CN107561061A - The assay method of potassium sodium Pb, Zn content in a kind of iron ore - Google Patents
The assay method of potassium sodium Pb, Zn content in a kind of iron ore Download PDFInfo
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- CN107561061A CN107561061A CN201710728782.4A CN201710728782A CN107561061A CN 107561061 A CN107561061 A CN 107561061A CN 201710728782 A CN201710728782 A CN 201710728782A CN 107561061 A CN107561061 A CN 107561061A
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Abstract
The present invention discloses a kind of assay method of potassium sodium Pb, Zn content in iron ore, and it includes：It is dissolved in after iron ore is decomposed with hydrofluoric acid, hydrochloric acid and perchloric acid in nitric acid medium, potassium sodium Pb, Zn content is determined using ICP plasma spectroscopies simultaneously.Using the assay method simple and fast, the range of linearity is wider, and agents useful for same is less, and interference is few, and analyze speed is fast, high sensitivity, and precision is good, and the degree of accuracy is high, meets the demand of research and production.
Description
Technical field
The present invention relates to metallurgical analysis field, the assay method of potassium sodium Pb, Zn content in more particularly to a kind of iron ore.
Background technology
With the maturation of modern smelting process for production, it is increasingly recognised that these four elements of potassium sodium lead zinc in iron ore
There is larger harm to blast furnace lining furnace bottom and smelting process, thus to the detection of four kinds of constituent contents of potassium sodium lead zinc in iron ore
Also element must be examined by turning into, while also turn into one of requirement when raw materials for production are settled accounts.
Through consulting normative document data, the method for determining potassium sodium in iron ore has atomic absorption spectrography (AAS), ICP plasmas
Spectroscopic methodology, X fluorescence spectrum method.The method of lead zinc has atomic absorption spectrography (AAS), scholar's ripple polarography, ICP plasmas in measure iron ore
Spectroscopic methodology, X fluorescence spectrum method.Wherein, enterprise's mark Q/BGJH-04-214-2008 atomic absorption spectroscopy determination potassium sodium lead zinc
It is to be extracted using hydrochloric acid, hydrofluoric acid, the molten sample of the acid of perchloric acid three, nitric acid, machine measurement absorbance on pure water constant volume.The linear model of this method
Enclose relative narrower, when measuring four kinds of elements can only one by one element determination thus time of measuring it is longer.Lu Yanrong etc. patent
Potassium lead zinc is in Muffle furnace 950~1000 using sodium carbonate-sodium tetraborate mixed flux in ICP plasma spectroscopies measurement iron ore
DEG C molten sample, acid extraction then upper machine measure.Thus this method can not measure sodium element content in iron ore simultaneously.National standard method
Potassium sodium hydrochloric acid hydrofluoric acid dissolution sample in GB 6730.49-1986 measurement iron ores, uses atomic absorption light in hydrochloric acid medium
Spectrometry measures, and measurement range K2O, Na2O is 0.005~1.50%.National standard method GB/T 6730.53-2004 and
GB/T 6730.54-2004 measure zinc in iron ore, lead content respectively, and with hydrochloric acid hydrofluoric acid dissolution sample, nitric acid oxidation, cigarette
Sour dissolved salts, filtering, MIBK extract and separate iron is used after handling residue, nitric acid destroys MIBK, dissolving with hydrochloric acid salt, inhaled in atom
Receive spectrophotometer measurement.This method data are accurate but flow is longer and largely uses MIBK reagents, and the reagent belongs to low toxicity
Class organic reagent, to personnel, environmental effects.Measurement range Pb：0.001~0.500%, Zn：0.001~0.5%.
The content of the invention
In view of this, the present invention provides a kind of assay method of potassium sodium Pb, Zn content in iron ore.
The present invention provides a kind of assay method of potassium sodium Pb, Zn content in iron ore, and it includes：
It is dissolved in after iron ore is decomposed with hydrofluoric acid, hydrochloric acid and perchloric acid in nitric acid medium, using ICP plasma lights
Spectrometry determines potassium sodium Pb, Zn content simultaneously.
