CN108375568A - Micro-wave digestion-inductive coupling plasma emission spectrograph method measures impurity element in rafifinal - Google Patents
Micro-wave digestion-inductive coupling plasma emission spectrograph method measures impurity element in rafifinal Download PDFInfo
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- CN108375568A CN108375568A CN201810176065.XA CN201810176065A CN108375568A CN 108375568 A CN108375568 A CN 108375568A CN 201810176065 A CN201810176065 A CN 201810176065A CN 108375568 A CN108375568 A CN 108375568A
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- 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
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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Abstract
Micro-wave digestion inductive coupling plasma emission spectrograph method measures impurity element in rafifinal, analysis and testing technology field.Applied microwave clears up the analysis method that instrument and inductive coupling plasma emission spectrograph (hereinafter referred to as ICP-OES) take calibration curve method to measure the totally 20 kinds of impurity elements of Ag, Ba, Bi, Cd, Co, Cu, Ga, Fe, In, Li, Mg, Mn, Mo, Pb, Sb, Ti, V, Sr, Zn, Zr in rafifinal.Sample is dissolved in enclosed high pressure micro-wave diminishing pot with appropriate amount of acid preferably extraneous factor to be avoided to pollute.It is tested by single factor and determines instrument optimum working parameter.And selection standard curve method test specimen, to reduce Matrix effects.Be one kind can 20 kinds of elements of single-time measurement and simplicity, it is quick, accurately modernize detection technique.
Description
Technical field
The invention belongs to analysis and testing technology fields, are related to applied microwave resolution instrument and inductively coupled plasma transmitting light
Spectrometer (hereinafter referred to as ICP-OES) take calibration curve method measure rafifinal in Ag, Ba, Bi, Cd, Co, Cu, Ga, Fe, In,
The analysis method of Li, Mg, Mn, Mo, Pb, Sb, Ti, V, Sr, Zn, Zr totally 20 kinds of impurity elements.
Background technology
Rafifinal has the performances such as many excellent performances, including low resistance of deformation, high conductivity and good plasticity,
Be applied primarily to scientific research, electronics industry, chemical industry and manufacture high purity alloys, laser material, aerospace and some
Other specific uses.The quality of rafifinal directly affects its performance in use and therefore rapidly and efficiently detects rafifinal
In impurity content have great importance.
Since the purity of rafifinal is very high, other elements content is very low, generally horizontal in micro or trace, at present rafifinal
Digestion procedure be all acid adding wet digestion method, but found in actual tests, since sample purity is very high, in dissolving rafifinal
When sample, acid adding wet digestion takes very long and easy pollution.This method is by the way of high-pressure sealed micro-wave digestion to height
Fine aluminium sample is cleared up, and not only sample decomposition is quickly, complete, volatile element loss is small, reagent consumes less, blank is low, goes back
Sample can be reduced with the extraneous time contacted to reduce the contaminated possibility of sample, this is very in trace element analysis
The important point.
The operation principle of ICP-OES tests is by sample solution by the control of computer software through being atomized into aerosol
After be brought into inductively coupled plasma, through the past it is molten, evaporation, dissociation, ionization, excitation, radiation etc. processes.Pass through light path system
Signal acquisition and signal conversion, so that it may go out the concentration value of element to be measured with sequentially determining.
Invention content
It is an object of the invention to invent a kind of applied microwave resolution instrument and inductive coupling plasma emission spectrograph point
The method for analysing rafifinal sample, this method can be with the content of 20 kinds of trace impurities in single-time measurement rafifinal.Experiment in order to
Reducing sample as far as possible is influenced in pretreatment process by outside contamination, and the reagent that experiment of the invention uses is all for top grade
Pure, deionized water used is 18.2 mega-ohms.The present invention test be using calibration curve method:By the standard of 20 kinds of impurity elements
Substance (liquid) is incorporated in same medium mixing and adds blank in the linear preparing standard solution that is incremented by with various concentration, and totally five
Part.Invention uses and rafifinal is put into the counteracting tank of polytetrafluoroethylene (PTFE), the method for high-pressure sealed resolution.This method can make high-purity
Aluminium dissolving is complete, more easy compared with conventional method, quickly, effectively.
It is determined through analysis of experiments, the resolution rafifinal sample that experiment condition used in the present invention can be quick and complete, most
The big possible outside contamination reduced suffered by sample and improve detection speed.
Specifically include the following conditions and step:
One, operating condition
(1) laboratory is dustless, 25 DEG C of temperature, humidity 30%-50%.
