CN109827952A - The ICP-AES detection method of micronutrient levels in a kind of lead concentrate - Google Patents
The ICP-AES detection method of micronutrient levels in a kind of lead concentrate Download PDFInfo
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Abstract
The present invention relates to a kind of ICP-AES detection methods of micronutrient levels in lead concentrate, microelement includes copper, zinc, cadmium, tin, bismuth, iron, aluminium, manganese, titanium, nickel, chromium, cobalt element, aim to solve the problem that lead concentrate carries out the detection inaccuracy of Determination of multiple metal elements, in particular for the problem of the assay inaccuracy of minor metallic element.This method includes preparing sample solution；Prepare the working curve standard solution of copper, zinc, cadmium, tin, bismuth, iron, aluminium, manganese, titanium, nickel, chromium, cobalt；Measure the mass concentration of sample solution, blank test solution；The content of copper, zinc, cadmium, tin, bismuth, iron, aluminium, manganese, titanium, nickel, chromium, cobalt element is calculated according to formula.It is accurate according to this measurement result, inspection range is big, can accurately measure the content of various trace elements, can be widely applied to testing agency, official or third party detection.
Description
Technical field
The invention belongs to mine trace element physical and chemical inspection technical field, relates generally to microelement in a kind of lead concentrate and contain
Amount, including copper, zinc, cadmium, tin, bismuth, iron, aluminium, manganese, titanium, nickel, chromium, cobalt element content ICP-AES measuring method.
Background technique
In recent years, with the continuous development of nonferrous production technology, to copper in non-ferrous metal, zinc, cadmium, tin, bismuth, iron,
Aluminium, manganese, titanium, nickel, chromium, the testing requirements of cobalt element are higher and higher, past during the assay of lead concentrate Determination of multiple metal elements
It is past sample to be measured using lead concentrate method to be specifically chosen according to the difference of its properties of samples, content height, for
When properties of samples and indefinite constituent content, us will be given to make troubles in the selection of measuring method, cause replication,
Take time and effort, if test method is not applicable, will result in sample to be tested resolution be not thorough, lead sulfate precipitation generate not exclusively, drop
Determine the problems such as terminal colour variation is unobvious, influences the accuracy of measurement result.Also there are no entirely accurate surveys in the prior art
How the method for measuring copper, zinc, cadmium, tin, bismuth, iron, aluminium, manganese, titanium, nickel, chromium, cobalt element in non-ferrous metal carries out lead concentrate more
The accurate detection of kind metallic element carries out Accurate Determining in particular for the content of minor metallic element, is the skill of urgent need to resolve
Art problem.
Summary of the invention
(1) technical problems to be solved
It is main it is a primary object of the present invention to propose a kind of ICP-AES measuring method of micronutrient levels in lead concentrate
It to include copper, zinc, cadmium, tin, bismuth, iron, aluminium, manganese, titanium, nickel, chromium, cobalt element, it is intended to solve existing measurement element species
Less, the technical problems such as result inaccuracy.
(2) technical solution
To achieve the above object, the present invention provides a kind of ICP-AES detection method of micronutrient levels in lead concentrate, institute
Stating microelement includes copper, zinc, cadmium, tin, bismuth, iron, aluminium, manganese, titanium, nickel, chromium, cobalt element, comprising the following steps:
S1, it prepares sample solution: being placed in a beaker firstly, weighing 0.2-0.5g lead concentrate sample, soaked with water, be added
4mL concentration 1.42g/mL nitric acid is added in the hydrochloric acid of 12mL concentration 1.19g/mL, and heating and temperature control is within the scope of 80 DEG C -100 DEG C
It is dissolved substantially to sample；The hydrofluoric acid of 10mL concentration 1.14g/mL, the perchloric acid of 2mL concentration 1.67g/mL, heating are added later
Temperature is controlled to emit dense white cigarette to perchloric acid within the scope of 250 DEG C -300 DEG C or steam to sample drying；If still having in the beaker black
Color residue is undissolved, repeats above step；Secondly, the heating of 4ml hydrochloric acid (1+1) solution small fire is added after the beaker is cooling
To solution without obvious residue；