Further, it is described iron ore is decomposed with hydrofluoric acid, hydrochloric acid and perchloric acid after be dissolved in nitric acid medium and be specially：
Weigh iron ore sample 0.1000g to be placed in 250mL polytetrafluoroethylene beakers, it is 1.13g/mL's to add 5mL concentration
Hydrofluoric acid, 10mL concentration is 1.19g/mL hydrochloric acid, after low-temperature heat decomposes sample, adds the height that 2mL concentration is 1.68g/mL
Chloric acid, continue to heat, make perchloric acid smoke cooling, add 5mL nitric acid and salt to dissolve nature and be cooled to below residual volume 1mL
After room temperature, it is transferred in 100mL volumetric flasks, is diluted to scale with pure water, shakes up.
Further, it is described to determine potassium sodium Pb, Zn content simultaneously using ICP plasma spectroscopies and be specially：
Prepare the standard liquid that the lead of sodium containing potassium zinc is following content：0%th, 0.005%, 0.010%, 0.050%,
0.100%th, 0.500%, 1.00%, 5.00%, 10.00%；
The spectrum line for selecting the element of K, Na, Pb, Zn tetra- be respectively 766.490nm, 589.592nm, 220.353nm,
The potassium sodium lead Zinc standard solution prepared is introduced Inductively coupled plasma optical emission spectrometer and surveyed by 202.548nm as analytical line
Fixed elemental signals intensity to be measured, using elemental signals intensity to be measured as ordinate, mass of ion percentage is abscissa, draws standard
Solution working curve；
Sample solution and blank solution are introduced into Inductively coupled plasma optical emission spectrometer and measure elemental signals intensity to be measured,
The mass percent of potassium sodium lead Zn-ef ficiency is obtained by the standard liquid working curve of known quality percentage；Calculation formula is as follows：W
(%)=Wi-W0
In formula, W is the weight/mass percentage composition of element in the sample；Wi is mass percent of the element in testing sample；
W0For mass percent of the element in blank solution to be measured.
Further, the assay method potassium sodium lead zinc measurement scope is as follows：K2O：0.005~10.00%, Na2O：
0.005~10.00%, Pb：0.005~10.00%, Zn：0.001~10.00%.
The beneficial effect of the assay method of potassium sodium Pb, Zn content is in a kind of iron ore provided by the invention：
1) iron ore standard specimen of the selection without potassium sodium lead zinc is as bottoming matrix, preparing standard solution working curve, to disappear
Except matrix element disturbs, make measurement result more accurate.
2) four kinds of constituent contents of potassium sodium lead zinc in iron ore are determined simultaneously using ICP ICPs, it is easy to operate quick,
Operating cost is low.
3) the inventive method agents useful for same is less, thus has fewer environmental impacts；The range of linearity is wider, and interference is few, accurate
Spend, the degree of accuracy is high.Measure relative standard deviation and be less than 5%, the rate of recovery is between 96~104.3%.
Embodiment
The invention discloses a kind of assay method of potassium sodium Pb, Zn content in iron ore, those skilled in the art can use for reference this
Literary content, it is suitably modified technological parameter realization.In particular, all similar replacements and change are to art technology
It is it will be apparent that they are considered as being included in the present invention for personnel.The method of the present invention and application are by preferable
Embodiment is described, related personnel substantially can not depart from present invention, in spirit and scope to side as described herein
Method and application are modified or suitably changed with combining, to realize and using the technology of the present invention.
The present invention provides a kind of assay method of potassium sodium Pb, Zn content in iron ore, and it includes：
It is dissolved in after iron ore is decomposed with hydrofluoric acid, hydrochloric acid and perchloric acid in nitric acid medium, using ICP plasma lights
Spectrometry determines potassium sodium Pb, Zn content simultaneously.
Further, it is described iron ore is decomposed with hydrofluoric acid, hydrochloric acid and perchloric acid after be dissolved in nitric acid medium and be specially：
Weigh iron ore sample 0.1000g to be placed in 250mL polytetrafluoroethylene beakers, it is 1.13g/mL's to add 5mL concentration
Hydrofluoric acid, 10mL concentration is 1.19g/mL hydrochloric acid, after low-temperature heat decomposes sample, adds the height that 2mL concentration is 1.68g/mL
Chloric acid, continue to heat, make perchloric acid smoke cooling, add 5mL nitric acid and salt to dissolve nature and be cooled to below residual volume 1mL
After room temperature, it is transferred in 100mL volumetric flasks, is diluted to scale with pure water, shakes up.
