CN110514643A - A kind of method that inductively coupled plasma emission spectrography measures trace element in high purity magnesium base oxide - Google Patents

A kind of method that inductively coupled plasma emission spectrography measures trace element in high purity magnesium base oxide Download PDF

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CN110514643A
CN110514643A CN201910825841.9A CN201910825841A CN110514643A CN 110514643 A CN110514643 A CN 110514643A CN 201910825841 A CN201910825841 A CN 201910825841A CN 110514643 A CN110514643 A CN 110514643A
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CN110514643B (en
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王景凤
黎永娟
胡燕秀
李颜君
岳萍
罗仙平
吴敏
王春英
梁金凤
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QINGHAI WEST MINING ENGINEERING TECHNOLOGY RESEARCH Co Ltd
Western Mining Group Science And Technology Development Co Ltd
Western Mining Co Ltd
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QINGHAI WEST MINING ENGINEERING TECHNOLOGY RESEARCH Co Ltd
Western Mining Group Science And Technology Development Co Ltd
Western Mining Co Ltd
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/62Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
    • G01N21/71Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light thermally excited
    • G01N21/73Systems 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

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Abstract

The invention discloses the methods of trace element in a kind of inductively coupled plasma emission spectrography measurement high purity magnesium base oxide, sample first passes through pretreatment, then the standard solution of aluminium, calcium, potassium, sodium, boron, iron, manganese, cadmium, lead, the multielement standard mixed solution of sulphur or single element silicon is added, hydrochloric acid is added, is diluted, finally series standard solution is measured with inductively coupled plasma atomic emission spectrometer.Utilize the universal law of aluminium, calcium, potassium, sodium, boron, iron, manganese, cadmium, lead, sulphur, the element silicon emission spectrum in inductively coupled plasma, simulate high-purity serial magnesium-based oxide matrix, coexistence elements and background emission spectral investigation are carried out, medium, analysis spectral line screening, matrix is measured and eliminates test and condition optimizing containing interfering with each other between miscellaneous element spectral line, establishes optimal sample determination condition;Using standard addition method as technological means, the measurement of trace impurity in high-purity serial magnesium-based oxide samples is realized.

Description

Trace in a kind of inductively coupled plasma emission spectrography measurement high purity magnesium base oxide The method of secondary element
Technical field
The present invention relates to the technical field of analysis and detection of salt lake chemical industry, and in particular to one kind by inductive coupling etc. from The method of trace element in daughter emission spectrographic determination high purity magnesium base oxide.
Background technique
Salt lake resources are the advantage and characteristic resources of China Qinghai Area, and deep development utilizes salt lake resources, and salt lake mentions magnesium Key technology makes a breakthrough, and western magnesium industry product yield and quality reach " five the first in the world ", for examining for puzzlement Qinghai many years You provide another new way by the comprehensive development and utilization of sweat Bischofite in Salt lake waste material, and " magnesium evil " becomes " magnesium It is precious ".To solve " magnesium evil " problem present in exploit resources of salt lakes utilization, industry has had developed high-purity serial magnesium-based oxygen in succession Compound, wherein highly-purity magnesite fills the domestic gaps, high-purity as the downstream of carrier using 100,000 tons/year of high purity magnesium hydroxides and using it The exploitation of product is also just in development like a raging fire.However, existing product does not generate significant benefit to enterprise, head is because being a lack of Detection method and cannot being provided to user's especially Foreign User suffice to show that product quality containing miscellaneous index.Carry out high-purity magnesium-based In oxide coexistence elements spectral signature and law study in inductively coupled plasma body flame be solve this drawback it is effective Means.
High-purity serial magnesium-based oxide of Qinghai Western Magnesium Technology Co., Ltd.'s production mainly has magnesia, magnesium hydroxide and just In the magnesium carbonate and magnesium metal of exploitation, product (main content be greater than 99.9%) containing miscellaneous many kinds of, such as, calcium, potassium, sodium, boron, The content of iron, manganese, cadmium, lead, sulphur, silicon etc., these impurity elements will have a direct impact on the performance of product, using effect and price, together When, content is little, and mass percentage is usually 10-3-10-4The order of magnitude, and the matrix of sample is at concentrations up to 100-10-1%, These characteristics become the technical bottleneck of the detection above-mentioned element of trace.Appropriate dilute sample solution can reduce matrix in a certain range The influence of effect, but the concentration of analytical element is reduced while dilution, limit the use of the technological means.
