CN105973873A - Method for determination of contents of metal elements in nodular cast iron by ICP-OES method - Google Patents
Method for determination of contents of metal elements in nodular cast iron by ICP-OES method Download PDFInfo
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- CN105973873A CN105973873A CN201610273169.3A CN201610273169A CN105973873A CN 105973873 A CN105973873 A CN 105973873A CN 201610273169 A CN201610273169 A CN 201610273169A CN 105973873 A CN105973873 A CN 105973873A
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- G—PHYSICS
- G01—MEASURING; TESTING
- 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
Abstract
The invention relates to a method for determination of the contents of metal elements in nodular cast iron by an ICP-OES method, wherein the method comprises the following steps: (1) preparing a sample solution; (2) preparing a blank solution; (3) preparing a standard solution; (4) drawing a standard curve; and (5) using ICP-OES, determining the sample solution prepared in the step (1) and the blank solution prepared in the step (2), combining with the work curve obtained in the step (4), and thus obtaining the contents of Mn, Cu, Mg, Co, V, Ti, Ni and Cr in the sample. The detection method is easy to operate and high in sensitivity.
Description
Technical field
The present invention relates to a kind of measure the method for metal element content in spheroidal graphite cast-iron, be specifically related to a kind of utilization
ICP-OES method measures the method for metal element content in spheroidal graphite cast-iron, belongs to chemical analysis technology field.
Background technology
Spheroidal graphite cast-iron is a kind of grey cast-iron with excellent mechanical properties.Machine building industry obtains
Extensively application.Along with development, user is more and more higher to prescription, thus fast to the chemical element of material
It is essential that speed is analyzed, and in spheroidal graphite cast-iron, the element such as copper, manganese, magnesium, cobalt, vanadium, chromium, nickel, titanium generally uses former
Sub-absorption process, volumetric method, spectrophotography is measured respectively, but above-mentioned method of testing required time is relatively
Long, process is relatively complicated.
Summary of the invention
The technical problem to be solved is for state of the art offer is a kind of simple to operate and accuracy rate is high
ICP-OES method measure the method for metal element content in spheroidal graphite cast-iron.
A kind of ICP-OES method of the present invention measures the method for metal element content in spheroidal graphite cast-iron, including
Following steps:
(1) configuration test liquid；Sample is completely dissolved in inorganic mixed acid, prepares and be completely dissolved liquid, the most molten
Solve in liquid, sample: ratio=0.2g:10～30mL of inorganic mixed acid, the described liquid that is completely dissolved is moved to capacity
In Ping, constant volume, prepare test liquid, be completely dissolved liquid: volume ratio=10 of test liquid～30:100；
(2) configuration blank solution；According to step (1), high purity iron is processed by the processing procedure of sample, prepare sky
White liquor；
(3) configuration standard solution；It is respectively configured the series mark of Mn, Cu, Mg, Co, V, Ti, Ni, Cr
Quasi-solution；
(4) standard curve is drawn；The standard solution configured for step (3), utilizes ICP-OES to be measured,
Obtain the working curve of signal intensity and each concentration of element；
(5) utilize ICP-OES, select the optimized analysis ripple of Mn, Cu, Mg, Co, V, Ti, Ni, Cr
Long, test liquid that determination step (1) configures and the blank solution that step (2) configures, the work that integrating step (4) obtains
Curve, obtains the content of Mn, Cu, Mg, Co, V, Ti, Ni, Cr in sample.
Preferably, described inorganic mixed acid is the mixture of hydrochloric acid and nitric acid；
Preferably, to be respectively top grade pure for described hydrochloric acid and/or nitric acid；
Preferably, hydrochloric acid: volume ratio=1 of nitric acid～5:1, preferably 3:1.
Preferably, in step (1), the configuration process of test liquid is: is dissolved in hydrochloric acid by sample, is heated to emitting
Bubble, adds nitric acid, continues to heat until sample is completely dissolved, cooling, prepares and be completely dissolved liquid, will
The described liquid that is completely dissolved moves in volumetric flask, uses water constant volume, prepares test liquid；
Preferably, first sample is dissolved in salt aqueous acid, is heated to effervescent, add nitric acid, continue
Continuous heating, until sample is completely dissolved, cools down, and prepares and is completely dissolved liquid, moves to hold by the described liquid that is completely dissolved
In measuring bottle, use water constant volume, prepare test liquid；
Preferably, in described salt aqueous acid, water: volume ratio=1 of hydrochloric acid～5:3, preferably 2:3.