Further, it is described to determine potassium sodium Pb, Zn content simultaneously using ICP plasma spectroscopies and be specially：
Prepare the standard liquid that the lead of sodium containing potassium zinc is following content：0%th, 0.005%, 0.010%, 0.050%,
0.100%th, 0.500%, 1.00%, 5.00%, 10.00%；
The spectrum line for selecting the element of K, Na, Pb, Zn tetra- be respectively 766.490nm, 589.592nm, 220.353nm,
The potassium sodium lead Zinc standard solution prepared is introduced Inductively coupled plasma optical emission spectrometer and surveyed by 202.548nm as analytical line
Fixed elemental signals intensity to be measured, using elemental signals intensity to be measured as ordinate, mass of ion percentage is abscissa, draws standard
Solution working curve；
Sample solution and blank solution are introduced into Inductively coupled plasma optical emission spectrometer and measure elemental signals intensity to be measured,
The mass percent of potassium sodium lead Zn-ef ficiency is obtained by the standard liquid working curve of known quality percentage；Calculation formula is as follows：W
(%)=Wi-W0
In formula, W is the weight/mass percentage composition of element in the sample；Wi is mass percent of the element in testing sample；
W0 is mass percent of the element in blank solution to be measured.
In said determination method provided by the invention, potassium sodium lead zinc measurement scope is as follows：K2O：0.005~10.00%,
Na2O：0.005~10.00%, Pb：0.005~10.00%, Zn：0.001~10.00%.
The present invention provides a kind of assay method of potassium sodium Pb, Zn content in iron ore, and this method is by iron ore sample hydrochloric acid hydrogen
Fluoric acid perchloric acid is decomposed, and potassium sodium Pb, Zn content can be determined simultaneously using ICP plasma spectroscopies in nitric acid medium.Analysis method
Simple and fast, the range of linearity is wider, and agents useful for same is less, and interference is few, and analyze speed is fast, high sensitivity, and precision is good, the degree of accuracy
Height, meet the demand of research and production.
The present invention is a kind of assay method of potassium sodium lead Zn-ef ficiency content in iron ore, is specifically completed by following steps：Claim sample
→ dissolving → extraction, constant volume → upper machine measure.
The beneficial effect of the assay method of potassium sodium Pb, Zn content is in a kind of iron ore provided by the invention：
1) iron ore standard specimen of the selection without potassium sodium lead zinc is as bottoming matrix, preparing standard solution working curve, to disappear
Except matrix element disturbs, make measurement result more accurate.
2) four kinds of constituent contents of potassium sodium lead zinc in iron ore are determined simultaneously using ICP ICPs, it is easy to operate quick,
Operating cost is low.
3) the inventive method agents useful for same is less, thus has fewer environmental impacts；The range of linearity is wider, and interference is few, accurate
Spend, the degree of accuracy is high.Measure relative standard deviation and be less than 5%, the rate of recovery is between 96~104.3%.
With reference to embodiment, the present invention is expanded on further：
Embodiment
1st, method summary
Weigh iron ore sample 0.1000g to be placed in 250mL polytetrafluoroethylene beakers, hydrogenation fluoric acid hydrochloric acid low-temperature heat makes
After sample decomposes, increase chloric acid and continue to heat, make perchloric acid smoke to below residual volume 1mL, it is slightly cold, add nitric acid to make salt
Dissolving, after being cooled to room temperature naturally, is transferred in 100mL volumetric flasks, is diluted to scale with pure water, shakes up.Determined using ICP-AES methods
The constituent content of potassium sodium lead zinc four.
2nd, analyrical reagent, standard liquid, instrument are prepared.
2.1 hydrochloric acid (ρ 1.19, GR), hydrofluoric acid (ρ 1.13, GR), perchloric acid (ρ 1.68, GR), nitric acid (2+3, GR), by than
Example is prepared with pure water；
2.2 experimental waters are two level pure water
2.3 potassium sodium lead Zinc standard solutions：With 1000 μ g/mL potassium sodium lead Zinc standard solution (in national ferrous materials test
Heart Iron and Steel Research Geueral Inst), it is diluted to 100.0 μ g/mL, 10.0 μ g/mL, 1.0 μ g/mL standard liquid step by step respectively.
