CN105223050B - 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, more particularly to a kind of micro-wave digestion inductively coupled plasma spectrometry
The method that 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 rareness and very
The rare metal scandium for arriving high-purity leads to its costliness.The scandium preservation in the world 90~95% is in bauxite, phosphorus ore rock and iron according to statistics
In titanium ore；So valuable element of the scandium as association in bauxite, comprehensive utilization increasingly obtains the attention of enterprise, can increase
Add the economic benefit of enterprise, environmental protection can also be promoted.
Since bauxite has stronger chemical stability, often containing a small amount of corundum, belong to than sample difficult to deal with.It passes
The conventional alumina sample ore analysis method of system and non-ferrous metal industry standard YS/T575-2007 are decomposed using strong basicity flux, such as
Natrium carbonicum calcinatum or natrium carbonicum calcinatum+boric acid mixed flux melt 20min, sodium hydroxide in 1000 DEG C or so of high temperature furnace
Or potassium hydroxide melts 750 DEG C of melting 10min of 20min and sodium peroxide in 750 DEG C, then each Major And Minor Elements are carried out respectively
It measures.However, these sample decomposition methods all introduce a large amount of flux, cause in the Determination of Trace Scandium for measuring association, matrix is done
It disturbs seriously, instrument fluctuation is big, measurement result bigger error.It is interfered in spite of by the way of Matrix Match to eliminate, but a large amount of
The presence of inorganic salts still has the risk for causing instrument sample introduction cone blocking plug or slowly blocking.
According to another report, " the molten sample inductively coupled plasma emission spectrography of tetracid measures the scandium in geological sample, and rock ore deposit is surveyed
Examination ", " ICP-AES methods measure Determination of Trace Scandium in vanadium titano-magnetite and metallurgical slag, University of Science ＆ Technology, Beijing's journal ", " ICP-AES is measured
Microamounts of Scandium selenium rhenium in uranium ore, University Of Nanhua's journal " etc. uses acid extracting：Hydrochloric acid, nitric acid, sulfuric acid, hydrofluoric acid, perchloric acid etc. are low
Warm electric hot plate dissolves scandium, however helpless for the decomposition of bauxite, needless to say to the Accurate Determining of Determination of Trace Scandium.Therefore
Be badly in need of exploitation it is a kind of accurately and efficiently suitable for bauxite trace element scandium analysis method.
Micro-wave digestion has that simple and quick, reagent dosage is few, blank value is low as a kind of emerging Sample Pretreatment Technique
The advantages that, it is widely used in the sample pre-treatments of various trace element analysis.Scandium measure in related bauxite is had no at present
Relevant report.
At present, there is Publication No. CN104111207A, publication date is the Chinese invention patent document on October 22nd, 2014,
Entitled " content assaying method of activated silica in a kind of bauxite " is disclosed and is divided using sodium hydroxide as micro-wave digestion liquid
The scheme of bauxite is solved, equally, it may appear that the drawbacks of aforementioned high-temperature fusion sample, in addition to it thoroughly cannot decompose sample, largely
The stability there are severe jamming instrument of salt is unfavorable for the Accurate Determining in trace hole.
Invention content
It is a kind of for measuring the analysis method of trace element scandium in bauxite it is an object of the invention to develop, pass through hydrogen fluorine
Acid, nitric acid, hydrogen peroxide and phosphoric acid clear up sample, ultra-pure water constant volume, inductively coupled plasma atomic emission under microwave action
Instrument measures Sc, realizes the Accurate Determining to trace element Sc in bauxite sample.The present invention is few with reagent dosage, sample blank
It is low, the advantages that detection limit is low, high sensitivity, the range of linearity is wide.
