volumetric flask, scale is diluted to ultrapure water, is mixed.The mixed standard solution amount of pipetting is respectively as follows: 1000 μ g/ based on mL
The Al:0 of mL, 2.5,3.0,4.0,4.5,5.0；Si:0,2.5,2,1.5,1,0.5 of 100 μ g/mL；The Cr:0 of 100 μ g/mL,
6、5、4、3、2。
Preferably, inductive coupling plasma emission spectrograph operating condition in step (3) specifically: RF power:
1150W, secondary air: 0.5L/min, nebulizer gas flow: 0.7L/min, cooling gas flow: 12L/min, pump speed is rinsed
100rpm, analysis pump speed 50rpm, analytical element wavelength are respectively as follows: Al-396.152nm, Si-250.690nm, Cr-
357.869nm。
Preferably, aluminium, silicon, chromated oxide conversion coefficient be successively are as follows: and 1.8895,2.1393,1.4615, three oxidation after conversion
Two aluminium mass fraction % contents are as follows: 47.238,56.685,75.580,85.028,94.475；Silica quality score contains
Measure % are as follows: 5.348,4.279,3.209,2.139,1.070；Chrome green mass fraction content % are as follows: 8.769,7.308,
5.846、4.385、2.923。
Compared with the prior art, the advantages of the present invention are as follows: present invention micro-wave digestion pre-treatment sample, using hydroxide
Sodium liquid (5%)+hydrochloric acid+mL nitric acid can make main amount member using sodium hydroxide by sample digestion to limpid bright as Acid system
Plain oxide is converted into acid anhydrides sodium, then uses acid dissolution, obtains soluble single element ion, can thoroughly dissolve high alumina containing chromium
Fire resistant materials avoid being lost using platinum crucible, can substantially reduce testing cost.
Agents useful for same sodium hydroxide, hydrochloric acid and nitric acid of the present invention are laboratory common agents, discharge dirt again after diluting
Dye is smaller, more environmentally-friendly.Preparing calibration curve using standard solution, not only dosage is few and has very high flexibility ratio, by prepare liquid
Ten times of dilution can make main element analysis content be up to 95%, and operation is quickly, pollution-free to sample, and measurement precision is high, can
Effectively improve detection working efficiency.
Specific embodiment
Present invention is further described in detail with reference to embodiments.
A kind of ICP-AES of the invention quickly measures Main elements aluminum oxide, two in high alumina refractories containing chromium
The method of silica and chromic oxide content, includes the following steps:
Test device therefor: U.S. Thermo Fisher6500Duo composes direct-reading inductively coupled plasma atomic emission entirely
Instrument；U.S. CE M Mars6 microwave dissolver；German Sai Duolisi electronic balance；GT-30 type Laboratory Pure Water machine.
Test agents useful for same: hydrochloric acid (excellent pure grade)；Nitric acid (excellent pure grade)；Sodium hydroxide solution (5%)；Ultrapure water (from
System)；Standard reserving solution: the Standard Stock solutions of Al, Si, Cr are provided by national Iron and Steel Research Geueral Institute, and concentration value is 1000 μ
g/mL；It is stand-by that the Standard Stock solutions of Si, Cr are diluted to 100 μ g/mL.
For the accuracy for verifying the method for the present invention measurement result, pink fused alumina chamotte is chosen as example 1, BH0140 alumina is made
For example 2, GSBD4401-92 aluminium oxide standard sample is as example 3.
The measuring method of aluminum oxide, silica in example 1~3 and chromic oxide content includes following step
It is rapid:
1) sample decomposes: accurately weighing sample 0.1000g, is accurate to 0.1mg, be placed in TFM counteracting tank, is put into HTC peace
It in full cover, is soaked, is added 2mL caustic lye of soda (5%), weak vibrations tank body with a small amount of ultrapure water, 10mL salt is added after 2min
Acid stands 5min, is eventually adding 5mL nitric acid, gently shakes solution, run out of its portion gas, covers TFM lid and safety spring
Piece tightens lid with torque spanner, is put into microwave cavity, connects temperature sensor, be put into microwave dissolver by table 1
Micro-wave digestion program is cleared up.After clearing up EP (end of program), 30 DEG C are cooled to hereinafter, digestion solution is transferred to 100mL volumetric flask
In, it is settled to scale with ultrapure water, is shaken up, is stood, is prepared into prepare liquid after 10 times of dilution.
