CN106290317A - Potassium, lead and Direct spectrophotometry method in iron ore, slag and ion dust mud contaning - Google Patents
Potassium, lead and Direct spectrophotometry method in iron ore, slag and ion dust mud contaning Download PDFInfo
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- CN106290317A CN106290317A CN201610736677.0A CN201610736677A CN106290317A CN 106290317 A CN106290317 A CN 106290317A CN 201610736677 A CN201610736677 A CN 201610736677A CN 106290317 A CN106290317 A CN 106290317A
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/71—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light thermally excited
- G01N21/73—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light thermally excited using plasma burners or torches
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
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Abstract
In the open a kind of iron ore of the present invention, slag and ion dust mud contaning, potassium, lead and Direct spectrophotometry method, comprising: sodium carbonate and sodium tetraborate are mixed, be laid in mixed flux in platinum crucible, weigh in testing sample platinum crucible, then cover mixed flux;In another platinum crucible, add mixed flux and ferric oxide does blank sample;Melt in will be equipped with the platinum crucible of blank sample and being placed in Muffle furnace equipped with the platinum crucible of testing sample, take out cooling;Constant volume after frit is dissolved;Potassium, lead and zinc single element standards calibration curve solution and blank sample solution are introduced inductive coupling plasma emission spectrograph, draws K, Zn, Pb calibration curve;Specimen sample solution, blank sample solution are introduced inductive coupling plasma emission spectrograph standard solution, obtains the content of K, Zn, Pb in sample solution according to calibration curve.The method has range of linearity width, highly sensitive, easy and simple to handle, analysis result feature accurate, reliable.
Description
Technical field
The present invention relates to Ferrous Metallurgy analysis field, particularly to potassium in a kind of iron ore, slag and ion dust mud contaning, lead and
Direct spectrophotometry method.
Background technology
Ion dust mud contaning kind mainly includes sintering dirt mud, pelletizing dirt mud, blast furnace dust, blast furnace gas mud, steel-making
Dirt mud, converter mud, electricity (turning) stove dedusting ash, cold (hot) roll mud, steel rolling scale oxide, structure, stock yard dust
With cast house dust, flyash etc..
Sodium, lead, Direct spectrophotometry in iron ore are had both at home and abroad to some researchs, wherein company standard Q/BGJH-04-
214-2008, method uses hydrochloric acid, Fluohydric acid. to decompose sample, and perchloric acid smoked, dilute nitric acid dissolution salt, at atomic absorption spectrophotometry
Photometer measurement absorbance, measurement range Na of method2O:0.010~5.00%, K2O:0.010~10.00%, Pb:0.010
~1.00%, Zn:0.001~1.00%, the method needs to use substantial amounts of perchloric acid;National standard method 6730.49-86,
Iron ore sample salt acid+hydrofluoric acid decomposes, in hydrochloric acid medium, in measuring potassium content, method at atomic absorption spectrophotometer
Measurement range 0.005~1.50%;National standard method GB/T6730.54-2004 and GB/T6730.53-2004 surveys respectively
Determining lead in iron ore, zinc, sample hydrochloric acid and Fluohydric acid. decompose, nitric acid oxidation, nicotinic acid dissolved salts, filter, process residue after,
With MIBK extract and separate ferrum, nitric acid destroys MIBK, and dissolving with hydrochloric acid salt, in atomic absorption spectrophotometer measurement, the method
Need to use substantial amounts of organic solvent, measurement range Pb:0.001 of method~0.500%, Zn:0.001~0.5%;Ding Hong etc.
Discussed " potassium, sodium in atomic absorption spectroscopy determination ion dust mud contaning ", owing to the Pulse sample introduction device range of linearity is narrow, right
In the sample that content is higher, after dissolving, need stepwise dilution, complex operation, reduce the accuracy of measurement result.And for
The sample that carbon containing is higher, addition perchloric acid is fuming and is easily caught fire.Leeization have studied that " it is miscellaneous that ICP-AES method measures trace in mud entirely
Prime element copper, zinc, cadmium, nickel, lead ", the method is mainly for the mud of sewage treatment plant.Above several method is not satisfied by respectively
Plant potassium, lead and the analysis demand of zinc in iron ore, slag, ion dust mud contaning.
Summary of the invention
In view of this, potassium, lead and Direct spectrophotometry method during the present invention provides a kind of iron ore, slag and ion dust mud contaning.
