CN106918588A - The emission spectrographic analysis method of trace impurity in ultra-pure graphite powder - Google Patents
The emission spectrographic analysis method of trace impurity in ultra-pure graphite powder Download PDFInfo
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- CN106918588A CN106918588A CN201510993521.6A CN201510993521A CN106918588A CN 106918588 A CN106918588 A CN 106918588A CN 201510993521 A CN201510993521 A CN 201510993521A CN 106918588 A CN106918588 A CN 106918588A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- 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
- G01N21/66—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light electrically excited, e.g. electroluminescence
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/286—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/44—Sample treatment involving radiation, e.g. heat
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/286—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising
- G01N2001/2866—Grinding or homogeneising
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Abstract
The present invention relates to a kind of emission spectrographic analysis method of trace impurity in ultra-pure graphite powder.The method comprises the following steps：(1) imperfect combustion：Ultra-pure graphite powder sample is weighed, is placed in silica crucible, by silica crucible placement Muffle furnace, burning stops burning gradually to remove graphite matrix to surplus, is taken out after cooling, precise burns remaining test portion, and be placed on grinding in tetrafluoro mortar it is uniform after it is stand-by；(2) emission spectrographic analysis：Gained is burnt during remaining test portion adds graphite electrode carries out emission spectrographic analysis.This invention takes the imperfect combustion method of graphite matrix, the impurity enriched that will be remained is in the remaining graphite matrix that burns, powder method emission spectrographic analysis is directly carried out after grinding is uniform, greatly reduce the Determination Limit of analysis method, the trace impurity analysis in 5N even more high-purity graphite powders can be carried out, method is simple and easy to apply.
Description
Technical field
The present invention relates to a kind of analysis method of trace impurity in ultra-pure graphite powder, more particularly to a kind of ultra-pure stone
The emission spectrographic analysis method of trace impurity in ink powder.
Background technology
With the continuous improvement of high purity graphite purification technique level and quality requirement.It is corresponding to this, set up corresponding point
Analysis method is particularly important.Purity w>Ultra-pure graphite of 99.999% (abbreviation 5N), due to wherein usual
Still remaining has Fe, Si, Mg, Ca, Al, the Ni of contents level extremely low (μ g/g-ng/g grades, even lower),
The plurality of impurities such as Cu.Therefore, set up it is a kind of can be while determining the analysis of various trace impurities in ultra-pure graphite
Method is requirement very high and be very necessary.
Ge Peng etc. is using the ash content after the high purity graphite burning of ESEM and power spectrum (99.913%) relatively low to purity
Middle Si, Al, Fe, Ca, Mg are analyzed.Zhang Aibin etc. determines ash using sequential scan ICP-AES methods
14 kinds of impurity metallic elementses in point (Al, Ca, Cd, Co, Cr, Cu, Fe, Mg, Mn, Mo, Ni, Ti,
V, Zn), but Si is not analyzed.Merchant waits quietly using ICP-MS methods in high purity graphite 31 and 35 seed scars
The measure for measuring impurity element is studied, but lacks Fe, Si, Mg, Ca to often containing in high purity graphite,
The analysis of Al.Single element analysis method cannot be realized to analysis, multiple units while multielement in ultrapure graphite powder
Plain analysis method is used in combination then cumbersome bothersome.Neutron activation analysiss (NAA) and spark source mass spectrometry (SSMS)
Though with very low determination limit (up to 10-8%), condition requirement is high, it is difficult to popularization and application.
The present inventor attempts being analyzed ultra-pure graphite powder with highly sensitive GD-MS instrument, but finds
Graphite powder cannot briquet, cause analysis to carry out.
Pre-treatment is carried out to ultrapure graphite powder using combustion method, the purpose that volatilization matrix is enriched with impurity can be reached, can be big
The Determination Limit of width reduction analysis method.Common combustion method is burnt after volatilizing using acid completely mostly by graphite matrix
Dissolved impurity is measured.The shortcoming of this method is：Through after high-temp combustion residual impurities (such as Mo, V,
Cr, Sn, Pb etc.) cannot be completely dissolved with acid, partial impurities (such as Cr, Fe, Si etc.) are waved caused by molten sample
Hair loss, the problems such as reagent blank is high.
Therefore it provides a kind of simple and easy to apply, trace is miscellaneous in greatly improving ultra-pure graphite powder of sensitivity of analytical method
The analysis method of matter just turns into the technical barrier that the technical field is badly in need of solving.
The content of the invention
It is simple and easy to apply it is an object of the invention to provide one kind, greatly improve ultra-pure graphite of sensitivity of analytical method
The analysis method of trace impurity in powder.
To achieve the above object, the present invention takes following technical scheme：
A kind of emission spectrographic analysis method of trace impurity in ultra-pure graphite powder, its step is as follows：
(1) imperfect combustion：Ultra-pure graphite powder sample is weighed, is placed in silica crucible, silica crucible is put
Put in Muffle furnace, burning stops burning gradually to remove graphite matrix to surplus, is taken out after cooling, precise
Burn remaining test portion, and is placed on stand-by after grinding is uniform in tetrafluoro mortar；
(2) emission spectrographic analysis：Sent out during step (1) the gained remaining test portion of burning is added into graphite electrode
Penetrate spectrum analysis.
In step (1), described ignition temperature is 800-850 DEG C；The remaining test portion of burning is sample
1-2wt%
In step (1), the silica crucible is placed in quartz holder device, and with the quartzy fluffy holder device
It is placed in Muffle furnace together.
Described quartz holder device includes quartzy base plate and quartzy top board, and the quartzy base plate is provided with quartz cylinder
Ring.
In step (2), the graphite electrode carried out the empty burning of high current before emission spectrographic analysis is carried out.
When carrying out emission spectrographic analysis, standard specimen and sample weigh 10mg, are fitted into Φ 4mm × 3mm electrodes, use
Grinding tool is compacted；It is 290V in direct-current arc voltage using plane-grating spectrograph, excitation current is 12A, electrode
Distance is 5.0mm, and the time for exposure to take the photograph spectrum under conditions of 85s, develops, is fixed, impurity element is analyzed.
Advantages of the present invention：
Imperfect combustion method this invention takes graphite matrix (removes most of graphite-based by high-temp combustion
Body), the impurity enriched that will be remained directly carries out powder method hair in the remaining graphite matrix that burns after grinding is uniform
Spectrum analysis is penetrated, the Determination Limit of analysis method is greatly reduced, in can carrying out 5N even more high-purity graphite powders
Trace impurity analysis, method is simple and easy to apply.
Below by the drawings and specific embodiments, the present invention will be further described, but is not meant to the present invention
The limitation of protection domain.
Brief description of the drawings
Fig. 1 is the quartz holder dress in the emission spectrographic analysis method of trace impurity in ultra-pure graphite powder of the invention
The structural representation put.
Fig. 2 be trace impurity in ultra-pure graphite powder of the invention emission spectrographic analysis method in impurity Mn S-lgc
Working curve.
Specific embodiment
Embodiment 1
1. instrument and reagent
Atomic Emission Spectrometer AES：The PGS-2 plane-grating spectrographs of German Zeiss companies production, including spectrum projector,
Microphotometer.
The cup-shaped graphite electrode of spectroscopic pure：Φ4mm×3mm；Ultra-pure graphite powder：Spectroscopic pure (purity w>5N)；
The ultraviolet II type photographic plate of the long-range photosensitive material company production in Tianjin.
Impurity standard specimen.Using the oxide or its sponge state simple substance of each impurity (impurity element is shown in Table 1) during preparation,
According to amount of calculation, principal mark sample is first prepared, then with ultra-pure graphite powder stepwise dilution, obtain mass fraction and be respectively
0.05%, 0.01%, 0.005%, 0.001%, 0.0005% impurity graphite Sample series.(for Cu, Mg,
Ag, and other impurities phase ratios, its mass fraction order of magnitude lower, respectively 0.005%, 0.001%, 0.0005%,
0.0001%, 0.00005%).
2. experimental technique
Each standard specimen claims 1 part of sample, sample to claim 2 parts of sample, standard specimen and sample to weigh 10mg, load Φ 4mm × 3mm
In electrode, it is compacted with grinding tool.Direct-current arc voltage 290V, excitation current 12A, electrode distance 5.0mm, expose
Spectrum is taken the photograph under the conditions of light time 85s.Development, the fixing dark room operation according to standard are carried out.
3. experimental result and discussion
The impurity element of 3.1 analyses and the analytical line of selection
The impurity element of the analysis of table 1 and the analysis of line wavelength of selection
3.2 reduce graphite electrode blank assay
By remaining there are the impurity such as the Si of trace, Mg, Fe in the graphite electrode that is used, high current can be taken empty
Burning method is removed.This experiment is from calcination electric current 20A, time 20s.Graphite electrode after non-calcination and calcination is simultaneously
Carry out taking the photograph spectrum and compare, the change of its blackness is shown in Table 2.
Blackness situation of change of the impurity such as Si in the graphite electrode of table 2, Mg, Fe before and after calcination
| Element | Mg | Si | Fe | Al | Ca | Cu | Ni |
| Impurity blackness in non-calcination electrode | 63 | 51 | 17 | 24 | 13 | 25 | 16 |
| Impurity blackness in electrode after calcination | 13 | 11 | 10 | 22 | 17 | 31 | 19 |
| Electrode background blackness after calcination | 7 | 6 | 8 | 17 | 13 | 19 | 19 |
Compare and understand, non-calcination takes the photograph spectrum it was observed that Si, Mg, Fe impurity line blackness with the graphite electrode after calcination
Substantially reduce, do not observe Si in the graphite electrode after calcination substantially, Mg, Fe impurity line, density of spectral line is very
Weak, suitable with background value, these impurity are removed by calcination in illustrating graphite.Other impurity such as Al, Ca,
Cu, Ni etc. do not observe significant changes then, substantially suitable with background value.
3.3 imperfect combustions (volatilization matrix enrichment impurity) method experiment
3.3.1 quartz holder device and contrast experiment are used in burning
The calcination of various samples is carried out due to the Muffle furnace used in laboratory, the volatilization of sample, drops during calcination
Deng pollution is caused to muffle furnace hearth, pollution may be formed to the ultrapure graphite powder burnt in Muffle furnace.For
This present invention devises ultrapure graphite powder combustion experiment quartz holder device, as shown in figure 1, being superelevation of the present invention
The structural representation of the quartz holder device in pure graphite powder in the emission spectrographic analysis method of trace impurity, on figure
Circle represent and be welded on quartz cylinder ring on quartzy base plate, for placing silica crucible.The device can prevent Muffle
Pollution of micro- (dirt/powder) or the material of lower section volatilization that stove burner hearth top is dropped to sample.Graphite is will be equipped with during experiment
The silica crucible of powder is placed in quartz holder, then is put in Muffle furnace burning and is burnt with being placed directly in Muffle furnace
Graphite powder sample be analyzed, to understand experiment effect of the device to sample pre-treatments.Comparing result is shown in
Table 3.
Table 3 directly burn and under quartz holder unit protection the comparative analysis of burning graphite powder blackness data
As can be seen that the sample after being burnt under two ways, wherein Mg, Si, Fe, Al, Ca, Cu, Ni
Impurity blackness has no significant difference.Directly Ag is detected in the sample after burning, and the sample after another way burning
Ag is not detected in product.Illustrate that quartz holder device is served and protect sample from dirt that may be present in furnace muffle
The pollution that dye thing (such as Ag) is caused to it.
3.3.2 imperfect combustion method experimental technique and impurity enriched effect
The burning graphite powder under the conditions of high temperature blowing air, can make graphite generate carbon dioxide with oxygen reaction, so that
Removal matrix centrated impurities are reached, the purpose of sensitivity of analytical method is improved.The present invention is removed using imperfect combustion method
Most of graphite matrix is removed, is enriched in DC-AES method Direct Analysis miscellaneous in the remaining a small amount of graphite matrix of burning
Matter.
Experimental technique：
(1) the ultra-pure graphite powders of 5g accurately are weighed, is placed in silica crucible, silica crucible is placed on quartzy branch
In rack device (see Fig. 1), it is placed in Muffle furnace with device, in burning gradually to remove stone at 800-850 DEG C
Black matrix stops burning to test portion about residue 0.1g.Taken out after cooling, the remaining test portion of precise burning, and
Grinding is uniform rear stand-by in being placed on tetrafluoro mortar.
(2) by foregoing 2. experimental technique test, and with do not remove matrix be enriched with impurity graphite powder former state comparative analysis.
Compare impurity element density of spectral line, be shown in Table 4, to understand concentration effect.
In the ultra-pure graphite powder of table 4 before and after impurity enriched comparative analysis blackness data
| Impurity element | Mg | Si | Fe | Ni | Al | Ca | Cu |
| As former state | 34 | 31 | 16 | 15 | 19 | 35 | 28 |
| Sample after burning | 133 | 128 | 103 | 112 | 39 | 67 | 76 |
It can be seen that, the density of spectral line of all impurity elements is increased substantially in the sample after burning, illustrates impurity enriched
Effect is significant.By impurity quantitative analysis, the impurity blackness after enrichment can be linear in impurity working curve
In the range of.Therefore, carrying out the analysis pre-treatment of ultra-pure graphite from imperfect combustion method, analysis is reduced with this
Method Determination Limit.
3.3.3 recovery of standard addition
Experimental technique：2 parts of the ultra-pure graphite powders of 5g (being accurate to 0.0001g) are weighed, is placed in silica crucible, by quartz
Crucible is placed under quartz holder device, is placed in Muffle furnace with device, in being burnt at 800-850 DEG C, to examination
Material about 0.1g stops burning, is taken out after cooling, precise remaining sample, and is placed on grinding in tetrafluoro mortar
It is stand-by after uniform.Impurity is introduced in graphite standard specimen (containing 25 kinds of impurity) mode when mark-on is tested, and carries out double parallel reality
Test.Impurity graphite standard series and the test portion handled well and mark-on sample are carried out by 2. experimental techniques.Rate of recovery result
It is shown in Table 5.1-5.3：Impurity introduces the recovery of standard addition % for obtaining with graphite standard specimen and solution standard specimen mode respectively.Mode
1. represent weigh 100mg mass fractions for 0.005% (Ag, Cu, Mg are impurity graphite standard specimen 0.0005%),
After being added in the ultra-pure graphite powders of 5g, burnt at 800-850 DEG C to about 100mg.2. mode represents directly burning 100mg
Mass fraction is that (Ag, Cu, Mg mass fraction are for 0.0001%) to remaining about 20mg for 0.001% impurity graphite standard specimen.
The impurity of table 5.1 introduces the recovery of standard addition for obtaining (%) with graphite standard specimen and solution standard specimen mode respectively
The impurity of table 5.2 introduces the recovery of standard addition for obtaining (%) with graphite standard specimen and solution standard specimen mode respectively
The impurity of table 5.3 introduces the recovery of standard addition for obtaining (%) with graphite standard specimen and solution standard specimen mode respectively
As can be seen from Table 5, to more they tend to 100% with the rate of recovery that 1. 2. mode obtain compared with mode attached for impurity graphite standard specimen
Closely, reason has been mode rate of recovery experiment only scaling loss the 4/5 of matrix 2., and impurity cycles of concentration (5 times) is relatively low,
Burning time is short, so the loss of most impurity is seldom (rate of recovery is 100% or so), but Ca, Mo,
Cu, Ag still have significantly loss (rate of recovery only has 50% or so).Whole burning time is long when 1. mode introduces,
The most of loss of partial impurities (such as Pb, Bi, V, Mo, Ag), partial impurities (such as Sn, Ti, Ca, Cu,
Sb, Ga, In, Ge) there is the loss of about half, other impurity (Mg, Si, Fe, Mn, Cr, Ru, Ni,
Al, Ir, Pt, Au, Co) substantially without significantly sacrificing.
3.3.4 working curve
By taking impurity Mn as an example, its working curve as shown in Figure 2, the hair of trace impurity in ultra-pure graphite powder of the invention
Penetrate the S-lgc working curves of impurity Mn in spectroscopic analysis methods.S=70.841lgc+288.84, R2=0.9983.Its
The working curve of its impurity element is similar.
3.3.5 precision
10 parallel determinations are carried out to the sample after enrichment, its precision data is shown in Table 6.
The impurity precision (n=10) of table 6
| Impurity element | Mg | Si | Fe | Ni | Al | Ca | Cu |
| RSD/% | 4.2 | 4.3 | 23 | 23 | 14 | 8.7 | 7.1 |
It can be seen that RSD is between 4.2%-23%, the precision of Fe, Ni is poor.
3.2.3.6 as former state in impurity content
Impurity content can obtain the mass fraction of impurity in original graphite sample after conversion in the enrichment sample for measuring, as a result
It is shown in Table 7.
The mass fraction (%) of impurity in the ultra-pure graphite powder of table 7 former state
| Impurity element | Mg | Si | Fe | Ni |
| Mass fraction | ||||
| Impurity element | Al | Cu | Ca | Other impurity |
| Mass fraction | Do not detect |
It can be seen that, the purity of ultra-pure graphite powder reaches 5N5.
The present invention can be greatly improved after removing most of graphite matrix as pre-treating method using imperfect combustion method
Sensitivity of analytical method, is enriched in direct-current arc emission spectrographic analysis miscellaneous in the remaining graphite matrix of burning
Matter, realizes the purity analysis of 5N and the ultra-pure graphite powder of the above.In graphite standard specimen (containing 25 kinds of impurity) mode
Introduce adding for 11 kinds of impurity such as impurity, wherein Mg, Si, Fe, Mn, Cr, Ru, Ni, Al, Ir, Pt, Au
The mark rate of recovery is respectively between 82.3%~122.8%.Mg, Si, Fe, Ni, Al, Ca, Cu impurity determination RSD
Between 4.2%-23%.Ultra-pure graphite powder purity of analysis reaches 5N5.Method simple practical.In addition, this hair
It is bright by designed combustion quartz holder device, secondary pollution of the combustion process to sample can also be avoided.
Claims (7)
1. in a kind of ultra-pure graphite powder trace impurity emission spectrographic analysis method, comprise the following steps：
(1) imperfect combustion：Ultra-pure graphite powder sample is weighed, is placed in silica crucible, silica crucible is put
Put in Muffle furnace, burning stops burning gradually to remove graphite matrix to surplus, is taken out after cooling, precise
Burn remaining test portion, and is placed on stand-by after grinding is uniform in tetrafluoro mortar；
(2) emission spectrographic analysis：Gained is burnt during remaining test portion adds graphite electrode carries out emission spectrum point
Analysis.
2. in ultra-pure graphite powder according to claim 1 trace impurity emission spectrographic analysis method, its
It is characterised by：Described ignition temperature is 800-850 DEG C.
3. in ultra-pure graphite powder according to claim 2 trace impurity emission spectrographic analysis method, its
It is characterised by：The described remaining test portion of burning is the 1-2wt% of sample.
4. in ultra-pure graphite powder according to claim 1 trace impurity emission spectrographic analysis method, its
It is characterised by：Described silica crucible is placed in quartz holder device, and is put with the quartzy fluffy holder device
In Muffle furnace.
5. in ultra-pure graphite powder according to claim 4 trace impurity emission spectrographic analysis method, its
It is characterised by：Described quartz holder device includes quartzy base plate and quartzy top board, and the quartzy base plate is provided with stone
English cylinder ring.
6. in ultra-pure graphite powder according to claim 1 trace impurity emission spectrographic analysis method, its
It is characterised by：Described graphite electrode carried out the empty burning of high current before emission spectrographic analysis is carried out.
7. in ultra-pure graphite powder according to claim 1 trace impurity emission spectrographic analysis method, its
It is characterised by：When carrying out emission spectrographic analysis, standard specimen and sample weigh 10mg, load Φ 4mm × 3mm electrodes
In, it is compacted with grinding tool；It is 290V in direct-current arc voltage using plane-grating spectrograph, excitation current is 12A,
Electrode distance is 5.0mm, and the time for exposure to take the photograph spectrum under conditions of 85s, develops, is fixed, impurity element is carried out
Analysis.
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Citations (4)
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|---|---|---|---|---|
| CN102095198A (en) * | 2009-12-11 | 2011-06-15 | 通用电气公司 | Impurity detection in combustor systems |
| CN202886171U (en) * | 2012-11-05 | 2013-04-17 | 北京有色金属研究总院 | Device for enriching trace impurities in sulfur |
| CN104406943A (en) * | 2014-11-26 | 2015-03-11 | 四川大学 | Pretreatment method for liquid sample in laser-induced breakdown spectrum detection technology |
| CN104515766A (en) * | 2013-09-27 | 2015-04-15 | 中核北方核燃料元件有限公司 | Method for measuring impurity elements in graphite slurry |
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2015
- 2015-12-25 CN CN201510993521.6A patent/CN106918588A/en not_active Withdrawn
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102095198A (en) * | 2009-12-11 | 2011-06-15 | 通用电气公司 | Impurity detection in combustor systems |
| CN202886171U (en) * | 2012-11-05 | 2013-04-17 | 北京有色金属研究总院 | Device for enriching trace impurities in sulfur |
| CN104515766A (en) * | 2013-09-27 | 2015-04-15 | 中核北方核燃料元件有限公司 | Method for measuring impurity elements in graphite slurry |
| CN104406943A (en) * | 2014-11-26 | 2015-03-11 | 四川大学 | Pretreatment method for liquid sample in laser-induced breakdown spectrum detection technology |
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| 墨淑敏: "原子发射光谱法测定焦炭中的15种微量杂质元素", 《光谱实验室》 * |
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Application publication date: 20170704 |