CN117629985A - Alloy impurity phase quantitative detection method - Google Patents

Alloy impurity phase quantitative detection method Download PDF

Info

Publication number
CN117629985A
CN117629985A CN202311647222.8A CN202311647222A CN117629985A CN 117629985 A CN117629985 A CN 117629985A CN 202311647222 A CN202311647222 A CN 202311647222A CN 117629985 A CN117629985 A CN 117629985A
Authority
CN
China
Prior art keywords
alloy
concentration
standard curve
impurity
calculating
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN202311647222.8A
Other languages
Chinese (zh)
Inventor
佘昌俊
丁志东
张钰
易栓
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
ZHENJIANG PRODUCT QUALITY SUPERVISION INSPECTION CENTER
Original Assignee
ZHENJIANG PRODUCT QUALITY SUPERVISION INSPECTION CENTER
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by ZHENJIANG PRODUCT QUALITY SUPERVISION INSPECTION CENTER filed Critical ZHENJIANG PRODUCT QUALITY SUPERVISION INSPECTION CENTER
Priority to CN202311647222.8A priority Critical patent/CN117629985A/en
Publication of CN117629985A publication Critical patent/CN117629985A/en
Pending legal-status Critical Current

Links

Abstract

The invention discloses a quantitative detection method for alloy impurity phases, which comprises grinding, acid washing and dissolution, and application of photometry combined with flow injection analysis, so that quick and high-flux determination of impurities such as copper, zinc, nickel and the like in an alloy is realized. The method has the advantages that multiple steps are completed through a single instrument, the use cost and the operation complexity of the instrument are reduced, and meanwhile, the accuracy and the reliability of the method are improved through sensitivity calculation, relative error evaluation and a data processing algorithm. The innovative method provides a solution with stronger feasibility and higher efficiency for alloy impurity analysis, and is expected to be widely applied in practical application.