Mainly there is the method containing miscellaneous element in measurement high purity metal oxides and high pure metal: spectrophotometry, atom are inhaled Receipts method, inductive coupling plasma emission spectrum method etc..Spectrophotometry can only measure the oligo-elements such as iron, can only measure list every time One element, work efficiency are low, at high cost;Atomic absorption method is adapted only to measure most metallic elements, and is difficult to measure boron, sulphur, silicon Equal nonmetalloids, and the detection limit of part minor metallic element is not high, it is difficult to meet accuracy requirement;Inductively coupled plasma Body emission spectrometry have high sensitivity, detection limit is low, accuracy is good, the range of linearity is wide, can measure simultaneously in a sample Multiple element.
Currently, inductive coupling plasma emission spectrum method trace element in measuring high-purity serial magnesium-based oxide does not have state The national standard substance of family's standard, provincial standard or same matrix carrys out implementation quality control, and most the method referring to value is oxygen Change the measurement national standard HG/T 2573-2012 of magnesium and the measurement standard HG/T 3607-2007 of magnesium hydroxide.Regrettably, Lack in two standards deliming, iron, outside manganese (without in magnesia) other elements measurement, and calcium using high level (most Lower bound 10-1The order of magnitude) EDTA titration, detection limit is unable to reach 10-4The requirement of order of magnitude content, meanwhile, both methods In lack the reproducibility and reproducibility index of quality control requirement, laboratory to itself testing result lack reliability judge according to According to.Currently, not seen the report of impurity element in inductive coupling plasma emission spectrum method measurement high purity magnesium base oxide, In In close research few in number, Tao Meijuan using interference coefficient method have studied cadmium in magnesium and magnesium alloy, lead, nickel, aluminium, silicon, zirconium, The assay of 17 kinds of elements such as manganese, beryllium, copper, iron, titanium, lead, silver, calcium, yttrium, lanthanum, cerium and neodymium, Mei Tan use Matrix phase pair Magnesium and Silicon in Mg Alloys content are determined, and the mass percentage containing miscellaneous element is 10 in the two measurement sample-2The order of magnitude, Being not suitable for mass percentage is usually 10-4The measurement of order of magnitude high purity magnesium base oxide impurity element.
Summary of the invention
The technical problem to be solved by the present invention is in view of the shortcomings of the prior art, utilize sense coupled plasma optical emission spectrum Method, provide a kind of operating procedure is simple, sample treatment is simple and quick, measurement accuracy is high, can provide mass percentage down to for 10-4The analysis method of trace element in order of magnitude high purity magnesium base oxide.
In order to solve the above technical problems, the present invention adopts the following technical scheme: a kind of inductively coupled plasma body emits light The method that spectrometry measures trace element in high purity magnesium base oxide, it is characterised in that: sample first passes through pretreatment, is then added Calcium, potassium, sodium, boron, iron, manganese, cadmium, lead, sulphur, aluminium multielement standard solution or element silicon standard solution, be added hydrochloric acid, carry out it is dilute It releases, finally series standard solution is measured with inductively coupled plasma atomic emission spectrometer, specific determination step is such as Under,
1) prepare reagent: being mixed including hydrochloric acid and potassium, sodium, calcium, sulphur, boron, lead, iron, cadmium, manganese, aluminium multielement standard molten Liquid, element silicon standard solution;
2) preparing standard solution
A, potassium, sodium, calcium, sulphur, boron, lead, iron, cadmium, manganese, aluminium multielement mark accurately multielement standard mixed solution A 1: are pipetted Quasi- mixed solution, is diluted with water to scale, and constant volume shakes up to get multielement standard mixed solution A 1 is arrived;
Element silicon standard solution A2: accurately pipetting element silicon standard solution, is diluted with water to scale, constant volume, shake up to get To element silicon standard solution A2;
B, multielement standard mixed solution B1: accurately pipetting multielement standard mixed solution A 1, be diluted with water to scale, fixed Hold, shake up, obtains the multielement standard mixed solution B1 that concentration is 1 concentration 10% of multielement standard mixed solution A;
Element silicon standard solution B2: element silicon standard solution A2 accurately is pipetted, is diluted with water to scale, constant volume shakes up, and obtains It is the element silicon standard solution B2 of element silicon standard solution A2 concentration 10% to concentration;
