CN105067583A - Method for determination of content of lead in chrome ore - Google Patents
Method for determination of content of lead in chrome ore Download PDFInfo
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Abstract
A method for determination of the content of lead in a chrome ore comprises the steps: mixing sodium peroxide with the lead-containing chrome ore in a corundum crucible, melting at the temperature of 600-700 DEG C, then dissolving a precipitate and acidifying the melt with a hydrochloric acid solution and water, diluting with water, mixing evenly, and thus obtaining a sample solution; mixing evenly a hydrochloric acid solution and water with the same volume as that for preparation of the sample solution, to obtain a blank solution; respectively transferring at least five different volumes of lead standard solution with the mass concentration of 0.25 [mu]g/mL in a group of volumetric flasks, adding the blank solution, diluting with water, and thus obtaining the calibration solutions; and finally, testing in an atomic fluorescence spectrometer, to obtain a standard working curve of the calibration solutions, so as to test the content of lead in the chrome ore. With adopting of sodium peroxide to melt the chrome ore, the dissolution time is short, and the determination results are stable; the melting temperature is selected in the range of 600-700 DEG C, so that the sample complete melting can be met, and the molten sample result is stable; and with the calibration solutions as the benchmark, the measurement accuracy is improved.
Description
Technical field
The present invention relates to a kind of chrome ore detection method, particularly the assay method of lead content in a kind of chrome ore.
Background technology
Chrome ore is mainly used in controlling metal working industry, chemical industry and building industry, and can be used to alloying steel, fuel, chemical reagent, fire resistive material etc., is indispensable raw mineral materials in China's basic industries.The explored chrome ore geologic reserve of China occupies the 12nd in the world, belongs to deficient resources.The chrome ore that China uses is based on import, and the place of production comprises the countries and regions such as Africa south, Albania, Turkey, Pakistan, India, Iran, Philippine, Brazil, Australia, Indonesia.
Along with the continuous increase of China's chrome ore trade, product quality is very different, and environmental security is also day by day serious.Plumbous as a kind of harmful element, in smelting, alloy manufacture, not only severe contamination is caused to health and environment, the plasticity of product, impact resistance also can be made to reduce.Therefore, find one fast, plumbous assay method in chrome ore accurately, to promotion environmental protection, improve the quality of products all significant.
About assay method plumbous in chrome ore, there is no relevant report at present.Assay method many employings acid system plumbous in other mineral common is cleared up under normal pressure or microwave high pressure, adopt the analytical instrument such as Atomic absorption, test proves, most of chrome ore acid system is difficult to dissolve, and these common methods are not suitable for mensuration plumbous in chrome ore.
Summary of the invention
Technical matters to be solved by this invention is for the deficiencies in the prior art, provides a kind of reasonable in design, the method for lead content in the chrome ore measured exactly.
Technical matters to be solved by this invention is realized by following technical scheme, and the present invention is the assay method of lead content in a kind of chrome ore, is characterized in, its step is,
(1) preparation of sample solution
Take leaded chrome ore sample 0.2-0.7g, be placed in the corundum crucible of pre-add 0.8-1.2g sodium peroxide, then on sample, cover 0.8-1.2g sodium peroxide, corundum crucible being placed in temperature is melting 15-25min at 600-700 DEG C, takes out, is cooled to normal temperature;
The corundum crucible filling fused mass after cooling is put into beaker, add 45-55mL, temperature is that the hot water of 60 DEG C-100 DEG C embathes fused mass, the fused mass embathed is poured in beaker, and with hydrochloric acid solution and water, the fused mass remained inside and outside corundum crucible is rinsed in beaker, then add 8-12mL hydrochloric acid solution in beaker, dissolution precipitation acidifying, obtain fused mass solution, be cooled to normal temperature, fused mass solution is moved in 100mL volumetric flask, be diluted with water to scale, mixing;
From 100mL volumetric flask, pipette 3-7mL fused mass solution in 50mL volumetric flask, be diluted with water to scale, mixing, obtains sample solution;
(2) preparation of blank solution
Taking the sodium peroxide with step (1) equal in quality, after melting, then according to the step identical with preparing sample solution, obtaining blank solution;
(3) preparation of solution is calibrated
Pipette respectively at least 5 parts of different volumes, mass concentration be the plumbous standard solution of 0.25 μ g/mL in one group of 50mL volumetric flask, in each volumetric flask, all add 8-12mL blank solution, be diluted with water to scale, mixing, obtain calibrate solution;
(4) examination with computer
In atomic fluorescence spectrometer, current-carrying is made with hydrochloric acid solution, solution of potassium borohydride makees reductive agent, with plumbous hollow cathode lamp for excitation source, successively fluorescence intensity test is carried out to calibration solution, sample solution and blank solution, to calibrate the lead concentration of solution for horizontal ordinate, fluorescence intensity is ordinate, draw the standard working curve of calibration solution, again according to the fluorescence intensity that sample solution obtains, with reference to the standard working curve of calibration solution, the lead in sample is carried out quantitatively, thus record content plumbous in chrome ore.
