CN105223050A - Method for measuring scandium in bauxite by microwave digestion inductively coupled plasma spectrometry - Google Patents
Method for measuring scandium in bauxite by microwave digestion inductively coupled plasma spectrometry Download PDFInfo
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Abstract
The invention provides a method for determining scandium in bauxite by microwave digestion inductively coupled plasma spectrometry, which comprises the steps of digesting a sample by hydrofluoric acid, nitric acid, hydrogen peroxide and phosphoric acid under the action of microwaves, fixing the volume by ultrapure water, and determining Sc by an inductively coupled plasma emission spectrometer, so that the accurate determination of trace element Sc in the bauxite sample is realized; the invention reduces the complicated operation process, digests the sample by adopting microwave, directly measures by an instrument without acid removal, and has the characteristics of simple operation steps, less reagent consumption and high analysis speed compared with the traditional sample treatment method. Meanwhile, the method adopts microwave to digest and decompose the sample, so that the dosage of the reagent can be greatly reduced, the blank of the reagent and the interference of a matrix are reduced, and the sensitivity and the accuracy of the analysis elements are improved.
Description
Technical field
The present invention relates to analysis determining technology field, particularly relate to a kind of method that micro-wave digestion inductively coupled plasma spectrometry method measures scandium in bauxite.
Background technology
Scandium is a kind of typical rare and scatter element, is widely used in each high-tech field, but because of its content rare and be difficult to obtain highly purified metal scandium, cause it expensive.The scandium in the world 90 ~ 95% is composed and is stored in bauxite, phosphorus ore rock and ferrotitanium ore according to statistics; So scandium is as the valuable element of association in bauxite, its comprehensive utilization more and more obtains the attention of enterprise, can increase the economic benefit of enterprise, can also promote environmental protection.
Because bauxite has stronger chemical stability, normal containing a small amount of corundum, belong to more unmanageable sample.The conventional alum clay sample ore analytical approach of tradition and non-ferrous metal industry standard YS/T575-2007 adopt strong basicity flux to decompose, as natrium carbonicum calcinatum or natrium carbonicum calcinatum+boric acid mixed flux, in the high temperature furnace of about 1000 DEG C, melting 20min, NaOH or potassium hydroxide are in 750 DEG C of melting 20min and sodium peroxide 750 DEG C of melting 10min, then measure each Major And Minor Elements respectively.But these sample decomposition methods all introduce a large amount of flux, cause when measuring the Determination of Trace Scandium of association, Matrix effects is serious, and instrument fluctuation is large, measurement result bigger error.Adopt the mode of Matrix Match to eliminate interference although have, the existence of a large amount of inorganic salts still has the risk causing instrument sample introduction cone blocking plug or slowly blocking.
Separately there is report, " four acid-soluble sample inductively coupled plasma emission spectrographies measure the scandium in geological sample; rock and mineral testing ", " ICP-AES method measures Determination of Trace Scandium in vanadium titano-magnetite and metallurgical slag; University of Science & Technology, Beijing's journal ", " ICP-AES measures Microamounts of Scandium selenium rhenium in uranium ore; University Of Nanhua's journal " etc. adopt acid extracting: the low temp. electric hot plates such as hydrochloric acid, nitric acid, sulfuric acid, hydrofluorite, perchloric acid dissolve scandium, but helpless for the decomposition of bauxite, say nothing of the Accurate Determining to Determination of Trace Scandium.Therefore a kind of analytical approach being applicable to trace element scandium in bauxite accurately and efficiently of exploitation is badly in need of.
Micro-wave digestion, as a kind of emerging Sample Pretreatment Technique, has the advantages such as simple and quick, reagent dosage is few, blank value is low, is widely used in the sample pre-treatments of various trace element analysis.Have no the relevant report about scandium in bauxite measures at present.