Finally, be transferred in 25mL volumetric flask after the solution is cooling, be diluted to scale with nitric acid (1+20), shake up, every
Night places or dry filtering, for use；In company with preparation blank test solution；Hydrochloric acid (1+1) solution refers to the concentration of same volume
36% hydrochloric acid solution and pure water mix；
Nitric acid (1+20) solution refers to that the nitric acid solution of 1 volume and the pure water of 20 volumes mix；
S2, the working curve standard solution for preparing copper, zinc, cadmium, tin, bismuth, iron, aluminium, manganese, titanium, nickel, chromium, cobalt:
Firstly, compound concentration is the hybrid standard of 100 μ g/mL copper, zinc, cadmium, tin, bismuth, iron, aluminium, manganese, titanium, nickel, chromium, cobalt
The normal storage solution of the copper of 1000 μ g/mL, zinc, cadmium, tin, bismuth, iron, aluminium, manganese, titanium, nickel, chromium, cobalt is diluted to by solution respectively
100μg/mL；
Secondly, preparing working curve standard solution: using copper, zinc, cadmium, tin, bismuth, iron, aluminium, manganese, titanium, nickel, chromium, cobalt it is mixed
Standardization solution prepares the series of tasks curve standard solution of 6 or more concentration in gradient respectively；
The mass concentration of S3, measurement sample solution, blank test solution: the working curve standard that the step S2 is configured
Solution is introduced into inductively coupled plasma atomic emission spectrometer, and at the wavelength that each element is selected, it is bent to measure the work
The spectral intensity of line standard solution produces the standard solution working curve of each element；When the linearly dependent coefficient of working curve
When >=0.999, the concentration of the sample solution concentration and the blank test solution is measured, according to the pass of spectral intensity and concentration
System obtains the lead concentrate sample, copper, zinc, cadmium, tin, bismuth, iron, aluminium, manganese, titanium, nickel, chromium, cobalt member in blank test solution respectively
Mass concentration c, the mass concentration c of elemento；
S4, according to formulaCalculate copper, zinc, cadmium,
The content of tin, bismuth, iron, aluminium, manganese, titanium, nickel, chromium, cobalt element；
In formula:
W (x) --- the mass fraction of element to be measured, unit are percentage；
C --- the mass concentration of element to be measured in sample solution, unit is micrograms per millilitre；
co--- the mass concentration of element to be measured in blank test solution, unit is micrograms per millilitre；
V --- sample solution volume, unit are milliliter；
m0--- the quality of sample, unit are gram；
R --- the coefficient of dilution.
Further, constituent content to be measured is selected to fall between the standard curve concentration of series standard solution drafting；Work as institute
State step S1 preparation constant volume after sample solution concentration range be more than or equal to 100 μ g/mL when, the step S1 preparation is determined
Sample solution carries out point taking dilution after appearance, and the constant volume sample solution concentration after point taking dilution is less than 100 μ g/mL.
Further, when the concentration range of sample solution is more than or equal to 100 μ g/mL after the constant volume of the step S1 preparation,
Sample solution after the constant volume of step S1 preparation is carried out point taking dilution, divides and takes the constant volume sample solution concentration after diluting little
In 80 μ g/mL.
Further, copper, zinc, cadmium, tin, bismuth, iron, aluminium, manganese, titanium, nickel, chromium, cobalt element series standard solution concentration difference
It is 0 μ g/mL, 0.1 μ g/mL, 0.5 μ g/mL, 2 μ g/mL, 10 μ g/mL, 50 μ g/mL.
Further, copper, zinc, cadmium, tin, bismuth, iron, aluminium, manganese, titanium, nickel, chromium, cobalt element series of tasks curve standard solution
Configuration method be: pipette respectively copper, zinc, cadmium, tin, bismuth, iron, aluminium, manganese, titanium, nickel, chromium, cobalt mixed standard solution 0.00mL,
0.05mL, 0.25mL, 1.00mL, 5.00mL, 25.00mL dilute constant volume in 50mL volumetric flask, with nitric acid；The nitric acid is 1
The pure water of the nitric acid solution of volume and 20 volumes mixes.
Further, in the step S2, the preparation dilution of the mixed standard solution dilutes constant volume using nitric acid；It is described
Nitric acid is that the nitric acid solution of 1 volume and the pure water of 20 volumes mix.
Further, in continuous mode, what is used is Cleaning analysis container, and acid is high purity acid, water is that quartzy sub- boiling is steamed
Distilled water, measuring result error when to avoid the element easy to pollute for measuring low content are excessive.
