CN101344487B - Method for simultaneously measuring elements of silicon, aluminum, calcium and barium - Google Patents
Method for simultaneously measuring elements of silicon, aluminum, calcium and barium Download PDFInfo
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- CN101344487B CN101344487B CN2008100489370A CN200810048937A CN101344487B CN 101344487 B CN101344487 B CN 101344487B CN 2008100489370 A CN2008100489370 A CN 2008100489370A CN 200810048937 A CN200810048937 A CN 200810048937A CN 101344487 B CN101344487 B CN 101344487B
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Abstract
The invention discloses a method that can simultaneously analyze various elements, aims at solving the defects that currently the analysis of various elements cannot be finished in one time, and consequently the analysis time is long and the reagent usage is large, and discloses a method that can simultaneously measure the elements of silicon, aluminum, calcium and barium, which comprises the following steps: a test sample is preprocessed by utilizing the acid dissolution method, microwave-digested, naturally cooled, and then placed into a volumetric flask with scales, diluted and shaken until well distributed, a solution with a standard working curve is prepared, an atomic emission spectrograph of inductance coupled plasmas is started and led to meet the measurement requirement, a plasma torch is lighted, the relative standard deviation of the plasma torch is led to be less than 5 percent, wavelength of each element is chosen, the working curves are plotted, and the content of each element is computed. The method combines the microwave digesting sample dissolution technique with the atomic emission spectrograph of inductance coupled plasmas, can simultaneously analyze nine elements including silicon, etc., is accurate and quick, has reduced reagent usage, and reduces the environmental pollution.
Description
Technical field
The present invention relates to chemical analysis, specifically more belong to the determination and analysis method of silicon aluminum calcium barium alloy silicon, aluminium, calcium, barium, iron, copper, manganese, magnesium, content of strontium.
Background technology
Silicon aluminum calcium barium alloy be a kind of in electric furnace and pneumatic steelmaking operation widespread usage novel deoxidizer in steel production, desulfurizing agent, it can make the oxygen in the steel drop to minimum; Forming the complicated snotter of calcium, barium, aluminium simultaneously floats from steel; Pure molten steel, the impact flexibility and the processing characteristics of raising steel.Therefore, the chemical constitution of accurately measuring silicon aluminum calcium barium alloy improves for smelting process and controllable quality has crucial meaning.
At present the mensuration of each constituent content in the silicon aluminum calcium barium alloy still there are not country and industry standard analytical approach.Through retrieving domestic document resource, comprising: SWIC (1989-now); The Chinese patent database (1985-now); Chinese academic dissertation database (1984-now); Chinese meeting paper database (1985-now); China's major scientific and technological achievement database (1986-now); Metallurgical Digest Database of China (1985-now) and metal Leader, world database (1998-now) etc., the document that retrieves at present has: " the ICP-AES method is measured elements such as aluminium, calcium, barium, phosphorus, copper in the Si-Al-Ca-Ba series alloy simultaneously ", the Tang Gang that " heavy steel technology " publishes in March, 2006 adopts that ICP-AES measures that aluminium and calcium and Anshan Iron and Steel Company in the NEW TYPE OF COMPOSITE deoxidizer silicon aluminum calcium barium alloy propose utilizes the ICP-AES method to analyse the method for calcium in the sial calcium strontium barium alloy, strontium, barium content.These more similar analytical approachs can be measured the element beyond the silica removal in the silicon aluminum calcium barium alloy, but silicon need adopt the chemical analysis method of gravimetric method or silicon fluoro acid potassium acid base titration to measure.These methods are all adopted conventional nitric acid, hydrofluoric acid dissolution simultaneously, and the mode that perchloric acid is smoldered is decomposed sample, and reagent dosage is many.
Summary of the invention
The objective of the invention is to overcome above-mentioned deficiency, provide a kind of employing ICP-AES method can measure nine elements such as silicon in the silicon aluminum calcium barium alloy, iron, aluminium, calcium, barium, copper, manganese, magnesium, strontium simultaneously, and measurement result accurately, reliably.