Specific technical solution of the present invention is as follows：
Micro-wave digestion induced coupled plasma atomic emission spectrometry measures scandium method in bauxite, it is characterised in that including walking as follows
Suddenly：
Step 1 weighs 0.2000~0.3000g bauxite samples to be measured, is placed in polytetrafluoroethylene (PTFE) teflon counteracting tank
Interior, addition is enough the ultra-pure water of bauxite sample wetness on a small quantity；
Step 2 fills toward step 1 and 5~8mL concentrated nitric acids (HNO is added in the counteracting tank of wetting shape bauxite sample3) and
The hydrogen peroxide of 1~3mL a concentration of 30%（H2O2）, the bauxite sample cleared up on top tank structure is washed into tank bottom, places 5min, is treated anti-
After answering completely, the dense hydrofluoric acid of 2~5mL (HF) and 2~3mL concentrated phosphoric acids are sequentially added, gently shakes polytetrafluoroethylene (PTFE) teflon
Counteracting tank is allowed to mixing, covers cover, is equipped with stent, is put on the sample turntable of microwave dissolver, temperature sensor is inserted
In the main control tank for entering polytetrafluoroethylene (PTFE) teflon counteracting tank, by setting micro-wave digestion program, the resolution of bauxite sample is carried out；
Step 3 waits after the completion of clearing up that standing is cooled to temperature in polytetrafluoroethylene (PTFE) teflon resolution main control tank and is less than 60
After DEG C, the digestion solution prepared in counteracting tank is transferred in 50.00 mL volumetric flasks, is shaken up with ultra-pure water constant volume to be measured；
Step 4, reagent blank experiment：It is placed in polytetrafluoroethylene (PTFE) teflon counteracting tank and adds in ultra-pure water, addition and step
Rapid one addition is identical；Sequentially add 5~8mL concentrated nitric acids (HNO3) and 1~3mL a concentration of 30% hydrogen peroxide（H2O2）,
5min is placed, after complete reaction, the dense hydrofluoric acid of 2~5mL (HF) and 2~3mL concentrated phosphoric acids is sequentially added, gently shakes poly- four
Vinyl fluoride teflon counteracting tank is allowed to mixing, covers cover, is equipped with stent, is put on the sample turntable of microwave dissolver, will
Temperature sensor is inserted into the main control tank of polytetrafluoroethylene (PTFE) teflon counteracting tank, and by setting micro-wave digestion program, it is empty to carry out reagent
White resolution；It waits after the completion of clearing up, standing is cooled in polytetrafluoroethylene (PTFE) teflon resolution main control tank temperature less than after 60 DEG C, will
The digestion solution prepared in counteracting tank is transferred in 50.00 mL volumetric flasks, is shaken up with ultra-pure water constant volume to be measured；
Step 5, using the solution to be measured that the direct determination step three of induced coupled plasma atomic emission spectrometry and step 4 are made,
Obtain measurement result.
The ultra-pure water used in step 1 meets GB6682-92《The specification and test method of Experiment of Analytical Chemistry room water》
Middle two level water requirement.
Because considering that microwave dissolver optimum reagent usage amount is 7~20mL in step 2, the concentrated nitric acid of the invention added in
(HNO3), hydrogen peroxide（H2O2）, dense hydrofluoric acid (HF), the sum of concentrated phosphoric acid total volume should be maintained at 10~15mL.Micro-wave digestion program
Control process is：It is warming up to 120 DEG C first, keeps 2min；Then persistently overheating to 180 DEG C, 5min is kept；Finally continue to heat up
To 220 DEG C, 10min is kept；Wherein, being warming up to 120 DEG C needs 5min, and being warming up to 180 DEG C needs 5min, is warming up to 220 DEG C of need
Want 5min.
Operating condition and selected analytical line of the inductive coupling plasma emission spectrograph by setting in step 5, successively
Bioassay standard sequence, step 3 and the made solution to be measured of step 4, sample solution measurement result subtract reagent blank after be
Sample analysis result.
Selected instrument operating condition and standard sequence are as follows：
Instrument：PE 8300V type inductive coupling plasma emission spectrographs；
Inductive coupling plasma emission spectrograph (ICP-OES) sampling system：Hydrofluoric acid resistant；
Inductive coupling plasma emission spectrograph (ICP-OES) operating condition：1300 W of RF power；Cool down gas 15.0
L/min；0.8 L/min of atomization gas flow；0.2 L/min of secondary air amount；Sample introduction flow velocity：1.5 mL/min；Irrigation flow rate：
3.0mL/min；Analytical line：Sc361.383nm.
The preparation of standard series：
Scandium oxide standard reserving solution ρ (Sc2O3The mg/mL of)=1.00 weighs the scandium oxide through 600 DEG C of 2 h of calcination
0.2500g is placed in 250 mL beakers, with dissolving with hydrochloric acid, is moved into 250 mL volumetric flasks, is diluted with water to scale, shakes up.
Standard series：Configuration point takes the scandium oxide standard solution of the 50ug/mL of 0.5 and 5mL in the volumetric flask of 50mL
In, add 5mL concentrated nitric acids (HNO3) and 2mL concentrated phosphoric acids（H3PO4）, then constant volume scale again.It is a concentration of to be configured to scandium oxide
0.5th, the standard sequence of 5 μ g/mL.