Description

Alloy impurity phase quantitative detection method
Technical Field
The invention relates to a quantitative detection method for alloy impurity phases.
Background
Conventional alloy impurity detection methods typically involve complex pretreatment steps and the use of multiple instruments, such as spark spectroscopy, atomic absorption spectroscopy, and the like. These methods suffer from the following drawbacks:
cumbersome pretreatment: the pretreatment process in the traditional method comprises the steps of grinding, acid washing, dissolving and the like, and the steps are time-consuming and labor-consuming, and are easy to introduce external pollution to influence accuracy.
The multi-instrument use: the combined use of various instruments adds complexity and cost to the analysis as well as increasing the technical difficulty of operation.
Limiting high throughput analysis: conventional methods generally require long analysis times, fail to meet the requirements for high throughput analysis, and limit the ability to monitor and react quickly in real time.
Technical limitations: in conventional methods, it is often limited by the sensitivity and stability of the instrument, which results in difficulties in accurate determination of low concentrations of impurities. Meanwhile, the control of experimental conditions and the establishment of a standard curve in the traditional method also face some technical difficulties.
Disclosure of Invention
The invention aims to provide a quantitative detection method for alloy impurity phases.
In order to achieve the above purpose, the invention is implemented according to the following technical scheme:
the invention comprises the following steps:
s1: grinding, pickling and dissolving an alloy sample containing impurities to be detected for later use; the grinding particle size was 200 mesh. The pickling is carried out by adopting a mixed solution of nitric acid and hydrochloric acid. The ratio of nitric acid to hydrochloric acid is 1:3, heating to 60-70 ℃ during pickling.
S2: preparing a corresponding reagent as a color reagent according to impurities to be detected; adding the solution in the step S1 into a color developing agent to form a color developing complex; measuring absorbance of the chromogenic complex using a spectrophotometer; according to a known standard curve, calculating the concentration of impurities to be detected in the sample;
s3: calculating the slope and intercept of a standard curve according to the sensitivity of the instrument and the measurement noise, determining the impurity concentration of the minimum reliable measurement according to the slope of the standard curve, comparing with the existing method, determining the relative error of the method, and evaluating the accuracy of the method; optimizing instrument parameters according to the result; the relative error is calculated using the following formula:
the accuracy of the evaluation method comprises reliability evaluation of the results, reliability and repeatability of the measurement results are evaluated by calculating relative error results, and for the data of multiple measurements, a control chart is drawn to monitor the stability of the method.
S4: comparing experimental results under different conditions, and calculating the average value and standard deviation of experimental data; and calculating the concentration of the impurity to be detected of the alloy sample by adopting a data processing algorithm on the detection data. For each experimental dataset under measurement conditions, the average value of the samples was calculatedAnd standard deviation s
Where n is the number of samples, x i Is the i-th data point.
The data processing algorithm carries out standard curve fitting and concentration calculation, and when the standard curve fitting is carried out, the fitting equation is as follows: y=mx=b
Wherein y is absorbance, x is concentration, m is slope, b is intercept, and the concentration of the impurity to be detected of the alloy sample is calculated according to a fitting equation.
The beneficial effects of the invention are as follows:
compared with the prior art, the method has the following technical effects:
simplifying the pretreatment steps:
according to the technical scheme, the sample pretreatment step is simplified by using the grinding step with the grinding granularity of 200 meshes, the acid washing of the nitric acid and hydrochloric acid mixed solution and the dissolution by selecting a proper solvent. This not only improves the efficiency of the experiment, but also reduces the possibility of external contamination.
A single instrument implements multiple steps:
the spectrophotometry is combined with flow injection analysis, and a plurality of steps of impurity detection including color development, absorbance measurement, standard curve fitting and the like are realized through a single instrument. This reduces the cost and complexity of instrument use while improving the reproducibility of the experiment.
Sensitivity and accuracy are improved:
the minimum reliably measured impurity concentration is determined by calculating the slope and intercept of the standard curve. The calculation of the relative error and the comparison with the traditional method further evaluate the accuracy of the method. By optimizing the instrument parameters, the sensitivity and accuracy of measurement are improved.
High throughput analysis and real-time monitoring:
by adopting flow injection analysis and combining a rapid and reliable photometry, the rapid and high-flux analysis of impurities to be detected in the alloy is realized. This makes the method suitable not only for laboratory environments, but also for applications where real-time monitoring is required.
Stability and reliability are improved:
the stability and the reliability of the method are evaluated through statistical analysis of experimental data, drawing of a control chart and calculation of relative errors. The repeatability and the credibility of the experimental result are ensured, and more reliable data support is provided for practical application.
By overcoming the defects of the traditional method, the technical scheme has higher efficiency, simpler and more convenient operation and better performance in the aspect of quantitative detection of alloy impurity phases.
Drawings
Fig. 1 is a flow chart of the present invention.
Detailed Description
The invention will be further described with reference to the accompanying drawings and specific embodiments, wherein the exemplary embodiments and descriptions of the invention are for purposes of illustration, but are not intended to be limiting.
As shown in fig. 1: the invention comprises the following steps:
s1: grinding, pickling and dissolving an alloy sample containing impurities to be detected for later use; the grinding particle size was 200 mesh. The pickling is carried out by adopting a mixed solution of nitric acid and hydrochloric acid. The ratio of nitric acid to hydrochloric acid is 1:3, heating to 60-70 ℃ during pickling.
S2: preparing a corresponding reagent as a color reagent according to impurities to be detected; adding the solution in the step S1 into a color developing agent to form a color developing complex; measuring absorbance of the chromogenic complex using a spectrophotometer; according to a known standard curve, calculating the concentration of impurities to be detected in the sample;
s3: calculating the slope and intercept of a standard curve according to the sensitivity of the instrument and the measurement noise, determining the impurity concentration of the minimum reliable measurement according to the slope of the standard curve, comparing with the existing method, determining the relative error of the method, and evaluating the accuracy of the method; optimizing instrument parameters according to the result; the relative error is calculated using the following formula:
the accuracy of the evaluation method comprises reliability evaluation of the results, reliability and repeatability of the measurement results are evaluated by calculating relative error results, and for the data of multiple measurements, a control chart is drawn to monitor the stability of the method.
S4: comparing experimental results under different conditions, and calculating the average value and standard deviation of experimental data; and calculating the concentration of the impurity to be detected of the alloy sample by adopting a data processing algorithm on the detection data. For each experimental dataset under measurement conditionsCalculating the average value of the samplesAnd standard deviation s
Where n is the number of samples, x i Is the i-th data point.
The data processing algorithm carries out standard curve fitting and concentration calculation, and when the standard curve fitting is carried out, the fitting equation is as follows: y=mx=b
Wherein y is absorbance, x is concentration, m is slope, b is intercept, and the concentration of the impurity to be detected of the alloy sample is calculated according to a fitting equation.
Embodiment one: determination of copper content