Technical scheme of the present invention is achieved in that it combines the molten appearance technology of micro-wave digestion with inductively coupled plasma atomic emission spectrometer, measure silicon in the silicon aluminum calcium barium alloy, aluminium, calcium, barium, iron, copper, manganese, magnesium, strontium simultaneously.
Realize the technical measures of purpose:
A kind of method that can measure Si-Al-Ca-Ba silicon, aluminium, calcium, barium, iron, copper, manganese, magnesium, strontium simultaneously, its step:
6) adopt the acid method of dissolving that sample is carried out pre-service:
A) get 0.1～1.0 the gram sample place the micro-wave digestion jar;
B) the micro-wave digestion jar is placed temperature＜20 ℃ water, with deionized water that sample is moistening, and add at least 5 milliliters nitric acid;
C) drip 1 milliliter hydrofluorite;
D) treat that vigorous reaction stops after, add 1 milliliter hydrofluorite again, and add a cover lid, specimen temperature is controlled at 30～＜58 ℃;
7) carry out micro-wave digestion
At first heat, make the temperature in the micro-wave digestion jar reach 100～140 ℃, the control programming rate is at 20～25 ℃/min;
Clear up: continue heating, make the temperature in the micro-wave digestion jar reach 180～220 ℃, the control programming rate is at 10～15 ℃/min;
Clear up: in temperature is to be incubated 5～15min under 180～220 ℃ of conditions again;
Lower the temperature: make the temperature in the micro-wave digestion jar reach 140～160 ℃, the control cooling rate is at 5～10 ℃/min; Carry out air draft, discharge the waste gas in the micro-wave digestion stove;
8) after micro-wave digestion finishes, adopt the natural cooling mode that sample is cooled to be lower than 38 ℃;
9) cooled sample is inserted in the volumetric flask of 100 milliliters of scales, be diluted to 100 milliliters scale and shake even with plasma water;
10) configuration of working curve standard solution:
In the volumetric flask of 100 milliliters of scales, add with sample and handle same acid, prepare serial working curve according to the content range of different elements; Wherein copper, manganese, magnesium, four distribution of trace elements of strontium are 0.00%～0.500%; Being distributed as of principal element silicon, aluminium, calcium, barium, iron: silicon 0.00～60%, iron 0.00～40.00%; Aluminium, calcium and barium be distributed as 0.00～25.00%;
6) open inductively coupled plasma atomic emission spectrometer, make each item index of this spectrometer reach its measurement requirement;
7) light plasmatorch, result's the relative standard deviation that makes continuous coverage 10 times is less than 5%;
8) wavelength of selection silicon, aluminium, calcium, barium, iron, copper, manganese, magnesium, strontium;
9) drawing curve: line strength of in inductively coupled plasma atomic emission spectrometer, measuring silicon, aluminium, calcium, barium, iron, copper, manganese, magnesium, strontium in the standard solution of variable concentrations respectively; Concentration with silicon, aluminium, calcium, barium, iron, copper, manganese, magnesium, strontium is horizontal ordinate; Line strength is an ordinate, the drawing curve;
10) calculate silicon, aluminium, calcium, barium, iron, copper, manganese, magnesium, content of strontium: under the condition identical, measure the intensity of silicon, aluminium, calcium, barium, iron, copper, manganese, magnesium, strontium spectral line in the sample solution, computing machine with drawing curve step
Automatically confirm the content of silicon, aluminium, calcium, barium, iron, copper, manganese, magnesium, strontium in each solution according to working curve.
It is: heating first makes the temperature in the micro-wave digestion jar reach 110～130 ℃.
It is: clear up: continue heating, make the temperature in the micro-wave digestion jar reach 200～220 ℃.
It is: clear up the temperature that makes in the micro-wave digestion jar again and under 200～220 ℃ of conditions, be incubated 8～10min.