At present, publication number is had to be CN104111207A, publication date is the Chinese invention patent document on October 22nd, 2014, name is called the content assaying method of activated silica " in a kind of bauxite ", discloses the scheme adopting NaOH to carry out decomposing bauxite as micro-wave digestion liquid, equally, there will be the drawback of aforesaid high-temperature fusion sample, except can not thoroughly decompose except sample, the stability that there is severe jamming instrument of a large amount of salt, be unfavorable for the Accurate Determining that trace is cheated.
Summary of the invention
The object of the invention is to develop a kind of analytical approach for measuring trace element scandium in bauxite, under microwave action, sample is cleared up by hydrofluorite, nitric acid, hydrogen peroxide and phosphoric acid, ultrapure water constant volume, inductive coupling plasma emission spectrograph measures Sc, realizes the Accurate Determining to trace element Sc in bauxite sample.The advantages such as it is few that the present invention has reagent dosage, and sample blank is low, and detection limit is low, highly sensitive, and the range of linearity is wide.
The concrete technical scheme of the present invention is as follows:
Micro-wave digestion induced coupled plasma atomic emission spectrometry measures scandium method in bauxite, it is characterized in that comprising the steps:
Step one, takes 0.2000 ~ 0.3000g bauxite sample to be measured, is placed in teflon teflon counteracting tank, adds the ultrapure water be enough to bauxite sample wetness on a small quantity;
Step 2, fills toward step one in the counteracting tank of wetting shape bauxite sample and adds 5 ~ 8mL red fuming nitric acid (RFNA) (HNO
3) and 1 ~ 3mL concentration be 30% hydrogen peroxide (H
2o
2), bauxite sample on counteracting tank inwall is washed at the bottom of tank, places 5min, after question response is complete, add the dense hydrofluorite of 2 ~ 5mL (HF) and 2 ~ 3mL strong phosphoric acid more successively, shake teflon teflon counteracting tank gently and make it mixing, cover cover, be equipped with support, put on the sample rotating disk of microwave dissolver, temperature sensor is inserted in the main control tank of teflon teflon counteracting tank, by setting micro-wave digestion program, carry out clearing up of bauxite sample;
Step 3, after having cleared up, has left standstill and has been cooled to teflon teflon and clears up in main control tank temperature lower than after 60 DEG C, be transferred to by the digestion solution prepared in 50.00mL volumetric flask, shake up to be measured with ultrapure water constant volume in counteracting tank;
Step 4, reagent blank is tested: be placed in teflon teflon counteracting tank and add ultrapure water, addition is identical with the addition of step one; Add 5 ~ 8mL red fuming nitric acid (RFNA) (HNO more successively
3) and 1 ~ 3mL concentration be 30% hydrogen peroxide (H
2o
2), place 5min, after question response is complete, then add the dense hydrofluorite of 2 ~ 5mL (HF) and 2 ~ 3mL strong phosphoric acid successively, shake teflon teflon counteracting tank gently and make it mixing, cover cover, be equipped with support, put on the sample rotating disk of microwave dissolver, temperature sensor is inserted in the main control tank of teflon teflon counteracting tank, by setting micro-wave digestion program, carry out clearing up of reagent blank; After having cleared up, leave standstill and be cooled to teflon teflon and clear up in main control tank temperature lower than after 60 DEG C, the digestion solution prepared has been transferred in 50.00mL volumetric flask, shakes up to be measured with ultrapure water constant volume in counteracting tank;
Step 5, adopts induced coupled plasma atomic emission spectrometry direct determination step three and the made solution to be measured of step 4, obtains measurement result.
The ultrapure water adopted in step one meets secondary water requirement in GB6682-92 " specification of Experiment of Analytical Chemistry room water and test method ".