Further, the lead bullion sample ore product should be pre-processed before the step S1: firstly, passing through the hole 0.149mm
The standard screen of diameter screens；Then, in 105 DEG C of -115 DEG C of drying 2h；Later, be placed in drier be cooled to room temperature it is spare.
Further, the light-splitting chamber of the inductive coupling plasma emission spectrograph has the function of to vacuumize or purging,
Running parameter are as follows: power 1200W, fog chamber press 32Psi, pump 1.2mL/min, time of integration 25S.
Further, the beaker material is polytetrafluoroethylene (PTFE)；Assay balance sensibility reciprocal 0.1mg, drying box accuracy of temperature control ± 5
℃。
The beneficial effect that the present invention is implemented is: measurement result is accurate, inspection range is big, can accurately measure lot of trace member
The content of element, can be widely applied to testing agency, official.
Detailed description of the invention
The attached drawing for constituting a part of the invention patent is used to provide to further understand the invention patent, and the present invention is special
The illustrative embodiments and their description of benefit are used to explain the present invention patent, do not constitute the improper restriction to the invention patent.
Fig. 1 is a kind of ICP-AES measuring method schematic diagram of micronutrient levels in lead concentrate.
Specific embodiment
The invention patent is described in detail below, the description of this part be only it is exemplary and explanatory, should not be to this
The protection scope of patent of invention has any restriction effect.
Embodiment
The present invention provides a kind of ICP-AES measuring method of micronutrient levels in lead concentrate, and specific embodiment is as follows:
One, reagent and instrument:
(1) reagent
This standard agents useful for same and water refer both to analytical reagents and GB/T 6682 are provided when not indicating other and requiring
Tertiary effluent.
1.1 hydrofluoric acid (ρ=1.14g/mL), excellent pure grade.
1.2 hydrochloric acid (ρ=1.19g/mL), excellent pure grade.
1.3 nitric acid (ρ=1.42g/mL), excellent pure grade.
1.4 perchloric acid (ρ=1.67g/mL), excellent pure grade.
1.5 hydrochloric acid (1+1), (hydrochloric acid (1+1) solution refers to 36% hydrochloric acid solution of concentration of same volume and pure to excellent pure grade
Water mixes).
1.6 nitric acid (1+20) (nitric acid (1+20) solution refer to 1 volume nitric acid solution and 20 volumes pure water mixing and
At.)
1.9 sodium hydroxides, excellent pure grade.
1.10 metallic coppers (Cu >=99.99%).
1.11 metallic zincs (Zn >=99.99%).
1.12 cadmium metals (Cd >=99.99%).
1.13 metallic tins (Sn >=99.99%).
1.14 bismuth metals (Bi >=99.99%).
1.15 metallic irons (Fe >=99.99%).
1.16 potassium bichromates (standard reagent or excellent pure grade).
1.17 metallic aluminiums (Al >=99.99%).
1.18 manganese metals (Mn >=99.99%).
1.19 Titaniums (Ti >=99.99%).
1.20 metallic nickels (Ni >=99.99%).
1.21 metallic cobalts (Co >=99.99%).
1.22 standard solution (100ug/ml) are prepared by 602 method of GB/T, or following preparation:
Copper normal storage solution (1.0mg/mL): commercially available to have copper standard solution (1000 μ for demonstrate,proving national liquid standard sample
G/mL it) obtains.
1.23 zinc normal storage solution (1.0mg/mL): commercially available to have the Zinc standard solution for demonstrate,proving national liquid standard sample
(1000 μ g/mL) is obtained.
1.24 cadmium normal storage solution (1.0mg/mL): commercially available to have the cadmium standard solution for demonstrate,proving national liquid standard sample
(1000 μ g/mL) is obtained.
1.25 tin normal storage solution (1.0mg/mL): commercially available to have the tin standard solution for demonstrate,proving national liquid standard sample
(1000 μ g/mL) is obtained.
1.26 bismuth normal storage solution (1.0mg/mL): commercially available to have the bismuth standard solution for demonstrate,proving national liquid standard sample
(1000 μ g/mL) is obtained.
1.27 iron normal storage solution (1.0mg/mL): commercially available to have the iron standard solution for demonstrate,proving national liquid standard sample
(1000 μ g/mL) is obtained.
1.28 aluminium normal storage solution (1.0mg/mL): commercially available to have the aluminum standard solution for demonstrate,proving national liquid standard sample
(1000 μ g/mL) is obtained.
