CN104502179A - Test sample treatment method for simultaneously measuring content of silicon and phosphor in silicon-manganese alloy by ICP - Google Patents
Test sample treatment method for simultaneously measuring content of silicon and phosphor in silicon-manganese alloy by ICP Download PDFInfo
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- CN104502179A CN104502179A CN201410707207.2A CN201410707207A CN104502179A CN 104502179 A CN104502179 A CN 104502179A CN 201410707207 A CN201410707207 A CN 201410707207A CN 104502179 A CN104502179 A CN 104502179A
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- 238000012360 testing method Methods 0.000 title claims abstract description 18
- 238000000034 method Methods 0.000 title claims abstract description 15
- 229910052710 silicon Inorganic materials 0.000 title claims abstract description 15
- 239000010703 silicon Substances 0.000 title claims abstract description 15
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 title claims abstract description 12
- 229910000914 Mn alloy Inorganic materials 0.000 title abstract 6
- PYLLWONICXJARP-UHFFFAOYSA-N manganese silicon Chemical compound [Si].[Mn] PYLLWONICXJARP-UHFFFAOYSA-N 0.000 title abstract 6
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 30
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 21
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000008367 deionised water Substances 0.000 claims abstract description 14
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 14
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 13
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 11
- 239000010439 graphite Substances 0.000 claims abstract description 11
- 229910052742 iron Inorganic materials 0.000 claims abstract description 10
- 238000001914 filtration Methods 0.000 claims abstract description 9
- 238000001816 cooling Methods 0.000 claims abstract description 8
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims abstract description 7
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000004327 boric acid Substances 0.000 claims abstract description 7
- 239000000706 filtrate Substances 0.000 claims abstract description 7
- 238000002156 mixing Methods 0.000 claims abstract description 7
- 238000005406 washing Methods 0.000 claims abstract description 7
- 239000012046 mixed solvent Substances 0.000 claims abstract description 3
- 239000000523 sample Substances 0.000 claims description 58
- 238000002844 melting Methods 0.000 claims description 20
- 230000008018 melting Effects 0.000 claims description 20
- 238000003672 processing method Methods 0.000 claims description 16
- 239000011521 glass Substances 0.000 claims description 9
- 229910052698 phosphorus Inorganic materials 0.000 claims description 9
- 239000011574 phosphorus Substances 0.000 claims description 9
- 239000012488 sample solution Substances 0.000 claims description 8
- 230000004907 flux Effects 0.000 claims description 6
- 239000006210 lotion Substances 0.000 claims description 6
- 238000011002 quantification Methods 0.000 claims description 6
- 229910052799 carbon Inorganic materials 0.000 claims description 2
- 239000000155 melt Substances 0.000 claims 1
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 abstract description 6
- 239000002253 acid Substances 0.000 abstract description 2
- 238000004140 cleaning Methods 0.000 abstract 1
- 238000007500 overflow downdraw method Methods 0.000 abstract 1
- 238000004806 packaging method and process Methods 0.000 abstract 1
- 239000002245 particle Substances 0.000 abstract 1
- 238000005303 weighing Methods 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 11
- 238000009616 inductively coupled plasma Methods 0.000 description 10
- 238000004090 dissolution Methods 0.000 description 7
- 238000004458 analytical method Methods 0.000 description 6
- 239000000126 substance Substances 0.000 description 5
- 230000004927 fusion Effects 0.000 description 3
- 238000005259 measurement Methods 0.000 description 3
- 230000003595 spectral effect Effects 0.000 description 3
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 2
- 241001062472 Stokellia anisodon Species 0.000 description 2
- 238000009614 chemical analysis method Methods 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 229910017604 nitric acid Inorganic materials 0.000 description 2
- VLTRZXGMWDSKGL-UHFFFAOYSA-N perchloric acid Chemical compound OCl(=O)(=O)=O VLTRZXGMWDSKGL-UHFFFAOYSA-N 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- WICBODZZQQCSQP-UHFFFAOYSA-N Cl.[O-2].[O-2].[Mn+4] Chemical compound Cl.[O-2].[O-2].[Mn+4] WICBODZZQQCSQP-UHFFFAOYSA-N 0.000 description 1
- PXGOKWXKJXAPGV-UHFFFAOYSA-N Fluorine Chemical compound FF PXGOKWXKJXAPGV-UHFFFAOYSA-N 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 239000012482 calibration solution Substances 0.000 description 1
- 238000004737 colorimetric analysis Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 239000011737 fluorine Substances 0.000 description 1
- 229910052731 fluorine Inorganic materials 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000012452 mother liquor Substances 0.000 description 1