(2) the various vessel used are both needed to be boiled with hydrochloric acid and cleaned with deionized water.
Two, element is measured
Ag, Ba, Bi, Cd, Co, Cu, Ga, Fe, In, Li, Mg, Mn, Mo, Pb, Sb, Ti, V, Sr, Zn, Zr totally 20 kinds of elements.
Three, the preparation of reagent and standard solution agent standard curve
(1) hydrochloric acid and nitric acid are top pure grade;
(2) test water is ultra-pure water;
(3) Ag, Ba, Bi, Cd, Co, Cu, Ga, Fe, In, Li, Mg, Mn, Mo, Pb, Ti, V, Sr, Zn, Zr system are weighed respectively
For at respective standard reserving solution, concentration is 1000 μ g/mL, can be carried by national steel material test center Iron and Steel Research Geueral Inst
For;A concentration of 500 μ g/mL of Sb standard reserving solutions are provided by national steel material test center Iron and Steel Research Geueral Inst.
Then by Ag, Ba, Bi, Cd, Co, Cu, Ga, Fe, In, Li, Mg, Mn, Mo, Pb, Sb, Ti, V, Sr, Zn, Zr standard
Storing solution mixes and is prepared into mixed standard solution, Ag, Ba in mixed standard solution, Bi, Cd, Co, Cu, Ga, Fe, In, Li,
The concentration of Mg, Mn, Mo, Pb, Sb, Ti, V, Sr, Zn, Zr are 50.0 μ g/mL;
Pipette respectively 5.00mL Ag, Ba, Bi, Cd, Co, Cu, Ga, Fe, In, Li, Mg, Mn, Mo, Pb, Ti, V, Sr, Zn,
Zr standard reserving solutions (1000 μ g/mL), 10mL Sb standard reserving solutions (500 μ g/mL) add 5mL hydrochloric acid in 100mL volumetric flasks,
It is diluted with water to scale, mixing;
(4) mixed standard solution 0,1.00,2.00,6.00,10.00mL is pipetted successively, is separately added into the appearance of 5 100mL
In measuring bottle (A grades), it is separately added into 5mL hydrochloric acid, with deionized water constant volume to scale;The working curve of preparation is 0,0.50,1.00,
3.00,5.00 μ g/mL standard liquid series;The working curve can cover the content range of 20 kinds of elements in rafifinal;By standard
Solution series sequentially enters to be measured in ICP-OES instruments, further obtains each mark of impurity element intensity about concentration
Directrix curve;
Four, the processing of sample to be tested
Rafifinal sample 5.00g (being accurate to ± 0.0001g) to be measured is weighed in 100mL polytetrafluoroethylene (PTFE) counteracting tanks,
5mL hydrochloric acid and 1mL nitric acid is added, capping, which is placed in microwave dissolver, is cleared up;It is taken after resolution program (being shown in Table 1)
Go out, after cooling can opening, with deionized water constant volume in 100mL volumetric flasks, shakes up to obtain solution A, into ICP-OES instruments
It measures, obtains each impurity element intensity, each impurity member in solution A is further obtained then in conjunction with the intensity in step 3 (4)
The concentration of element;
Five, the mass percentage for weighing each impurity element in rafifinal sample to be measured is calculated, calculation formula is as follows:
Further preferably:
Each Determination of Impurity Elements wavelength is as follows:
Observed altitude
Observed altitude is adjusted by nebulizer pressure and highly to be set.Using Mn, Ni and Fe and relevant
The best observation point of chemistry disruption is avoided in adjustment.Therefore we measure 20 kinds of elements simultaneously, it is impossible to distinguish to each element
An observation point is designed, " compound observed altitude " can only be used.
The test condition of microwave dissolver:
1 micro-wave digestion condition of table
The test condition of ICP-OES instruments:
It is preferred that 7300 types of PE companies of U.S. Optima.Operating wavelength range 167-782nm, resolution capability are reachable
0.003nm;The halophilic jewel concentric atomizer of resistance to HF acid, triple channel peristaltic pump;Beam splitting system:Echelle grating, vertical square
Pipe designs, radial survey mode;Gases used is high-purity argon (99.99% or more).Instrumentation choosing conditions are shown in Table 2.
Analysis and Control software is opened, after instrument is preheated half an hour, plant capacity, cooling gas flow, secondary air are set
Amount, wriggling pump speed, sample promote time, the sample time of integration.Point opens " plasma " button, forms stable plasmatorch
Flame.Calibration curve solution and blank and sample solution (concentration is from low to high) are sucked successively by pump line, you can obtain to be measured
The intensity value and concentration value of element.