1.29 manganese normal storage solution (1.0mg/mL): commercially available to have the manganese standard solution for demonstrate,proving national liquid standard sample
(1000 μ g/mL) is obtained.
1.30 titanium normal storage solution (1.0mg/mL): commercially available to have the titanium standard solution for demonstrate,proving national liquid standard sample
(1000 μ g/mL) is obtained.
1.31 nickel normal storage solution (1.0mg/mL): commercially available to have the nickel standard solution for demonstrate,proving national liquid standard sample
(1000 μ g/mL) is obtained.
1.32 chromium normal storage solution (1.0mg/mL): commercially available to have the chromium standard solution for demonstrate,proving national liquid standard sample
(1000 μ g/mL) is obtained.
1.33 cobalt normal storage solution (1.0mg/mL): commercially available to have the cobalt standard solution for demonstrate,proving national liquid standard sample
(1000 μ g/mL) is obtained.
1.34 standard solution A: normal storage solution (1.22-1.33) is diluted to 100 μ g/mL, and molten with normal storage
The acidity (used time dilution) that liquid is consistent.
1.35 mixed standard solutions: being diluted to 100 μ g/mL with nitric acid (1.6) for normal storage solution (1.22-1.33),
And the acidity (used time dilution) being consistent with normal storage solution.
(2) instrument and equipment
1, inductive coupling plasma emission spectrograph.
2, light-splitting chamber has the function of to vacuumize or purging.
3, light source: plasma source uses power 750W~1750W.The operating condition of instrument is referring to the following table 2.
2 instrument operating condition of table
| Power/W | Assist gas/(L/min) | Fog chamber's pressure/Psi | Pump/(mL/min) | Sample injection time/s | The time of integration/s | Observed pattern |
| 1200 | 0.3 | 31~35 | 1.0-1.3 | 20~30 | 25 | Level observation |
4, the recommendation analysis spectral line of each element is shown in Table 3
The recommendation analytical line of the element to be measured of table 3
| Element | Analytical line/nm | Element | Analytical line/nm |
| Cu | 327.754 | Al | 396.152 |
| Zn | 202.548 | Mn | 293.306 |
| Cd | 226.502 | Ti | 336.122 |
| Sn | 235.484 | Ni | 231.604 |
| Bi | 223.061 | Cr | 267.716 |
| Fe | 234.350 | Co | 228.615 |
5, polytetrafluoroethylene beaker: 250mL
6, temperature controllable electric hot plate: 100 DEG C -400 DEG C
7, assay balance: sensibility reciprocal 0.1mg
8, measurement range:
The measurement concentration range of the element to be measured of table 4
| Element | Measurement range | Element | Measurement range |
| Copper | 0.00013~1.00 | Bismuth | 0.00079~1.00 |
| Zinc | 0.00011~0.500 | Iron | 0.00039~1.00 |
| Cadmium | 0.000033~0.500 | Aluminium | 0.00056~1.00 |
| Tin | 0.00098~1.00 | Manganese | 0.000056~1.00 |
| Titanium | 0.00010~1.00 | Nickel | 0.000052~1.00 |
| Chromium | 0.00013~1.00 | Cobalt | 0.000038~1.00 |
Two, sample test step:
(1) sample
Weighing sample amount and constant volume and should meeting the regulation of table 4 for different elements is analyzed, weighing amount is accurate to
0.0001g。
4 weighing amount of table, constant volume
Blank test is done in company with sample.
(2) specific steps
S1, it prepares sample solution: lead concentrate being placed in 250mL polytetrafluoroethylene beaker, is soaked with little water, be added
12mL hydrochloric acid (1.2) is added 4mL nitric acid (1.3) and heats sample in 80 DEG C of -100 DEG C of holding low temperature ranges to basic dissolution, adds
Enter 10mL hydrofluoric acid (1.1), 2mL perchloric acid (1.4), be placed on electric hot plate, temperature is that emit perchloric acid dense for 250 DEG C of -300 DEG C of heating
White cigarette, if sample still has black residue undissolved, repeats above step until steaming is closely dry to sample.It is slightly cold, 4ml hydrochloric acid is added
Solution (1.5) low-grade fever dissolved salts are to solution without obvious residue.It is cooling, it is transferred in 25mL volumetric flask, is diluted to nitric acid (1.6)
Scale shakes up, placement overnight or dry filtering, to point take or directly upper machine measurement.When measuring the element easy to pollute of low content, make
With high purity acid and quartzy sub-boiling distillation water, clean analyzing container is used.To prevent cross contamination, the utensil contacted with sample is answered
All use 10%HNO3It impregnates 24 hours (generating except corroding), with ultrapure water 3 times, dries spare.