3) sample pretreatment: accurately weighing sample, and little water is added to soak, a small amount of repeatedly to add in the case where glass bar is stirred continuously Enter hydrochloric acid (1+1), until sample is completely dissolved, solution is limpid, rinses wall of cup with a small amount of water, heats on low temperature electric hot plate slightly boiled 2min is removed, cooling, is moved into volumetric flask, and (1+1) hydrochloric acid is added and is shaken up with water constant volume, obtains sample solution;
4) production of standard addition method working curve
The production of multielement working curve: successively accurately pipette respectively multielement standard mixed solution B1:0mL, 0.25mL, The good sample of above-mentioned pretreatment is successively accurately added in one group of 25mL volumetric flask in 0.50mL, 1.25mL, 2.50mL, 5.00mL Solution 2.50mL is added hydrochloric acid 0.5mL, is diluted with water to scale, constant volume shakes up;The corresponding potassium of this working curve, sodium, calcium, Sulphur, boron, lead, iron, cadmium, manganese, aluminium element concentration be respectively 0ug/mL, 0.10ug/mL, 0.20ug/mL, 0.50ug/mL, 1.00ug/mL,2.00ug/mL;
The production of element silicon standard working solution: accurately pipette element silicon standard solution B2:0mL, 0.25mL, 0.50mL, The good sample solution 2.50mL of above-mentioned pretreatment is accurately added in one group of 25mL volumetric flask in 1.25mL, 2.50mL, 5.00mL, It is diluted with water to scale, constant volume shakes up;This working curve correspond to element silicon concentration be respectively 0ug/mL, 0.10ug/mL, 0.20ug/mL,0.50ug/mL,1.00ug/mL,2.00ug/mL;
5) it measures: successively series standard solution being measured with inductively coupled plasma atomic emission spectrometer, with Concentration 0ug/mL, 0.10ug/mL of the corresponding standard solution of each element, 0.20ug/mL, 0.50ug/mL, 1.00ug/mL, 2.00ug/mL is abscissa, using corresponding intensity of emission spectra under each concentration as ordinate, maps, obtains each element mark The intersection point of the standard curve of quasi- addition method, curve and axis of abscissas is the concentration of element to be measured in sample, multiplied by corresponding dilute Multiple is released to get the content of element to be measured in sample.
Key instrument and operating condition:
Inductively coupled plasma atomic emission spectrometer: iCAP 7000SERIES type, silent winged your science and technology of generation of U.S.'s match have Limit company;
Electronic balance: ME204E type, sensibility reciprocal 0.0001g, Switzerland Mei Teletuo benefit measuring technique Co., Ltd;
Thermo7400, RF frequency 27.12MHz, efficient concentric atomizer, plasma observed pattern: vertical (diameter ), wave-length coverage 166-847nm, optical resolution (FHW)≤0.007nm, at 200nm;At 0.014nm, 400nm; At 0.021nm, 600nm;Semiconductor refrigerating CID detector, detection unit > 290000.
Thermoelectricity ICP7400, power 950W, cooling air 12L/min assist gas 0.5L/min, carrier gas 0.5L/min, and observation is high Spend 12mm;The time of integration: long wave 5S, shortwave 15S;Pump speed: rinsing 50rpm, analyzes pump speed 50rpm.
In step 5), each analytical element and corresponding wavelength are as follows: Al 167.079nm, B 249.773nm, Ca are 393.366nm, Cd 228.802nm, Fe 238.204nm, K 766.490nm, Mn 257.610nm, Na are 589.592nm, Pb 220.353nm, S 182.034nm, Si 251.611nm.
In step 3), the sample amount of pipetting is 5.0000g, and 1+1 hydrochloric acid additional amount is 30 milliliters, is added when necessary few drops;In Slightly boiled 2min is heated with 200 DEG C of temperature on low temperature electric hot plate, is moved into after cooling in 50 milliliters of volumetric flask and adds (1+1) salt 5 milliliters of acid, with water constant volume, shakes up.
The concentration of element silicon standard solution is 1000ug/mL, potassium, sodium, calcium, sulphur, boron, lead, iron, cadmium, manganese, aluminium multielement mark The concentration of quasi- mixed solution is 1000ug/mL, and the concentration of multielement standard mixed solution A 1 is 100ug/mL, and element silicon standard is molten The concentration of liquid A2 is 100ug/mL, and the concentration of multielement standard mixed solution B1 is 10ug/mL, and element silicon standard solution B2's is dense Degree is 10ug/mL.
Co-existing element interference is investigated: having investigated magnesium-based bulk concentration in high purity magnesium base oxide is respectively 10mg/mL, 20mg/ Interference of the magnesium matrix to element to be measured when mL, 30mg/mL, it is determined that magnesium-based bulk concentration is when being not more than 20mg/mL, to member to be measured Element is noiseless;
Detection limit situation: being blank METHOD FOR CONTINUOUS DETERMINATION 11 times with 2%HCL under the conditions of laboratory apparatus of the present invention, to measure knot Detection limit of the 3 times of standard deviations of fruit as this method, using 10 times of Determination Limits as this method of standard deviation;
Detection limit: Al:0.0283ug/mL;B:0.0077ug/mL;Ca:0.00216ug/mL;Cd:0.0018ug/mL; Fe:0.0194ug/mL;K:0.0147ug/mL;Mn:0.0009ug/mL;Na:0.0250ug/mL;Pb:0.0120ug/mL;Si: 0.0175ug/mL;S:0.0291ug/mL;
Determination Limit: Al:0.0942ug/mL;B:0.0256g/mL;Ca:0.0721ug/mL;Cd:0.0059ug/mL; Fe:0.0648ug/mL;K:0.0490ug/mL;Mn:0.0030ug/mL;Na:0.0832ug/mL;Pb:0.0401ug/mL;Si: 0.0582ug/mL;S:0.0971ug/mL.
