CN102393369B - Temperature increment method for measuring content of ferric oxide in silicon carbide through adopting atomic absorption method - Google Patents
Temperature increment method for measuring content of ferric oxide in silicon carbide through adopting atomic absorption method Download PDFInfo
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- CN102393369B CN102393369B CN 201110350021 CN201110350021A CN102393369B CN 102393369 B CN102393369 B CN 102393369B CN 201110350021 CN201110350021 CN 201110350021 CN 201110350021 A CN201110350021 A CN 201110350021A CN 102393369 B CN102393369 B CN 102393369B
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Abstract
The invention discloses a temperature increment method for measuring content of ferric oxide in silicon carbide through adopting the atomic absorption method. A sample is sent into a graphite furnace and heated to realize the sample atomization. The temperature increment method is realized in the following steps of: increasing the temperature to 100 to 110 DEG C at a speed of 8 DEG C/s, and preserving the temperature for 6 to 15s; increasing the temperature to 115 to 125 DEG C at a speed of 3 DEG C/s, and preserving the temperature for 9 to 17s; increasing the temperature to 135 to 145 DEG C at a speed of 5 DEG C/s, and preserving the temperature for 4 to 12s; increasing the temperature to 642 to 654 DEG C at a speed of 50 DEG C/s, and preserving the temperature for 16 to 23s; increasing the temperature to 1447 to 1456 DEG C at a speed of 250 DEG C/s, and preserving the temperature for 24 to 36s; and instantly increasing the temperature to 2596 to 2606 DEG C, and heating for 4 to 11s.The light wave intensity is detected and the content of the ferric oxide is calculated. Through controlling the temperature and the temperature increment speed, the to-be-analyzed element is atomizedin the same chemical form, so that the interference is greatly reduced, and favorable analysis result can be obtained; and the method has the advantages of short analysis time, high precision, simplicity in operation, and the like.
Description
Technical field
The present invention relates to the atomic absorption spectrometry of ferric oxide content in the silicon carbide micro-powder, specifically the temperature-rising method of ferric oxide content in the aas determination silit.
Background technology
Method for detection of ferric oxide content in the silicon carbide micro-powder mainly contains colourimetry and atomic absorption method at present, and colourimetry has manually, big, the shortcomings such as detection time is long, efficient is low, environment difference of apparatus factor influence; The principle of atomic absorption method is: the Atomic Absorption Spectrometer device is provided the light of elemental characteristic spectral line to be measured from radiation of light source, is absorbed by element ground state atom to be measured in the steam during by sample steam.The degree that is weakened by radiation feature spectral line light is measured the content of element to be measured in the sample.Atom absorbs the absorbing phenomenon that characteristic spectral line that the atom pair refer to be gaseous state goes out by similar atomic radiation has.When radiation projects on the atomic vapour, if equaling atom, the corresponding energy of radiation wavelength during to the excited state energy needed, then can cause the absorption of atom pair radiation by ground state transition, produce absorption spectrum.Ground state atom has absorbed energy, and outermost electron production transition transits to excited state from low-energy state.Atomic absorption method mostly adopts the liquid sample introduction, flame atomization, and solution atomization was dissociated into ground state atom by molecular vapors then to being evaporated to the molecule steam before this, this testing process, the sample requirement is more, and condensation rate is lower.Can not or be difficult to analyze higher lower of solid or viscosity.Sensitivity is lower, because combustion gas and combustion-supporting gas be the sample Macrodilution, thereby sensitivity is restricted.Sample temperature in the heating engineering is too high, the too fast meeting that heats up causes sample to splash, and the atomization effect is bad; Temperature is crossed low removal of contamination fully again, so the temperature-rising method of sample in heating process be the key factor that influences element loss amount to be measured and contaminant removal effect in the sample, direct impact analysis result's precision.
Summary of the invention
Technical matters to be solved by this invention provides the temperature-rising method of ferric oxide content in a kind of aas determination silit, can improve the precision of measurement.