Blank assay is carried out in company with sample.
S2, the working curve standard solution for preparing copper, zinc, cadmium, tin, bismuth, iron, aluminium, manganese, titanium, nickel, chromium, cobalt:
Firstly, the normal storage solution of preparation copper, zinc, cadmium, tin, bismuth, iron, aluminium, manganese, titanium, nickel, chromium, cobalt is respectively 1000 μ
g/mL；Prepare mixed standard solution again: by the copper of 1000 μ g/mL, zinc, cadmium, tin, bismuth, iron, aluminium, manganese, titanium, nickel, chromium, cobalt mark
Quasi- storage is diluted to 100 μ g/mL with nitric acid (1.6) solution respectively；
Secondly, preparing working curve standard solution: the mixed standard solution is added in one group of 50mL volumetric flask and matches respectively
Copper processed, zinc, cadmium, tin, bismuth, iron, aluminium, manganese, titanium, nickel, chromium, cobalt 6 or more concentration in gradient series of tasks curve standard
Solution is diluted to scale with water and shakes up.Sample standard solution is not added is typically chosen constituent content to be measured as blank solution
Falling among the standard curve that the series standard solution is drawn is advisable, and the quantity of series standard solution is determined by required precision.
Standard solution preparation can refer to the following table 5 (need dilute sample except).
5 mixed standard solution concentration of table and element to be measured (μ g/mL)
It can also also be may be selected according to the grade of lead concentrate sample corresponding standard sample (having card standard specimen), by step S1 system
Preparation Method prepares series standard solution, and the quantity of series standard solution is determined by required precision, generally takes 6.
The mass concentration of S3, measurement sample solution, blank test solution:
(1) determination condition
According to the suitable argon flow of instrument situation selection.
(2) series standard solution prepared by step S2 is introduced into inductively coupled plasma atomic emission spectrometer, it is defeated
Enter according to selected instrument optimum determining condition is tested, at the wavelength that each element is selected, measures each in series standard solution
The intensity of element draws the standard working curve of each element；When the linearly dependent coefficient of working curve >=0.999, institute is measured
The concentration for stating sample solution concentration and the blank test solution obtains the lead concentrate sample according to the relationship of luminous intensity and concentration
The mass concentration c of the mass concentration c of each element in product, blank test solution, each elemento；
S4, according toCalculate copper, zinc, cadmium, tin,
The content of bismuth, iron, aluminium, manganese, titanium, nickel, chromium, cobalt element；
In formula:
W (x) --- the mass fraction of element to be measured, unit are percentage；
C --- the mass concentration of element to be measured in sample solution, unit is micrograms per millilitre；
co--- the mass concentration of element to be measured in blank test solution, unit is micrograms per millilitre；
V --- sample solution volume, unit are milliliter；
m0--- the quality of sample, unit are gram；
R --- the coefficient of dilution.
Calculated result retains three effective digitals, and it is consistent with detection limit that when testing result < 0.01 retains digit, the data obtained
The revision of the convention abides by 8170 numerical value rule for rounding off of GB/T.
When the concentration range of sample solution is more than or equal to 100 μ g/mL after the constant volume of step S1 preparation, to the step
Sample solution carries out point taking dilution after the constant volume of rapid S1 preparation, divides and takes the constant volume sample solution concentration after diluting less than 100 μ g/
mL；Especially divide the constant volume sample solution concentration after taking dilution no more than 80 μ g/mL.
Copper, zinc, cadmium, tin, bismuth, iron, aluminium, manganese, titanium, nickel, chromium, cobalt element series of tasks curve concentration of standard solution are respectively
0μg/mL、0.1μg/mL、0.5μg/mL、2μg/mL、10μg/mL、50μg/mL。
The configuration method of copper, zinc, cadmium, tin, bismuth, iron, aluminium, manganese, titanium, nickel, chromium, cobalt element series of tasks curve standard solution
Be: pipette respectively the copper, zinc, cadmium, tin, bismuth, iron, aluminium, manganese, titanium, nickel, chromium, cobalt mixed standard solution 0.00mL,
0.05mL, 0.25mL, 1.00mL, 5.00mL, 25.00mL dilute constant volume in 50mL volumetric flask, with nitric acid (1.6).