2.4 key instruments and test condition
2.4.1 PE companies in the U.S. produce, Optima5300DV inductively-coupled plasma spectrometers.
2.4.2 instrument parameter：See running parameter table 1：
The inductively-coupled plasma spectrometer running parameter of table 1
2.4.3 the analysis of line wavelength of the element of K, Na, Pb, Zn tetra- using 766.490nm, 589.592nm, 220.353nm,
202.548nm。
3rd, determine
3.1 analytical procedure
Weigh iron ore sample 0.1000g to be placed in 250mL polytetrafluoroethylene beakers, add 5mL hydrofluoric acid (ρ 1.13),
10mL hydrochloric acid (ρ 1.19), after low-temperature heat decomposes sample, add 2mL perchloric acid (ρ 1.68), continue to heat, make perchloric acid smoke
It is slightly cold to below residual volume 1mL, after adding 5mL nitric acid (2+3), salt dissolving nature to be cooled to room temperature, it is transferred to 100mL volumetric flasks
In, scale is diluted to pure water, is shaken up.Reagent blank is done in company with sample.
The preparation of 3.2 working curve standard liquids
In nine 250mL polytetrafluoroethylene beakers, weigh iron ore standard specimens of eight parts of 0.1000g without potassium sodium lead zinc and make
For bottoming matrix (not weighing bottoming standard specimen in a beaker, be blank), by the acid adding of analytical procedure 3.1 carry out sample decomposition,
Perchloric acid smoked, nitric acid (2+3) dissolved salts, are cooled to after room temperature and shift respectively in nine 100mL plastics volumetric flasks, Ran Houfen
Potassium sodium lead Zinc standard solution is not taken in nine 100mL volumetric flasks, it is dilute to scale with pure water, shake up.It is configured to the lead zinc of sodium containing potassium
For the working curve of the standard liquid of following content：
0%th, 0.005%, 0.010%, 0.050%, 0.100%, 0.500%, 1.00%, 5.00%, 10.00%.
3.3 use ICP-AES method determination sample potassium sodium Pb, Zn contents
With reference to the modulating apparatus condition of running parameter table 1, the spectrum line for selecting the element of K, Na, Pb, Zn tetra- is respectively
As analytical line, the potassium sodium lead zinc standard that 3.2 are prepared is molten by 766.490nm, 589.592nm, 220.353nm, 202.548nm
Liquid introduces Inductively coupled plasma optical emission spectrometer and determines elemental signals intensity to be measured, is sat using elemental signals intensity to be measured to be vertical
Mark, mass of ion percentage is abscissa, draws standard liquid working curve.
Sample solution and blank solution are introduced into Inductively coupled plasma optical emission spectrometer and measure elemental signals intensity to be measured,
The mass percent of potassium sodium lead Zn-ef ficiency is obtained by the standard liquid working curve of known quality percentage.
3.4W (tested component) (%)=Wi-W0
In formula：W is the weight/mass percentage composition of element in the sample；Wi is mass percent of the element in testing sample；
W0For mass percent of the element in blank solution to be measured.
4 preci-sion and accuracies are tested
To 1# samples, 2# samples, empirically method measures the precision test of 11 times.Analysis result is shown in Table 2.
The precision test result of table 2
Accuracy test is carried out to three standards for iron ore materials according to the inventive method, while uses atom absorption method
(AAS) accuracy test contrasted has been made, have also been made mark-on reclaims experiment, experimental result is shown in Table 3.
The accuracy test result of table 3
Note：* the value marked is less than the inventive method analysis lower limit.
5th, conclusion
It can be seen from table 2,3 method of testing relative standard deviation provided by the invention be less than 5%, standard specimen measured value with
Standard value is consistent；It is consistent with atom absorption method measured value；Recovery of standard addition is between 96~104.3%.Thus this hair
Bright method has higher precision and the preferable degree of accuracy, great application value.
Described above is only the preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, under the premise without departing from the principles of the invention, some improvements and modifications can also be made, these improvements and modifications also should
It is considered as protection scope of the present invention.
Claims (4)
- A kind of 1. assay method of potassium sodium Pb, Zn content in iron ore, it is characterised in that including：It is dissolved in after iron ore is decomposed with hydrofluoric acid, hydrochloric acid and perchloric acid in nitric acid medium, it is same using ICP plasma spectroscopies When determine potassium sodium Pb, Zn content.