Advantage of the present invention is as follows：
The present invention reduces cumbersome operating process, and using micro-wave digestion sample, instrument directly measures, without catching up with acid, compared with
Traditional sample treatment, the present invention have the characteristics of operating procedure is simple and direct, and reagent consumption is few, and analyze speed is fast.This law simultaneously
Sample is decomposed using micro-wave digestion, reagent dosage can be greatly reduced, reagent blank and Matrix effects is reduced, improves analytical element
Sensitivity and accuracy.
Specific embodiment
Micro-wave digestion induced coupled plasma atomic emission spectrometry measures scandium method in bauxite, is as follows：
Step 1 weighs 0.2000~0.3000g bauxite samples to be measured, is placed in polytetrafluoroethylene (PTFE) teflon counteracting tank
Interior, addition is enough the ultra-pure water of bauxite sample wetness on a small quantity；
Step 2 fills toward step 1 and 5~8mL concentrated nitric acids (HNO is added in the counteracting tank of wetting shape bauxite sample3) and
The hydrogen peroxide of 1~3mL a concentration of 30%（H2O2）, the bauxite sample cleared up on top tank structure is washed into tank bottom, places 5min, is treated anti-
After answering completely, the dense hydrofluoric acid of 2~5mL (HF) and 2~3mL concentrated phosphoric acids are sequentially added, gently shakes polytetrafluoroethylene (PTFE) teflon
Counteracting tank is allowed to mixing, covers cover, is equipped with stent, is put on the sample turntable of microwave dissolver, temperature sensor is inserted
In the main control tank for entering polytetrafluoroethylene (PTFE) teflon counteracting tank, the resolution of program progress bauxite sample is cleared up by table 1；
1 micro-wave digestion program of table
Step 3 waits after the completion of clearing up that standing is cooled to temperature in polytetrafluoroethylene (PTFE) teflon resolution main control tank and is less than 60
After DEG C, the digestion solution prepared in counteracting tank is transferred in 50.00 mL volumetric flasks, is shaken up with ultra-pure water constant volume to be measured；
Step 4, reagent blank experiment：It is placed in polytetrafluoroethylene (PTFE) teflon counteracting tank and adds in ultra-pure water, addition and step
Rapid one addition is identical；Sequentially add 5~8mL concentrated nitric acids (HNO3) and 1~3mL a concentration of 30% hydrogen peroxide（H2O2）,
5min is placed, after complete reaction, the dense hydrofluoric acid of 2~5mL (HF) and 2~3mL concentrated phosphoric acids is sequentially added, gently shakes poly- four
Vinyl fluoride teflon counteracting tank is allowed to mixing, covers cover, is equipped with stent, is put on the sample turntable of microwave dissolver, will
Temperature sensor is inserted into the main control tank of polytetrafluoroethylene (PTFE) teflon counteracting tank, and clearing up program by table 1 carries out, and carries out reagent blank
Resolution；It waits after the completion of clearing up, standing, which is cooled to temperature in polytetrafluoroethylene (PTFE) teflon resolution main control tank, less than after 60 DEG C, will disappear
The digestion solution prepared in solution tank is transferred in 50.00 mL volumetric flasks, is shaken up with ultra-pure water constant volume to be measured；
Step 5 using operating condition of the induced coupled plasma atomic emission spectrometry by setting and selected analytical line, is surveyed successively
Determine standard sequence with Step 3: the made solution to be measured of step 4, sample solution measurement result subtract reagent blank after be sample
Product analysis result.Selected instrument operating condition and standard sequence are as follows：
Instrument：PE 8300V type inductive coupling plasma emission spectrographs；
Inductive coupling plasma emission spectrograph (ICP-OES) sampling system：Hydrofluoric acid resistant；
Inductive coupling plasma emission spectrograph (ICP-OES) operating condition：1300 W of RF power；Cool down gas 15.0
L/min；0.8 L/min of atomization gas flow；0.2 L/min of secondary air amount；Sample introduction flow velocity：1.5 mL/min；Irrigation flow rate：
3.0mL/min；Analytical line：Sc361.383nm.
The preparation of standard series：
Scandium oxide standard reserving solution ρ (Sc2O3The mg/mL of)=1.00 weighs the scandium oxide through 600 DEG C of 2 h of calcination
0.2500g is placed in 250 mL beakers, with dissolving with hydrochloric acid, is moved into 250 mL volumetric flasks, is diluted with water to scale, shakes up.
Standard series：Configuration point takes the scandium oxide standard solution of the 50ug/mL of 0.5 and 5mL in the volumetric flask of 50mL
In, add 5mL concentrated nitric acids (HNO3) and 2mL concentrated phosphoric acids（H3PO4）, then constant volume scale again.It is a concentration of to be configured to scandium oxide
0.5th, the standard sequence of 5 μ g/mL.