Because considering that microwave dissolver optimum reagent use amount is 7 ~ 20mL, the red fuming nitric acid (RFNA) (HNO that the present invention adds in step 2
3), hydrogen peroxide (H
2o
2), dense hydrofluorite (HF), strong phosphoric acid cumulative volume sum should remain on 10 ~ 15mL.Micro-wave digestion programmed control process is: be first warmed up to 120 DEG C, keeps 2min; Then persistently overheating to 180 DEG C, keep 5min; Finally continue to be warmed up to 220 DEG C, keep 10min; Wherein, be warming up to 120 DEG C of needs 5min, be warming up to 180 DEG C of needs 5min, be warming up to 220 DEG C of needs 5min.
In step 5, inductive coupling plasma emission spectrograph is by the condition of work set and selected analytical line, the solution to be measured that sequentially determining standard sequence, step 3 and step 4 are made, sample solution measurement result is sample analysis result after deducting reagent blank.
Selected instrument condition of work and standard sequence as follows:
Instrument: PE8300V type inductive coupling plasma emission spectrograph;
Inductive coupling plasma emission spectrograph (ICP-OES) sampling system: hydrofluoric acid resistant;
Inductive coupling plasma emission spectrograph (ICP-OES) condition of work: RF power 1300W; Cold gas 15.0L/min; Atomization gas flow 0.8L/min; Assisted gas flow 0.2L/min; Sample introduction flow velocity: 1.5mL/min; Irrigation flow rate: 3.0mL/min; Analytical line: Sc361.383nm.
The preparation of standard series:
Scandium oxide standard reserving solution ρ (Sc
2o
3)=1.00mg/mL takes the scandium oxide 0.2500g through 600 DEG C of calcination 2h, is placed in 250mL beaker, with dissolving with hydrochloric acid, moves in 250mL volumetric flask, is diluted with water to scale, shakes up.
Standard series: configuration divides the scandium oxide standard solution of the 50ug/mL getting 0.5 and 5mL in the volumetric flask of 50mL, adds 5mL red fuming nitric acid (RFNA) (HNO
3) and 2mL strong phosphoric acid (H
3pO
4), and then constant volume scale.Be configured to the standard sequence that scandium oxide concentration is 0.5,5 μ g/mL.
Advantage of the present invention is as follows:
The present invention reduces loaded down with trivial details operating process, adopt micro-wave digestion sample, instrument directly measures, and without the need to catching up with acid, more traditional sample treatment, the present invention has simplified operational procedure, and reagent consumption is few, the feature that analysis speed is fast.This law adopts micro-wave digestion to decompose sample simultaneously, greatly can reduce reagent dosage, reduces reagent blank and Matrix effects, improves sensitivity and the accuracy of analytical element.
Embodiment
Micro-wave digestion induced coupled plasma atomic emission spectrometry measures scandium method in bauxite, and concrete steps are as follows:
Step one, takes 0.2000 ~ 0.3000g bauxite sample to be measured, is placed in teflon teflon counteracting tank, adds the ultrapure water be enough to bauxite sample wetness on a small quantity;
Step 2, fills toward step one in the counteracting tank of wetting shape bauxite sample and adds 5 ~ 8mL red fuming nitric acid (RFNA) (HNO
3) and 1 ~ 3mL concentration be 30% hydrogen peroxide (H
2o
2), bauxite sample on counteracting tank inwall is washed at the bottom of tank, place 5min, after question response is complete, then add the dense hydrofluorite of 2 ~ 5mL (HF) and 2 ~ 3mL strong phosphoric acid successively, shake teflon teflon counteracting tank gently and make it mixing, cover cover, be equipped with support, put on the sample rotating disk of microwave dissolver, temperature sensor is inserted in the main control tank of teflon teflon counteracting tank, clear up program by table 1 and carry out clearing up of bauxite sample;
Table 1 micro-wave digestion program
Step 3, after having cleared up, has left standstill and has been cooled to teflon teflon and clears up in main control tank temperature lower than after 60 DEG C, be transferred to by the digestion solution prepared in 50.00mL volumetric flask, shake up to be measured with ultrapure water constant volume in counteracting tank;