It is: the wavelength of selected silicon, aluminium, calcium, barium, iron, copper, manganese, magnesium, strontium is: silicon: 221.667nm, aluminium: 394.401nm, calcium: 317.933nm, barium: 230.424nm, iron: 233.280nm, copper: 327.396nm, manganese: 259.610nm, magnesium: 279.553nm, strontium 407.771nm.
The present invention is dissolved micro-wave digestion in the appearance technology and is combined with inductively coupled plasma atomic emission spectrometer, measures silicon in the silicon aluminum calcium barium alloy sample, iron, aluminium, calcium, barium, copper, manganese, magnesium, nine elements of strontium simultaneously, and it has characteristics accurately and rapidly.When the present invention adopted the microwave digestion technology pretreatment sample, reagent dosage was compared the conventional appearance technology of dissolving and has been reduced more than 50%, has significantly reduced the pollution of chemical reagent to environment.When decomposing sample, the control decomposition temperature guarantees that the measurement result of silicon is more accurate, can satisfy the requirement of detection.
Description of drawings
The working curve of Fig. 1 elemental silicon
The working curve of Fig. 2 element aluminum
The working curve of Fig. 3 element calcium
The working curve of Fig. 4 Elements Barium
The working curve of Fig. 5 elemental iron
The working curve of Fig. 6 elemental copper
The working curve of Fig. 7 element manganese
The working curve of Fig. 8 element magnesium
The working curve of Fig. 9 elements strontium
Embodiment
1, uses instrument
IRIS Advantage composes the direct-reading plasma emission spectrometer entirely; Microwave digestion system, MILESTONE ETHOSTC type high-pressure microwave is cleared up stove;
2, use reagent
Agents useful for same all adopts top grade pure; Experimental water is a deionized water;
3, the standard inventory solution of nine elements: all adopt the corresponding standard material preparation of purity >=99.99%, content is 1.000mg/mL.
A kind of method that can measure elements of silicon, aluminum, calcium and barium simultaneously, its step:
1) adopt the acid method of dissolving that sample is carried out pre-service:
A) get 0.2000 the gram sample place the micro-wave digestion jar;
B) place temperature to be 18 ℃ of water in the micro-wave digestion jar, with deionized water that sample is moistening, and in cold water, add 5 milliliters nitric acid;
C) drip 1 milliliter hydrofluorite;
D) treat that vigorous reaction stops after, add 1 milliliter hydrofluorite again, and add a cover lid, control specimen temperature at 58 ℃;
2) carry out micro-wave digestion:
At first heat, make the temperature in the micro-wave digestion jar reach 100 ℃, the control programming rate is at 20 ℃/min;
Clear up: continue heating, make the temperature in the micro-wave digestion jar reach 180 ℃, the control programming rate is at 10 ℃/min;
Clear up: in temperature is to be incubated 15 minutes under 180 ℃ of conditions again;
Lower the temperature: make the temperature in the micro-wave digestion jar reach 140 ℃, the control cooling rate is at 5 ℃/min;
Carry out air draft, discharge the waste gas in the micro-wave digestion stove;
3) after micro-wave digestion finishes, adopt the natural cooling mode that sample is cooled to 38 ℃;
4) cooled sample is inserted in the volumetric flask of 100 milliliters of scales, be diluted to 100 milliliters scale and shake even with plasma water;
5) configuration of working curve standard solution:
In the volumetric flask of 100 milliliters of scales, add with sample and handle same acid, prepare serial working curve according to the content range of different elements; Wherein copper, manganese, magnesium, four distribution of trace elements of strontium are 0.00%, being distributed as of each element of principal element: silicon 0.00%, iron 0.00%, aluminium, calcium and barium be distributed as 0.00%;
6) open inductively coupled plasma atomic emission spectrometer, make each item index of this spectrometer reach its measurement requirement;
7) light plasmatorch, the relative standard deviation that makes copper, manganese, magnesium, 10 measurement results of four elements of four trace elements of strontium is less than 5%;
8) select the wavelength of each element: silicon: 221.667nm, aluminium: 394.401nm, calcium: 317.933nm, barium: 230.424nm, iron: 233.280nm, copper: 327.396nm, manganese: 259.610nm, magnesium: 279.553nm, strontium 407.771 nm;
9) drawing curve: use the hybrid standard working solution of preparation, under table 1 instrument condition of work, measure, the computer automatic drafting calibration curve is seen Fig. 1-Fig. 9.