Technical matters to be solved by this invention can also be realized further by following technical scheme, the assay method of lead content in described chrome ore: in the examination with computer described in step (4), fluorescence intensity test negative high voltage be 230-270mV, lamp current is 55-65mA, atomizer height is 6-10mm, assisted gas flow is 380-420mL/min, shield gas flow amount is carried out under being the condition of 700-900mL/min.
Technical matters to be solved by this invention can also be realized further by following technical scheme, the assay method of lead content in described chrome ore: in the sample solution preparation process described in step (1), is accurate to 0.0001g when taking leaded chrome ore sample.
Technical matters to be solved by this invention can also be realized further by following technical scheme, the assay method of lead content in described chrome ore: in the sample solution preparation process described in step (1), hydrochloric acid solution used is for being that 2:3-4:1 is formulated by concentrated hydrochloric acid and water according to volume ratio.
Technical matters to be solved by this invention can also be realized further by following technical scheme, the assay method of lead content in described chrome ore: in the examination with computer described in step (4), hydrochloric acid solution used is for being that 1:199-1:49 is formulated by concentrated hydrochloric acid and water according to volume ratio.
Technical matters to be solved by this invention can also be realized further by following technical scheme, the assay method of lead content in described chrome ore: in the sample solution preparation process described in step (1), rinses and fills that the corundum crucible of fused mass hydrochloric acid solution used is 10-14mL, water is 5-10mL.
Technical matters to be solved by this invention can also be realized further by following technical scheme, the assay method of lead content in described chrome ore: in the examination with computer described in step (4), and the concentration of described solution of potassium borohydride is 10-25g/L.
Compared with prior art, the present invention adopts sodium peroxide chrome ore, easily operates, and dissolution time is short, and measurement result is stablized; Melt temperature is selected at 600-700 DEG C, solves the too short and melting of molten sample time incomplete, long, lose time and the problem of the energy, will melt sample time controling at 20min, and sample melted can be met complete, and melt sample result stable; If blank solution, get rid of the impact of experiment agents useful for same, improve the precision measured, if calibration solution, as a benchmark of the fluorescence intensity of sample solution, the solution environmental of solution environmental and the sample solution of calibration solution is close, ensures the stability of mensuration, it is reasonable in design, improves quantitative accuracy plumbous in chrome ore.
Accompanying drawing explanation
Fig. 1 is the standard working curve figure of embodiment 14 alignment solution.
Embodiment
Further describe concrete technical scheme of the present invention, so that those skilled in the art understands the present invention further, and do not form the restriction to its right.