2 ICP of table-OES instrument operating conditions
It is an advantage of the invention that:
1, due to the micro-wave digestion inductive coupling plasma emission spectrograph ICP-OES employed in the method for the present invention
It is limited with lower detection, can accurately, accurately measure the impurity in high-purity material, the present invention has selected suitable spectral line, made
Inductive coupling plasma emission spectrograph is obtained under the premise of eliminating spectral line interference, it can be with 20 in single-time measurement rafifinal
The content of kind trace impurity, can not only reduce workload, and finding speed is fast, and accuracy is high, and precision is good.
2, the external world of pre-treating method and experiment condition maximum possible used in the present invention reduced suffered by sample
Pollution, therefore it is high to detect authenticity.
Description of the drawings
Fig. 1 is the canonical plotting that impurity Pb in rafifinal is measured with micro-wave digestion-plasma atomic emission spectrometer.
Specific implementation mode
To make the objectives, technical solutions, and advantages of the present invention clearer, below in conjunction with specific embodiment to this hair
Bright further description.
Sample 5g is weighed in polytetrafluoroethylene (PTFE) counteracting tank, 5mL hydrochloric acid 1mL nitric acid is added, capping is placed on micro-wave digestion
It is cleared up, is taken out after resolution program (being shown in Table 1), after cooling can opening, with deionized water constant volume in 100mL capacity in instrument
Bottle, shakes up to be measured.Blank is done in company with sample.
ICP-OES instruments are opened, point opens " plasma ", sucks calibration curve solution successively by pump line, determines calibration
After curve, blank and sample solution are measured, checks data, calculates content.
Wherein computer disposal calculate method be:
Embodiment 1:
Experimental procedure:
1, sample is cleaned
It is rinsed well with deionized water, dried for standby.
2, sample dissolves
Rafifinal sample 5g (being accurate to ± 0.0001g) is weighed in 100mL polytetrafluoroethylene (PTFE) counteracting tanks, 5mL salt is added
Sour 1mL nitric acid, capping, which is placed in microwave dissolver, is cleared up.It takes out after resolution program (being shown in Table 1), opens after cooling
Tank shakes up to be measured with deionized water constant volume in 100mL volumetric flasks.Blank is done in company with sample.
3, instrumentation
Analysis and Control software is opened, after instrument is preheated half an hour, setting plant capacity is 1.0Kw, cooling gas flow
15L/min, secondary air amount 0.2L/min, atomizing pressure 50psi (1psi=6.89kPa), sample promote speed 1.2ml/
Min, point open " plasma " button, form stable plasmatorch flame.Calibration curve prepare liquid (concentration is from low to high) is logical
It crosses pump line to suck successively, generates four test points, the curve formed to this several points is corrected confirmation, and linear coefficient is made to exist
0.995 or more.Blank and sample solution are sucked successively by pump line, you can obtain the concentration of element to be measured on data mode column
Value.
The confirmation curve for measuring and being obtained when Pb impurity elements is shown in Fig. 1, and linear coefficient 0.9998 clicks result
Output, you can obtain the concentration value C of Pb elements on data mode column.
The elemental profiles to be surveyed are confirmed respectively, concentration of element to be measured is calculated by software:
According to calculation formula
The content for finally obtaining various elements to be measured is as follows:
Element | Ag | Ba | Bi | Cd | Co | Cu | Ga | Fe |
Percentage composition % | 6.3E-05 | 1.1E-05 | 8.2E-04 | 1.1E-05 | 1.7E-04 | 2.0E-04 | 1.4E-05 | 1.3E-05 |
Element | In | Li | Mg | Mn | Mo | Pb | Sb | Ti |
Percentage composition % | 1.4E-05 | 1.3E-04 | 1.7E-04 | 6.3E-04 | 5.0E-05 | 3.3E-05 | 1.5E-05 | 1.8E-05 |
Element | V | Sr | Zn | Zr | ||||
Percentage composition % | 1.2E-05 | 1.1E-05 | 2.2E-05 | 7.5E-05 |
Method reliability demonstration:
Using recovery test come the reliability of verification method.Be separately added into three parallel samples of rafifinal silver, barium,
20 elements to be measured such as bismuth, cadmium make its mass concentration increase separately 0.5,2.0,5.0 μ g/mL, are carried out in company with sample preparation
Analysis measures, and calculates average recovery rate.Experiments have shown that the rate of recovery of each element is between 91.9%~102.4%, specifically such as
Following table.