10) calculate a constituent content: under the condition identical with drawing curve step, measure the intensity of each element spectral line in the sample solution, computing machine is confirmed the content of each element in each solution automatically according to working curve.
Embodiment 2
A kind of method that can measure elements of silicon, aluminum, calcium and barium simultaneously, its step:
1) adopt the acid method of dissolving that sample is carried out pre-service:
E) get 0.2000 the gram sample place the micro-wave digestion jar;
F) place temperature to be 18 ℃ of water in the micro-wave digestion jar, with deionized water that sample is moistening, and in cold water, add 5 milliliters nitric acid;
G) drip 1 milliliter hydrofluorite;
B) treat that vigorous reaction stops after, add 1 milliliter hydrofluorite again, and add a cover lid, control specimen temperature at 50 ℃;
2) carry out micro-wave digestion:
At first heat, make the temperature in the micro-wave digestion jar reach 110 ℃, the control programming rate is at 21 ℃/min; Clear up: continue heating, make the temperature in the micro-wave digestion jar reach 195 ℃, the control programming rate is at 12 ℃/min;
Clear up: in temperature is to be incubated 12min under 195 ℃ of conditions again;
Lower the temperature: make the temperature in the micro-wave digestion jar reach 150 ℃, the control cooling rate is at 8 ℃/min;
Carry out air draft, discharge the waste gas in the micro-wave digestion stove;
3) after micro-wave digestion finishes, adopt the natural cooling mode that sample is cooled to 35 ℃;
4) cooled sample is inserted in the volumetric flask of 100 milliliters of scales, be diluted to 100 milliliters scale and shake even with plasma water;
5) configuration of working curve standard solution:
In the volumetric flask of 100 milliliters of scales, add with sample and handle same acid, prepare serial working curve according to the content range of different elements; Wherein copper, manganese, magnesium, four distribution of trace elements of strontium are 0.01%, being distributed as of each element of principal element: silicon 15.00%, iron 10.00%, aluminium, calcium and barium be distributed as 5.00%;
6) open inductively coupled plasma atomic emission spectrometer, make each item index of this spectrometer reach its measurement requirement;
7) light plasmatorch, the relative standard deviation of 10 measurement results that makes silicon, aluminium, calcium, barium, five principal elements of iron is less than 1%;
8) select the wavelength of each element: silicon: 221.667nm, aluminium: 394.401nm, calcium: 317.933nm, barium: 230.424nm, iron: 233.280nm, copper: 327.396nm, manganese: 259.610nm, magnesium: 279.553nm, strontium 407.771nm;
9) drawing curve: use the hybrid standard working solution of preparation, under table 1 instrument condition of work, measure, the computer automatic drafting calibration curve is seen Fig. 1-Fig. 9.
10) calculate a constituent content: under the condition identical with drawing curve step, measure the intensity of each element spectral line in the sample solution, computing machine is confirmed the content of each element in each solution automatically according to working curve.