Precision situation: being 1 μ g/mL with concentration after electronics coupled plasma atomic emission spectrometer preheats 30min Standard solution duplicate measurements 11 times, relative standard deviation≤1.5%.
The rate of recovery experiment: to high purity magnesium base oxide sample carry out recovery testu, obtain Al, B, Ca, Cd, Fe, K, The rate of recovery of Mn, Na, Pb, Si, S respectively 98.24~104.60%, 98.20~103.27%, 97.26~104.70%, 98.36~102.00%, 98.19~102.40%, 96.96~103.50%, 98.23~102.50%, 95.05~ 104.11%, 97.40~102.50%, 97.93~103.80%, 97.19~102.20%, fully meet wanting for analysis method It asks.
Steadiness: being respectively 1 μ with concentration after electronics coupled plasma atomic emission spectrometer preheats 30min The aluminium of g/mL, calcium, potassium, sodium, boron, iron, manganese, cadmium, lead, sulphur multielement standard mixed solution, the element silicon mark that concentration is 1 μ g/mL Quasi- solution is measured 1 time at interval of 20min, is measured 12 times altogether, relative standard deviation≤3%, the linear phase of working curve in 4h Close coefficients R >=0.999.
Sample of the present invention first passes through pretreatment, and potassium, sodium, calcium, sulphur, boron, lead, iron, cadmium, manganese, aluminium multielement mark is then added The standard solution of quasi- solution or element silicon is added hydrochloric acid, is diluted, finally uses inductively coupled plasma atomic emission spectrum Instrument is measured series standard solution.Using magnesium, calcium, potassium, sodium, boron, iron, manganese, cadmium, lead, sulphur, element silicon in inductive coupling etc. The universal law of emission spectrum in ion simulates high-purity serial magnesium-based oxide matrix, carries out coexistence elements and background emission light It composes research, measurement medium, analysis spectral line screening, matrix and elimination is tested and condition is excellent containing interfering with each other between miscellaneous element spectral line Change, establishes optimal sample determination condition;Using standard addition method as technological means, realize in high-purity serial magnesium-based oxide samples It is measured while trace impurity, enters internationalization market for China's advantage salt lake resources high-end product and technical support is provided, Meanwhile the method improves work efficiency, and reduces the labor intensity of operator, thus there is significant social benefit.
The present invention also has the positive effect that: (1) in the prior art, inductive coupling plasma emission spectrum method is measuring Trace element does not have the national standard substance of national standard, provincial standard or same matrix real in high-purity series magnesium-based oxide Quality control is applied, and the method for the invention utilizes aluminium, calcium, potassium, sodium, boron, iron, manganese, cadmium, lead, sulphur, element silicon in inductive coupling The universal law of emission spectrum in plasma simulates high-purity serial magnesium-based oxide matrix, carries out coexistence elements and background emission Spectral investigation, measurement medium, analysis spectral line screening, matrix and containing between miscellaneous element spectral line interfering with each other elimination test and condition it is excellent Change, establishes optimal sample determination condition;Using standard addition method as technological means, high-purity serial magnesium-based oxide samples are realized The measurement of middle trace impurity.(2) the method for the invention can detect Simultaneous Determination of Trace Elements in high purity magnesium base oxide simultaneously, Being suitable for mass percentage is usually 10-4The measurement of order of magnitude high purity magnesium base oxide impurity element, and the essence of testing result Density is high, and stability is good in instrument detection process, and enterprise's detection pressure can be effectively relieved in the method for the present invention, not only has important Meaning, and it is very necessary.It include magnesia, hydrogen for high-purity serial magnesium-based oxide of Qinghai Western Magnesium Technology Co., Ltd.'s production The detection of trace impurity provides technical support in magnesia and magnesium carbonate being developed and magnesium metal product sample.(3) It being difficult to handle high-purity serial magnesium-based oxide samples using existing method, the method for the present invention is handled sample by hydrochloric acid, The sample solution of high-purity serial magnesium-based oxide is obtained, is measured using standard addition method, is not directed to phase in the prior art Like method, there is not any enlightenment, sample treatment of the present invention is obtained by test of many times, has practical behaviour yet Make application value.