The above-mentioned processing method to sample is applicable to not contain the sample not allowing carbide.
When, containing when not allowing carbide in sample, need sample does following process: described inorganic mixed acid
Mixture for perchloric acid, hydrochloric acid and nitric acid；
Preferably, one or more in described perchloric acid, hydrochloric acid, nitric acid are that top grade is pure；
Preferably, perchloric acid: hydrochloric acid: volume ratio=0.5 of nitric acid～3:0.5～3:0.5～3, preferably 1:1:1.
In step (1), the configuration process of test liquid is: sample is dissolved in perchloric acid, is heated to height of smoldering
Chloric acid cigarette, cooling, then it is separately added into hydrochloric acid and nitric acid, heating, until sample is completely dissolved, cools down, and prepares
It is completely dissolved liquid, the described liquid that is completely dissolved is moved in volumetric flask, uses water constant volume, prepare test liquid；
Preferably, sample is dissolved in perchloric acid, is heated to perchloric acid cigarette of smoldering, cooling, it is separately added into
Salt aqueous acid and nitric acid, heating until sample is completely dissolved, cools down, prepares and be completely dissolved liquid, by institute
State and be completely dissolved liquid and move in volumetric flask, use water constant volume, prepare test liquid；
Preferably, in described salt aqueous acid, water: volume ratio=1 of hydrochloric acid～5:1, preferably 2:1.
Preferably, in step (2), in described high purity iron, the mass fraction of ferrum is more than 99.98%.
Preferably, the parameter of ICP-OES is set to: nebulizer gas flow is 0.3～2L/min, waits in vitro
Radio-frequency power is 1100～1500W, and plasma gas flow amount is 10～15L/min, and auxiliary gas flow amount is
0.1～0.8L/min, pump discharge is 1～3mL/min；
Preferably, the parameter of ICP-OES is set to: nebulizer gas flow is 0.55L/min, waits and penetrates in vitro
Frequently power is 1300W, and plasma gas flow amount is 12L/min, and auxiliary gas flow amount is 0.2L/min,
Pump discharge is 1.5mL/min.
Preferably, in step (3), the series standard solution of Mn, Cu, Mg, Co, V, Ti, Ni, Cr
Configuration process be according to step (1), 6 parts of high purity irons to be processed by the processing procedure of sample respectively, system
Obtain 6 parts for the treatment of fluids, respectively 6 parts of described treatment fluids moved in 100mL volumetric flask, prepare 6 parts of initial liquid,
In every part of initial liquid, the standard of Mn, Cu, Mg, Co, V, Ti, Ni, Cr is added respectively according to following table
Solution, constant volume, prepare the series standard solution of each metallic element；
In technique scheme, corresponding every kind of metallic element to be measured has been respectively configured 6 parts of standard solution, and
The addition graded of standard solution so that standard solution curve point is the most, the most intensive, curve is the most accurate,
The most representative, and then the scope of measurement is the widest.
Preferably, in step (3), in described high purity iron, the mass fraction of ferrum is more than 99.98%.
Compared with prior art, it is an advantage of the current invention that: Inductively coupled plasma optical emission spectrometer (ICP)
Being the new tool of modern analysis, ICP-OES method has highly sensitive, the detection limit end, and measurement range is wide, soon
Speed, the advantage such as multielement simultaneous determination.It is now widely used for geology, environmental protection, chemical industry, biological medicine, food
Product, metallurgical, in the aspect sample such as agricultural, element is qualitative, quantitative analysis.
This method of testing is compared with other method of testings, and it is simple to operate, and accuracy rate is high.
Detailed description of the invention
Below in conjunction with embodiment, the present invention is described in further detail.
The present embodiment specifically uses ICP-OES method to measure the content of metallic element in spheroidal graphite cast-iron, specifically uses
The ICP-OES-8000 type spectrogrph that equipment is Perkinelmer Instruments LLC, the parameter of instrument is set to:
Quarter bend: the quartzy standard quarter bend of instrument first wife；Nebulizer gas flow: 0.55L/min.Etc. in vitro radio frequency merit
Rate: 1300W. plasma gas flow amount: 12L/min；Auxiliary gas flow amount: 0.2L/min；Pump discharge:
1.5mL/min；Sample feeding analyze time delay: 20 seconds；Number of repetition: 2.