Embodiment 3
A kind of method that can measure elements of silicon, aluminum, calcium and barium simultaneously, its step:
1) adopt the acid method of dissolving that sample is carried out pre-service:
A) get 0.2000 the gram sample place the micro-wave digestion jar;
B) place temperature to be 18 ℃ of water in the micro-wave digestion jar, with deionized water that sample is moistening, and in cold water, add 5 milliliters nitric acid;
C) drip 1 milliliter hydrofluorite;
D) treat that vigorous reaction stops after, add 1 milliliter hydrofluorite again, and add a cover lid, control specimen temperature at 45 ℃;
2) carry out micro-wave digestion:
At first heat, make the temperature in the micro-wave digestion jar reach 120 ℃, the control programming rate is at 23 ℃/min; Clear up: continue heating, make the temperature in the micro-wave digestion jar reach 210 ℃, the control programming rate is at 12 ℃/min;
Clear up: in temperature is to be incubated 10min under 210 ℃ of conditions again;
Lower the temperature: make the temperature in the micro-wave digestion jar reach 155 ℃, the control cooling rate is at 8 ℃/min;
Carry out air draft, discharge the waste gas in the micro-wave digestion stove;
3) after micro-wave digestion finishes, adopt the natural cooling mode that sample is cooled to be lower than 32 ℃;
4) cooled sample is inserted in the volumetric flask of 100 milliliters of scales, be diluted to 100 milliliters scale and shake even with plasma water;
5) configuration of working curve standard solution: in the volumetric flask of 100 milliliters of scales, add with sample and handle same acid, prepare serial working curve according to the content range of different elements; Wherein copper, manganese, magnesium, four distribution of trace elements of strontium are 0.05%, being distributed as of each element of principal element: silicon 30.00%, iron 20.00%, aluminium, calcium and barium be distributed as 10.00%;
6) open inductively coupled plasma atomic emission spectrometer, make each item index of this spectrometer reach its measurement requirement;
7) light plasmatorch, the relative standard deviation of 10 measurement results that makes silicon, aluminium, calcium, barium, five principal elements of iron is less than 1%;
8) select the wavelength of each element: silicon: 221.667nm, aluminium: 394.401nm, calcium: 317.933nm, barium: 230.424nm, iron: 233.280nm, copper: 327.396nm, manganese: 259.610nm, magnesium: 279.553nm, strontium 407.771nm;
9) drawing curve: use the hybrid standard working solution of preparation, under table 1 instrument condition of work, measure, the computer automatic drafting calibration curve is seen Fig. 1-Fig. 9.
10) calculate a constituent content: under the condition identical with drawing curve step, measure the intensity of each element spectral line in the sample solution, computing machine is confirmed the content of each element in each solution automatically according to working curve.
Embodiment 4
A kind of method that can measure elements of silicon, aluminum, calcium and barium simultaneously, its step:
1) adopt the acid method of dissolving that sample is carried out pre-service:
I) get 0.2000 the gram sample place the micro-wave digestion jar;
J) place temperature to be 10 ℃ of water in the micro-wave digestion jar, with deionized water that sample is moistening, and in cold water, add 5 milliliters nitric acid;
K) drip 1 milliliter hydrofluorite;
L) treat that vigorous reaction stops after, add 1 milliliter hydrofluorite again, and add a cover lid, control specimen temperature at 38 ℃;
2) carry out micro-wave digestion:
At first heat, make the temperature in the micro-wave digestion jar reach 130 ℃, the control programming rate is at 23 ℃/min; Clear up: continue heating, make the temperature in the micro-wave digestion jar reach 215 ℃, the control programming rate is at 14 ℃/min; Clear up: in temperature is to be incubated 8min under 215 ℃ of conditions again;
Lower the temperature: make the temperature in the micro-wave digestion jar reach 150 ℃, the control cooling rate is at 8 ℃/min;
Carry out air draft, discharge the waste gas in the micro-wave digestion stove;
3) after micro-wave digestion finishes, adopt the natural cooling mode that sample is cooled to be lower than 30 ℃;
4) cooled sample is inserted in the volumetric flask of 100 milliliters of scales, be diluted to 100 milliliters scale and shake even with plasma water;
5) configuration of working curve standard solution: in the volumetric flask of 100 milliliters of scales, add with sample and handle same acid, prepare serial working curve according to the content range of different elements; Wherein copper, manganese, magnesium, four distribution of trace elements of strontium are 0.10%, being distributed as of each element of principal element: silicon 40.00%, iron 30.00%, aluminium, calcium and barium be distributed as 20.00%;
6) open inductively coupled plasma atomic emission spectrometer, make each item index of this spectrometer reach its measurement requirement;
7) light plasmatorch, the relative standard deviation of 10 measurement results that makes silicon, aluminium, calcium, barium, five principal elements of iron is less than 1%;
8) select the wavelength of each element: silicon: 221.667nm, aluminium: 394.401nm, calcium: 317.933nm, barium: 230.424nm, iron: 233.280nm, copper: 327.396nm, manganese: 259.610nm, magnesium: 279.553nm, strontium 407.771nm;
9) drawing curve: use the hybrid standard working solution of preparation, under table 1 instrument condition of work, measure, the computer automatic drafting calibration curve is seen Fig. 1-Fig. 9.