The present invention solves the problems of the technologies described above the technical scheme that adopts to be: the temperature-rising method of ferric oxide content in the aas determination silit; adopt Atomic Absorption Spectrometer as testing tool; feeding pressure to the graphite furnace of Atomic Absorption Spectrometer is that the argon gas of 0.5MPa is as blanket gas; then silicon carbide sample to be measured is sent in the graphite furnace; connect the power supply of graphite furnace; control strength of current heats up graphite furnace gradually; the heating silicon carbide sample; make sample atomsization, pass the content that weakens quantitative determination place di-iron trioxide of the light wave intensity of atom vapor by detection.The temperature-rising method of graphite furnace is: improve strength of current gradually, make graphite furnace be warming up to 100-110 ℃ with the speed of 8 ℃/s, keep 6-15s under this temperature; Speed with 3 ℃/s is warming up to 115-125 ℃ then, insulation 9-17s; Speed with 5 ℃/s is warming up to 135-145 ℃ again, insulation 4-12s; Speed with 50 ℃/s is warming up to 642-654 ℃ afterwards, insulation 16-23s; Speed with 250 ℃/s is warming up to 1447-1456 ℃ again, insulation 24-36s; Moment is warming up to 2596-2606 ℃ afterwards, continues heating 4-11s with this temperature, and detect light wave intensity to the back heat time heating time, and calculates ferric oxide content according to sample addition and testing result; Heat up with the speed of 500 ℃/s more at last, continue calcining 1-5s after being warming up to 2697-2708 ℃, namely finish the temperature-rise period of graphite furnace.
Adopt Atomic Absorption Spectrometer to detect the silicon carbide micro-powder sample, change atomic absorption instrument spectrometer traditional liquid sample introduction, directly adopt solid sampling, sample is introduced graphite-pipe with solid forms, by the electric current of controlling by graphite-pipe graphite-pipe is heated because of its resistance, produce high temperature below 3000 ℃ with sample drying, ashing, final atomization.Oxidized when the high temperature for fear of graphite-pipe, in inside and outside blanketing with inert gas of graphite-pipe.According to the degree that radiation light-wave intensity weakens, carry out data and handle.
The invention has the beneficial effects as follows: by temperature and the programming rate of control heating process, make element to be analyzed enter atomized stage with identical chemical form, and the matrix coexisting substances all is removed, and gas chemistry disturbs and the background absorption interference reduces significantly, obtains good analysis result.Have analysis time short, degree of accuracy is high, simple to operate, reduce to detect cost; Before detection, need not add reagent such as hydrofluorite, nitric acid, sulfuric acid sample is handled, can realize remarkable advantages such as direct solid sample introduction.Thoroughly avoided simultaneously in the colorimetric method for determining di-iron trioxide process crossing mistake by what equipment, personnel, reagent etc. produced, avoided in testing process owing to add reagent such as hydrofluorite, nitric acid, sulfuric acid to the influence of the healthy generation of testing staff, thereby improved the quality index of product, also improved testing staff's working environment simultaneously.
Embodiment
Specify the temperature-rising method of ferric oxide content in the aas determination silit of the present invention.The atomic absorption spectrometry of ferric oxide content adopts Atomic Absorption Spectrometer as testing tool in the silit; graphite furnace in the Atomic Absorption Spectrometer is the heater block of sample; sample is introduced graphite furnace with solid-state form; by the flow through electric current of graphite furnace of control graphite furnace is heated because of its resistance, adopting pressure in the heating process is that the argon gas of 0.5MPa is as the blanket gas of graphite furnace.When measuring; the argon gas that first graphite furnace feeding pressure to Atomic Absorption Spectrometer is 0.5MPa is as blanket gas; then silicon carbide sample to be measured is sent in the graphite furnace; connect the power supply of graphite furnace; control strength of current heats up graphite furnace gradually; the heating silicon carbide sample makes sample atomsization, passes the content that weakens quantitative determination place di-iron trioxide of the light wave intensity of atom vapor by detection.The temperature-rising method of graphite furnace is: improve strength of current gradually, make graphite furnace be warming up to 100-110 ℃ with the speed of 8 ℃/s, keep 6-15s under this temperature; Speed with 3 ℃/s is warming up to 115-125 ℃ then, insulation 9-17s; Speed with 5 ℃/s is warming up to 135-145 ℃ again, insulation 4-12s; Speed with 50 ℃/s is warming up to 642-654 ℃ afterwards, insulation 16-23s; Speed with 250 ℃/s is warming up to 1447-1456 ℃ again, insulation 24-36s; Moment is warming up to 2596-2606 ℃ afterwards, continues heating 4-11s with this temperature, and detect light wave intensity to the back heat time heating time, and calculates ferric oxide content according to sample addition and testing result; Heat up with the speed of 500 ℃/s more at last, continue calcining 1-5s after being warming up to 2697-2708 ℃, namely finish the temperature-rise period of graphite furnace.