In the sample treatment
1st, the usage amount selection of nitric acid
Nitric acid is widely used in the decomposition of sample as a kind of acid with strong oxidizing property.The present invention use proportion for 1.40 it is dense
Nitric acid, result of the test show when the dosage of nitric acid is more than 5mL, you can decompose the scandium in alumina sample ore completely, try
Test result such as table 2.
2 nitric acid usage amount of table is to scandium amount determination influences in bauxite sample
Note：The mass fraction of scandium is 34 × 10 in bauxite standard specimen GBW (E) 070036 selected by experiment-6
2nd, the dosage choice experiment of hydrogen peroxide
Hydrogen peroxide is a kind of strong oxidizer, very strong oxidation, it may have certain solubilization-aid effect, the present invention use
30% hydrogen peroxide, result of the test show when the dosage of 30% hydrogen peroxide is more than 1mL, you can by the scandium energy in alumina sample ore
It decomposes completely, but the dosage for working as hydrogen peroxide increases to 4mL, since reaction is too acutely easy to cause during micro-wave digestion
PTFE（Polytetrafluoroethylene (PTFE)）Teflon counteracting tank explodes, therefore suggests that the dosage of general 30% hydrogen peroxide is no more than 3mL, result of the test
Such as table 3.
3 hydrogen peroxide usage amount of table is to scandium amount determination influences in bauxite sample
Note：The mass fraction of scandium is 34 × 10 in bauxite standard specimen GBW (E) 070036 selected by experiment-6
3rd, the dosage choice experiment of hydrofluoric acid
Hydrofluoric acid has very strong corrosivity, can corrode silicate and generate gaseous ocratation, effectively remove sample
Middle silicate, the present invention use proportion, and for 1.12 dense hydrofluoric acid, result of the test shows to be more than 2mL when the dosage of hydrofluoric acid
When, you can the scandium in alumina sample ore can be decomposed completely, result of the test such as table 4.
4 hydrofluoric acid usage amount of table is to scandium amount determination influences in bauxite sample
Note：The mass fraction of scandium is 34 × 10 in bauxite standard specimen GBW (E) 070036 selected by experiment-6
4th, phosphoric acid dosage is tested
The present invention use proportion for 1.69 concentrated phosphoric acid, when result of the test shows dosage when phosphoric acid more than 2mL,
Scandium in alumina sample ore can be decomposed completely, but after the dosage of phosphoric acid is more than 3mL, since phosphoric acid itself is than great, added
Dosage it is big, leading to prepare the viscosity of digestion solution increases, and can not will prepare digestion solution and be transferred in volumetric flask completely, at the same compared with
Big viscosity, the sample feeding pipe and atomizer for easily causing plasma spectrometer block, therefore select phosphoric acid dosage as 2~3mL, test
As a result such as table 5.
5 phosphoric acid usage amount of table is to scandium amount determination influences in bauxite sample
Note：The mass fraction of scandium is 34 × 10 in bauxite standard specimen GBW (E) 070036 selected by experiment-6
5th, method contrast test
Different bauxite sample ores is weighed, is compared using this method dissolved mineral sample and same sodium hydroxide, sodium peroxide,
It can be obtained by the data result analysis of table 6, the measurement result of this method is the same as there are no significant between alkali fusion measurement result difference, side
Method accuracy meets requirement of experiment, and this method is feasible.
Table 6
6th, method precision is tested
We select bauxite national standard substance GBW (E) 070036, using the molten ore deposit method of tradition and microwave digestion method
5 parallel laboratory tests are carried out to standard substance, the scandium in sample is measured.
Table 7
Microwave Digestion effectively reduces matrix effect it can be seen from 7 data of table, and the precision of method has obtained significantly
Raising.