Element average recovery rate statistics to be measured
Precision test:
To rafifinal sample, sample is handled according to analytical procedure, 10 measurement has been carried out, has obtained result and RSD see the table below.
Relative standard deviation is less than 3%.
Analysis result and precision
Claims (4)
1. the method that a kind of micro-wave digestion-inductive coupling plasma emission spectrograph method measures impurity element in rafifinal,
It is characterized in that, specifically includes the following conditions and step:
One, operating condition
(1) laboratory is dustless, 25 DEG C of temperature, humidity 30%-50%;
(2) the various vessel used are both needed to be boiled with hydrochloric acid and cleaned with deionized water;
Two, element is measured
Ag, Ba, Bi, Cd, Co, Cu, Ga, Fe, In, Li, Mg, Mn, Mo, Pb, Sb, Ti, V, Sr, Zn, Zr totally 20 kinds of elements;
Three, the preparation of reagent and standard solution agent standard curve
(1) hydrochloric acid and nitric acid are top pure grade;
(2) test water is ultra-pure water;
(3) Ag, Ba, Bi, Cd, Co, Cu, Ga, Fe, In, Li, Mg, Mn, Mo, Pb, Ti, V, Sr, Zn, Zr is weighed respectively to be prepared into
Respective standard reserving solution, concentration are 1000 μ g/mL;A concentration of 500 μ g/mL of Sb standard reserving solutions;
Then by Ag, Ba, Bi, Cd, Co, Cu, Ga, Fe, In, Li, Mg, Mn, Mo, Pb, Sb, Ti, V, Sr, Zn, Zr standard inventory
Liquid mixes and is prepared into mixed standard solution, Ag, Ba in mixed standard solution, Bi, Cd, Co, Cu, Ga, Fe, In, Li, Mg, Mn,
The concentration of Mo, Pb, Sb, Ti, V, Sr, Zn, Zr are 50.0 μ g/mL;
5.00mL Ag, Ba, Bi, Cd, Co, Cu, Ga, Fe, In, Li, Mg, Mn, Mo, Pb, Ti, V, Sr, Zn, Zr mark are pipetted respectively
Quasi- storing solution, 10mL Sb standard reserving solutions (500 μ g/mL) add 5mL hydrochloric acid, are diluted with water to scale in 100mL volumetric flasks,
Mixing;
(4) mixed standard solution 0,1.00,2.00,6.00,10.00mL is pipetted successively, is separately added into the volumetric flask of 5 100mL
In, it is separately added into 5mL hydrochloric acid, with deionized water constant volume to scale;The working curve of preparation is 0,0.50,1.00,3.00,5.00
μ g/mL standard liquid series;The working curve can cover the content range of 20 kinds of elements in rafifinal;By standard liquid series according to
It is measured in secondary entrance ICP-OES instruments, further obtains each standard curve of impurity element intensity about concentration;
Four, the processing of sample to be tested
Rafifinal sample 5.00g to be measured is weighed in 100mL polytetrafluoroethylene (PTFE) counteracting tanks, 5mL hydrochloric acid and 1mL nitric acid is added,
Capping, which is placed in microwave dissolver, is cleared up;It is taken out after resolution EP (end of program), after cooling can opening, with deionized water constant volume
It in 100mL volumetric flasks, shakes up to obtain solution A, into being measured in ICP-OES instruments, obtains each impurity element intensity, then
The concentration of each impurity element in solution A is further obtained in conjunction with the intensity in step 3 (4);
Five, the mass percentage for weighing each impurity element in rafifinal sample to be measured is calculated, calculation formula is as follows:
2. a kind of micro-wave digestion described in accordance with the claim 1-inductive coupling plasma emission spectrograph method measures rafifinal
The method of middle impurity element, which is characterized in that each Determination of Impurity Elements wavelength is as follows:
3. a kind of micro-wave digestion described in accordance with the claim 1-inductive coupling plasma emission spectrograph method measures rafifinal
The method of middle impurity element, which is characterized in that the test condition of microwave dissolver:
1 micro-wave digestion condition of table
4. a kind of micro-wave digestion described in accordance with the claim 1-inductive coupling plasma emission spectrograph method measures rafifinal
The method of middle impurity element, which is characterized in that the test condition of ICP-OES instruments:
Operating wavelength range 167-782nm, resolution capability is up to 0.003nm;The halophilic jewel concentric atomizer of resistance to HF acid, three
Multi-channel peristaltic pump;Beam splitting system:Echelle grating, vertical quarter bend design, radial survey mode;Gases used is high-purity argon
99.99% or more;Instrumentation choosing conditions are shown in Table 2;
Analysis and Control software is opened, after instrument is preheated half an hour, plant capacity is set, and cooling gas flow, secondary air amount is compacted
Dynamic pump speed, sample promote time, the sample time of integration;Point opens " plasma " button, forms stable plasmatorch flame;High-ranking officers
Directrix curve solution and testing sample solution are sucked successively by pump line, you can obtain the intensity value and concentration value of element to be measured.