10) calculate a constituent content: under the condition identical with drawing curve step, measure the intensity of each element spectral line in the sample solution, computing machine is confirmed the content of each element in each solution automatically according to working curve.
A kind of method that can measure elements of silicon, aluminum, calcium and barium simultaneously, its step:
1) adopt the acid method of dissolving that sample is carried out pre-service:
A) get 0.2000 the gram sample place the micro-wave digestion jar;
B) place temperature to be 10 ℃ of water in the micro-wave digestion jar, with deionized water that sample is moistening, and in cold water, add 5 milliliters nitric acid;
C) drip 1 milliliter hydrofluorite;
D) treat that vigorous reaction stops after, add 1 milliliter hydrofluorite again, and add a cover lid, control specimen temperature at 30 ℃;
2) carry out micro-wave digestion:
At first heat, make the temperature in the micro-wave digestion jar reach 140 ℃, the control programming rate is at 25 ℃/min; Clear up: continue heating, make the temperature in the micro-wave digestion jar reach 220 ℃, the control programming rate is at 15 ℃/min;
Clear up: in temperature is to be incubated 5min under 220 ℃ of conditions again;
Lower the temperature: make the temperature in the micro-wave digestion jar reach 160 ℃, the control cooling rate is at 10 ℃/min; Carry out air draft, discharge the waste gas in the micro-wave digestion stove, and fast cooling;
3) after micro-wave digestion finishes, adopt the natural cooling mode that sample is cooled to be lower than 28 ℃;
4) cooled sample is inserted in the volumetric flask of 100 milliliters of scales, be diluted to 100 milliliters scale and shake even with plasma water;
5) configuration of working curve standard solution: in the volumetric flask of 100 milliliters of scales, add with sample and handle same acid, prepare serial working curve according to the content range of different elements; Wherein copper, manganese, magnesium, four distribution of trace elements of strontium are 0.500%, being distributed as of each element of principal element: silicon 60.00%, iron 40.00%; Aluminium, calcium and barium be distributed as 25.00%;
6) open inductively coupled plasma atomic emission spectrometer, make each item index of this spectrometer reach its measurement requirement;
7) light plasmatorch, the relative standard deviation of 10 measurement results that makes silicon, aluminium, calcium, barium, five principal elements of iron is less than 1%;
8) select the wavelength of each element: silicon: 221.667nm, aluminium: 394.401nm, calcium: 317.933nm, barium: 230.424nm, iron: 233.280nm, copper: 327.396nm, manganese: 259.610nm, magnesium: 279.553nm, strontium 407.771nm;
9) drawing curve: use the hybrid standard working solution of preparation, under table 1 instrument condition of work, measure, the computer automatic drafting calibration curve is seen Fig. 1-Fig. 9.
10) calculate a constituent content: under the condition identical with drawing curve step, measure the intensity of each element spectral line in the sample solution, computing machine is confirmed the content of each element in each solution automatically according to working curve.