Specific embodiment
It is described further With reference to embodiment:
In the present embodiment,
1, key instrument and operating condition:
Inductively coupled plasma atomic emission spectrometer: iCAP 7000SERIES type, silent winged your science and technology of generation of U.S.'s match have Limit company;
Electronic balance: ME204E type, sensibility reciprocal 0.0001g, Switzerland Mei Teletuo benefit measuring technique Co., Ltd;
Thermo7400, RF frequency 27.12MHz, efficient concentric atomizer, plasma observed pattern: vertical (diameter ), wave-length coverage 166-847nm, optical resolution (FHW)≤0.007nm, at 200nm;At 0.014nm, 400nm; At 0.021nm, 600nm;Semiconductor refrigerating CID detector, detection unit > 290000.
Thermoelectricity ICP7400, power 950W, cooling air 12L/min assist gas 0.5L/min, carrier gas 0.5L/min, and observation is high Spend 12mm;The time of integration: long wave 5S, shortwave 15S;Pump speed: rinsing 50rpm, analyzes pump speed 50rpm.
Analytical element and wavelength is measured accordingly:
2, main agents
Hydrochloric acid: GR, Sichuan western Gansu Province science Co., Ltd;
Potassium, sodium, calcium, sulphur, boron, lead, iron, cadmium, manganese, aluminium multielement standard mixed solution: 1000ug/mL, number: GNM- M104320-2013, national non-ferrous metal and electronic material Institute of Analysis;
Element silicon standard solution: 1000ug/mL, number: GSB 04-1752-2004 (a), national non-ferrous metal and electronics Material analysis test center;
3, standard solution
The preparation A of standard solution:
Multielement standard mixed solution A 1 (100ug/mL): potassium, sodium, calcium, sulphur, boron, lead, iron, cadmium, manganese, aluminium are accurately pipetted Multielement standard mixed solution (10000ug/mL) 10.00mL is diluted with water to scale, constant volume shakes in 100ml volumetric flask It is even.
Element silicon standard solution A2 (100ug/mL): accurately pipette 10.00mL silicon standard solution (1000ug/mL) in In 100ml volumetric flask, it is diluted with water to scale, constant volume shakes up.
The preparation B of standard solution:
Multielement standard mixed solution B1 (10ug/mL): the above-mentioned multielement standard mixed solution A 1 of 10.00mL is accurately pipetted In 100mL volumetric flask, it is diluted with water to scale, constant volume shakes up.
Element silicon standard solution (10ug/mL) B2: the above-mentioned element silicon standard solution A2 of 10.00mL accurately is pipetted in 100ml In volumetric flask, it is diluted with water to scale, constant volume shakes up.
4, sample pretreatment
5.0000g sample is accurately weighed, in 250mL beaker, little water is added to soak, it is few in the case where glass bar is stirred continuously Repeatedly hydrochloric acid (1+1) is added in amount, until sample is completely dissolved, solution is limpid, and (1+1 hydrochloric acid theoretical addition amount is 30 milliliters, when necessary It adding few drops), rinses wall of cup with a small amount of water, (200 DEG C) the slightly boiled 2min of heating, are removed on low temperature electric hot plate, and it is cooling, move into 50 In milliliter volumetric flask, 5 milliliters of (1+1) hydrochloric acid is added, with water constant volume, shakes up.
The production of standard addition method working curve:
The production of multielement working curve: it is more that potassium, sodium, calcium, sulphur, boron, lead, iron, cadmium, manganese, aluminium are successively accurately pipetted respectively Elemental standards mixed solution B1 (10ug/mL): 0mL, 0.25mL, 0.50mL, 1.25mL, 2.50mL, 5.00mL, in one group of 25mL In volumetric flask, the good sample solution 2.50mL of above-mentioned pretreatment is successively accurately added, hydrochloric acid 0.5mL is added, is diluted with water to quarter Degree, constant volume shake up.The corresponding potassium of this working curve, sodium, calcium, sulphur, boron, lead, iron, cadmium, manganese, aluminium element concentration be respectively 0ug/mL、0.10ug/mL、0.20ug/mL、0.50ug/mL、1.00ug/mL、2.00ug/mL。
The production of element silicon standard working solution: accurately pipette element silicon standard solution B2 (10ug/mL): 0mL, It is good that above-mentioned pretreatment is accurately added in one group of 25mL volumetric flask in 0.25mL, 0.50mL, 1.25mL, 2.50mL, 5.00mL Sample solution 2.50mL, is diluted with water to scale, and constant volume shakes up.The concentration that this working curve corresponds to element silicon is respectively 0ug/ mL、0.10ug/mL、0.20ug/mL、0.50ug/mL、1.00ug/mL、2.00ug/mL。
The operating condition optimized according to instrument, the wavelength of element to be measured, with ICP-OES successively to series standard solution into Row measurement, with concentration 0ug/mL, 0.10ug/mL of the corresponding standard solution of each element, 0.20ug/mL, 0.50ug/mL, 1.00ug/mL, 2.00ug/mL are that abscissa is mapped, obtained using corresponding intensity of emission spectra under each concentration as ordinate To the standard curve of each element standard addition method.The intersection point of curve and axis of abscissas is the concentration of element to be measured in sample, is multiplied With corresponding extension rate, (after 5.0000g sample pretreatment constant volume in 50mL volumetric flask, pipette 2.50mL sample constant volume in In 25mL volumetric flask) to get the content of element to be measured in sample.