In the heating process of sample, heat in strict accordance with heating rate of the present invention and temperature, leading portion adopts the slope to heat up, and keeps temperature heating certain hour after temperature arrives and sets again.Adopt ladder-elevating temperature at the back segment of heating process, temperature moment is risen to setting value, finish the atomization of sample.After measuring ferric oxide content, continue graphite furnace heating certain hour, residual to remove sample, prepare for detect next time.
Embodiment 1
The temperature-rising method of ferric oxide content in the aas determination silit, adopt Atomic Absorption Spectrometer as testing tool, feeding pressure to the graphite furnace of Atomic Absorption Spectrometer is that the argon gas of 0.5MPa is as blanket gas, then silicon carbide sample to be measured is sent in the graphite furnace, connect the power supply of graphite furnace, control strength of current heats up graphite furnace gradually, the heating silicon carbide sample, make sample atomsization, pass the content that weakens quantitative determination place di-iron trioxide of the light wave intensity of atom vapor by detection, the temperature-rising method of graphite furnace is: improve strength of current gradually, make graphite furnace be warming up to 100 ℃ with the speed of 8 ℃/s, keep 8s under this temperature; Speed with 3 ℃/s is warming up to 117 ℃ then, insulation 12s; Speed with 5 ℃/s is warming up to 137 ℃ again, insulation 11s; Speed with 50 ℃/s is warming up to 642 ℃ afterwards, insulation 19s; Speed with 250 ℃/s is warming up to 1452 ℃ again, insulation 33s; Moment is warming up to 2598 ℃ afterwards, continues heating 9s with this temperature, and detect light wave intensity to the back heat time heating time, and calculates ferric oxide content according to sample addition and testing result; Heat up with the speed of 500 ℃/s more at last, continue calcining 3s after being warming up to 2701 ℃, namely finish the temperature-rise period of graphite furnace.
Embodiment 2
The temperature-rising method of ferric oxide content in the aas determination silit, adopt Atomic Absorption Spectrometer as testing tool, feeding pressure to the graphite furnace of Atomic Absorption Spectrometer is that the argon gas of 0.5MPa is as blanket gas, then silicon carbide sample to be measured is sent in the graphite furnace, connect the power supply of graphite furnace, control strength of current heats up graphite furnace gradually, the heating silicon carbide sample, make sample atomsization, pass the content that weakens quantitative determination place di-iron trioxide of the light wave intensity of atom vapor by detection, the temperature-rising method of graphite furnace is: improve strength of current gradually, make graphite furnace be warming up to 104 ℃ with the speed of 8 ℃/s, keep 6s under this temperature; Speed with 3 ℃/s is warming up to 115 ℃ then, insulation 9s; Speed with 5 ℃/s is warming up to 135 ℃ again, insulation 4s; Speed with 50 ℃/s is warming up to 648 ℃ afterwards, insulation 16s; Speed with 250 ℃/s is warming up to 1447 ℃ again, insulation 24s; Moment is warming up to 2596 ℃ afterwards, continues heating 4s with this temperature, and detect light wave intensity to the back heat time heating time, and calculates ferric oxide content according to sample addition and testing result; Heat up with the speed of 500 ℃/s more at last, continue calcining 5s after being warming up to 2697 ℃, namely finish the temperature-rise period of graphite furnace.
Embodiment 3
The temperature-rising method of ferric oxide content in the aas determination silit, adopt Atomic Absorption Spectrometer as testing tool, feeding pressure to the graphite furnace of Atomic Absorption Spectrometer is that the argon gas of 0.5MPa is as blanket gas, then silicon carbide sample to be measured is sent in the graphite furnace, connect the power supply of graphite furnace, control strength of current heats up graphite furnace gradually, the heating silicon carbide sample, make sample atomsization, pass the content that weakens quantitative determination place di-iron trioxide of the light wave intensity of atom vapor by detection, the temperature-rising method of graphite furnace is: improve strength of current gradually, make graphite furnace be warming up to 110 ℃ with the speed of 8 ℃/s, keep 15s under this temperature; Speed with 3 ℃/s is warming up to 125 ℃ then, insulation 17s; Speed with 5 ℃/s is warming up to 145 ℃ again, insulation 12s; Speed with 50 ℃/s is warming up to 654 ℃ afterwards, insulation 23s; Speed with 250 ℃/s is warming up to 1456 ℃ again, insulation 36s; Moment is warming up to 2606 ℃ afterwards, continues heating 11s with this temperature, and detect light wave intensity to the back heat time heating time, and calculates ferric oxide content according to sample addition and testing result; Heat up with the speed of 500 ℃/s more at last, continue calcining 1s after being warming up to 2708 ℃, namely finish the temperature-rise period of graphite furnace.