Sample preparation S1:
and (3) selecting an aluminum alloy sample containing copper impurities for mechanical grinding, and grinding the aluminum alloy sample into 200 meshes of particle fineness.
Acid washing and dissolution: the mixture of nitric acid and hydrochloric acid is used for pickling, and the ratio is 1:3. The pickling is carried out at the temperature of 65 ℃ to ensure that surface oxides and other pollutants are effectively removed. The sample is dissolved, and a proper solvent is selected to ensure complete dissolution of copper impurities.
Reagent preparation and color development S2:
BCA reagent was prepared as a color developer for copper ions.
Measurement of chromogenic Complex: the solution of step S1 is added to the BCA developer to form a color developing complex. The absorbance of the chromogenic complex was measured using a spectrophotometer.
Concentration calculation: the concentration of copper impurities in the sample was calculated spectrophotometrically using a known standard curve.
Sensitivity calculation and relative error evaluation S3:
sensitivity and relative error: the slope and intercept of the standard curve are calculated to determine the minimum reliably measured copper concentration. The accuracy of the method is evaluated using a relative error formula.
Optimizing instrument parameters: and optimizing instrument parameters according to the comparison result with the existing method.
Data statistics and processing S4:
statistical analysis of experimental data: and comparing experimental results under different conditions, and calculating the average value and standard deviation of experimental data.
Data processing algorithm: standard curve fitting and concentration calculation were performed using data processing algorithms. And calculating the concentration of copper impurities in the aluminum alloy sample according to the fitting equation.
Reliability evaluation of results: the relative error results are used to evaluate the reliability and repeatability of the measurement results. For data from multiple measurements, a control chart is drawn to monitor the stability of the method.
Standard curve equation: a=0.101 [ cu ] +0.017
Absorbance A of sample to be measured sample =0.325
Calculation of copper concentration from standard curve
The calculation results are as follows:
by simplifying the pretreatment steps and adopting the flow injection analysis combined photometry, the rapid and high-throughput analysis of the copper content is realized. Multiple steps are realized by a single instrument, so that the cost and the operation complexity are reduced, and the repeatability of the experiment is improved. By optimizing instrument parameters and evaluating relative errors, the accuracy and stability of the method are improved.
Embodiment two: determination of Zinc content
Sample preparation S1:
and (3) selecting an aluminum alloy sample containing zinc impurities for mechanical grinding, and grinding the aluminum alloy sample into 200 meshes of particle fineness.
Acid washing and dissolution: the mixture of nitric acid and hydrochloric acid is used for pickling, and the ratio is 1:3. The pickling is carried out at the temperature of 65 ℃ to ensure that surface oxides and other pollutants are effectively removed. The sample is dissolved, and proper solvent is selected to ensure that zinc impurities are completely dissolved.
Reagent preparation and color development S2:
a soft red reagent was prepared as a color developer for copper ions.
Measurement of chromogenic Complex: and (3) adding the solution obtained in the step (S1) into a soft red reagent color developing agent to form a color developing complex. The absorbance of the chromogenic complex was measured using a spectrophotometer.
Concentration calculation: the concentration of zinc impurities in the sample was calculated spectrophotometrically using a known standard curve.
Sensitivity calculation and relative error evaluation S3:
sensitivity and relative error: the slope and intercept of the standard curve are calculated to determine the minimum reliably measured zinc concentration. The accuracy of the method is evaluated using a relative error formula.
Optimizing instrument parameters: and optimizing instrument parameters according to the comparison result with the existing method.
Data statistics and processing S4:
statistical analysis of experimental data: and comparing experimental results under different conditions, and calculating the average value and standard deviation of experimental data.
Data processing algorithm: standard curve fitting and concentration calculation were performed using data processing algorithms. And calculating the concentration of zinc impurities in the aluminum alloy sample according to the fitting equation.
Reliability evaluation of results: the relative error results are used to evaluate the reliability and repeatability of the measurement results. For data from multiple measurements, a control chart is drawn to monitor the stability of the method.
Standard curve equation: a=0.202 [ zn ] +0.012
Absorbance A of sample to be measured sample =0.265
According to the standardCurve calculation of copper concentration
The calculation results are as follows:
by simplifying the pretreatment steps and adopting the flow injection analysis combined photometry, the rapid and high-flux analysis of the zinc content is realized. Multiple steps are realized by a single instrument, so that the cost and the operation complexity are reduced, and the repeatability of the experiment is improved. By optimizing instrument parameters and evaluating relative errors, the accuracy and stability of the method are improved.
Embodiment III: determination of Nickel content
Sample preparation S1:
and (3) selecting an aluminum alloy sample containing nickel impurities for mechanical grinding, and grinding the aluminum alloy sample into 200 meshes of particle fineness.
Acid washing and dissolution: the mixture of nitric acid and hydrochloric acid is used for pickling, and the ratio is 1:3. The pickling is carried out at the temperature of 65 ℃ to ensure that surface oxides and other pollutants are effectively removed. The sample is dissolved, and a proper solvent is selected to ensure that the nickel impurities are completely dissolved.
Reagent preparation and color development S2:
a soft red reagent was prepared as a color developer for copper ions.
Measurement of chromogenic Complex: and (3) adding the solution obtained in the step (S1) into a soft red reagent color developing agent to form a color developing complex. The absorbance of the chromogenic complex was measured using a spectrophotometer.
Concentration calculation: the concentration of nickel impurities in the sample was calculated spectrophotometrically using a known standard curve.
Sensitivity calculation and relative error evaluation S3:
sensitivity and relative error: the slope and intercept of the standard curve are calculated to determine the minimum reliably measured nickel concentration. The accuracy of the method is evaluated using a relative error formula.
Optimizing instrument parameters: and optimizing instrument parameters according to the comparison result with the existing method.
Data statistics and processing S4:
statistical analysis of experimental data: and comparing experimental results under different conditions, and calculating the average value and standard deviation of experimental data.
Data processing algorithm: standard curve fitting and concentration calculation were performed using data processing algorithms. And calculating the concentration of the nickel impurities in the aluminum alloy sample according to the fitting equation.
Reliability evaluation of results: the relative error results are used to evaluate the reliability and repeatability of the measurement results. For data from multiple measurements, a control chart is drawn to monitor the stability of the method.
Standard curve equation: a=0.046 [ n ] i ]+0.012
Absorbance A of sample to be measured sample =0.316
Calculation of copper concentration from standard curve
The calculation results are as follows:
by simplifying the pretreatment steps and adopting the flow injection analysis combined photometry, the rapid and high-throughput analysis of the nickel content is realized. Multiple steps are realized by a single instrument, so that the cost and the operation complexity are reduced, and the repeatability of the experiment is improved. By optimizing instrument parameters and evaluating relative errors, the accuracy and stability of the method are improved.
These three examples demonstrate the superiority of the newly proposed quantitative detection method of the alloy impurity phase over the conventional method. The novel method has greater feasibility and practicability in practical application by simplifying operation steps, reducing cost and improving experimental efficiency and accuracy.
The technical scheme of the invention is not limited to the specific embodiment, and all technical modifications made according to the technical scheme of the invention fall within the protection scope of the invention.