The present invention provides potassium, lead and Direct spectrophotometry method in a kind of iron ore, slag and ion dust mud contaning, comprising:
Step a, mixes sodium carbonate and sodium tetraborate, obtains mixed flux;Described mixed flux is laid in platinum earthenware
In crucible, weigh in platinum crucible described in testing sample, then cover described mixed flux;Add described in another platinum crucible
Mixed flux and ferric oxide do blank sample;
Step b, will be equipped with the platinum crucible of described blank sample and the platinum crucible equipped with described testing sample is placed in horse
Not melt in stove, take out cooling;
Step c, puts in beaker by sample and crucible after cooling, and addition high purity water, hydrochloric acid are in low temp. electric hot plate, by frit
Constant volume in volumetric flask is moved into after dissolving, standby;
Step d, configuration potassium, lead and zinc single element standard solution, obtain standards calibration curve solution;
Step e, the blank sample solution that described standards calibration curve solution and step b are obtained introduce inductive etc. from
Daughter emission spectrometer, measures the signal intensity treating measured ion, and with mass percent as abscissa, the signal intensity of ion is vertical
Coordinate draws K, Zn, Pb calibration curve;
Step f, specimen sample solution step c obtained, blank sample solution introduce inductively coupled plasma and launch
Spectrogrph, measures the signal intensity treating measured ion, according to K, Zn, Pb standard solution calibration curve of known quality percent, asks
Go out the content of K, Zn, Pb in sample solution.
Further, described step a specifically includes:
By sodium carbonate: sodium tetraborate mixes with the weight ratio of 2:1, obtains mixed flux standby;Weigh and mix described in 1.0g
Flux is laid in platinum crucible, weighs 0.1000g testing sample and is placed in above platinum crucible, then covers mixing described in 0.5g
Flux;
Separately take a platinum crucible and add mixed flux described in 1.5g, be weighed into 0.050g iron sesquioxide, make blank sample.
Further, in described step b, arranging Muffle in-furnace temperature is 950 DEG C~1000 DEG C, and dissolution time is 15min.
Further, described step c particularly as follows:
Sample after cooling and crucible are put in 300mL beaker, add 80mL temperature be 60 DEG C~the high purity water of 70 DEG C,
20mL hydrochloric acid is in low temp. electric hot plate, and after being dissolved by frit, solution moves into 250mL volumetric flask constant volume, shakes up, standby.
Further, described step d specifically includes, weigh 6 parts of weight be the high purity iron of 0.040g in 300mL beaker,
Move in 250mL volumetric flask after adding 3mL hydrochloric acid, 3mL nitric acid, 20mL high purity water heating for dissolving so that in solution, mer weight is
Fe40%, then be separately added into potassium, lead, Zinc standard solution so that potassium in solution, content of Pb&Zn be respectively 0,0.050%,
0.1%, 0.5%, 1.0%, 5.0%, 12.0%, it is diluted to scale with high purity water, shakes up, obtain standards calibration curve solution.
Further, in described step f, in testing sample, the content of K, Zn, Pb is calculated as follows:
W%=Wi-W0
In formula: W is the weight/mass percentage composition of element in sample;
W0For element mass percent in blank solution to be measured;
WiFor element mass percent in sample to be measured.
Further, in described testing sample the content of potassium, lead and zinc all in the range of 0.005at~12.0at%.
The assay method that the present invention provides is to be decomposed by sample by sodium carbonate and sodium tetraborate mixed flux, hydrochloric acid-heat
After water extraction frit acidifying, ICP-AES is utilized directly, simultaneously to measure potassium, lead and the Zn content in sample solution.The method
Expanded the analysis upper limit of potassium, lead and zinc, be more suitable for potassium, lead, zinc, slag that carbon content is higher, ion dust mud contaning sample point
Analysis.The present invention uses Matrix Match to eliminate matrix interference, has range of linearity width, highly sensitive, easy and simple to handle, and analysis result is accurate
Really, reliable feature.
It is demonstrated experimentally that potassium, lead and zinc in iron ore, slag, ion dust mud contaning are surveyed by the method using the present invention to provide
Fixed, it is possible to have measured in 4 hours simultaneously, shorten sample processing time, the scope of analysis method up to 0.005at~
12.0at%.The assay method of the present invention has the advantage that precision is high, accuracy is high, fast and convenient, it is easy to accomplish producing
In promote the use of.
Detailed description of the invention
The invention discloses potassium, lead and Direct spectrophotometry method, art technology in a kind of iron ore, slag and ion dust mud contaning
Personnel can use for reference present disclosure, is suitably modified technological parameter and realizes.Special needs to be pointed out is, all similar replacements and changing
Dynamic apparent to those skilled in the art, they are considered as being included in the present invention.The method of the present invention and should
With being described by preferred embodiment, related personnel substantially can be without departing from present invention, spirit and scope
Method described herein and application it is modified or suitably changes and combine, realize and apply the technology of the present invention.