The present embodiment ICP-OES method measures the method for metal element content in spheroidal graphite cast-iron, comprises the steps:
(1) configuration test liquid；Weigh about 0.2000g sample to be placed in 200mL beaker, add 10mL water and 15mL
Hydrochloric acid (top grade is pure), cap upper surface ware, it is placed on warm table and is slowly heated to emitting air pocket, warm table temperature
Degree controls at 200～300 DEG C, is cooled to room temperature and is carefully added into 5mL nitric acid (top grade is pure), continues heating
Decompose completely to sample.Contain as samples and do not allow carbide, 5mL perchloric acid (top grade is pure) can be added, heating
To emitting perchloric acid cigarette 3～5min, adding 10mL water after cooling, 5mL hydrochloric acid (top grade is pure) shakes up, then adds 5mL
Nitric acid, heating for dissolving salt, it is cooled to room temperature, moves to solution, in 100mL volumetric flask, be diluted with water to
Scale mixes, and prepares test liquid.
The acidity of test liquid prepared by this step substantially about 10%, this acidity can guarantee that obtain stronger clean
Intensity.
The present embodiment is when determining test liquid acidity, through experimental verification: prepare a series of a certain amount of respectively
Concentration of element, Mn (2mg/L), Cu (2mg/L), Mg (2mg/L), Co (2mg/L), V (2mg/L),
Ti (2mg/L), Ni (2mg/L), Cr (2mg/L), be separately added into different amounts of HCl, HNO3,
Deduct HCl, HNO simultaneously3Blank, obtains the plain intensity of the unit under different acidity, and test proves along with acidity
Increase, clean strength decrease.
(2) configuration blank solution；Weighing 0.2g high purity iron, in high purity iron, the mass fraction of ferrum is more than 99.98%,
According to step (1), high purity iron is processed by the processing procedure of sample, prepare blank solution；
Because spheroidal graphite cast-iron contains substantial amounts of ferrum, would have to consider the interference problem of ferrum in an experiment, use
High purity iron replaces blank, and is processed into aqueous standard method curve with the high purity iron of equal quality and sample simultaneously
The interference of ferrum can be eliminated.
(3) configuration standard solution；It is respectively configured the series mark of Mn, Cu, Mg, Co, V, Ti, Ni, Cr
Quasi-solution；Concrete configuration process is: (in high purity iron, the mass fraction of ferrum is more than to weigh about 0.2g high purity iron
99.98%) 6 parts are respectively placed in 200ml beaker, according to step (1) to the processing procedure of sample respectively to 6
Part high purity iron carries out processing dissolving, is cooled to room temperature, prepares 6 parts for the treatment of fluids, respectively by 6 parts of described process
Liquid moves in 100mL volumetric flask, prepares 6 parts of initial liquid, adds respectively according to following table in every part of initial liquid
The standard solution of Mn, Cu, Mg, Co, V, Ti, Ni, Cr, constant volume, prepare each metallic element is
Row standard solution；
| Metallic element | Concentration of standard solution (mg/L) | Every part of initial liquid adds the volume/ml of standard solution |
| Mn | 1000 | 0.1,0.2,0.4,0.8,1.6,3.2 |
| Cu | 100 | 0.2,0.4,0.8,1.6,3.2,6.4 |
| Mg | 100 | 0.1,0.2,0.4,0.8,1.6,3.2 |
| Co | 100 | 0.05,0.1,0.2,0.4,0.8,1.6 |
| V | 100 | 0.1,0.2,0.4,0.8,1.6,3.2 |
| Ti | 200 | 0.1,0.2,0.4,0.8,1.6,3.2 |
| Ni | 100 | 0.1,0.2,0.4,0.8,1.6,3.2 |
| Cr | 100 | 0.1,0.2,0.4,0.8,1.6,3.2 |
Configured the series standard solution of each element according to above table after, it is ensured that in series standard solution,
The mass percent of each metallic element lays respectively at following scope: Mn 0.05～1.6%, Cu 0.01～0.32%,
Mg 0.005～0.16%, Co 0.0025～0.08%, V 0.005～0.16%, Ti 0.01～0.32%, Ni
0.005～0.16%, Cr 0.005～0.16%.In above-mentioned series standard solution, the content of each element can ensure sample
In each element content within the above range.