5, it measures: successively series standard solution being measured with inductively coupled plasma atomic emission spectrometer, with Concentration 0ug/mL, 0.10ug/mL of the corresponding standard solution of each element, 0.20ug/mL, 0.50ug/mL, 1.00ug/mL, 2.00ug/mL is abscissa, using corresponding intensity of emission spectra under each concentration as ordinate, maps, obtains each element mark The intersection point of the standard curve of quasi- addition method, curve and axis of abscissas is the concentration of element to be measured in sample, multiplied by corresponding dilute Multiple is released to get the content of element to be measured in sample.
In steps of 5, each analytical element and corresponding wavelength are as follows: Al 167.079nm, B 249.773nm, Ca are 393.366nm, Cd 228.802nm, Fe 238.204nm, K 766.490nm, Mn 257.610nm, Na are 589.592nm, Pb 220.353nm, S 182.034nm, Si 251.611nm.
In step 4, the sample amount of pipetting is 5.0000g, and 1+1 hydrochloric acid additional amount is 30 milliliters, is added when necessary few drops;Low Slightly boiled 2min is heated with 200 DEG C of temperature on warm electric hot plate, is moved into after cooling in 50 milliliters of volumetric flask and adds (1+1) hydrochloric acid It 5 milliliters, with water constant volume, shakes up.
The concentration of element silicon standard solution is 1000ug/mL, potassium, sodium, calcium, sulphur, boron, lead, iron, cadmium, manganese, aluminium multielement mark The concentration of quasi- mixed solution is 1000ug/mL, and the concentration of multielement standard mixed solution A 1 is 100ug/mL, and element silicon standard is molten The concentration of liquid A2 is 100ug/mL, and the concentration of multielement standard mixed solution B1 is 10ug/mL, and element silicon standard solution B2's is dense Degree is 10ug/mL.
Co-existing element interference is investigated
Magnesium matrix when magnesium-based bulk concentration is respectively 10mg/mL, 20mg/mL, 30mg/mL in high purity magnesium base oxide is investigated Interference to element to be measured, it is determined that magnesium-based bulk concentration is noiseless to element to be measured when being not more than 20mg/mL.
Detection limit situation
It is blank METHOD FOR CONTINUOUS DETERMINATION 11 times with 2%HCL under the conditions of laboratory apparatus of the present invention, with 3 times of standards of measurement result Deviation is as detection limit, using 10 times of Determination Limits as this method of standard deviation;
Detection limit: Al:0.0283ug/mL;B:0.0077ug/mL;Ca:0.00216ug/mL;Cd:0.0018ug/mL; Fe:0.0194ug/mL;K:0.0147ug/mL;Mn:0.0009ug/mL;Na:0.0250ug/mL;Pb:0.0120ug/mL;Si: 0.0175ug/mL;S:0.0291ug/mL;
Determination Limit: Al:0.0942ug/mL;B:0.0256g/mL;Ca:0.0721ug/mL;Cd:0.0059ug/mL; Fe:0.0648ug/mL;K:0.0490ug/mL;Mn:0.0030ug/mL;Na:0.0832ug/mL;Pb:0.0401ug/mL;Si: 0.0582ug/mL;S:0.0971ug/mL.
Precision situation
After electronics coupled plasma atomic emission spectrometer preheats 30min, the standard solution for being 1 μ g/mL with concentration Duplicate measurements 11 times, relative standard deviation≤1.5%.