- 229920001296 polysiloxane Polymers 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- ABTOQLMXBSRXSM-UHFFFAOYSA-N silicon tetrafluoride Chemical compound F[Si](F)(F)F ABTOQLMXBSRXSM-UHFFFAOYSA-N 0.000 description 1
- 239000012086 standard solution Substances 0.000 description 1
- 230000001360 synchronised effect Effects 0.000 description 1
- 239000012085 test solution Substances 0.000 description 1
- 238000012549 training Methods 0.000 description 1
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- Sampling And Sample Adjustment (AREA)
Abstract
The invention discloses a test sample treatment method for simultaneously measuring content of silicon and phosphor in a silicon-manganese alloy by ICP. The test sample treatment method comprises the following steps: weighing 0.1000g of a silicon-manganese alloy test sample with particle size of 160-200mesh, putting the silicon-manganese alloy test sample into filter paper which is pre-filled with 2.0-2.5g of a mixed solvent of anhydrous sodium carbonate and boric acid in a ratio of 2 to 1, uniformly mixing, packaging and putting into an iron crucible with a graphite layer bottom for fusing for 12-18 minutes at 800-900 DEG C, cooling for 2-3 minutes to obtain a sample, putting the sample into a container which is pre-filled with 90-110ml of a diluted hydrochloric acid solution consisting of hydrochloric acid and water in a ratio of 1 to 3, dissolving clinkers, filtering the obtained sample through rapid quantitative filter paper into a 250ml volumetric flask, cleaning the sample containing container and the filter paper with deionized water, and adding deionized water to the scale after cooling the filtrate and washing liquor. According to the test sample treatment method, the silicon-manganese alloy test sample is fused and decomposed through an alkaline fusion method, thereby avoiding volatilization loss of silicon when hydrofluoric acid is added to dissolve the test sample through an acid dissolving method; the test sample is completely decomposed without interference or dissipation, so that the analyzed results are accurate and stable; moreover, an ICP spectrograph is used for simultaneously measuring the content of silicon and phosphor in the silicon-manganese alloy.
Description
Technical field
The invention belongs to metallurgical material test and analysis technology field, be specifically related to the sample processing method of silicon, phosphorus content in a kind of ICP Simultaneously test silicomangan.
Background technology
The chemical composition of domestic and international detection silicomangan mainly adopts traditional chemical analysis, the chemical analysis method such as measuring silicon has two-way differential colorimetry, phosphorus content P-Mo blue photometric method measures, chemical analysis method operating process is long, consuming time many, for the mensuration of batch samples, no matter be vessel or finding speed, all cannot meet the needs that fast pace is produced, and analysis result there is larger difference because of the difference of operating personnel.Phosphorus content in present silicomangan also can use ICP(inductively coupled plasma atomic emission spectrometer) measure.By sample nitric acid, hydrofluoric acid dissolution, perchloric acid smoked drives fluorine.By hydrochloric acid manganese dioxide reduction precipitation, after test solution is filtered constant volume, ICP spectrometer is measured the spectral intensity of P elements, processed by instrument data process software, its working curve calculates the massfraction of P elements in sample.But in sample course of dissolution, add nitric acid due to the method and hydrofluorite decomposes sample jointly, chemical reaction is comparatively fierce, silicon and hydrofluorite form silicon tetrafluoride and easily volatilize in beaker, cause measurement result on the low side, therefore can not simultaneously for measuring the silicone content in sample.Therefore, be necessary to research and develop one without heterogeneous interference, without dissipating, and simple and efficient sample processing method, realize the synchronous detection of silicon in silicomangan, P elements, analyze data in real time, reliably for smelt production provides.
Summary of the invention
The object of the present invention is to provide the sample processing method of silicon, phosphorus content in a kind of ICP Simultaneously test silicomangan.
The object of the present invention is achieved like this, and the sample processing method of silicon, phosphorus content in described ICP Simultaneously test silicomangan, comprises melting, dissolving and filter progress, specifically comprise:
A, melting: taking 0.1000g granularity is 160 ~ 200 object silicomangan samples, be placed in the natrium carbonicum calcinatum that 2.0 ~ 2.5g is altogether housed in advance: the filter paper of the mixed flux of boric acid=2:1, mixing puts into the rebasing iron crucible of graphite linings after wrapping, in 800 ~ 900 DEG C of melting 12 ~ 18min, take out cooling 2 ~ 3min, obtain sample a.