Step 4, reagent blank is tested: be placed in teflon teflon counteracting tank and add ultrapure water, addition is identical with the addition of step one; Add 5 ~ 8mL red fuming nitric acid (RFNA) (HNO more successively
3) and 1 ~ 3mL concentration be 30% hydrogen peroxide (H
2o
2), place 5min, after question response is complete, then add the dense hydrofluorite of 2 ~ 5mL (HF) and 2 ~ 3mL strong phosphoric acid successively, shake teflon teflon counteracting tank gently and make it mixing, cover cover, be equipped with support, put on the sample rotating disk of microwave dissolver, temperature sensor is inserted in the main control tank of teflon teflon counteracting tank, clear up program by table 1 to carry out, carry out clearing up of reagent blank; After having cleared up, leave standstill and be cooled to teflon teflon and clear up in main control tank temperature lower than after 60 DEG C, the digestion solution prepared has been transferred in 50.00mL volumetric flask, shakes up to be measured with ultrapure water constant volume in counteracting tank;
Step 5, adopts induced coupled plasma atomic emission spectrometry by the condition of work of setting and selected analytical line, the solution to be measured that sequentially determining standard sequence and step 3, step 4 are made, and sample solution measurement result is sample analysis result after deducting reagent blank.Selected instrument condition of work and standard sequence as follows:
Instrument: PE8300V type inductive coupling plasma emission spectrograph;
Inductive coupling plasma emission spectrograph (ICP-OES) sampling system: hydrofluoric acid resistant;
Inductive coupling plasma emission spectrograph (ICP-OES) condition of work: RF power 1300W; Cold gas 15.0L/min; Atomization gas flow 0.8L/min; Assisted gas flow 0.2L/min; Sample introduction flow velocity: 1.5mL/min; Irrigation flow rate: 3.0mL/min; Analytical line: Sc361.383nm.
The preparation of standard series:
Scandium oxide standard reserving solution ρ (Sc
2o
3)=1.00mg/mL takes the scandium oxide 0.2500g through 600 DEG C of calcination 2h, is placed in 250mL beaker, with dissolving with hydrochloric acid, moves in 250mL volumetric flask, is diluted with water to scale, shakes up.
Standard series: configuration divides the scandium oxide standard solution of the 50ug/mL getting 0.5 and 5mL in the volumetric flask of 50mL, adds 5mL red fuming nitric acid (RFNA) (HNO
3) and 2mL strong phosphoric acid (H
3pO
4), and then constant volume scale.Be configured to the standard sequence that scandium oxide concentration is 0.5,5 μ g/mL.
in this sample treatment
1, the use amount of nitric acid is selected
Nitric acid, as a kind of acid with strong oxidizing property, is widely used in the decomposition of sample.The present invention adopt proportion be 1.40 red fuming nitric acid (RFNA), test findings shows, when the consumption of nitric acid is greater than 5mL time, the scandium in alum clay sample ore can be decomposed completely, test findings is as table 2.
Table 2 nitric acid use amount is on scandium quantitative determination impact in bauxite sample
Note: in the selected bauxite standard specimen GBW (E) 070036 of test, the massfraction of scandium is 34 × 10
-6
2, the consumption choice experiment of hydrogen peroxide
Hydrogen peroxide is a kind of strong oxidizer, very strong oxidation, also there is certain solubilization-aid effect, the present invention adopts 30% hydrogen peroxide, test findings shows, when the consumption of 30% hydrogen peroxide is greater than 1mL time, scandium in alum clay sample ore can be decomposed completely, but when the consumption of hydrogen peroxide is increased to 4mL, because reaction too acutely easily causes PTFE(teflon in micro-wave digestion process) blast of teflon counteracting tank, therefore advise that the consumption of general 30% hydrogen peroxide is no more than 3mL, test findings is as table 3.