Embodiment 1, the assay method of lead content in a kind of chrome ore, its step is,
(1) preparation of sample solution
Take leaded chrome ore sample 0.2g, be placed in the corundum crucible of pre-add 0.8g sodium peroxide, then on sample, cover 0.8g sodium peroxide, corundum crucible being placed in temperature is melting 15min at 600 DEG C, takes out, is cooled to normal temperature;
The corundum crucible filling fused mass after cooling is put into beaker, add 45mL, temperature is that the hot water of 60 DEG C embathes fused mass, the fused mass embathed is poured in beaker, and with hydrochloric acid solution and water, the fused mass remained inside and outside corundum crucible is rinsed in beaker, then add 8-12mL hydrochloric acid solution in beaker, dissolution precipitation acidifying, obtain fused mass solution, be cooled to normal temperature, fused mass solution is moved in 100mL volumetric flask, be diluted with water to scale, mixing;
From 100mL volumetric flask, pipette 3mL fused mass solution in 50mL volumetric flask, be diluted with water to scale, mixing, obtains sample solution;
(2) preparation of blank solution
Taking the sodium peroxide with step (1) equal in quality, after melting, then according to the step identical with preparing sample solution, obtaining blank solution;
(3) preparation of solution is calibrated
Pipette respectively 0mL, 5mL, 10mL, 15mL, 20mL, 25mL mass concentration be the plumbous standard solution of 0.25 μ g/mL in one group of 50mL volumetric flask, in each volumetric flask, all add 8mL blank solution, be diluted with water to scale, mixing, obtain calibrate solution;
(4) examination with computer
In atomic fluorescence spectrometer, current-carrying is made with hydrochloric acid solution, solution of potassium borohydride makees reductive agent, with plumbous hollow cathode lamp for excitation source, successively fluorescence intensity test is carried out to calibration solution, sample solution and blank solution, to calibrate the lead concentration of solution for horizontal ordinate, fluorescence intensity is ordinate, draw the standard working curve of calibration solution, again according to the fluorescence intensity that sample solution obtains, with reference to the standard working curve of calibration solution, the lead in sample is carried out quantitatively, thus record content plumbous in chrome ore.
Embodiment 2, the assay method of lead content in a kind of chrome ore, its step is,
(1) preparation of sample solution
Take leaded chrome ore sample 0.7g, be placed in the corundum crucible of pre-add 1.2g sodium peroxide, then on sample, cover 1.2g sodium peroxide, corundum crucible being placed in temperature is melting 25min at 700 DEG C, takes out, is cooled to normal temperature;
The corundum crucible filling fused mass after cooling is put into beaker, add 45mL, temperature is that the hot water of 100 DEG C embathes fused mass, the fused mass embathed is poured in beaker, and with hydrochloric acid solution and water, the fused mass remained inside and outside corundum crucible is rinsed in beaker, then add 12mL hydrochloric acid solution in beaker, dissolution precipitation acidifying, obtain fused mass solution, be cooled to normal temperature, fused mass solution is moved in 100mL volumetric flask, be diluted with water to scale, mixing;
From 100mL volumetric flask, pipette 7mL fused mass solution in 50mL volumetric flask, be diluted with water to scale, mixing, obtains sample solution;
(2) preparation of blank solution
Taking the sodium peroxide with step (1) equal in quality, after melting, then according to the step identical with preparing sample solution, obtaining blank solution;
(3) preparation of solution is calibrated
Move respectively 1mL, 3mL, 5mL, 7mL, 9mL, 11mL mass concentration be the plumbous standard solution of 0.25 μ g/mL in one group of 50mL volumetric flask, in each volumetric flask, all add 12mL blank solution, be diluted with water to scale, mixing, obtain calibrate solution;
(4) examination with computer
In atomic fluorescence spectrometer, current-carrying is made with hydrochloric acid solution, solution of potassium borohydride makees reductive agent, with plumbous hollow cathode lamp for excitation source, successively fluorescence intensity test is carried out to calibration solution, sample solution and blank solution, to calibrate the lead concentration of solution for horizontal ordinate, fluorescence intensity is ordinate, draw the standard working curve of calibration solution, again according to the fluorescence intensity that sample solution obtains, with reference to the standard working curve of calibration solution, the lead in sample is carried out quantitatively, thus record content plumbous in chrome ore.