Rate of recovery experiment
To high purity magnesium base oxide sample carry out recovery testu, obtain Al, B, Ca, Cd, Fe, K, Mn, Na, Pb, Si, The rate of recovery of S respectively 98.24~104.60%, 98.20~103.27%, 97.26~104.70%, 98.36~ 102.00%, 98.19~102.40%, 96.96~103.50%, 98.23~102.50%, 95.05~104.11%, 97.40~102.50%, 97.93~103.80%, 97.19~102.20%, fully meet the requirement of analysis method;
Steadiness is respectively 1 μ with concentration after electronics coupled plasma atomic emission spectrometer preheats 30min The aluminium of g/mL, calcium, potassium, sodium, boron, iron, manganese, cadmium, lead, sulphur multielement standard mixed solution, the element silicon mark that concentration is 1 μ g/mL Quasi- solution is measured 1 time at interval of 20min, is measured 12 times altogether, relative standard deviation≤3%, the linear phase of working curve in 4h Coefficients R >=0.999 is closed, Precision test result is shown in Table 1, and detection limit and Determination Limit measurement result are shown in Table 2, determination of recovery rates knot Fruit is shown in Table 3.
The Precision test result (%) of 1 the method for the present invention of table
The detection limit and Determination Limit (ug/mL) of 2 the method for the present invention of table
3 mark-on reclaims of table test (%)
The above has been described in detail, described above, is only a preferred embodiment of the present invention, when cannot Limit practical range of the invention, i.e., it is all according to the made equivalent changes and modifications of the application range, it should still belong to the present invention and cover model In enclosing.

Claims (8)

1. the method for trace element, feature in a kind of inductively coupled plasma emission spectrography measurement high purity magnesium base oxide Be: sample first passes through pretreatment, and then addition aluminium, calcium, potassium, sodium, boron, iron, manganese, cadmium, lead, the multielement standard mixing of sulphur are molten The standard solution of liquid or element silicon is added hydrochloric acid, is diluted, finally with inductively coupled plasma atomic emission spectrometer pair Series standard solution is measured, and specific determination step is as follows,
1) prepare reagent: including hydrochloric acid and potassium, sodium, calcium, sulphur, boron, lead, iron, cadmium, manganese, aluminium multielement standard mixed solution, Element silicon standard solution;
2) preparing standard solution
A, it is mixed that potassium, sodium, calcium, sulphur, boron, lead, iron, cadmium, manganese, aluminium multielement standard accurately multielement standard mixed solution A 1: are pipetted Solution is closed, scale is diluted with water to, constant volume shakes up to get multielement standard mixed solution A 1 is arrived;
Element silicon standard solution A2: accurately pipetting element silicon standard solution, is diluted with water to scale, and constant volume shakes up to get silicon is arrived Elemental standard solution A2;
B, multielement standard mixed solution B1: accurately pipetting multielement standard solution A1, be diluted with water to scale, and constant volume shakes up, Obtain the multielement standard mixed solution B1 that concentration is multielement standard solution A1 concentration 10%;
Element silicon standard solution B2: element silicon standard solution A2 accurately is pipetted, is diluted with water to scale, constant volume shakes up, and obtains dense Degree is the silicon standard solution B2 of silicon standard solution A2 concentration 10%;
3) sample pretreatment: accurately weighing sample, and little water is added to soak, a small amount of that salt is repeatedly added in the case where glass bar is stirred continuously Sour (1+1), until sample is completely dissolved, solution is limpid, rinses wall of cup with a small amount of water, slightly boiled 2min is heated on low temperature electric hot plate, It removes, it is cooling, it moves into volumetric flask, (1+1) hydrochloric acid is added and is shaken up with water constant volume, obtains sample solution;
4) production of standard addition method working curve
The production of multielement working curve: successively accurately pipette respectively multielement standard solution B1:0mL, 0.25mL, 0.50mL, The good sample solution of above-mentioned pretreatment is successively accurately added in one group of 25mL volumetric flask in 1.25mL, 2.50mL, 5.00mL 2.50mL is added hydrochloric acid 0.5mL, is diluted with water to scale, constant volume shakes up;The corresponding potassium of this working curve, sodium, calcium, sulphur, boron, Lead, iron, cadmium, manganese, aluminium element concentration be respectively 0ug/mL, 0.10ug/mL, 0.20ug/mL, 0.50ug/mL, 1.00ug/mL, 2.00ug/mL;
The production of element silicon standard working solution: accurately pipette element silicon standard solution B2:0mL, 0.25mL, 0.50mL, The good sample solution 2.50mL of above-mentioned pretreatment is accurately added in one group of 25mL volumetric flask in 1.25mL, 2.50mL, 5.00mL, It is diluted with water to scale, constant volume shakes up;This working curve correspond to element silicon concentration be respectively 0ug/mL, 0.10ug/mL, 0.20ug/mL,0.50ug/mL,1.00ug/mL,2.00ug/mL;
5) it measures: successively series standard solution being measured with inductively coupled plasma atomic emission spectrometer, Yi Geyuan Concentration 0ug/mL, 0.10ug/mL, 0.20ug/mL, 0.50ug/mL, 1.00ug/mL, 2.00ug/ of the corresponding standard solution of element ML is abscissa, using corresponding intensity of emission spectra under each concentration as ordinate, maps, obtains each element standard addition method Standard curve, the intersection point of curve and axis of abscissas is the concentration of element to be measured in sample, multiplied by corresponding extension rate, i.e., The content of element to be measured in sample.