Table 3 hydrogen peroxide use amount is on scandium quantitative determination impact in bauxite sample
Note: in the selected bauxite standard specimen GBW (E) 070036 of test, the massfraction of scandium is 34 × 10
-6
3, the consumption choice experiment of hydrofluorite
Hydrofluorite has very strong corrosivity, can silicate be corroded and generate the silicon tetrafluoride of gaseous state, effective removal sample mesosilicic acid salt, the present invention adopt proportion be 1.12 dense hydrofluorite, test findings shows, when the consumption of hydrofluorite is greater than 2mL time, the scandium in alum clay sample ore can be decomposed completely, test findings is as table 4.
Table 4 hydrofluorite use amount is on scandium quantitative determination impact in bauxite sample
Note: in the selected bauxite standard specimen GBW (E) 070036 of test, the massfraction of scandium is 34 × 10
-6
4, phosphoric acid consumption experiment
The present invention adopt proportion be 1.69 strong phosphoric acid, test findings shows, when the consumption of phosphoric acid is greater than 2mL time, scandium in alum clay sample ore can be decomposed completely, but after the consumption of phosphoric acid is greater than 3mL, because phosphoric acid self is than great, in addition consumption is large, the viscosity preparing digestion solution is caused to increase, cannot be transferred to preparing digestion solution completely in volumetric flask, simultaneously larger viscosity, easily causing sample feeding pipe and the atomizer blocking of plasma-speetrometer, therefore select phosphoric acid consumption to be 2 ~ 3mL, test findings is as table 5.
Table 5 phosphoric acid use amount is on scandium quantitative determination impact in bauxite sample
Note: in the selected bauxite standard specimen GBW (E) 070036 of test, the massfraction of scandium is 34 × 10
-6
5, method contrast test
Take different bauxite sample ores, this method dissolved mineral sample same NaOH, sodium peroxide is adopted to contrast, can be drawn by the data result analysis of table 6, the measurement result of this method is with between alkali fusion measurement result, there are no significant difference, method accuracy meets requirement of experiment, and the method is feasible.
Table 6
6, method precision experiment
We select bauxite national standard material GBW (E) 070036, adopt the molten ore deposit method of tradition and microwave digestion method to carry out 5 parallel laboratory tests to standard substance, measure the scandium in sample.
Table 7
As can be seen from table 7 data, Microwave Digestion effectively reduces matrix effect, and the precision of method is significantly improved.
Claims (6)
1. micro-wave digestion induced coupled plasma atomic emission spectrometry measures scandium method in bauxite, it is characterized in that comprising the steps:
Step one, takes 0.2000 ~ 0.3000g bauxite sample to be measured, is placed in teflon teflon counteracting tank, adds the ultrapure water be enough to bauxite sample wetness on a small quantity;
Step 2, fill toward step one in the counteracting tank of wetting shape bauxite sample and add 5 ~ 8mL red fuming nitric acid (RFNA) and 1 ~ 3mL concentration is the hydrogen peroxide of 30%, bauxite sample on counteracting tank inwall is washed at the bottom of tank, place 5min, after question response is complete, add the dense hydrofluorite of 2 ~ 5mL and 2 ~ 3mL strong phosphoric acid more successively, shake teflon teflon counteracting tank gently and make it mixing, cover cover, be equipped with support, put on the sample rotating disk of microwave dissolver, temperature sensor is inserted in the main control tank of teflon teflon counteracting tank, by setting micro-wave digestion program, carry out clearing up of bauxite sample,
Step 3, after having cleared up, has left standstill and has been cooled to teflon teflon and clears up in main control tank temperature lower than after 60 DEG C, be transferred to by the digestion solution prepared in 50.00mL volumetric flask, shake up to be measured with ultrapure water constant volume in counteracting tank;
Step 4, reagent blank is tested: be placed in teflon teflon counteracting tank and add ultrapure water, addition is identical with the addition of step one; Add 5 ~ 8mL red fuming nitric acid (RFNA) more successively and 1 ~ 3mL concentration is the hydrogen peroxide of 30%, place 5min, after question response is complete, add the dense hydrofluorite of 2 ~ 5mL and 2 ~ 3mL strong phosphoric acid more successively, shake teflon teflon counteracting tank gently and make it mixing, cover cover, be equipped with support, put on the sample rotating disk of microwave dissolver, temperature sensor is inserted in the main control tank of teflon teflon counteracting tank, clear up program by setting and clear up; After having cleared up, leave standstill and be cooled to teflon teflon and clear up in main control tank temperature lower than after 60 DEG C, the digestion solution prepared has been transferred in 50.00mL volumetric flask, shakes up to be measured with ultrapure water constant volume in counteracting tank;
Step 5, adopts induced coupled plasma atomic emission spectrometry direct determination step three and the made solution to be measured of step 4, obtains measurement result.
