CN104316512A - Method for measuring content of barium element in nucleating agent by adopting ICP-AES - Google Patents

Abstract

The invention relates to a method for measuring the content of barium element in a nucleating agent, and in particular relates to a method for measuring the content of the barium element in the nucleating agent by adopting an ICP-AES. The method comprises the steps of preparing a standard curve solution of the barium, preparing the standard curve solution, and measuring the standard curve solution on an inductively coupled plasma emission spectrometer; drawing a working curve by taking the concentration of the barium in the standard curve solution as the abscissa and the intensity of an emission spectrum of the barium in the standard curve solution as the ordinate; measuring liquid to be measured under the measurement condition being the same as that the former step; and finding the concentration of the barium in the liquid to be measured in the working curve, and then calculating the content of the barium in a sample to be measured. The method is simple in steps, low in cost, slight in pollution and short in flow process, is especially suitable for analyzing low-content elements, and is high in analysis speed, high in accuracy and suitable for production and detection; furthermore, the classical chemical analysis method can be replaced by adopting the method, so that the detection flow process is shortened, and the detection efficiency is improved.

Description

A kind of ICP-AES method measures the method for barium constituent content in inovulant

Technical field

The present invention relates to a kind of method measuring barium constituent content in inovulant, especially relate to a kind of method that ICP-AES method measures barium constituent content in inovulant.

Background technology

Inovulant is applied to the history that cast iron industry has nearly 80 years.Its Main Function to promote graphitization, reduces chilling tendency, and increase eutectic cell quantity, crystal grain thinning, uniform formation, improves graphite form and distribution situation.Wherein barium is comparatively ideal constituent element, and have the stronger anti-ageing ability of moving back and very strong nucleation ability, and baric inovulant fusing point is low, easily absorbed, during process, scum silica frost is few.

The mensuration of inoculant element now mainly adopts classical chemical analysis method, as barium content in inovulant adopts barium sulfategravimetry to measure, must through the chemical treatment of complexity, sense cycle is long, complex operation, application reagent is many, and the result recorded is not felt quite pleased, and can not meet the requirement of high added value ironcasting to high-purity raw and auxiliary material impurity analysis.

Also do not overcome the method for above-mentioned defect at present.

Summary of the invention

The object of the invention is the defect overcoming prior art, there is provided a kind of step simple, be that a cost is low, pollute few, flow process is short, the analysis, the analysis speed that are particularly useful for Minor element are fast, accuracy is high, is applicable to produce and detect, the chemico-analytic method of alternative classics simultaneously, shorten testing process, a kind of ICP-AES method improving detection efficiency measures the method for barium constituent content in inovulant.

The present invention realizes in the following way:

ICP-AES method measures a method for barium constituent content in inovulant, it is characterized in that: the method comprises the steps:

A. the typical curve solution of barium is prepared;

B. configuration standard curve solution: take many parts with the high purity iron of sample to be tested Matrix Match as iron-based body original pattern, the barium Standard Stock solutions that 0 ~ 10mL concentration is 1000 μ g/mL is added successively in many parts of iron-based body original patterns, prepare the typical curve solution of many parts of barium again according to step a, its concentration range is 8 ~ 14 μ g/mL;

C. typical curve solution is measured on inductive coupling plasma emission spectrograph, with the concentration of the barium in typical curve solution for horizontal ordinate, the intensity of emission spectra of the barium in the typical curve solution measured is ordinate drawing curve, wherein, the analysis spectral line measuring the barium selected is 233.527nm;

D. measure test solution to be measured with the condition determination that step c is same, from described working curve, check in the concentration of barium in test solution to be measured, then calculate the content of barium in sample to be tested;

The described typical curve solution methods preparing barium is for taking 0.1000g sample in 200mL polytetrafluoroethylene beaker, use a small amount of water-wet, add 8 ~ 12mL nitric acid, about 5mL hydrofluorite is carefully dripped with plastic tube, stop to intense reaction, add 6 ~ 8mL hydrochloric acid, be placed on electric furnace and be slowly heated to test portion dissolving completely, add 6 ~ 10mL perchloric acid, low-temperature heat is to emitting perchloric acid cigarette, wall of cup is rinsed with water, continuing low-temperature heat smolders to surplus about 2mL ~ 3mL solution, slightly cold, add 15 ~ 30mL hydrochloric acid, heating for dissolving salt, be cooled to room temperature, test solution is moved in 500mL volumetric flask, scale is diluted to ultrapure water, shake up,