Through experiment, its result:
Through nine interference tests of measuring between the element, there is not interference each other, can measure simultaneously; The precision test: appoint and get two samples by test method replicate determination 11 times, carry out the precision test, the relative standard deviation of each element is all less than 1.5%; Accuracy test: the present domestic silicon aluminum calcium barium alloy standard model that do not have temporarily; Chosen standard models such as the silico-calcium barium similar, sial barium and silico-calcium barium strontium during test and carried out accuracy test with the Si-Al-Ca-Ba matrix, adopt this method to the measurement result of the standard model chosen all in the scope of standard deviation.
Select two standard models (numbering is respectively YSB14610 and YSB14611) to make an experiment.Measurement result is seen table 1.
Table 1 experimental result
Data by table 1 can be found out; Between the measured value of nine elements of two standard models and the standard value good consistance is arranged all; And the relative standard deviation of measuring (RSD): high-load all less than 1%, trace element all less than 5%, can satisfy the detection requirement fully.
The influence of solution temperature: the experiment counteracting tank be positioned in the cooling bath of ice cube with air in same sample (choice criteria sample YSB14610:Si 53.39%) is added acid reaction under two kinds of situation; All put into then and measure after clearing up in the micro-wave digestion stove, the measurement result of silicon is seen table 2 in two kinds of methods.
The measurement result (%) of the silicon under two kinds of conditions of table 2
| ? | In the cooling bath | In the air |
| Measured value | 53.45?53.47 53.39?53.42 53.28?53.33 | 51.49?52.28 52.68?51.93 52.45?52.89 |
| Mean value | 53.39 | 52.29 |
| RSD | 0.14 | 0.98 |
The data of table 2 show: the low precision of measuring when not taking in cooling bath, to add the acid treatment sample as a result, and analysis result is on the low side.
Accuracy experiment (reclaiming experiment) about method:
That select to produce is numbered the YSB14612 standard model, adds silicon, iron, aluminium, calcium, barium, copper, manganese, the magnesium of certain content, the standard solution of nine elements of strontium, presses the sample analysis procedure, carries out recovery test, and measurement result is seen table 3.
Table 3 standard model mark-on reclaims experiment (%)
Experimental result: recovery scope: Si 98.1～101.6, Al 98.9%～101.9%, Ca98.4%～102.2%, Ba 98.4%～101.2%, Fe 99.1%～102.0%, Mn 99.7%～104.0%, Cu 99.5%～105.5%Mg 96.5%～107.0%Sr 96.0%～105.0% satisfy the detection needs.
Claims (4)
1. the method that can measure Si-Al-Ca-Ba iron copper manganese magnesium strontium element simultaneously, its step:
1) adopt the acid method of dissolving that sample is carried out pre-service:
E) get 0.2 the gram sample place the micro-wave digestion jar;
F) the micro-wave digestion jar is placed 10～18 ℃ of water of temperature, with deionized water that sample is moistening, and add at least 5 milliliters nitric acid;
G) drip 1 milliliter hydrofluorite;
H) treat that vigorous reaction stops after, add 1 milliliter hydrofluorite again, and add a cover lid, specimen temperature is controlled at 30～58 ℃;
6) carry out micro-wave digestion
At first heat, make the temperature in the micro-wave digestion jar reach 100～140 ℃, 20～25 ℃/min of control programming rate;
Clear up: continue heating, make the temperature in the micro-wave digestion jar reach 180～220 ℃, 10～15 ℃/min of control programming rate;
Clear up: in temperature is to be incubated 5～15 minutes under 180～220 ℃ of conditions again;
Lower the temperature: make the temperature in the micro-wave digestion jar reach 140～160 ℃, the control cooling rate is at 5～10 ℃/min;
Carry out air draft, discharge the waste gas in the micro-wave digestion stove;
7) after micro-wave digestion finishes, adopt the natural cooling mode that sample is cooled to be lower than 38 ℃;
8) cooled sample is inserted in the volumetric flask of 100 milliliters of scales, be diluted to 100 milliliters scale and shake even with deionized water;