(4) standard curve is drawn；The series standard solution configured for step (3), utilizes ICP-OES to survey
Fixed, obtain the working curve of signal intensity and each concentration of element；Wherein, abscissa is each metallic element series
The concentration (mg/L) of standard solution, vertical coordinate is that plasma emission spectroscopy is to each element variable concentrations
Emissive porwer, OES-8000 system automatically generates；
(5) utilize ICP-OES, select the optimized analysis ripple of Mn, Cu, Mg, Co, V, Ti, Ni, Cr
Long, test liquid that determination step (1) configures and the blank solution that step (2) configures, the work that integrating step (4) obtains
Curve, obtains the content of Mn, Cu, Mg, Co, V, Ti, Ni, Cr in sample.
Wherein, optimized analysis wavelength and the corresponding detection limit of each metallic element are as shown in table 1；Each metal
The computing formula of constituent content is: [A × V × f × 10-6/mo] × 100, wherein A is the concentration (mg/L) recorded,
V be constant volume (mL), f be extension rate, moFor sample mass.
The optimized analysis wavelength of each metallic element of table 1. and corresponding detection limit
| Metallic element | Wavelength (nm) | Detection limit DL (mg/L) |
| Cu | 327.393 | 0.02 |
| Mg | 285.213 | 0.0016 |
| Mn | 257.610 | 0.02 |
| Ni | 231.604 | 0.04 |
| Cr | 267.716 | 0.05 |
| V | 310.230 | 0.02 |
| Co | 228.616 | 0.03 |
| Ti | 307.864 | 0.03 |
Table 2～9 is the present embodiment detection method and the compareing, by table 2～9 of each metallic element traditional test methods
Understanding, this detection method accuracy is higher.
Table 2. this method and GB/T223.4-2008 constant-current titration or visual titration measuring manganese result synopsis
Table 3. this method is analyzed method Flame Atomic Absorption Spectrometry with GB/T223.53-1987 iron and steel and alloy and is divided
Light Photometric Determination of Copper result synopsis
Table 4. this method analyzes method Flame Atomic Absorption Spectrometry light splitting light with GB/T223.53-1987 iron and steel and alloy
Degree method measures magnesium result synopsis
Table 5. method analyzes method nitroso-R-salt spectrphotometric method for measuring cobalt result with GB/T223.22 iron and steel and alloy
Synopsis
Table 6. method analyzes method measuring vanadium by ferrous ammonium sulfate capacitance result with GB/T223.13 iron and steel and alloy
Synopsis
Table 7. method analyzes method chromotropic acid spectrophotometry titanium result with GB/T223.16 iron and steel and alloy
Synopsis
Table 8. method is analyzed method nickel dimethylglyoximate Cerium-group REE with GB/T223.23 iron and steel and alloy and is measured nickel
Result synopsis
Table 9. method and GB/T223.11 iron and steel and alloy are analyzed method Ammonium persulfate. oxidation volumetric method and are measured chromium knot
Really synopsis
Above content is only presently preferred embodiments of the present invention, for those of ordinary skill in the art, according to this
The thought of invention, the most all will change, and this specification content is not
It is interpreted as limitation of the present invention.
Claims (9)
1. an ICP-OES method measures the method for metal element content in spheroidal graphite cast-iron, it is characterised in that
Comprise the steps:
(1) configuration test liquid；Sample is completely dissolved in inorganic mixed acid, prepares and be completely dissolved liquid, the most molten
Solve in liquid, sample: ratio=0.2g:10～30mL of inorganic mixed acid, the described liquid that is completely dissolved is moved to capacity
In Ping, constant volume, prepare test liquid, be completely dissolved liquid: volume ratio=10 of test liquid～30:100；
(2) configuration blank solution；According to step (1), high purity iron is processed by the processing procedure of sample, prepare sky
White liquor；
(3) configuration standard solution；It is respectively configured the series mark of Mn, Cu, Mg, Co, V, Ti, Ni, Cr
Quasi-solution；
(4) standard curve is drawn；The standard solution configured for step (3), utilizes ICP-OES to be measured,
Obtain the working curve of signal intensity and each concentration of element；
(5) utilize ICP-OES, select the optimized analysis ripple of Mn, Cu, Mg, Co, V, Ti, Ni, Cr
Long, test liquid that determination step (1) configures and the blank solution that step (2) configures, the work that integrating step (4) obtains
Curve, obtains the content of Mn, Cu, Mg, Co, V, Ti, Ni, Cr in sample.