1 micro-wave digestion program of table
| Embodiment | Time (min) | Power (W) | Temperature (DEG C) | Pressure (psi) |
| 1 | 15 | 800 | 220 | 800 |
| 2 | 20 | 800 | 220 | 800 |
(2) standard solution working curve prepare: pipette 2mL caustic lye of soda (5%), 10mL hydrochloric acid, 5mL nitric acid in
In 100mL volumetric flask, use after ultrapure water constant volume as reagent blank.Dilute silicon, chromium standard reserving solution to 100 respectively with ultrapure water
μ g/mL is stand-by.6 100mL volumetric flasks separately are taken, sequentially add aluminium, silicon, chromium series standard solution, then pipette 10mL reagent blank
Solution is separately added into 6 100mL volumetric flasks, is diluted to scale with ultrapure water, is mixed.By single element quality in standard curve point
Number content is scaled oxide mass fractional content, and each oxide elements content is shown in Table 2 in standard curve.
Each element mass fraction content (%) in 2 standard curve of table
| Element | Standard 1 | Standard 2 | Standard 3 | Standard 4 | Standard 5 | Standard 6 |
| Al2O3 | 0 | 47.238 | 56.685 | 75.580 | 85.028 | 94.475 |
| SiO2 | 0 | 5.348 | 4.279 | 3.209 | 2.139 | 1.070 |
| Cr2O3 | 0 | 8.769 | 7.308 | 5.846 | 4.385 | 2.923 |
The measurement of ICP host element: optimization instrument parameter makes instrument be in optimum state: RF power: 1150W, secondary air:
0.5L/min, nebulizer gas flow: 0.7L/min, cooling gas flow: 12L/min, pump speed 100rpm, analysis pump speed are rinsed
50rpm, choosing Al-396.152nm, Si-250.690nm, Cr-357.869nm is analysis spectral line.Sequentially determining blank in order
Solution, mixed standard solution and prepare liquid, using the mass fraction content of oxide elements as abscissa, intensity value is quasi- for ordinate
Zygonema linearity curve calculates aluminum oxide, silica and chromic oxide content in chromate-containing materials.
Linear relationship and detection limit: the related coefficient of each element is respectively Al2O3、SiO2、Cr2O30.9999: 0.9999,
0.9999；Detection limit (%) Al2O3、SiO2、Cr2O3: 0.078,0.012,0.020, testing result is referring to table 3.
3 preci-sion and accuracy of table (n=8) %
Note: the Al in example 12O3、SiO2、Cr2O3Comparison data by GB/T3044-2007 white fused alumina, pink fused alumina chemistry
Analysis method is provided；Cr is free of in "-" representative instance 2,32O3, only it is further verifying Al2O3、SiO2Accuracy.
According to testing result, the Al detected using the application2O3、SiO2、Cr2O3Result and using press GB/T3044-
2007 detected values are very close, very close with standard value, and accuracy in detection is high.
The Applicant declares that the present invention illustrates detection method process of the invention by examples detailed above, but the present invention is not
It is confined to aforesaid operations step, that is, does not mean that the present invention must rely on aforesaid operations process and could implement.Technical field
Technical staff it will be clearly understood that any improvement in the present invention, adds reagent equivalence replacement and analytical element used in the present invention
Add, all of which fall within the scope of protection and disclosure of the present invention.
Claims (8)
1. a kind of ICP-AES quickly measures Main elements aluminum oxide, silica and three in high alumina refractories containing chromium
The method for aoxidizing two chromium contents, it is characterised in that: key step is as follows:
(1) sample is accurately weighed, is placed in TFM counteracting tank, is put into HTC safety guard, is soaked with a small amount of ultrapure water, hydrogen-oxygen is added
Change sodium liquid, hydrochloric acid is added after reacting a period of time in weak vibrations tank body, stands, is eventually adding nitric acid, gently shakes solution, make
Portion gas is run out of, and TFM lid and safety spring piece are covered, and is tightened lid with torque spanner, is put into microwave cavity, connects temperature
Sensor is put into microwave dissolver and is cleared up, and after clearing up EP (end of program), is cooled to 30 DEG C hereinafter, digestion solution is transferred to
In volumetric flask, it is settled to scale, is shaken up, is stood, dilution is prepared into prepare liquid；
(2) standard solution working curve is prepared: according to the resolution dosage of sample, pipetting the caustic lye of soda, hydrochloric acid, nitric acid of equivalent
In volumetric flask, use after ultrapure water constant volume as reagent blank；It is stand-by to dilute silicon, chromium standard reserving solution respectively with ultrapure water, separately
Several identical volumetric flasks are taken, aluminium, silicon, chromium series standard solution is sequentially added, refers again to the dilution of prepare liquid in step (1)
Multiple pipettes blank reagent solution and is separately added into several volumetric flasks, is diluted to scale with ultrapure water, mixes；
(3) ICP instrument is opened, after each index of instrument meets the requirements and stabilization of lighting a fire, establishes sample according to the operating condition of ICP
Analysis method, optimize the pressure of two pump folders, by single element mass fraction content convert oxidation material in method foundation
Fractional content is measured, sequentially determining blank solution, mixed standard solution and prepare liquid, are contained in order with element oxide mass fraction
Amount is abscissa, and spectral intensity values are ordinate linear curve, can directly calculate the fire resisting of High-Alumina containing chromium to be measured automatically
The content of aluminum oxide, silica and chrome green in material.