The invention provides potassium, lead and Direct spectrophotometry method in a kind of iron ore, slag and ion dust mud contaning, comprising:
Step a, mixes sodium carbonate and sodium tetraborate, obtains mixed flux;Described mixed flux is laid in platinum earthenware
In crucible, weigh in platinum crucible described in testing sample, then cover described mixed flux;Add described in another platinum crucible
Mixed flux and ferric oxide do blank sample;
Step b, will be equipped with the platinum crucible of described blank sample and the platinum crucible equipped with described testing sample is placed in horse
Not melt in stove, take out cooling;
Step c, puts in beaker by sample and crucible after cooling, and addition high purity water, hydrochloric acid are in low temp. electric hot plate, by frit
Constant volume in volumetric flask is moved into after dissolving, standby;
Step d, configuration potassium, lead and zinc single element standard solution, obtain standards calibration curve solution;
Step e, the blank sample solution that described standards calibration curve solution and step b are obtained introduce inductive etc. from
Daughter emission spectrometer, measures the signal intensity treating measured ion, and with mass percent as abscissa, the signal intensity of ion is vertical
Coordinate draws K, Zn, Pb calibration curve;
Step f, specimen sample solution step c obtained, blank sample solution introduce inductively coupled plasma and launch
Spectrogrph, measures the signal intensity treating measured ion, according to K, Zn, Pb standard solution calibration curve of known quality percent, asks
Go out the content of K, Zn, Pb in sample solution.
Preferably, above-mentioned steps a specifically includes:
By sodium carbonate: sodium tetraborate mixes with the weight ratio of 2:1, obtains mixed flux standby;Weigh and mix described in 1.0g
Flux is laid in platinum crucible, weighs 0.1000g testing sample and is placed in above platinum crucible, then covers mixing described in 0.5g
Flux;
Separately take a platinum crucible and add mixed flux described in 1.5g, be weighed into 0.050g iron sesquioxide, make blank sample.
In above-mentioned steps b, being preferably provided with Muffle in-furnace temperature is 950 DEG C~1000 DEG C, and dissolution time is 15min.
Further, described step c particularly as follows:
During after cooling, 300mL beaker put into by sample and crucible, adding 80mL temperature is 60 DEG C~the high purity water of 70 DEG C, 20mL
Hydrochloric acid is in low temp. electric hot plate, and after being dissolved by frit, solution moves into 250mL volumetric flask constant volume, shakes up, standby.
Preferably, in described step d, weigh 6 parts of weight be the high purity iron of 0.040g in 300mL beaker, add 3mL salt
Move in 250mL volumetric flask after acid, 3mL nitric acid, 20mL high purity water heating for dissolving so that in solution, mer weight is Fe40%, then
Be separately added into potassium, lead, Zinc standard solution so that potassium in solution, content of Pb&Zn be respectively 0,0.050%, 0.1%, 0.5%,
1.0%, 5.0%, 12.0%, it is diluted to scale with high purity water, shakes up, obtain standards calibration curve solution.
In described step f, in testing sample, the content of K, Zn, Pb may be calculated as:
W%=Wi-W0
In formula: W is the weight/mass percentage composition of element in sample;
W0For element mass percent in blank solution to be measured;
WiFor element mass percent in sample to be measured.
The present invention is supplied to assay method and is applicable to the content of potassium, lead and zinc all in the range of 0.005at~12.0at%
The mensuration of iron ore, slag and ion dust mud contaning.
Below in conjunction with embodiment, the present invention it is expanded on further:
[reagent]
Hydrochloric acid: top grade is pure;
Sodium carbonate: top grade is pure;Sodium tetraborate: top grade is pure;Sodium carbonate: sodium tetraborate=2:1 mixing
Potassium, lead, zinc single element standard solution: concentration is 1000 μ g/mL, derives from State center for standard matter;
High purity iron (purity is more than 99.9%);
250mL volumetric flask;300mL beaker;Argon: purity of argon >=99.9%.
Iron sesquioxide: standard reagent;
Compressed air.
[equipment]
Sense coupled plasma optical emission spectrogrph model is PE company Optima 5300V;
ICP-AES Instrument working parameter is listed in table 1:
Table 1ICP-AES Instrument working parameter
Parameter name | Numerical value |
RF power (W) | 1300 |
Cooling gas flow (mL/min) | 15 |
Secondary air amount (mL/min) | 0.2 |
Atomization gas flow (mL/min) | 0.8 |
Input mode | Peristaltic pump sample introduction |
Sample mode | Jump peak mode to sample |
Number of repetition | 3 |
Observed pattern | Level is observed |
Washing time (s) | 30 |
Integration (calculating) pattern | Potassium is Peak Area;Lead, zinc are peak height; |
[sample analysis]
1, weigh 1.0g sodium carbonate and sodium tetraborate mixed flux is laid in platinum crucible, weigh 0.1000g and treat test sample
Product are placed in above platinum crucible, then cover 0.5g sodium carbonate and sodium tetraborate mixed flux.