Claims (5)
1. micro-wave digestion-induced coupled plasma atomic emission spectrometry measures scandium method in bauxite, it is characterised in that includes the following steps：
Step 1 weighs 0.2000~0.3000g bauxite samples to be measured, is placed in polytetrafluoroethylene (PTFE) teflon counteracting tank, adds
Enter and be enough on a small quantity by the ultra-pure water of bauxite sample wetness；
Step 2 fills toward step 1 and 5~8mL concentrated nitric acids and 1~3mL concentration is added in the counteracting tank of wetting shape bauxite sample
For 30% hydrogen peroxide, the bauxite sample cleared up on top tank structure is washed into tank bottom, places 5min, after complete reaction, then successively
The dense hydrofluoric acid of 2~5mL and 2~3mL concentrated phosphoric acids are added in, polytetrafluoroethylene (PTFE) teflon counteracting tank is gently shaken and is allowed to mixing, cover
Cover is equipped with stent, is put on the sample turntable of microwave dissolver, and temperature sensor insertion polytetrafluoroethylene (PTFE) teflon is disappeared
In the main control tank for solving tank, by setting micro-wave digestion program, the resolution of bauxite sample is carried out；The micro-wave digestion program controlled
Cheng Wei：It is warming up to 120 DEG C first, keeps 2min；Then persistently overheating to 180 DEG C, 5min is kept；Finally continue to be warming up to 220
DEG C, keep 10min；Wherein, being warming up to 120 DEG C needs 5min, and being warming up to 180 DEG C needs 5min, is warming up to 220 DEG C of needs
5min；
Step 3 waited after the completion of clearing up, and standing is cooled to after temperature is less than 60 DEG C in polytetrafluoroethylene (PTFE) teflon resolution main control tank,
The digestion solution prepared in counteracting tank is transferred in 50.00 mL volumetric flasks, is shaken up with ultra-pure water constant volume to be measured；
Step 4, reagent blank experiment：It is placed in polytetrafluoroethylene (PTFE) teflon counteracting tank and adds in ultra-pure water, addition and step 1
Addition it is identical；The hydrogen peroxide of 5~8mL concentrated nitric acids and 1~3mL a concentration of 30% are sequentially added, 5min is placed, waits to react
After completely, the dense hydrofluoric acid of 2~5mL and 2~3mL concentrated phosphoric acids are sequentially added, gently shakes polytetrafluoroethylene (PTFE) teflon counteracting tank
Mixing is allowed to, covers cover, is equipped with stent, is put on the sample turntable of microwave dissolver, temperature sensor is inserted into poly- four
In the main control tank of vinyl fluoride teflon counteracting tank, cleared up by setting resolution program；It waits after the completion of clearing up, standing is cooled to poly-
After temperature is less than 60 DEG C in tetrafluoroethene teflon resolution main control tank, the digestion solution prepared in counteracting tank is transferred to 50.00
In mL volumetric flasks, shaken up with ultra-pure water constant volume to be measured；
Step 5 using the solution to be measured that the direct determination step three of induced coupled plasma atomic emission spectrometry and step 4 are made, obtains
Measurement result.
2. micro-wave digestion according to claim 1-induced coupled plasma atomic emission spectrometry measures scandium method in bauxite, special
Sign is：The ultra-pure water used in step 1 meets GB6682-92《The specification and test method of Experiment of Analytical Chemistry room water》
Middle two level water requirement.
3. micro-wave digestion according to claim 1-induced coupled plasma atomic emission spectrometry measures scandium method in bauxite, special
Sign is：Microwave dissolver optimum reagent usage amount is 7~20mL in step 2, therefore concentrated nitric acid, hydrogen peroxide, the dense hydrogen added in
The sum of fluoric acid, concentrated phosphoric acid total volume should be maintained at 10~15mL.
4. micro-wave digestion according to claim 1-induced coupled plasma atomic emission spectrometry measures scandium method in bauxite, special
Sign is：Operating condition and selected analytical line of the inductive coupling plasma emission spectrograph by setting in step 5, successively
Bioassay standard sequence, step 3 and the made solution to be measured of step 4, sample solution measurement result subtract reagent blank after be
Sample analysis result.
5. micro-wave digestion according to claim 1-induced coupled plasma atomic emission spectrometry measures scandium method in bauxite, special
Sign is that selected instrument operating condition is：
Instrument：PE 8300V type inductive coupling plasma emission spectrographs；
Inductive coupling plasma emission spectrograph sampling system：Hydrofluoric acid resistant；
Inductive coupling plasma emission spectrograph operating condition：1300 W of RF power；Cool down 15.0 L/min of gas；Atomization air flow
Measure 0.8 L/min；0.2 L/min of secondary air amount；Sample introduction flow velocity：1.5 mL/min；Irrigation flow rate：3.0mL/min；Analysis
Line：Sc361.383nm；
The preparation of standard series：
The mg/mL of scandium oxide standard reserving solution ρ=1.00 weighs the scandium oxide 0.2500g through 600 DEG C of 2 h of calcination, puts
In 250 mL beakers, with dissolving with hydrochloric acid, move into 250 mL volumetric flasks, be diluted with water to scale, shake up；
Standard series：Configuration point takes the scandium oxide standard solution of the 50ug/mL of 0.5 and 5mL to be mended in the volumetric flask of 50mL
Add 5mL concentrated nitric acids and 2mL concentrated phosphoric acids, then constant volume scale again, be configured to the standard of a concentration of 0.5,5 μ g/mL of scandium oxide
Sequence.
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