The present invention is by keeping the time of heating after controlling temperature, the heating rate in the sample heating process and being raised to predetermined temperature, realized removing fully impurity element, and make element to be analyzed enter atomized stage with identical chemical form, reduce gas chemistry interference and background absorption significantly and disturb, obtained good analysis result.Accuracy of detection obviously improves, and foreshortens to detection time below 10 minutes.
Claims (1)
1. the temperature-rising method of ferric oxide content in the aas determination silit, adopt Atomic Absorption Spectrometer as testing tool, feeding pressure to the graphite furnace of Atomic Absorption Spectrometer is that the argon gas of 0.5MPa is as blanket gas, then silicon carbide sample to be measured is sent in the graphite furnace, connect the power supply of graphite furnace, control strength of current heats up graphite furnace gradually, the heating silicon carbide sample, make sample atomsization, the weakening of light wave intensity that passes atom vapor by detection measures the content of making di-iron trioxide, it is characterized in that: the temperature-rising method of graphite furnace is: improve strength of current gradually, make graphite furnace be warming up to 100-110 ℃ with the speed of 8 ℃/s, under this temperature, keep 6-15s; Speed with 3 ℃/s is warming up to 115-125 ℃ then, insulation 9-17s; Speed with 5 ℃/s is warming up to 135-145 ℃ again, insulation 4-12s; Speed with 50 ℃/s is warming up to 642-654 ℃ afterwards, insulation 16-23s; Speed with 250 ℃/s is warming up to 1447-1456 ℃ again, insulation 24-36s; Moment is warming up to 2596-2606 ℃ afterwards, continues heating 4-11s with this temperature, and detect light wave intensity to the back heat time heating time, and calculates ferric oxide content according to sample addition and testing result; Heat up with the speed of 500 ℃/s more at last, continue calcining 1-5s after being warming up to 2697-2708 ℃, namely finish the temperature-rise period of graphite furnace.
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| CN103344595A (en) * | 2013-07-26 | 2013-10-09 | 武汉钢铁(集团)公司 | Method for rapidly detecting content of ferric oxide in limestone or dolomite by adopting atomic absorption spectrometry |
| CN103439213B (en) * | 2013-09-02 | 2016-07-20 | 武汉钢铁(集团)公司 | The system detecting method of industry carborundum component |
Citations (2)
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| US4730925A (en) * | 1985-09-20 | 1988-03-15 | Nippon Steel Corporation | Method of spectroscopically determining the composition of molten iron |
| CN101738376A (en) * | 2008-11-25 | 2010-06-16 | 中国第一重型机械集团公司 | Method for measuring graphite oven atomic absorption spectrum of arsenic element in steel |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4730925A (en) * | 1985-09-20 | 1988-03-15 | Nippon Steel Corporation | Method of spectroscopically determining the composition of molten iron |
| CN101738376A (en) * | 2008-11-25 | 2010-06-16 | 中国第一重型机械集团公司 | Method for measuring graphite oven atomic absorption spectrum of arsenic element in steel |
Non-Patent Citations (5)
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| Determination of heavy metals in fish samples of the middle Black Sea (Turkey) by graphite furnace atomic absorption spectrometry;Mustafa Tüzen;《Food Chemistry》;20031231;第80卷;全文 * |
| HirotsuguMinami等.SimultaneousDirectDeterminationofAluminum Calcium and Iron in Silicon Carbide and Silicon Nitride Powders by Slurry-Sampling Graphite Furnace AAS.《Analytical Sciences》.2004 |
| Mustafa Tüzen.Determination of heavy metals in fish samples of the middle Black Sea (Turkey) by graphite furnace atomic absorption spectrometry.《Food Chemistry》.2003,第80卷 |
| Simultaneous Direct Determination of Aluminum, Calcium and Iron in Silicon Carbide and Silicon Nitride Powders by Slurry-Sampling Graphite Furnace AAS;Hirotsugu Minami 等;《Analytical Sciences》;20040331;第20卷;全文 * |
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