Blank experiment: weigh 0.050g iron sesquioxide, does blank experiment in company with sample.
2, will be equipped with testing sample the platinum crucible of blank sample to put into Muffle furnace and melt (950 DEG C~1000 DEG C)
15min, takes out cooling.
3, after cooling, sample and crucible are put in 300mL beaker, add 80mL high purity water (60 DEG C~70 DEG C), 20mL hydrochloric acid
In low temp. electric hot plate, after being dissolved by frit, solution moves in 250mL volumetric flask, is diluted to scale with high purity water, shakes up, and waits
Upper machine.
4, the configuration of standards calibration curve solution
Potassium, lead, zinc single element standard solution: concentration is 1000 μ g/mL, derives from State center for standard matter;
In order to reduce matrix effect, weigh 6 parts of high purity irons (purity is more than 99.9%) 0.040g and, in 300mL beaker, add
Move in 250mL volumetric flask after entering 3mL hydrochloric acid, 3mL nitric acid, 20mL high purity water heating for dissolving and make the mer weight in solution to be
Fe40%, then be separately added into potassium, lead, Zinc standard solution so that potassium in solution, content of Pb&Zn be respectively 0,0.050%,
0.1%, 0.5%, 1.0%, 5.0%, 12.0%, it is diluted to scale with high purity water, shakes up.This solution makes standard curve and uses.
5, modulating equipment, refers to above-mentioned table 1.
6, selecting spectral line, select K 766.49nm, Zn 202.55nm, Pb220.35nm do analytical line.
7, calibration curve is drawn: standards calibration curve solution and blank sample solution are introduced inductively coupled plasma and sends out
Penetrating spectrogrph, measure the signal intensity treating measured ion, with mass percent as abscissa, the signal intensity of ion is that vertical coordinate is painted
K, Zn, Pb calibration curve processed.
8, specimen sample solution, blank sample solution introduce inductive coupling plasma emission spectrograph, measure to be measured from
Son signal intensity, according to K, Zn, Pb standard solution calibration curve of known quality percent, obtain K in sample solution, Zn,
The content of Pb.
In sample, the content of K, Zn, Pb is calculated as follows:
W%=Wi-W0
In formula: the weight/mass percentage composition of element in W-sample;
W0-element is mass percent in blank solution to be measured;
Wi-element mass percent in sample solution to be measured;
This method detection range: K, Zn, Pb are 0.005at~12.0at%.
Embodiment 1
Making working curve as stated above, curve correlation coefficient r is more than 0.999, and empirically method prepares 11 parts of blank
Solution divides 3 times and is measured, the detection limit formula C defined according to IUPAC (IUPAC)L=3Sb/k
(SbFor blank standard deviation, k is corresponding Slope of Calibration Curve) calculate method detection and be limited to K, Zn, Pb 0.0005%.
Embodiment 2
Weigh potassium feldspar (GBW03116), lode tin raw ore (BY0108-1), iron ore (GSBH30001-97), iron ore
(GSBH30005), iron ore (GSB03-2025-2006), polymetallic ore (GBW07163), blast furnace slag (YSBC28552-98)
It is measured as stated above, the results are shown in Table 2.
Table 2 standard sample measurement result
Note: * represents, asserting value analyzes lower limit less than this patent.
Embodiment 3
Weigh iron ore (GSB03-2025-2006), blast furnace slag (YSBC28552-98), iron ore (GSBH30004) mark
The some parts of quasi-sample and mud sample, slag sample, gas ash sample, adhesive sample, be separately added into K, Zn, Pb standard molten
Liquid, is measured as stated above, the results are shown in Table 3.
The measurement result that table 3 standard sample mark-on reclaims
Embodiment 4
Claim iron ore 1#, 2# sample, dedusting ash 2# sample, slag 1# sample, iron scale 1# sample, flyash 1# sample
It is measured as stated above, the results are shown in Table 4.