2 ICP of table-OES instrument operating conditions
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Cited By (9)
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CN109444248A (en) * | 2018-11-20 | 2019-03-08 | 中国地质大学(武汉) | A kind of method that the solution based on laser degrades that sample introduction is analyzed |
CN109632933A (en) * | 2018-12-29 | 2019-04-16 | 上海微谱化工技术服务有限公司 | A kind of analysis method of fat emulsion injection |
CN110514645A (en) * | 2019-09-24 | 2019-11-29 | 中国航发哈尔滨轴承有限公司 | The method of impurity element As, Sb content in silicon bronze is accurately measured with ICP-AES |
CN110954394A (en) * | 2019-12-31 | 2020-04-03 | 河钢股份有限公司 | Method for measuring content of nickel, copper, aluminum, chromium and molybdenum in recarburizing agent by ICP-AES (inductively coupled plasma-atomic emission Spectrometry) |
CN110987906A (en) * | 2019-12-16 | 2020-04-10 | 上海电气电站设备有限公司 | ICP-OES analysis method for determining trace silicon in nickel-based superalloy by using FACT correction technology |
CN111398257A (en) * | 2020-04-15 | 2020-07-10 | 首钢京唐钢铁联合有限责任公司 | Method for measuring content of trace elements in silicon-aluminum alloy |
CN113504291A (en) * | 2021-06-16 | 2021-10-15 | 宁波锦越新材料有限公司 | Sample preparation method and detection method for determining impurities in ultra-high-purity aluminum by utilizing ICP-MS (inductively coupled plasma-mass spectrometry) |
CN114184445A (en) * | 2021-12-09 | 2022-03-15 | 四川阿格瑞新材料有限公司 | Method for measuring content of residual metal elements in OLED material |
CN114749042A (en) * | 2022-04-12 | 2022-07-15 | 宁波江丰电子材料股份有限公司 | Dissolving method of AgCuTi alloy |
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CN109444248A (en) * | 2018-11-20 | 2019-03-08 | 中国地质大学(武汉) | A kind of method that the solution based on laser degrades that sample introduction is analyzed |
CN109632933A (en) * | 2018-12-29 | 2019-04-16 | 上海微谱化工技术服务有限公司 | A kind of analysis method of fat emulsion injection |
CN109632933B (en) * | 2018-12-29 | 2021-11-16 | 上海微谱化工技术服务有限公司 | Analysis method of fat emulsion injection |
CN110514645A (en) * | 2019-09-24 | 2019-11-29 | 中国航发哈尔滨轴承有限公司 | The method of impurity element As, Sb content in silicon bronze is accurately measured with ICP-AES |
CN110987906A (en) * | 2019-12-16 | 2020-04-10 | 上海电气电站设备有限公司 | ICP-OES analysis method for determining trace silicon in nickel-based superalloy by using FACT correction technology |
CN110954394A (en) * | 2019-12-31 | 2020-04-03 | 河钢股份有限公司 | Method for measuring content of nickel, copper, aluminum, chromium and molybdenum in recarburizing agent by ICP-AES (inductively coupled plasma-atomic emission Spectrometry) |
CN111398257A (en) * | 2020-04-15 | 2020-07-10 | 首钢京唐钢铁联合有限责任公司 | Method for measuring content of trace elements in silicon-aluminum alloy |
CN113504291A (en) * | 2021-06-16 | 2021-10-15 | 宁波锦越新材料有限公司 | Sample preparation method and detection method for determining impurities in ultra-high-purity aluminum by utilizing ICP-MS (inductively coupled plasma-mass spectrometry) |
CN114184445A (en) * | 2021-12-09 | 2022-03-15 | 四川阿格瑞新材料有限公司 | Method for measuring content of residual metal elements in OLED material |
CN114184445B (en) * | 2021-12-09 | 2023-09-08 | 四川阿格瑞新材料有限公司 | Method for measuring content of residual metal element in OLED material |
CN114749042A (en) * | 2022-04-12 | 2022-07-15 | 宁波江丰电子材料股份有限公司 | Dissolving method of AgCuTi alloy |
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