In continuous mode, what is used is Cleaning analysis container, and acid is high purity acid, water is quartzy sub-boiling distillation water, to keep away
Measuring result error when exempting to measure the element easy to pollute of low content is excessive.
The lead bullion sample ore product should be pre-processed before the step S1: firstly, passing through the standard screen in the aperture 0.149mm
Screening；Then, in 105 DEG C of -115 DEG C of drying 2h；Later, be placed in drier be cooled to room temperature it is spare.
Optimization experiment condition is: the light-splitting chamber of the inductive coupling plasma emission spectrograph, which has, to be vacuumized or purging
Function, running parameter are as follows: power 1200W, fog chamber press 32Psi, pump 1.2mL/min, time of integration 25S；The beaker material is
Polytetrafluoroethylene (PTFE)；Drying box accuracy of temperature control ± 5 DEG C.
Finally it should be noted that the above examples are only used to illustrate the technical scheme of the present invention and are not limiting, although reference
Preferred embodiment describes the invention in detail, it will be appreciated by those skilled in the art that can be to technical side of the invention
Case is modified or replaced equivalently, and without departing from the spirit and scope of the technical solution of the present invention, should all be covered in this hair
In bright scope of the claims.
Claims (10)
1. the ICP-AES detection method of micronutrient levels in a kind of lead concentrate, the microelement include copper, zinc, cadmium, tin,
Bismuth, iron, aluminium, manganese, titanium, nickel, chromium, cobalt element, which comprises the following steps:
S1, it prepares sample solution: being placed in a beaker firstly, weighing 0.2-0.5g lead concentrate sample, soaked with water, it is dense that 12mL is added
The hydrochloric acid of 1.19g/mL is spent, 4mL concentration 1.42g/mL nitric acid is added, heating and temperature control is within the scope of 80 DEG C -100 DEG C to sample
Basic dissolution；The hydrofluoric acid of 10mL concentration 1.14g/mL, the perchloric acid of 2mL concentration 1.67g/mL, computer heating control temperature are added later
Degree emits dense white cigarette to perchloric acid within the scope of 250 DEG C -300 DEG C or steams to sample drying；If still having black residue in the beaker
It is undissolved, repeat above step；Secondly, 4ml hydrochloric acid (1+1) solution small fire is added and is heated to solution after the beaker is cooling
Without obvious residue；Finally, being transferred in 25mL volumetric flask after the solution is cooling, being diluted to scale with nitric acid (1+20), shake
It is even, placement overnight or dry filtering, for use；In company with preparation blank test solution；Hydrochloric acid (1+1) solution refers to the dense of same volume
It spends 36% hydrochloric acid solution and pure water mixes；
Nitric acid (1+20) solution refers to that the nitric acid solution of 1 volume and the pure water of 20 volumes mix；
S2, the working curve standard solution for preparing copper, zinc, cadmium, tin, bismuth, iron, aluminium, manganese, titanium, nickel, chromium, cobalt:
Firstly, compound concentration is the mixed standard solution of 100 μ g/mL copper, zinc, cadmium, tin, bismuth, iron, aluminium, manganese, titanium, nickel, chromium, cobalt,
The normal storage solution of the copper of 1000 μ g/mL, zinc, cadmium, tin, bismuth, iron, aluminium, manganese, titanium, nickel, chromium, cobalt is diluted to 100 μ respectively
g/mL；
Secondly, prepare working curve standard solution: using copper, zinc, cadmium, tin, bismuth, iron, aluminium, manganese, titanium, nickel, chromium, cobalt mixing mark
Quasi- solution prepares the series of tasks curve standard solution of 6 or more concentration in gradient respectively；
The mass concentration of S3, measurement sample solution, blank test solution: the working curve standard solution that the step S2 is configured
It is introduced into inductively coupled plasma atomic emission spectrometer, at the wavelength that each element is selected, measures the working curve mark
The spectral intensity of quasi- solution produces the standard solution working curve of each element；When working curve linearly dependent coefficient >=
When 0.999, the concentration of the sample solution concentration and the blank test solution is measured, according to the relationship of spectral intensity and concentration
The lead concentrate sample is obtained respectively, copper, zinc, cadmium, tin, bismuth, iron, aluminium, manganese, titanium, nickel, chromium, cobalt element in blank test solution
Mass concentration c, mass concentration co；
S4, according to formulaCalculate copper, zinc, cadmium, tin, bismuth,
The content of iron, aluminium, manganese, titanium, nickel, chromium, cobalt element；
In formula:
W (x) --- the mass fraction of element to be measured, unit are percentage；
C --- the mass concentration of element to be measured in sample solution, unit is micrograms per millilitre；
co--- the mass concentration of element to be measured in blank test solution, unit is micrograms per millilitre；
V --- sample solution volume, unit are milliliter；
m0--- the quality of sample, unit are gram；
R --- the coefficient of dilution.