- 2. the assay method of potassium sodium Pb, Zn content in iron ore according to claim 1, it is characterised in that described by iron ore Being dissolved in nitric acid medium after being decomposed with hydrofluoric acid, hydrochloric acid and perchloric acid is specially：Weigh iron ore sample 0.1000g to be placed in 250mL polytetrafluoroethylene beakers, add the hydrogen fluorine that 5mL concentration is 1.13g/mL Acid, 10mL concentration is 1.19g/mL hydrochloric acid, after low-temperature heat decomposes sample, adds the perchloric acid that 2mL concentration is 1.68g/mL, Continue to heat, make perchloric acid smoke cooling, add 5mL nitric acid and salt to dissolve nature and be cooled to room temperature to below residual volume 1mL Afterwards, it is transferred in 100mL volumetric flasks, is diluted to scale with pure water, shakes up.
- 3. the assay method of potassium sodium Pb, Zn content in iron ore according to claim 1, it is characterised in that described to use ICP Plasma spectroscopy determines potassium sodium Pb, Zn content simultaneously：Prepare the standard liquid that the lead of sodium containing potassium zinc is following content：0%th, 0.005%, 0.010%, 0.050%, 0.100%, 0.500%th, 1.00%, 5.00%, 10.00%；The spectrum line for selecting the element of K, Na, Pb, Zn tetra- is respectively that 766.490nm, 589.592nm, 220.353nm, 202.548nm make For analytical line, the potassium sodium lead Zinc standard solution prepared is introduced into Inductively coupled plasma optical emission spectrometer and determines element letter to be measured Number intensity, using elemental signals intensity to be measured as ordinate, mass of ion percentage is abscissa, and it is bent to draw standard liquid work Line；Sample solution and blank solution are introduced into Inductively coupled plasma optical emission spectrometer and measure elemental signals intensity to be measured, by Know that the standard liquid working curve of mass percent obtains the mass percent of potassium sodium lead Zn-ef ficiency；Calculation formula is as follows：W (%) =Wi-W0In formula, W is the weight/mass percentage composition of element in the sample；Wi is mass percent of the element in testing sample；W0For member Mass percent of the element in blank solution to be measured.
- 4. the assay method of potassium sodium Pb, Zn content in the iron ore according to claims 1 to 3 any one, it is characterised in that The assay method potassium sodium lead zinc measurement scope is as follows：K2O：0.005~10.00%, Na2O：0.005~10.00%, Pb： 0.005~10.00%, Zn：0.001~10.00%.
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| CN108627374A (en) * | 2018-04-25 | 2018-10-09 | 山西建龙实业有限公司 | The assay method of Zn content in a kind of iron ore |
| CN111829864A (en) * | 2020-01-15 | 2020-10-27 | 包头钢铁（集团）有限责任公司 | Method for measuring contents of potassium, sodium, lead, zinc and copper in serpentine |
| CN113252644A (en) * | 2021-04-19 | 2021-08-13 | 青海西钢特殊钢科技开发有限公司 | Method for measuring zinc element in electroslag steel by ICP-OES |
| CN113295676A (en) * | 2021-04-06 | 2021-08-24 | 包头钢铁（集团）有限责任公司 | Method for measuring calcium, aluminum and barium in deoxidizer |
| CN113418970A (en) * | 2021-05-14 | 2021-09-21 | 包头钢铁（集团）有限责任公司 | Method for measuring fluorine in magnesium refractory material |
| CN113702358A (en) * | 2021-08-10 | 2021-11-26 | 包头钢铁（集团）有限责任公司 | Method for measuring content of potassium and sodium in silica |
| CN114354580A (en) * | 2021-12-13 | 2022-04-15 | 包头钢铁（集团）有限责任公司 | Method for measuring contents of potassium, sodium, lead, zinc and copper elements in iron ore, furnace slag, blast furnace dust and iron-containing tail mud |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108627374A (en) * | 2018-04-25 | 2018-10-09 | 山西建龙实业有限公司 | The assay method of Zn content in a kind of iron ore |
| CN111829864A (en) * | 2020-01-15 | 2020-10-27 | 包头钢铁（集团）有限责任公司 | Method for measuring contents of potassium, sodium, lead, zinc and copper in serpentine |
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| CN113252644A (en) * | 2021-04-19 | 2021-08-13 | 青海西钢特殊钢科技开发有限公司 | Method for measuring zinc element in electroslag steel by ICP-OES |
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| CN114354580A (en) * | 2021-12-13 | 2022-04-15 | 包头钢铁（集团）有限责任公司 | Method for measuring contents of potassium, sodium, lead, zinc and copper elements in iron ore, furnace slag, blast furnace dust and iron-containing tail mud |
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