Claims (7)

1. The quantitative detection method of the alloy impurity phase is characterized by comprising the following steps of:
s1: grinding, pickling and dissolving an alloy sample containing impurities to be detected for later use;
s2: preparing a corresponding reagent as a color reagent according to impurities to be detected; adding the solution in the step S1 into a color developing agent to form a color developing complex; measuring absorbance of the chromogenic complex using a spectrophotometer; according to a known standard curve, calculating the concentration of impurities to be detected in the sample;
s3: calculating the slope and intercept of a standard curve according to the sensitivity of the instrument and the measurement noise, determining the impurity concentration of the minimum reliable measurement according to the slope of the standard curve, comparing with the existing method, determining the relative error of the method, and evaluating the accuracy of the method; optimizing instrument parameters according to the result;
s4: comparing experimental results under different conditions, and calculating the average value and standard deviation of experimental data; and calculating the concentration of the impurity to be detected of the alloy sample by adopting a data processing algorithm on the detection data.
2. The method for quantitatively detecting the impurity phase of an alloy according to claim 1, characterized by comprising the steps of: the grinding granularity in the step S1 is 200 meshes.
3. The method for quantitatively detecting the impurity phase of an alloy according to claim 1, characterized by comprising the steps of: and in the step S1, the pickling is performed by adopting a mixed solution of nitric acid and hydrochloric acid.
4. The method for quantitatively detecting the impurity phase of an alloy according to claim 3, wherein: the ratio of nitric acid to hydrochloric acid is 1:3, heating to 60-70 ℃ during pickling.
5. The method for quantitatively detecting the impurity phase of an alloy according to claim 1, characterized by comprising the steps of: in the step S3, the relative error is calculated using the following formula:
the accuracy of the evaluation method comprises reliability evaluation of the results, reliability and repeatability of the measurement results are evaluated by calculating relative error results, and for the data of multiple measurements, a control chart is drawn to monitor the stability of the method.
6. The method for quantitatively detecting the impurity phase of an alloy according to claim 1, characterized by comprising the steps of: in step S4, for each experimental data set under the measurement condition, an average value of the samples is calculatedAnd standard deviation s
Where n is the number of samples, x i Is the i-th data point.
7. The method for quantitatively detecting the impurity phase of an alloy according to claim 6, wherein: and (3) performing standard curve fitting and concentration calculation by a data processing algorithm in the step (S4), wherein when the standard curve fitting is performed, a fitting equation is as follows: y=mx=b
Wherein y is absorbance, x is concentration, m is slope, b is intercept, and the concentration of the impurity to be detected of the alloy sample is calculated according to a fitting equation.
CN202311647222.8A 2023-12-04 2023-12-04 Alloy impurity phase quantitative detection method Pending CN117629985A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202311647222.8A CN117629985A (en) 2023-12-04 2023-12-04 Alloy impurity phase quantitative detection method