2. the method for claim 1, it is characterised in that: described inorganic mixed acid is hydrochloric acid and nitric acid
Mixture；
Preferably, to be respectively top grade pure for described hydrochloric acid and/or nitric acid；
Preferably, hydrochloric acid: volume ratio=1 of nitric acid～5:1, preferably 3:1.
3. method as claimed in claim 2, it is characterised in that: in step (1), the configuration process of test liquid
For: sample is dissolved in hydrochloric acid, is heated to effervescent, add nitric acid, continue heating until sample is complete
Dissolve, cooling, prepare and be completely dissolved liquid, the described liquid that is completely dissolved is moved in volumetric flask, constant volume, prepare
Test liquid；
Preferably, first sample is dissolved in salt aqueous acid, is heated to effervescent, add nitric acid, continue
Continuous heating, until sample is completely dissolved, cools down, and prepares and is completely dissolved liquid, moves to hold by the described liquid that is completely dissolved
In measuring bottle, constant volume, prepare test liquid；
Preferably, in described salt aqueous acid, water: volume ratio=1 of hydrochloric acid～5:3, preferably 2:3.
4. the method for claim 1, it is characterised in that: described inorganic mixed acid is perchloric acid, salt
Acid and the mixture of nitric acid；
Preferably, one or more in described perchloric acid, hydrochloric acid, nitric acid are that top grade is pure；
Preferably, perchloric acid: hydrochloric acid: volume ratio=0.5 of nitric acid～3:0.5～3:0.5～3, preferably 1:1:1.
5. method as claimed in claim 4, it is characterised in that: in step (1), the configuration process of test liquid
For: sample being dissolved in perchloric acid, is heated to smoldering, be separately added into hydrochloric acid and nitric acid after cooling again, heating is straight
It is completely dissolved to sample, cooling, prepares and be completely dissolved liquid, the described liquid that is completely dissolved is moved in volumetric flask,
Constant volume, prepares test liquid；
Preferably, sample is dissolved in perchloric acid, is heated to smoldering, cooling, it is separately added into salt aqueous acid
And nitric acid, heating until sample is completely dissolved, cools down, prepares and be completely dissolved liquid, be completely dissolved liquid by described
Move in volumetric flask, constant volume, prepare test liquid；
Preferably, in described salt aqueous acid, water: volume ratio=1 of hydrochloric acid～5:1, preferably 2:1.
6. the method for claim 1, it is characterised in that: in step (2), ferrum in described high purity iron
Mass fraction is more than 99.98%.
7. the method for claim 1, it is characterised in that the parameter of ICP-OES is set to: atomization
Device gas flow is 0.3～2L/min, and waiting in vitro radio-frequency power is 1100～1500W, plasma gas flow amount
Being 10～15L/min, auxiliary gas flow amount is 0.1～0.8L/min, and pump discharge is 1～3mL/min；
Preferably, the parameter of ICP-OES is set to: nebulizer gas flow is 0.55L/min, waits and penetrates in vitro
Frequently power is 1300W, and plasma gas flow amount is 12L/min, and auxiliary gas flow amount is 0.2L/min,
Pump discharge is 1.5mL/min.
8. the method for claim 1, it is characterised in that: in step (3), Mn, Cu, Mg,
The configuration process of the series standard solution of Co, V, Ti, Ni, Cr is, according to the step (1) process to sample
6 parts of high purity irons are processed by process respectively, prepare 6 parts for the treatment of fluids, are moved by 6 parts of described treatment fluids respectively
To 100mL volumetric flask, prepare 6 parts of initial liquid, according to following table respectively in every part of initial liquid add Mn,
The standard solution of Cu, Mg, Co, V, Ti, Ni, Cr, constant volume, prepare the series standard of each metallic element
Solution；
9. method as claimed in claim 8, it is characterised in that: in step (3), ferrum in described high purity iron
Mass fraction is more than 99.98%.
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| CN110470654A (en) * | 2019-08-22 | 2019-11-19 | 北京星航机电装备有限公司 | A method of with multielement content in ICP-OES method measurement Cr12MoV material |
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Application publication date: 20160928 |