Embodiment 3, the assay method of lead content in chrome ore described in embodiment 1: in the examination with computer described in step (4), fluorescence intensity test negative high voltage be 230mV, lamp current is 55mA, atomizer height is 6mm, assisted gas flow is 380mL/min, shield gas flow amount is carried out under being the condition of 700mL/min.
Embodiment 4, the assay method of lead content in chrome ore described in embodiment 1: in the examination with computer described in step (4), fluorescence intensity test negative high voltage be 270mV, lamp current is 65mA, atomizer height is 10mm, assisted gas flow is 420mL/min, shield gas flow amount is carried out under being the condition of 900mL/min.
Embodiment 5, the assay method of lead content in chrome ore described in embodiment 1: in the examination with computer described in step (4), fluorescence intensity test negative high voltage be 250mV, lamp current is 60mA, atomizer height is 7mm, assisted gas flow is 400mL/min, shield gas flow amount is carried out under being the condition of 800mL/min.
Embodiment 6, the assay method of lead content in the chrome ore described in embodiment 1: in the sample solution preparation process described in step (1), is accurate to 0.0001g when taking leaded chrome ore sample.
Embodiment 7, the assay method of lead content in the chrome ore described in embodiment 1: in the sample solution preparation process described in step (1), hydrochloric acid solution used is for being that 2:3 is formulated by concentrated hydrochloric acid and water according to volume ratio.
Embodiment 8, the assay method of lead content in the chrome ore described in embodiment 1: in the sample solution preparation process described in step (1), hydrochloric acid solution used is for being that 4:1 is formulated by concentrated hydrochloric acid and water according to volume ratio.
Embodiment 9, the assay method of lead content in the chrome ore described in embodiment 1: in the examination with computer described in step (4), hydrochloric acid solution used is for being that 1:199 is formulated by concentrated hydrochloric acid and water according to volume ratio.
Embodiment 10, the assay method of lead content in the chrome ore described in embodiment 1: in the examination with computer described in step (4), hydrochloric acid solution used is for being that 1:49 is formulated by concentrated hydrochloric acid and water according to volume ratio.
Embodiment 11, the assay method of lead content in the chrome ore described in embodiment 1: in the sample solution preparation process described in step (1), rinses and fills that the corundum crucible of fused mass hydrochloric acid solution used is 10mL, water is 5mL.
Embodiment 12, the assay method of lead content in the chrome ore described in embodiment 1: in the sample solution preparation process described in step (1), rinses and fills that the corundum crucible of fused mass hydrochloric acid solution used is 14mL, water is 10mL.
Embodiment 13, the assay method of lead content in the chrome ore described in embodiment 1: in the sample solution preparation process described in step (1), rinses and fills that the corundum crucible of fused mass hydrochloric acid solution used is 12mL, water is 7mL.