B, dissolving: sample a is placed in the hydrochloric acid that 90 ~ 110ml is altogether housed in advance: the glass container of the dilute hydrochloric acid solution of water=1:3, treats that frit dissolves completely, obtain sample b.
C, filtration: by sample b with fast quantification Filter paper filtering in 250ml volumetric flask, clean the glass container and filter paper of containing sample b with deionized water, collect filtrate and washing lotion, be settled to scale with deionized water after being cooled to room temperature, shake up to obtain target sample solution.
The present invention adopts alkali fusion to carry out fusion and decomposition silicomangan sample, effectively prevent acid extracting in the volatilization loss adding silicon in hydrofluoric acid dissolution specimen, both ensure that sample decomposed completely, without heterogeneous interference, additionally reduce dissipation, make analysis result more accurate, stable, achieve with silicon, the phosphorus content in ICP spectrometer Simultaneously test silicomangan.Sample processing method of the present invention is easy, easy to operate, shortens the sample preparation time, improves analysis speed, can analyze data reliably in time, have good popularizing application prospect for smelt production provides.
Embodiment
The present invention is further illustrated below, but limited the present invention never in any form, and any conversion done based on training centre of the present invention or replacement, all belong to protection scope of the present invention.
The sample processing method of silicon, phosphorus content in ICP Simultaneously test silicomangan of the present invention, comprises melting, dissolving and filter progress, specifically comprises:
Described melting operation refers to that taking 0.1000g granularity is 160 ~ 200 object silicomangan samples, be placed in the natrium carbonicum calcinatum that 2.0 ~ 2.5g is altogether housed in advance: the filter paper of the mixed flux of boric acid=2:1, mixing puts into the rebasing iron crucible of graphite linings after wrapping, in 800 ~ 900 DEG C of melting 12 ~ 18min, take out cooling 2 ~ 3min, obtain sample a.
Described dissolution process refers to the hydrochloric acid being placed in by sample a and 90 ~ 110ml is altogether housed in advance: the glass container of the dilute hydrochloric acid solution of water=1:3, treats that frit dissolves completely, obtains sample b.
Described filter progress refers to sample b fast quantification Filter paper filtering in 250ml volumetric flask, the glass container and filter paper of containing sample b is cleaned with deionized water, collect filtrate and washing lotion, be settled to scale with deionized water after being cooled to room temperature, shake up to obtain target sample solution.
The granularity of the silicomangan sample described in melting operation is 180 orders.
The consumption of the mixed solvent described in melting operation is 2.0g.
Graphite carbon content > 99.85% described in melting operation, ignition residue≤0.15%, granularity≤30 μm.
The consumption of the graphite described in melting operation is 20 ~ 25g.
Melt temperature described in melting operation is 850 DEG C, and the melting time is 15min.
The fusion apparatus that melting operation adopts is high temperature box type resistance furnace.
The hydrochloric acid that dissolution process uses is commercial analysis net product.
The consumption of the dilute hydrochloric acid solution described in dissolution process is 100ml.
The temperature of the dilute hydrochloric acid solution described in dissolution process is 50 ~ 60 DEG C.
Room temperature described in filter progress is 18 ~ 26 DEG C.
After prepared by target sample solution, namely available ICP spectrometer measures according to working routine.Mainly comprise:
1, the preparation of working curve calibration solution: adopt similar standard substance solution drawing curve, take and severally form close silicomangan standard substance with sample to be tested, each unit have the measurement point of more than 4, its content distribution gradient as much as possible.Upper machine standardization after the standard substance weighed up is prepared mother liquor by operating process, carries out corresponding typical curve.With the degree of standard solution for horizontal ordinate, the mean value of spectral intensity is ordinate, is drawn the working curve respectively treating secondary element by instrument data process software.