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202311647222.8A CN117629985A (en) 2023-12-04 2023-12-04 Alloy impurity phase quantitative detection method

Publications (1)

Publication Number Publication Date
CN117629985A true CN117629985A (en) 2024-03-01

Family

ID=90019661

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202311647222.8A Pending CN117629985A (en) 2023-12-04 2023-12-04 Alloy impurity phase quantitative detection method

Country Status (1)

Country Link
CN (1) CN117629985A (en)

Similar Documents

Publication Publication Date Title
CN102033101A (en) Method for measuring metal impurities in high-purity MgO film material by using inductively coupled plasma mass spectrometer
CN103323412B (en) Thiocyanate spectrophotometry method for detecting iron content of high-temperature alloy
CN104237209A (en) Method for synchronously detecting copper, bismuth, iron, lead, tellurium, selenium, antimony and palladium in electrolytic silver through ICP-AES (Inductively Coupled Plasma-Atomic Emission Spectrometry)
CN110514643B (en) Method for measuring trace elements in high-purity magnesium-based oxide by inductively coupled plasma emission spectrometry
CN110940660A (en) Method for determining silver, arsenic, tin, boron, copper and zirconium in nickel-based superalloy
CN109632680B (en) Method for detecting phosphorus in water body based on permutation entropy
CN111443079A (en) Method for simultaneously detecting contents of trace As, Pb, Cd, Zn, Cr, Co and V elements in ferric trichloride
JP4434026B2 (en) Isotope ratio analysis method using plasma ion source mass spectrometer
Wengert Photometric determination of zirconium in magnesium alloys
CN109781684A (en) A kind of detection method of Mercury in Marine Sediment and arsenic
CN110220887B (en) Method for measuring lead, zinc, tin and nickel in waste circuit board stripping material resin powder
CN117629985A (en) Alloy impurity phase quantitative detection method
MacNEVIN et al. (Ethylenedinitrilo) tetraacetic Acid Chelation of Platinum Group Metals. Spectrophotometric Determination of Iridium
CN108956582A (en) A kind of emission spectrometry method of high-copper Phosphorus From Wastewater content
CN111474165A (en) Method for testing concentration content of lithium hexafluorophosphate in lithium ion functional electrolyte by using ICP (inductively coupled plasma)
CN112578071A (en) Quantitative analysis method for inorganic acid salt in electrolytic stripping powder
CN111141725A (en) Quantitative detection method for lithium hexafluorophosphate in lithium ion battery electrolyte
CN114354579B (en) Method for simultaneously detecting silver and palladium elements in silver and palladium mixture
van Staden et al. Determination of zinc in pharmaceutical products by use of a sequential injection analysis system
Wah Fong et al. Multi-elements (aluminium, copper, magnesium, manganese, selenium and zinc) determination in serum by dynamic reaction cell-inductively coupled plasma-mass spectrometry
Shen Determination of silver in copper concentrate by atomic absorption spectrometry
Goyal et al. Direct Determination of Cadmium in Nuclear-Grade Beryllium by GFAAS
CN116067939A (en) Quantitative detection method of lithium hexafluorophosphate
CN115356328A (en) Method for rapidly determining content of multiple elements in high-temperature nickel-based alloy
Maeda et al. Determination of Microgram Quantities of Tungsten in Iron, Molybdenum, and Titanium by X-Ray Fluorescence Analysis

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination