CN102033101A - Method for measuring metal impurities in high-purity MgO film material by using inductively coupled plasma mass spectrometer - Google Patents
Method for measuring metal impurities in high-purity MgO film material by using inductively coupled plasma mass spectrometer Download PDFInfo
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Abstract
The invention discloses a method for measuring metal impurities in a high-purity MgO film material by using an inductively coupled plasma mass spectrometer. The method comprises the following steps of: (1) preparing to-be-measured solution of the MgO film material; (2) preparing impurity-containing series standard solution samples of different concentrations; (3) selecting the working conditions of the inductively coupled plasma mass spectrometer, selecting isotopes of to-be-measured elements, measuring Ca, Fe and As in an H2 mode, measuring Al, Ti, V, Cr, Mn, Ni, Co, Cu, Zn, Zr, Mo, Cd, Sn, Sb, W, Pb and Bi in an Ar mode, analyzing the series standard solution samples to obtain working curves Yn=aXn+b of corresponding impurities, and analyzing the to-be-measured solution of the MgO film material to obtain the concentration values of the impurities; and (4) according to the concentration values of the impurities, obtaining the mass percentage of the to-be-measured impurity elements by calculating. The inductively coupled plasma mass spectrometer (ICP-MS) taking inductively coupled plasma as an excitation source and taking mass spectrum as a detector in the method has high sensitivity, low detection limit and good reproducibility, and can accurately measure the impurity elements in the high-purity material.
Description
Technical field
The present invention relates to the determination techniques of impurity in a kind of Coating Materials, relate in particular to a kind of method of using icp ms to measure metallic impurity in the high-purity MgO coating materials.
Background technology
The related method research of this invention is to launch greater than 99.99% MgO coating materials impurity analysis demand at the purity that the client provides.At present, the analysis to magnesium and magnesium alloy in the national standard method is that single element folk prescription method is carried out, and mostly is photometry and gravimetric method, and operating process is tediously long, and sample determination speed is too slow.Inductivity coupled plasma mass spectrometry has very strong advantage aspect the multielement mensuration, and the element detectability is very low, can better meet the needs that metallic impurity are analyzed in the high-purity MgO coating materials.
Summary of the invention
The purpose of this invention is to provide a kind of method that adopts icp ms to measure metallic impurity in the high-purity MgO coating materials, this method can realize that multiple element detects simultaneously, and the sample intermediate treatment is simple, and testing result is true and reliable.
For achieving the above object, the present invention takes following technical scheme:
With the method for metallic impurity in the icp ms mensuration high-purity MgO coating materials, this method comprises following operation steps:
(1), the MgO coating materials is dissolved in the dilute acid soln, add Cs, Tl inner mark solution, and use the deionized water constant volume, obtain the solution to be measured of MgO coating materials;
(2), preparation contains the series standard solution example of the variable concentrations of impurity A l, Cr, Mn, Ni, Co, Cu, Zn, Cd, Sn, Sb, Pb, Ca, Fe, As, BiV, Ti, Zr, Mo and W, and add the inner mark solution of Cs, Tl in each standard solution sample;
(3), the condition of work of selected icp ms, select element isotope to be measured, Ca, Fe and As are at H
2Measure under the pattern, Al, Ti, V, Cr, Mn, Ni, Co, Cu, Zn, Zr, Mo, Cd, Sn, Sb, W, Pb and Bi measure under the Ar pattern, from low to high the series standard solution example of each impurity element is analyzed according to concentration then, thereby obtained the working curve Y of corresponding impurity
n=aX
n+ b, its linearly dependent coefficient r all requires greater than 0.9990, wherein, X represents the concentration of certain impurity element, Y is the signal intensity rate of impurity element and internal standard element under this concentration, and n is a kind of among Al, Cr, Mn, Ni, Co, Cu, Zn, Cd, Sn, Sb, Pb, Ca, Fe, As, Bi, V, Ti, Zr, Mo and the W; Then the solution to be measured of MgO coating materials is analyzed, obtained the signal intensity rate Y of certain unknown element and internal standard element in the solution to be measured
u, the working curve of bringing this element into obtains the concentration value C of each element to be measured in the solution to be measured of MgO coating materials
u, obtain the concentration value of Al, Cr, Mn, Ni, Co, Cu, Zn, Cd, Sn, Sb, Pb, Ca, Fe, As, Bi, V, Ti, Zr, Mo and W successively;
(4), the concentration of impurity element to be measured in the sample solution that obtains according to step (3), by calculating the quality percentage composition of impurity element to be measured.
In described step (1), the Mg in the solution to be measured of described MgO coating materials
2+Concentration be 0.5～1mg/mL, the concentration of Cs and Tl is 10～20ng/mL.
In described step (2), the described series standard solution example that contains the variable concentrations of each impurity, be to be starting point with 0, and with 5-20ng/mL be each impurity in the series standard solution example concentration at interval, make the standard solution sample of the variable concentrations contain each impurity be at least three, and the Cs in each standard solution sample and the concentration of Tl are 10～20ng/mL.
Though Cs in the solution to be measured of MgO coating materials and the concentration of Tl are 10～20ng/mL, and the concentration of Cs in each standard solution sample and Tl also is 10～20ng/mL, and this is that the range of control of the concentration of Cs in concentration and the standard solution sample of Cs in the solution to be measured of MgO coating materials and Tl and Tl is identical.During metallic impurity in measuring same MgO coating materials, Cs in Cs in the solution to be measured of this MgO coating materials and the concentration of Tl and each standard solution sample and the concrete concentration of Tl also should be identical, promptly, when the concentration of Cs in the solution to be measured of MgO coating materials and Tl was 20ng/mL, Cs in each standard solution sample and the concentration of Tl also were 20ng/mL; When the concentration of Cs in the solution to be measured of MgO coating materials and Tl was 10ng/mL, Cs in each standard solution sample and the concentration of Tl also were 10ng/mL.
In described step (2), at first, with Al, Cr, Mn, Ni, Co, Cu, Zn, Cd, Sn, Sb, Pb, Ca, Fe, As, BiV, Ti, Zr, 20 kinds of elements of Mo and W are divided into Al, Cr, Mn, Ni, Co, Cu, Zn, Cd, Sn, Sb, Pb, Ca, Fe, one group and the V of As and Bi, Ti, Zr, another group of Mo and W, and make and contain Al, Cr, Mn, Ni, Co, Cu, Zn, Cd, Sn, Sb, Pb, Ca, Fe, first group the stock solution of As and Bi and contain V, Ti, Zr, second group the stock solution of Mo and W, and every group of stock solution made the series standard solution example of the variable concentrations that contains each impurity.
In described step (4), be to adopt following computing formula to calculate the quality percentage composition of impurity element to be measured, computing formula is: w%=C
u(ng/mL) * 10
-9* 100mL * 100/M (g)=C
u(ng/mL) * 10
-5/ M (g), wherein M represents the sample quality that takes by weighing.
In described step (1) and step (2), Cs, Tl be with
133Cs,
205Tl is an internal standard element.
In described step (1), dilute acid soln is preferably the hydrochloric acid solution of 8-15vt% concentration.Because the instrument condition of work does not allow, and does not generally select dilute sulfuric acid for use; And, generally do not select rare nitric acid for use yet, reason is that the course of dissolution of sample has the crystalline solid appearance.
The concentration that the present invention adopts icp ms to measure the impurity element storing solution that uses in the method for metallic impurity in the high-purity MgO coating materials is 1 μ g/mL, be to be that the impurity storing solution dilution of 1mg/mL obtains, and under 4 ℃ of conditions, preserve standby by concentration.In practical operation, use two groups of impurity element storing solutions, wherein, the stock solution that contains Al, Cr, Mn, Ni, Co, Cu, Zn, Cd, Sn, Sb, Pb, Ca, Fe, As and Bi is the stock solution of first group of impurity element, in the stock solution of first group of impurity element, impurity element is to be dissolved in HNO
3In the medium, the concentration of contained 15 kinds of impurity is 1 μ g/mL; The stock solution that contains V, Ti, Zr, Mo and W is the stock solution of second group of impurity element, and in the stock solution of second group of impurity element, impurity element is to be dissolved in HNO
3In the HF medium, HNO
3With the volume ratio of HF be 1: 1, the concentration of contained 5 kinds of impurity is 1 μ g/mL.
In preparation series standard solution example process, use above-mentioned two groups of impurity element storing solutions.In above-mentioned two groups of impurity element storing solutions, the concentration of contained various impurity is 1 μ g/mL, pipettes 0 respectively by series, 100,200,300, two groups of impurity element storing solutions of 400 μ L, that is to say, the stock solution of first group of impurity element is pipetted 0,100 respectively, 200,300,400 μ L pipette 0 respectively with the stock solution of second group of impurity element, 100,200,300,400 μ L, two groups of totally 8 samples, in these 8 samples, add 200 μ L concentration more respectively and be 1 μ g/mL Cs, the Tl inner mark solution is used the deionized water constant volume to the 10mL scale mark, thereby is obtained series standard solution.The series standard solution example of first group of impurity element is totally 5 standard points, and the concentration of 15 kinds of impurity is 0,10,20,30,40ng/mL, and the Cs in each standard solution sample, the concentration of Tl are 20ng/mL.The series standard solution example of second group of impurity element is totally 5 standard points, and the concentration of 5 kinds of impurity is 0,10,20,30,40ng/mL, and the Cs in each standard solution sample, the concentration of Tl are 20ng/mL.
Icp ms is measured the process of metallic impurity in the high-purity MgO coating materials and is among the present invention:
1) argon gas, hydrogen and recirculated cooling water are opened in icp ms is started shooting preheating, open Control Software, and the running parameter of instrument is set.After ready, click " igniting " shortcut, form stable plasmatorch.
2) edit methods program file mainly comprises the isotopic selection of element to be measured, Ar or H
2Concentration value of each standard point etc. on the setting of mode of operation and the input service curve;
3) under selected condition of work, according to concentration from low to high to each element be class standard analysis, thereby obtain corresponding work curve Y=aX+b, its linearly dependent coefficient r all requires greater than 0.9990.Wherein ordinate Y represents the signal intensity ratio of impurity element and internal standard element, and horizontal ordinate X represents the concentration of impurity element.Then unknown sample is analyzed, and obtained the concentration value C of each element to be measured in the unknown sample solution by working curve
u
4) concentration of element in the solution per sample is by calculating its percentage composition.
Adopt the method for matrix coupling to eliminate matrix effect among the present invention, the natural isotope of Mg does not have mass spectrum to disturb for the mensuration of element to be measured simultaneously.
Advantage of the present invention is:
1, the icp ms that adopts in the inventive method (ICP-MS) is excitaton source with the inductively coupled plasma, with the mass spectrum is detecting device, have highly sensitive, detectability is low, the advantage of favorable reproducibility, in conjunction with conventional chemical pre-treatment means, can measure the impurity element in the high-purity material accurately, accurately.The present invention selects suitable element isotope to measure according to abundance height, the little selection of interference, eliminating under the condition that matrix disturbs, mass spectrum disturbs, can measure more than 20 kind of trace metal impurity in the MgO coating materials simultaneously.Finding speed is fast, the accuracy height, and precision is good.
2, different elements adopt different mode determinations among the present invention, as Ca, Fe and As at H
2Under the pattern, with H
2For carrier gas is measured, effectively having avoided is separately under the carrier gas condition with Ar
40Ar,
40Ar
16O,
40Ar
35Cl for
40Ca,
56Fe,
75The interference of As has overcome the defective that Ca, Fe and As can not measure simultaneously with other element.
3, sample pre-treatments of the present invention is very simple, and directly application is convenient in the sample introduction analysis of the molten back of acid.
Description of drawings
Fig. 1 is a working curve of measuring metallic impurity Ca in the high-purity MgO coating materials with ICP-MS.
Embodiment
The present invention will be further described below in conjunction with specific embodiment:
Embodiment
The present invention is as follows with trace metal impurity concrete steps in the icp ms mensuration high-purity MgO coating materials:
Test experiments of the present invention carries out in high-purity laboratory;
1, The pretreatment
Take by weighing 0.1g MgO coating materials, be accurate to 0.0001g in the quartz beaker of 100mL, add rare HCl (1+9) 10mL, 50 ℃ of left and right sides heating for dissolving of low temperature, treat to change in the 100ml volumetric flask after sample dissolves fully, add 2mL concentration and be Cs, the Tl inner mark solution of 1 μ g/mL, to scale mark, it is C that this unknown sample GOLD FROM PLATING SOLUTION to be measured belongs to impurity concentration with the deionized water constant volume of 18.3 megaohms
u(ng/mL).
2, the preparation of standard solution
According to element character 20 kinds of elements are divided into two groups, wherein first group of impurities comprises: Al, Cr, Mn, Ni, Co, Cu, Zn, Cd, Sn, Sb, Pb, Ca, Fe, As, Bi are dissolved in these 15 kinds of impurity elements the HNO of 10vt%
3In the aqueous solution, prepare the stock solution of first group of impurity element, in the stock solution of first group of impurity element, the concentration of contained 15 kinds of impurity is 1 μ g/mL; Second group of impurities comprises: V, Ti, Zr, Mo, W.These 5 kinds of impurity elements are dissolved in the HNO that concentration is 10vt%
3With concentration be that (concentration is the HNO of 10vt% for the mixed aqueous solution of the HF of 10vt%
3With concentration be that the volume ratio of the HF of 10vt% is 1: 1) in, prepare the stock solution of second group of impurity element, in the stock solution of second group of impurity element, the concentration of contained 5 kinds of impurity is 1 μ g/mL.
Compound concentration is 0,10,20,30, during the series standard point of 40ng/mL, pipette the stock solution of first group of impurity element of 1 μ g/mL and the stock solution 0 of second group of impurity element respectively, 100,200,300,400 μ L are in the graduated tube of 10mL, obtain every group of 5 standard points, two groups totally 10, in these 10 standard points, add Cs, the Tl inner mark solution that 200 μ L concentration are 1 μ g/mL more respectively successively, use the deionized water constant volume to the 10mL scale mark.
3, Instrument measuring
1) argon gas, hydrogen and recirculated cooling water are opened in icp ms is started shooting preheating, open Control Software, and the running parameter of Agilent 7500ceICP-MS instrument is set:
Table 1 instrument parameter
After ready, click " igniting " shortcut, form stable plasmatorch.
2) edit methods mainly comprises the isotopic selection of element to be measured, Ar or H
2Concentration value of each standard point etc. on the selection of mode of operation and the input service curve; The concentration value of each impurity element standard point is 0,10,20,30,40ng/mL series.
Ca, Fe and As are at H
2Measure under the pattern, avoid under the Ar pattern
40Ar,
40Ar
16O,
40Ar
35Cl for
40Ca and
56Fe,
75The interference of As, Al, Ti, V, Cr, Mn, Ni, Co, Cu, Zn, Zr, Mo, Cd, Sn, Sb, W, Pb and Bi measure under the Ar pattern.
Prove through repetition test, select element mass number as shown in table 2 preferable:
The selection of table 2 metallic element isotopic mass to be measured number
| Element | Al | Ca | Ti | V | Cr | Mn | Fe | Ni | Co | Cu |
| Mass number | 27 | 40 | 48 | 51 | 52 | 55 | 56 | 58 | 59 | 63 |
| Element | Zn | As | Zr | Mo | Cd | Sn | Sb | W | Pb | Bi |
| Mass number | 64 | 75 | 90 | 98 | 113 | 120 | 121 | 184 | 208 | 209 |
When selecting element mass number as shown in table 2 for use, detection limit is low, and the working curve linearly dependent coefficient is good, and the mark-on recovering state is good.
3) from low to high the series standard solution of each element is analyzed according to concentration, thereby obtained the working curve Y of corresponding impurity element
n=aX
n+ b, its linearly dependent coefficient r all requires greater than 0.9990, and wherein, X represents the concentration of certain impurity element, and Y is the signal intensity rate of impurity element and internal standard element under this concentration.Then the solution to be measured of MgO coating materials is analyzed, obtained the signal intensity rate Y of certain unknown element and internal standard element in the solution to be measured
u, the working curve of bringing this element into obtains the concentration value C of each element to be measured in the solution to be measured of MgO coating materials
u
4, the concentration C of impurity element in the solution per sample
u(ng/mL), calculate the percentage composition w% of this element in the solid sample.
Computing formula is:
W%=C
u(ng/mL) * 10
-9* 100mL * 100/M (g)=C
u(ng/mL) * 10
-5/ M (g), wherein M represents the sample quality that takes by weighing.
Select isotope according to table 2, each impurity element in the series standard solution is analyzed, obtain the working curve of 20 kinds of impurity elements.Greater than 0.9990 o'clock, think linear good at linearly dependent coefficient, can be used for sample analysis.The curvilinear equation of each element, linearly dependent coefficient and detection limit see Table 3, and working curve diagram is example with Ca, and as shown in Figure 1, its linear equation is Y=0.0214X+0.1767, and linearly dependent coefficient is r=0.9997.
The mensuration of table 3 standard solution
Sample determination result and mark-on reclaim and the results are shown in Table 4.Mark-on reclaims investigates the reliability height that the result shows the inventive method.
The present invention selects suitable element isotope to measure according to abundance height, the little selection of interference, eliminating under the condition that matrix disturbs, mass spectrum disturbs, can measure 20 kinds of trace metallic impurity in the MgO coating materials simultaneously.Finding speed is fast, the accuracy height, and precision is good, the reliability height.
Table 4 sample determination and mark-on reclaim the result
Annotate: ND* is not for detecting.
The working curve of measuring metallic impurity Ca in the high-purity MgO coating materials with ICP-MS as shown in Figure 1.Its mensuration, analysis and computation process are as follows: at first metallic impurity Ca is carried out isotopic selection, according to table 2, metallic element Ca isotope to be measured is chosen as
40Ca, adopt icp ms under the Ar mode of operation, to measure metallic impurity Ca, according to concentration is 0,10,20,30, the value of 40ng/mL is analyzed the series standard solution example of impurity element Ca from low to high, thereby obtains impurity element Ca 0,10,20,30, (horizontal ordinate of seeing Fig. 1 is 0,10 with pairing four values of the signal intensity ratio of internal standard element under the 40ng/mL concentration, 20,30, the counting ratio of the pairing ordinate of 40ng/mL), utilize this four groups of corresponding values, make the working curve of measuring metallic impurity Ca in the high-purity MgO coating materials with ICP-MS, this working curve Y
Ca=0.0214X
Ca+ 0.1767 as shown in Figure 1, and its linearly dependent coefficient is r=0.9997, wherein, and X
CaThe concentration of expression Ca impurity element, Y
CaSignal intensity rate for Ca impurity element and internal standard element under a certain concentration.Adopt icp ms that the solution to be measured of MgO coating materials is analyzed then, obtain the signal intensity rate Y of Ca impurity element and internal standard element in the solution to be measured
u, bring the working curve of the Ca element among Fig. 1 into, obtain the concentration value C of Ca element to be measured in the solution to be measured of MgO coating materials
uConcentration C according to impurity Ca element to be measured in the solution to be measured
u(ng/mL), calculate the percentage mass content w% of this Ca element in the solid sample.According to computing formula: w%=C
u(ng/mL) * 10
-9* 100mL * 100/M (g)=C
u(ng/mL) * 10
-5/ M (g), wherein M represents the sample quality that takes by weighing, obtains the content 3.8 * 10 of the mass percent of impurity Ca element in the high-purity MgO coating materials
-4Quality %.
Claims (7)
1. measure the method for metallic impurity in the high-purity MgO coating materials with icp ms, it is characterized in that this method comprises following operation steps:
(1), the MgO coating materials is dissolved in the dilute acid soln, add Cs, Tl inner mark solution, and use the deionized water constant volume, obtain the solution to be measured of MgO coating materials;
(2), preparation contains the series standard solution example of the variable concentrations of impurity A l, Cr, Mn, Ni, Co, Cu, Zn, Cd, Sn, Sb, Pb, Ca, Fe, As, Bi, V, Ti, Zr, Mo and W, and add the inner mark solution of Cs, Tl in each standard solution sample;
(3), the condition of work of selected icp ms, select element isotope to be measured, Ca, Fe and As are at H
2Measure under the pattern, Al, Ti, V, Cr, Mn, Ni, Co, Cu, Zn, Zr, Mo, Cd, Sn, Sb, W, Pb and Bi measure under the Ar pattern, from low to high the series standard solution example of each impurity element is analyzed according to concentration then, thereby obtained the working curve Y of corresponding impurity
n=aX
n+ b, its linearly dependent coefficient r all requires greater than 0.9990, wherein, X represents the concentration of certain impurity element, Y is the signal intensity rate of impurity element and internal standard element under this concentration, and n is a kind of among Al, Cr, Mn, Ni, Co, Cu, Zn, Cd, Sn, Sb, Pb, Ca, Fe, As, Bi, V, Ti, Zr, Mo and the W; Then the solution to be measured of MgO coating materials is analyzed, obtained the signal intensity rate Y of certain unknown element and internal standard element in the solution to be measured
u, the working curve of bringing this element into obtains the concentration value C of each element to be measured in the solution to be measured of MgO coating materials
u, obtain the concentration value of Al, Cr, Mn, Ni, Co, Cu, Zn, Cd, Sn, Sb, Pb, Ca, Fe, As, BiV, Ti, Zr, Mo and W successively;
(4), the concentration of impurity element to be measured in the sample solution that obtains according to step (3), by calculating the quality percentage composition of impurity element to be measured.
2. the method with metallic impurity in the icp ms mensuration high-purity MgO coating materials according to claim 1 is characterized in that, in described step (1), and the Mg in the solution to be measured of described MgO coating materials
2+Concentration be 0.5～1mg/mL, the concentration of Cs and Tl is 10～20ng/mL.
3. the method for measuring metallic impurity in the high-purity MgO coating materials with icp ms according to claim 1, it is characterized in that, in described step (2), the described series standard solution example that contains the variable concentrations of each impurity, be to be starting point with 0, and with 5-20ng/mL be each impurity in the series standard solution example concentration at interval, make the standard solution sample of the variable concentrations contain each impurity be at least three, and the Cs in each standard solution sample and the concentration of Tl are 10～20ng/mL.
4. the method for measuring metallic impurity in the high-purity MgO coating materials with icp ms according to claim 3, it is characterized in that, in described step (2), at first, with Al, Cr, Mn, Ni, Co, Cu, Zn, Cd, Sn, Sb, Pb, Ca, Fe, As, BiV, Ti, Zr, Mo and W20 kind element are divided into Al, Cr, Mn, Ni, Co, Cu, Zn, Cd, Sn, Sb, Pb, Ca, Fe, one group and the V of As and Bi, Ti, Zr, another group of Mo and W, and make and contain Al, Cr, Mn, Ni, Co, Cu, Zn, Cd, Sn, Sb, Pb, Ca, Fe, first group the stock solution of As and Bi and contain V, Ti, Zr, second group the stock solution of Mo and W, and every group of stock solution made the series standard solution example of the variable concentrations that contains each impurity.
5. the method for measuring metallic impurity in the high-purity MgO coating materials with icp ms according to claim 1, it is characterized in that, in described step (4), be to adopt following computing formula to calculate the quality percentage composition of impurity element to be measured, computing formula is: w%=C
u(ng/mL) * 10
-9* 100mL * 100/M (g)=C
u(ng/mL) * 10
-5/ M (g), wherein M represents the sample quality that takes by weighing.
6. according to claim 1ly measure the method for metallic impurity in the high-purity MgO coating materials, it is characterized in that with icp ms, in described step (1) and step (2), Cs, Tl be with
133Cs,
205Tl is an internal standard element.
7. a kind of method that adopts icp ms to measure metallic impurity in the high-purity MgO coating materials according to claim 1 is characterized in that in described step (1), dilute acid soln is the hydrochloric acid solution of 8-15vt% concentration.
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2009
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