Embodiment 14, have chosen 26 the chrome ore samples of year April in September, 2014 to 2015 by the different importers of port, Lianyun Harbour import, different grade, and application this law is tested, and measure the content of its lead, its step is as follows,
1 test portion
1.1 instruments and reagent
1.1.1 instrument is selected: the atomic fluorescence spectrometer of Beijing Ji Tian company, model: AFS-9230;
1.1.2 reagent is selected: sodium peroxide, hydrochloric acid (ρ 1.19g/mL), hydrochloric acid solution, potassium hydroxide solution (10g/L), potassium ferricyanide solution (15g/L), solution of potassium borohydride (20g/L, take 20g potassium borohydride to be dissolved in 1000mL potassium hydroxide and potassium ferricyanide solution), plumbous standard solution (0.25 μ g/mL), corundum crucible 30mL;
The preparation of 1.2 samples
Should all by diameter 0.10mm(150 order by sample ore) standard sieve, choose the dry 1.5h of exsiccator that the sample ore leaked down is placed in 105 DEG C, be cooled to room temperature, for subsequent use as sample;
1.3 experimental technique
(1) preparation of sample solution
Take leaded chrome ore sample 0.5g, be placed in the corundum crucible of pre-add 1.0g sodium peroxide, then on sample, cover 1.0g sodium peroxide, corundum crucible being placed in temperature is melting 20min at 650 DEG C, takes out, is cooled to normal temperature;
The corundum crucible filling fused mass after cooling is put into beaker, add 50mL, temperature is that the hot water of 80 DEG C embathes fused mass, the fused mass embathed is poured in the beaker of 250mL, and be that the fused mass that corundum crucible inside and outside remain rinse in beaker by 1:1 formulated hydrochloric acid solution and 10mL water by concentrated hydrochloric acid and water according to volume ratio with 12mL, 10mL hydrochloric acid solution is added again in beaker, dissolution precipitation acidifying, obtain fused mass solution, be cooled to normal temperature, fused mass solution is moved in 100mL volumetric flask, be diluted with water to scale, mixing;
From 100mL volumetric flask, pipette 5mL fused mass solution in 50mL volumetric flask, be diluted with water to scale, mixing, obtains sample solution;
(2) preparation of blank solution
Taking the sodium peroxide with step (1) equal in quality, after melting, then according to the step identical with preparing sample solution, obtaining blank solution;
(3) preparation of solution is calibrated
Move respectively 0mL, 2mL, 4mL, 6mL, 8mL, 10mL mass concentration be the plumbous standard solution of 0.25 μ g/mL in one group of 50mL volumetric flask, in each volumetric flask, all add 10mL blank solution, be diluted with water to scale, mixing, obtain calibrate solution;
(4) examination with computer
In atomic fluorescence spectrometer, with being that the formulated hydrochloric acid solution of 1:99 makes current-carrying by concentrated hydrochloric acid and water according to volume ratio, the solution of potassium borohydride (containing the potassium hydroxide solution of 10g/L and the potassium ferricyanide solution of 15g/L) of 20g/L makees reductive agent, with plumbous hollow cathode lamp for excitation source, successively fluorescence intensity test is carried out to calibration solution, sample solution and blank solution, to calibrate the lead concentration of solution for horizontal ordinate, fluorescence intensity is ordinate, draw the standard working curve of calibration solution, content plumbous in chrome ore.
Under selected instrument condition of work, with concentration value
c(μ g/L) is horizontal ordinate, fluorescence intensity level
ifor ordinate, enter to measure to standard solution, drawing standard working curve, with reference to Fig. 1; Linear equation is:
i=132.0321 ×
c+ 17.0887, its related coefficient is 0.9998; Again according to the fluorescence intensity that sample solution obtains, with reference to the standard working curve of calibration solution, the lead in sample is carried out quantitatively, thus record from the chrome ore lead content scope of port, Lianyun Harbour import at 0.18 μ g/g-298.35 μ g/g.
Under the condition that experiment is selected, selected sample solution replicate determination 11 times, using the standard deviation of 3 times of concentration values as method detection limit, the method for calculating detects and is limited to 0.1ug/L, and corresponding to solid sample is 0.2ug/g.
The multiple molten sample loading mode due to laboratory examination, adopting hydrochloric acid-nitrate acid and hydrofluoric acid to add pressure at normal pressure and microwave all can not be complete by sample dissolution.Adopt sulfuric-phosphoric-perchloric acid-hydrofluorite to be heated to 230 DEG C at closed container sample segment to be cleared up, the corrosion-resistant requirement of the heat resisting and pressure resisting of this condition to instrument is higher, has certain risk.Select sodium peroxide, easily operate, melt the time short, measurement result is stablized.
The boiling point of sodium oxide molybdena is 657 DEG C, molten sample temperature is too low, sample can not be melted completely, and molten sample temperature is too high, the easy splash of sample, this law is by the molten sample thermal creep stress of test at 650 DEG C, and the molten sample time is too short, and melting is incomplete, long, lose time and the energy, to melt sample time controling at 20min, and can meet sample melted complete, molten sample result is stablized.