2. micro-wave digestion induced coupled plasma atomic emission spectrometry according to claim 1 measures scandium method in bauxite, it is characterized in that: the ultrapure water adopted in step one meets secondary water requirement in GB6682-92 " specification of Experiment of Analytical Chemistry room water and test method ".
3. micro-wave digestion induced coupled plasma atomic emission spectrometry according to claim 1 measures scandium method in bauxite, it is characterized in that: in step 2, microwave dissolver optimum reagent use amount is 7 ~ 20mL, the red fuming nitric acid (RFNA) therefore added, hydrogen peroxide, dense hydrofluorite, strong phosphoric acid cumulative volume sum should remain on 10 ~ 15mL.
4. micro-wave digestion induced coupled plasma atomic emission spectrometry according to claim 1 measures scandium method in bauxite, and it is characterized in that, micro-wave digestion programmed control process is: be first warmed up to 120 DEG C, keeps 2min; Then persistently overheating to 180 DEG C, keep 5min; Finally continue to be warmed up to 220 DEG C, keep 10min; Wherein, be warming up to 120 DEG C of needs 5min, be warming up to 180 DEG C of needs 5min, be warming up to 220 DEG C of needs 5min.
5. micro-wave digestion induced coupled plasma atomic emission spectrometry according to claim 1 measures scandium method in bauxite, it is characterized in that: in step 5, inductive coupling plasma emission spectrograph is by the condition of work set and selected analytical line, the solution to be measured that sequentially determining standard sequence, step 3 and step 4 are made, sample solution measurement result is sample analysis result after deducting reagent blank.
6. micro-wave digestion induced coupled plasma atomic emission spectrometry according to claim 1 measures scandium method in bauxite, and it is characterized in that, selected instrument condition of work is:
Instrument: PE8300V type inductive coupling plasma emission spectrograph;
Inductive coupling plasma emission spectrograph (ICP-OES) sampling system: hydrofluoric acid resistant;
Inductive coupling plasma emission spectrograph (ICP-OES) condition of work: RF power 1300W; Cold gas 15.0L/min; Atomization gas flow 0.8L/min; Assisted gas flow 0.2L/min; Sample introduction flow velocity: 1.5mL/min; Irrigation flow rate: 3.0mL/min; Analytical line: Sc361.383nm;
The preparation of standard series:
Scandium oxide standard reserving solution ρ (Sc
2o
3)=1.00mg/mL takes the scandium oxide 0.2500g through 600 DEG C of calcination 2h, is placed in 250mL beaker, with dissolving with hydrochloric acid, moves in 250mL volumetric flask, is diluted with water to scale, shakes up;
Standard series: configuration divides the scandium oxide standard solution of the 50ug/mL getting 0.5 and 5mL in the volumetric flask of 50mL, adds 5mL red fuming nitric acid (RFNA) and 2mL strong phosphoric acid, and then constant volume scale; Be configured to the standard sequence that scandium oxide concentration is 0.5,5 μ g/mL.
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