Described inductive coupling plasma emission spectrograph, its running parameter is: radio-frequency power 1300W, and assisted gas flow is 0.2L/min, and plasma flow is 15L/min, fog chamber pressure 0.55psi, pump speed 1.50r/min, multiplicity 3 times;

Described iron-based body original pattern comprises identical matrix composition with sample to be tested, but the content that described iron-based body original pattern does not comprise barium element or wherein barium element is known;

In described test specimens, the content of barium is ω M, calculates according to following formula,

${\mathrm{\ω}}_M=\frac{C_M\×V}{m\×{10}^6}\×100$

Wherein, C _mrepresent the concentration of barium in test solution to be measured, unit is mcg/ml; V represents the volume of test solution to be measured, and unit is milliliter; M represents the quality of sample to be tested, and unit is gram.

The present invention has following effect:

1) step is simple, that a cost is low, pollute few, the feature of environmental protection method that flow process is short: method provided by the invention comprises the steps: typical curve solution, the configuration standard curve solution of preparing barium: take many parts with the high purity iron of sample to be tested Matrix Match as iron-based body original pattern, the barium Standard Stock solutions that 0 ~ 10mL concentration is 1000 μ g/mL is added successively in many parts of iron-based body original patterns, prepare the typical curve solution of many parts of barium again according to step a, its concentration range is 8 ~ 14 μ g/mL; Typical curve solution is measured on inductive coupling plasma emission spectrograph, with the concentration of the barium in typical curve solution for horizontal ordinate, the intensity of emission spectra of the barium in the typical curve solution measured is ordinate drawing curve, wherein, the analysis spectral line measuring the barium selected is 233.527nm; Measure test solution to be measured with the condition determination that step c is same, from described working curve, check in the concentration of barium in test solution to be measured, then calculate the content of barium in sample to be tested.

2) accuracy is high, simple and efficient, meets the needs produced and detect: method provided by the invention is applied to the detection of barium element in inovulant, and accuracy is high, simple and efficient, meets the needs produced and detect, has novelty.

3) sense cycle significantly shortens: method provided by the invention is compared with traditional chemical detection method, the detection method sample pretreating process that application ICP-AES method of the present invention measures barium content in inovulant is simple, sense cycle significantly shortens, and can improve 60% with manual wet-way analysis relative efficiency.

4) be applicable to produce and detect, the chemico-analytic method of alternative classics simultaneously, shorten testing process, improve detection efficiency: the scope that method provided by the invention measures barium constituent content is 4% ~ 7%, and its analysis result is accurate, recovery of standard addition is 94.16% ~ 101.46%, error <0.2%, relative standard deviation is 0.72%, can meet barium in inovulant and contain quantitative analysis requirement, guarantee the composition of inovulant, for the quality control of foundry goods provides guarantee.

Embodiment

ICP-AES method measures a method for barium constituent content in inovulant, it is characterized in that: the method comprises the steps:

A. the typical curve solution of barium is prepared;

B. configuration standard curve solution: take many parts with the high purity iron of sample to be tested Matrix Match as iron-based body original pattern, the barium Standard Stock solutions that 0 ~ 10mL concentration is 1000 μ g/mL is added successively in many parts of iron-based body original patterns, prepare the typical curve solution of many parts of barium again according to step a, its concentration range is 8 ~ 14 μ g/mL;

C. typical curve solution is measured on inductive coupling plasma emission spectrograph, with the concentration of the barium in typical curve solution for horizontal ordinate, the intensity of emission spectra of the barium in the typical curve solution measured is ordinate drawing curve, wherein, the analysis spectral line measuring the barium selected is 233.527nm;

D. measure test solution to be measured with the condition determination that step c is same, from described working curve, check in the concentration of barium in test solution to be measured, then calculate the content of barium in sample to be tested.

The described typical curve solution methods preparing barium is for taking 0.1000g sample in 200mL polytetrafluoroethylene beaker, use a small amount of water-wet, add 8 ~ 12mL nitric acid, about 5mL hydrofluorite is carefully dripped with plastic tube, stop to intense reaction, add 6 ~ 8mL hydrochloric acid, be placed on electric furnace and be slowly heated to test portion dissolving completely, add 6 ~ 10mL perchloric acid, low-temperature heat is to emitting perchloric acid cigarette, wall of cup is rinsed with water, continuing low-temperature heat smolders to surplus about 2mL ~ 3mL solution, slightly cold, add 15 ~ 30mL hydrochloric acid, the concentration of hydrochloric acid is 1:3, heating for dissolving salt, be cooled to room temperature, test solution is moved in 500mL volumetric flask, scale is diluted to ultrapure water, shake up.