2. the ICP-AES detection method of micronutrient levels in lead concentrate according to claim 1, which is characterized in that choosing
Constituent content to be measured is selected to fall between the standard curve concentration of series standard solution drafting；After the constant volume of step S1 preparation
When the concentration range of sample solution is more than or equal to 100 μ g/mL, sample solution after the constant volume of step S1 preparation point take
Dilution divides the constant volume sample solution concentration after taking dilution less than 100 μ g/mL.
3. the ICP-AES detection method of micronutrient levels in lead concentrate according to claim 2, which is characterized in that institute
State step S1 preparation constant volume after sample solution concentration range be more than or equal to 100 μ g/mL when, the step S1 preparation is determined
Sample solution carries out point taking dilution after appearance, and the constant volume sample solution concentration after point taking dilution is no more than 80 μ g/mL.
4. the ICP-AES detection method of micronutrient levels in lead concentrate according to claim 1, which is characterized in that copper,
Zinc, cadmium, tin, bismuth, iron, aluminium, manganese, titanium, nickel, chromium, cobalt element series of tasks curve concentration of standard solution are 0 μ g/mL, 0.1 μ respectively
g/mL、0.5μg/mL、2μg/mL、10μg/mL、50μg/mL。
5. the ICP-AES detection method of micronutrient levels in lead concentrate according to claim 4, which is characterized in that copper,
Zinc, cadmium, tin, bismuth, iron, aluminium, manganese, titanium, nickel, chromium, cobalt element series of tasks curve standard solution configuration method be: pipette respectively
Copper, zinc, cadmium, tin, bismuth, iron, aluminium, manganese, titanium, nickel, chromium, mixed standard solution 0.00mL, 0.05mL of cobalt, 0.25mL, 1.00mL,
5.00mL, 25.00mL dilute constant volume in 50mL volumetric flask, with nitric acid；The nitric acid is the nitric acid solution and 20 volumes of 1 volume
Pure water mix.
6. the ICP-AES detection method of micronutrient levels in lead concentrate according to claim 1, which is characterized in that institute
It states in step S2, the preparation dilution of the mixed standard solution dilutes constant volume using nitric acid；The nitric acid is that the nitric acid of 1 volume is molten
Liquid and the pure water of 20 volumes mix.
7. the ICP-AES detection method of micronutrient levels in lead concentrate according to claim 1, which is characterized in that survey
During fixed, what is used is Cleaning analysis container, and acid is high purity acid, water is quartzy sub-boiling distillation water.
8. according to claim 1 in lead concentrate described in -7 micronutrient levels ICP-AES detection method, which is characterized in that
The lead bullion sample ore product should be pre-processed before the step S1: firstly, the standard screen by the aperture 0.149mm screens；So
Afterwards, in 105 DEG C of -115 DEG C of drying 2h；Later, be placed in drier be cooled to room temperature it is spare.
9. the ICP-AES detection method of micronutrient levels in lead concentrate according to claim 8, which is characterized in that institute
The light-splitting chamber for stating inductive coupling plasma emission spectrograph has the function of to vacuumize or purging, running parameter are as follows: power
1200W, fog chamber press 32Psi, pump 1.2mL/min, time of integration 25S.
10. the ICP-AES detection method of micronutrient levels in lead concentrate according to claim 9, which is characterized in that institute
Stating beaker material is polytetrafluoroethylene (PTFE)；Assay balance sensibility reciprocal 0.1mg, drying box accuracy of temperature control ± 5 DEG C.
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| CN110749486A (en) * | 2019-11-22 | 2020-02-04 | 长春黄金研究院有限公司 | Method for measuring tin content in crude lead |
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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 |
| CN114578028A (en) * | 2022-02-23 | 2022-06-03 | 复旦大学 | Simulation test and evaluation method for water resistance of vehicle transmission oil additive |
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