2. ICP-AES according to claim 1 quickly measures the oxidation of Main elements three two in high alumina refractories containing chromium
The method of aluminium, silica and chromic oxide content, it is characterised in that: the concentration of sodium hydroxide used is 2%-10%, salt
The volume by volume concentration of acid is 1:1~1:10, and the volume by volume concentration of nitric acid is 1:1~1:10.
3. ICP-AES according to claim 1 quickly measures the oxidation of Main elements three two in high alumina refractories containing chromium
The method of aluminium, silica and chromic oxide content, it is characterised in that: for weighing 0.1g sample, it is accurate to 0.1mg,
It is placed in TFM counteracting tank, is put into HTC safety guard, soaked with a small amount of ultrapure water, 2mL caustic lye of soda, weak vibrations tank is added
10mL hydrochloric acid is added after 2-5min for body, stands 2-10min, is eventually adding 5mL nitric acid, gently shakes solution, make its portion gas
It runs out of, then covers tightly counteracting tank, be put into microwave dissolver and cleared up；After clearing up EP (end of program), digestion solution is transferred to
Constant volume in 100mL volumetric flask is prepared into prepare liquid after 10 times of dilution.
4. ICP-AES according to claim 1 quickly measures the oxidation of Main elements three two in high alumina refractories containing chromium
The method of aluminium, silica and chromic oxide content, it is characterised in that: micro-wave digestion program is specifically arranged in step (1): disappearing
Solve power 800W, pressure 800psi or more, time-to-climb 10-3015min, retention time 20min or more, 200-220 DEG C of temperature.
5. ICP-AES according to claim 3 quickly measures the oxidation of Main elements three two in high alumina refractories containing chromium
The method of aluminium, silica and chromic oxide content, it is characterised in that: step (2) dilutes silicon, chromium standard with ultrapure water respectively
Stock solution is stand-by to 100 μ g/mL, separately takes 6 100mL volumetric flasks, sequentially adds aluminium, silicon, chromium series standard solution, then pipette
10mL blank reagent solution is separately added into 6 100mL volumetric flasks, is diluted to scale with ultrapure water, is mixed.
6. ICP-AES according to claim 5 quickly measures the oxidation of Main elements three two in high alumina refractories containing chromium
The method of aluminium, silica and chromic oxide content, it is characterised in that: the mixed standard solution amount of pipetting is respectively as follows: based on mL
Al:0,2.5,3.0,4.0,4.5,5.0 of 1000 μ g/mL；Si:0,2.5,2,1.5,1,0.5 of 100 μ g/mL；100 μ g/mL's
Cr:0,6,5,4,3,2.
7. ICP-AES according to claim 1 quickly measures the oxidation of Main elements three two in high alumina refractories containing chromium
The method of aluminium, silica and chromic oxide content, it is characterised in that: inductively coupled plasma body emits light in step (3)
Spectrometer operating condition specifically: RF power: 1150W, secondary air: 0.5L/min, nebulizer gas flow: 0.7L/min, cold
But throughput: pump speed 100rpm, analysis pump speed 50rpm 12L/min, are rinsed, analytical element wavelength is respectively as follows: Al-
396.152nm、Si-250.690nm、Cr-357.869nm。
8. ICP-AES according to claim 1 quickly measures the oxidation of Main elements three two in high alumina refractories containing chromium
The method of aluminium, silica and chromic oxide content, it is characterised in that: aluminium, silicon, chromated oxide conversion coefficient are successively are as follows:
1.8895,2.1393,1.4615, aluminum oxide mass fraction % content after conversion are as follows: 47.238,56.685,75.580,
85.028,94.475；Silica quality fractional content % are as follows: 5.348,4.279,3.209,2.139,1.070；Three oxidations two
Chromium matter amount fractional content % are as follows: 8.769,7.308,5.846,4.385,2.923.
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