9) configuration of working curve standard solution:
In the volumetric flask of 100 milliliters of scales, add with sample and handle same acid, prepare serial working curve according to the content range of different elements; Wherein copper, manganese, magnesium, four distribution of trace elements of strontium are 0.00%-0.500%; Being distributed as of principal element silicon, aluminium, calcium, barium, iron: silicon 0.00%-60.00%, iron 0.00%-40.00%; Aluminium, calcium and barium be distributed as 0.00%-25.00%;
6) open inductively coupled plasma atomic emission spectrometer, make each item index of this spectrometer reach its measurement requirement;
7) light plasmatorch, result's the relative standard deviation that makes continuous coverage 10 times is less than 5%;
8) wavelength of selection silicon, aluminium, calcium, barium, iron, copper, manganese, magnesium, strontium, the wavelength of selected each element is: silicon: 221.667nm, aluminium: 394.401nm, calcium: 317.933nm, barium: 230.424nm, iron: 233.280nm, copper: 327.396nm, manganese: 259.610nm, magnesium: 279.553nm, strontium 407.771nm;
9) drawing curve: line strength of in inductively coupled plasma atomic emission spectrometer, measuring silicon, aluminium, calcium, barium, iron, copper, manganese, magnesium, strontium in the standard solution of variable concentrations respectively; Concentration with silicon, aluminium, calcium, barium, iron, copper, manganese, magnesium, strontium is horizontal ordinate; Line strength is an ordinate, the drawing curve;
10) calculate silicon, aluminium, calcium, barium, iron, copper, manganese, magnesium, content of strontium: under the condition identical with drawing curve step; Measure the intensity of silicon, aluminium, calcium, barium, iron, copper, manganese, magnesium, strontium spectral line in the sample solution, computing machine is confirmed the content of silicon, aluminium, calcium, barium, iron, copper, manganese, magnesium, strontium in each solution automatically according to working curve.
2. a kind of method that can measure Si-Al-Ca-Ba iron copper manganese magnesium strontium element simultaneously as claimed in claim 1 is characterized in that: heating first makes the temperature in the micro-wave digestion jar reach 110～130 ℃.
3. a kind of method that can measure Si-Al-Ca-Ba iron copper manganese magnesium strontium element simultaneously as claimed in claim 1 is characterized in that: clear up: continue heating, make the temperature in the micro-wave digestion jar reach 200～220 ℃.
4. a kind of method that can measure Si-Al-Ca-Ba iron copper manganese magnesium strontium element simultaneously as claimed in claim 1 is characterized in that: clear up the temperature that makes in the micro-wave digestion jar again and under 200～220 ℃ of conditions, be incubated 8～10min.
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| Application Number | Priority Date | Filing Date | Title |
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| CN2008100489370A CN101344487B (en) | 2008-08-21 | 2008-08-21 | Method for simultaneously measuring elements of silicon, aluminum, calcium and barium |
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| CN2008100489370A CN101344487B (en) | 2008-08-21 | 2008-08-21 | Method for simultaneously measuring elements of silicon, aluminum, calcium and barium |
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| CN101344487A CN101344487A (en) | 2009-01-14 |
| CN101344487B true CN101344487B (en) | 2012-02-08 |
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| CN2008100489370A Expired - Fee Related CN101344487B (en) | 2008-08-21 | 2008-08-21 | Method for simultaneously measuring elements of silicon, aluminum, calcium and barium |
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| CN109030465B (en) * | 2018-08-17 | 2021-06-11 | 南京云开合金有限公司 | Method for detecting content of strontium, iron, barium, magnesium and calcium in zinc-strontium alloy |
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| CN114460065A (en) * | 2022-01-17 | 2022-05-10 | 包头钢铁（集团）有限责任公司 | Method for measuring strontium in deoxidizer such as silicon-aluminum-calcium-barium, silicon-aluminum-barium, silicon-calcium-barium and the like |
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