2. multielement in inductively coupled plasma emission spectrography measurement high purity magnesium base oxide according to claim 1 Method, it is characterised in that: in step 5), each analytical element and corresponding wavelength are as follows: Al 167.079nm, B are 249.773nm, Ca 393.366nm, Cd 228.802nm, Fe 238.204nm, K 766.490nm, Mn are 257.610nm, Na 589.592nm, Pb 220.353nm, S 182.034nm, Si 251.611nm.
3. multielement in inductively coupled plasma emission spectrography measurement high purity magnesium base oxide according to claim 1 Method, it is characterised in that: in step 3), the sample amount of pipetting be 5.0000g, (1+1) hydrochloric acid additional amount be 30 milliliters, when necessary It adds few drops;Slightly boiled 2min is heated with 200 DEG C of temperature on low temperature electric hot plate, is moved into after cooling in 50 milliliters of volumetric flask again 5 milliliters of (1+1) hydrochloric acid is added, with water constant volume, shakes up.
4. trace member in inductively coupled plasma emission spectrography measurement high purity magnesium base oxide according to claim 1 Element method, it is characterised in that: the concentration of element silicon standard solution be 1000ug/mL, potassium, sodium, calcium, sulphur, boron, lead, iron, cadmium, Manganese, aluminium multielement standard mixed solution concentration be 1000ug/mL, the concentration of multielement standard mixed solution A 1 is 100ug/ The concentration of mL, element silicon standard solution A2 are 100ug/mL, and the concentration of multielement standard mixed solution B1 is 10ug/mL, silicon member The concentration of plain standard solution B2 is 10ug/mL.
5. trace member in inductively coupled plasma emission spectrography measurement high purity magnesium base oxide according to claim 1 The method of element, it is characterised in that: with 2%HCL be blank METHOD FOR CONTINUOUS DETERMINATION 11 times, be used as this using 3 times of standard deviations of measurement result The detection limit of method, using 10 times of Determination Limits as this method of standard deviation;
Detection limit: Al:0.0283ug/mL;B:0.0077ug/mL;Ca:0.00216ug/mL;Cd:0.0018ug/mL;Fe: 0.0194ug/mL;K:0.0147ug/mL;Mn:0.0009ug/mL;Na:0.0250ug/mL;Pb:0.0120ug/mL;Si: 0.0175ug/mL;S:0.0291ug/mL;
Determination Limit: Al:0.0942ug/mL;B:0.0256g/mL;Ca:0.0721ug/mL;Cd:0.0059ug/mL;Fe: 0.0648ug/mL;K:0.0490ug/mL;Mn:0.0030ug/mL;Na:0.0832ug/mL;Pb:0.0401ug/mL;Si: 0.0582ug/mL;S:0.0971ug/mL.
6. trace member in inductively coupled plasma emission spectrography measurement high purity magnesium base oxide according to claim 1 The method of element, it is characterised in that: be 1 μ g/ with concentration after inductively coupled plasma atomic emission spectrometer preheats 30min The standard solution duplicate measurements of mL 11 times, makes its relative standard deviation≤1.5%.
7. trace member in inductively coupled plasma emission spectrography measurement high purity magnesium base oxide according to claim 1 Element method, it is characterised in that: to high purity magnesium base oxide sample carry out recovery testu, obtain Al, B, Ca, Cd, Fe, K, The rate of recovery of Mn, Na, Pb, Si, S is respectively 98.24~104.60%, 98.20~103.27%, 97.26~104.70%, 98.36~102.00%, 98.19~102.40%, 96.96~103.50%, 98.23~102.50%, 95.05~ 104.11%, 97.40~102.50%, 97.93~103.80%, 97.19~102.20%, to meet wanting for analysis method It asks.
8. trace member in inductively coupled plasma emission spectrography measurement high purity magnesium base oxide according to claim 1 The method of element, it is characterised in that: be respectively 1 with concentration after inductively coupled plasma atomic emission spectrometer preheats 30min The aluminium of μ g/mL, calcium, potassium, sodium, boron, iron, manganese, cadmium, lead, sulphur multielement standard mixed solution, the element silicon mark that concentration is 1 μ g/mL Quasi- solution is measured 1 time at interval of 20min, is measured 12 times altogether, relative standard deviation≤3%, the linear phase of working curve in 4h Close coefficients R >=0.999.
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