Described inductive coupling plasma emission spectrograph, its running parameter is: radio-frequency power 1300W, and assisted gas flow is 0.2L/min, and plasma flow is 15L/min, fog chamber pressure 0.55psi, pump speed 1.50r/min, multiplicity 3 times.

Described iron-based body original pattern comprises identical matrix composition with sample to be tested, but the content that described iron-based body original pattern does not comprise barium element or wherein barium element is known.

In described test specimens, the content of barium is ω M, calculates according to following formula,

${\mathrm{\&omega;}}_M=\frac{C_M\&times;V}{m\&times;{10}^6}\&times;100$

Wherein, C _mrepresent the concentration of barium in test solution to be measured, unit is mcg/ml (μ g/mL); V represents the volume of test solution to be measured, and unit is milliliter (mL); M represents the quality of sample to be tested, and unit is gram (g).

Claims (5)

1. ICP-AES method measures a method for barium constituent content in inovulant, it is characterized in that: the method comprises the steps:

A. the typical curve solution of barium is prepared;

B. configuration standard curve solution: take many parts with the high purity iron of sample to be tested Matrix Match as iron-based body original pattern, the barium Standard Stock solutions that 0 ~ 10mL concentration is 1000 μ g/mL is added successively in many parts of iron-based body original patterns, prepare the typical curve solution of many parts of barium again according to step a, its concentration range is 8 ~ 14 μ g/mL;

C. typical curve solution is measured on inductive coupling plasma emission spectrograph, with the concentration of the barium in typical curve solution for horizontal ordinate, the intensity of emission spectra of the barium in the typical curve solution measured is ordinate drawing curve, wherein, the analysis spectral line measuring the barium selected is 233.527nm;

D. measure test solution to be measured with the condition determination that step c is same, from described working curve, check in the concentration of barium in test solution to be measured, then calculate the content of barium in sample to be tested.

2. a kind of ICP-AES method as claimed in claim 1 measures the method for barium constituent content in inovulant, it is characterized in that: the described typical curve solution methods preparing barium is for taking 0.1000g sample in 200mL polytetrafluoroethylene beaker, use a small amount of water-wet, add 8 ~ 12mL nitric acid, about 5mL hydrofluorite is carefully dripped with plastic tube, stop to intense reaction, add 6 ~ 8mL hydrochloric acid, be placed on electric furnace and be slowly heated to test portion dissolving completely, add 6 ~ 10mL perchloric acid, low-temperature heat is to emitting perchloric acid cigarette, wall of cup is rinsed with water, continuing low-temperature heat smolders to surplus about 2mL ~ 3mL solution, slightly cold, add 15 ~ 30mL hydrochloric acid, heating for dissolving salt, be cooled to room temperature, test solution is moved in 500mL volumetric flask, scale is diluted to ultrapure water, shake up.

3. a kind of ICP-AES method as claimed in claim 1 measures the method for barium constituent content in inovulant, it is characterized in that: described inductive coupling plasma emission spectrograph, its running parameter is: radio-frequency power 1300W, assisted gas flow is 0.2L/min, plasma flow is 15L/min, fog chamber pressure 0.55psi, pump speed 1.50r/min, multiplicity 3 times.

4. a kind of ICP-AES method as claimed in claim 1 measures the method for barium constituent content in inovulant, it is characterized in that: described iron-based body original pattern comprises identical matrix composition with sample to be tested, but the content that described iron-based body original pattern does not comprise barium element or wherein barium element is known.

5. a kind of ICP-AES method as claimed in claim 1 measures the method for barium constituent content in inovulant, it is characterized in that: in described test specimens, the content of barium is ω _m, calculate according to following formula,

${\mathrm{\&omega;}}_M=\frac{C_M\&times;V}{m\&times;{10}^6}\&times;100$

Wherein, C _mrepresent the concentration of barium in test solution to be measured, unit is mcg/ml; V represents the volume of test solution to be measured, and unit is milliliter; M represents the quality of sample to be tested, and unit is gram.