The present invention adopts method of the present invention to measure carrying out plumbous in chrome ore, and accuracy is high, precision good; Carry out recovery testu according to step of the present invention, the recovery is between 96.4%-105.3%; To the sample determination of lead element different content, relative standard deviation (n=11) is 1.47%-3.68%, and the method detection limit reaches 0.1ug/L.
Claims (7)
1. the assay method of lead content in chrome ore, is characterized in that: its step is,
(1) preparation of sample solution
Take leaded chrome ore sample 0.2-0.7g, be placed in the corundum crucible of pre-add 0.8-1.2g sodium peroxide, then on sample, cover 0.8-1.2g sodium peroxide, corundum crucible being placed in temperature is melting 15-25min at 600-700 DEG C, takes out, is cooled to normal temperature;
The corundum crucible filling fused mass after cooling is put into beaker, add 45-55mL, temperature is that the hot water of 60 DEG C-100 DEG C embathes fused mass, the fused mass embathed is poured in beaker, and with hydrochloric acid solution and water, the fused mass remained inside and outside corundum crucible is rinsed in beaker, then add 8-12mL hydrochloric acid solution in beaker, dissolution precipitation acidifying, obtain fused mass solution, be cooled to normal temperature, fused mass solution is moved in 100mL volumetric flask, be diluted with water to scale, mixing;
From 100mL volumetric flask, pipette 3-7mL fused mass solution in 50mL volumetric flask, be diluted with water to scale, mixing, obtains sample solution;
(2) preparation of blank solution
Taking the sodium peroxide with step (1) equal in quality, after melting, then according to the step identical with preparing sample solution, obtaining blank solution;
(3) preparation of solution is calibrated
Pipette respectively at least 5 parts of different volumes, mass concentration be the plumbous standard solution of 0.25 μ g/mL in one group of 50mL volumetric flask, in each volumetric flask, all add 8-12mL blank solution, be diluted with water to scale, mixing, obtain calibrate solution;
(4) examination with computer
In atomic fluorescence spectrometer, current-carrying is made with hydrochloric acid solution, solution of potassium borohydride makees reductive agent, with plumbous hollow cathode lamp for excitation source, successively fluorescence intensity test is carried out to calibration solution, sample solution and blank solution, to calibrate the lead concentration of solution for horizontal ordinate, fluorescence intensity is ordinate, draw the standard working curve of calibration solution, again according to the fluorescence intensity that sample solution obtains, with reference to the standard working curve of calibration solution, the lead in sample is carried out quantitatively, thus record content plumbous in chrome ore.
2. the assay method of lead content in chrome ore according to claim 1, it is characterized in that: in the examination with computer described in step (4), fluorescence intensity test negative high voltage be 230-270mV, lamp current is 55-65mA, atomizer height is 6-10mm, assisted gas flow is 380-420mL/min, shield gas flow amount is carried out under being the condition of 700-900mL/min.
3. the assay method of lead content in chrome ore according to claim 1, is characterized in that: in the sample solution preparation process described in step (1), is accurate to 0.0001g when taking leaded chrome ore sample.
4. the assay method of lead content in chrome ore according to claim 1, is characterized in that: in the sample solution preparation process described in step (1), and hydrochloric acid solution used is for being that 2:3-4:1 is formulated by concentrated hydrochloric acid and water according to volume ratio.
5. the assay method of lead content in chrome ore according to claim 1, is characterized in that: in the examination with computer described in step (4), and hydrochloric acid solution used is for being that 1:199-1:49 is formulated by concentrated hydrochloric acid and water according to volume ratio.
6. the assay method of lead content in chrome ore according to claim 1, is characterized in that: in the sample solution preparation process described in step (1), rinses that the corundum crucible that fills fused mass hydrochloric acid solution used is 10-14mL, water is 5-10mL.
7. the assay method of lead content in chrome ore according to claim 1, it is characterized in that: in the examination with computer described in step (4), the concentration of described solution of potassium borohydride is 10-25g/L.
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