Table 4 sample specimens measurement result
Sample is decomposed by the assay method that the present invention provides by sodium carbonate and sodium tetraborate mixed flux, hydrochloric acid-hot water
After extracting frit and being acidified, ICP-AES is utilized directly, simultaneously to measure potassium, lead and the Zn content in sample solution.The method is opened up
Opened up the analysis upper limit of potassium, lead and zinc, be more suitable for potassium, lead and zinc, slag that carbon content is higher, ion dust mud contaning sample point
Analysis.The present invention uses Matrix Match to eliminate matrix interference, has range of linearity width, highly sensitive, easy and simple to handle, and analysis result is accurate
Really, reliable feature.
Checking by above-mentioned embodiment, it can be seen that use the method that the present invention provides to iron ore, slag, iron content
In dirt mud, potassium, lead and zinc are measured, it is possible to measured in 4 hours simultaneously, shorten sample processing time, analyze method
Scope up to 0.005at~12.0at%.The assay method of the present invention has that precision is high, accuracy is high, fast and convenient
Advantage, it is easy to accomplish promoting the use of aborning.
The above is only the preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For Yuan, under the premise without departing from the principles of the invention, it is also possible to make some improvements and modifications, these improvements and modifications also should
It is considered as protection scope of the present invention.
Claims (7)
1. potassium, lead and Direct spectrophotometry method in an iron ore, slag and ion dust mud contaning, it is characterised in that including:
Step a, mixes sodium carbonate and sodium tetraborate, obtains mixed flux;Described mixed flux is laid in platinum crucible,
Weigh in platinum crucible described in testing sample, then cover described mixed flux;Described mixing is added in another platinum crucible
Flux and ferric oxide do blank sample;
Step b, will be equipped with the platinum crucible of described blank sample and the platinum crucible equipped with described testing sample is placed in Muffle furnace
Interior melting, takes out cooling;
Step c, puts in beaker by sample and crucible after cooling, and frit, in low temp. electric hot plate, is dissolved by addition high purity water, hydrochloric acid
Constant volume in rear immigration volumetric flask, standby;
Step d, configuration potassium, lead and zinc single element standard solution, obtain standards calibration curve solution;
Step e, the blank sample solution described standards calibration curve solution and step b obtained introduces inductively coupled plasma
Emission spectrometer, measures the signal intensity treating measured ion, and with mass percent as abscissa, the signal intensity of ion is vertical coordinate
Draw K, Zn, Pb calibration curve;
Step f, specimen sample solution step c obtained, blank sample solution introduce inductively coupled plasma atomic emission
Instrument, measures the signal intensity treating measured ion, according to K, Zn, Pb standard solution calibration curve of known quality percent, obtains sample
The content of K, Zn, Pb in product solution.
Assay method the most according to claim 1, it is characterised in that described step a specifically includes:
By sodium carbonate: sodium tetraborate mixes with the weight ratio of 2:1, obtains mixed flux standby;Weigh mixed flux described in 1.0g
It is laid in platinum crucible, weighs 0.1000g testing sample and be placed in above platinum crucible, then it is molten to cover mixing described in 0.5g
Agent;
Separately take a platinum crucible and add mixed flux described in 1.5g, be weighed into 0.050g iron sesquioxide, make blank sample.
Assay method the most according to claim 1, it is characterised in that in described step b, arranging Muffle in-furnace temperature is
950 DEG C~1000 DEG C, dissolution time is 15min.
Assay method the most according to claim 1, it is characterised in that described step c particularly as follows:
Sample after cooling and crucible being put in 300mL beaker, adding 80mL temperature is 60 DEG C~the high purity water of 70 DEG C, 20mL salt
Acid is in low temp. electric hot plate, and after being dissolved by frit, solution moves into 250mL volumetric flask constant volume, shakes up, standby.
Assay method the most according to claim 1, it is characterised in that described step d specifically includes, weighing 6 parts of weight is
The high purity iron of 0.040g, in 300mL beaker, moves into 250mL after adding 3mL hydrochloric acid, 3mL nitric acid, 20mL high purity water heating for dissolving
In volumetric flask so that in solution, mer weight is Fe40%, then be separately added into potassium, lead, Zinc standard solution so that potassium in solution, lead,
Zn content is respectively 0,0.050%, 0.1%, 0.5%, 1.0%, 5.0%, 12.0%, is diluted to scale with high purity water, shakes up,
Obtain standards calibration curve solution.
Assay method the most according to claim 1, it is characterised in that in described step f, K, Zn, Pb in testing sample
Content is calculated as follows:
W%=Wi-W0
In formula: W is the weight/mass percentage composition of element in sample;
W0For element mass percent in blank solution to be measured;
WiFor element mass percent in sample to be measured.
Assay method the most according to claim 1, it is characterised in that in described testing sample, the content of potassium, lead and zinc is equal
In the range of 0.005at~12.0at%.
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