2, the spectral intensity of each element to be measured in measurement target sample solution on the working curve of previous step gained, is calculated the content value of each element to be measured, does blank test in company with sample by instrument data process software.
embodiment 1
Taking 0.1000g granularity is 160 object silicomangan samples, be placed in the natrium carbonicum calcinatum that 2.5g is altogether housed in advance: the filter paper of the mixed flux of boric acid=2:1, the iron crucible at the bottom of 25g graphite pads is put in mixing after wrapping, iron crucible is placed in high temperature box type resistance furnace in 800 DEG C of melting 18min, take out cooling 3min, obtain sample a.Sample a is placed in the hydrochloric acid that 110ml is altogether housed in advance: the 500ml beaker in tall form of the dilute hydrochloric acid solution of water=1:3, in the dilute hydrochloric acid solution of 60 DEG C, treats that frit dissolves completely, obtains sample b.By sample b with fast quantification Filter paper filtering in 250ml volumetric flask, clean the glass container and filter paper of containing sample b with deionized water, collect filtrate and washing lotion, be settled to scale with deionized water after being cooled to room temperature, shake up to obtain target sample solution.
embodiment 2
Taking 0.1000g granularity is 180 object silicomangan samples, be placed in the natrium carbonicum calcinatum that 2.0g is altogether housed in advance: the filter paper of the mixed flux of boric acid=2:1, the iron crucible at the bottom of 20g graphite pads is put in mixing after wrapping, iron crucible is placed in high temperature box type resistance furnace in 850 DEG C of melting 15min, take out cooling 2min, obtain sample a.Sample a is placed in the hydrochloric acid that 100ml is altogether housed in advance: the 500ml beaker in tall form of the dilute hydrochloric acid solution of water=1:3, in the dilute hydrochloric acid solution of 50 DEG C, treats that frit dissolves completely, obtains sample b.By sample b with fast quantification Filter paper filtering in 250ml volumetric flask, clean the glass container and filter paper of containing sample b with deionized water, collect filtrate and washing lotion, be settled to scale with deionized water after being cooled to room temperature, shake up to obtain target sample solution.
embodiment 3
Taking 0.1000g granularity is 200 object silicomangan samples, be placed in the natrium carbonicum calcinatum that 2.2g is altogether housed in advance: the filter paper of the mixed flux of boric acid=2:1, the iron crucible at the bottom of 24g graphite pads is put in mixing after wrapping, iron crucible is placed in high temperature box type resistance furnace in 900 DEG C of melting 12min, take out cooling 2.5min, obtain sample a.Sample a is placed in the hydrochloric acid that 90ml is altogether housed in advance: the 500ml beaker in tall form of the dilute hydrochloric acid solution of water=1:3, in the dilute hydrochloric acid solution of 56 DEG C, treats that frit dissolves completely, obtains sample b.By sample b with fast quantification Filter paper filtering in 250ml volumetric flask, clean the glass container and filter paper of containing sample b with deionized water, collect filtrate and washing lotion, be settled to scale with deionized water after being cooled to room temperature, shake up to obtain target sample solution.
Claims (9)
1., with a sample processing method for silicon, phosphorus content in ICP Simultaneously test silicomangan, it is characterized in that comprising melting, dissolving and filter progress, specifically comprise:
A, melting: taking 0.1000g granularity is 160 ~ 200 object silicomangan samples, be placed in the natrium carbonicum calcinatum that 2.0 ~ 2.5g is altogether housed in advance: the filter paper of the mixed flux of boric acid=2:1, the iron crucible at the bottom of graphite pads is put in mixing after wrapping, in 800 ~ 900 DEG C of melting 12 ~ 18min, take out cooling 2 ~ 3min, obtain sample a;
B, dissolving: sample a is placed in the hydrochloric acid that 90 ~ 110ml is altogether housed in advance: the glass container of the dilute hydrochloric acid solution of water=1:3, treats that frit dissolves completely, obtain sample b;
C, filtration: by sample b with fast quantification Filter paper filtering in 250ml volumetric flask, clean the glass container and filter paper of containing sample b with deionized water, collect filtrate and washing lotion, be settled to scale with deionized water after being cooled to room temperature, shake up to obtain target sample solution.
2. sample processing method according to claim 1, is characterized in that the granularity of the silicomangan sample described in operation A is 180 orders.
3. sample processing method according to claim 1, is characterized in that the consumption of the mixed solvent described in operation A is 2.0g.
4. sample processing method according to claim 1, is characterized in that the graphite carbon content > 99.85% described in operation A, ignition residue≤0.15%, granularity≤30 μm.
5. the sample processing method according to claim 1 or 4, is characterized in that the consumption of the graphite described in operation A is 20 ~ 25g.
6. sample processing method according to claim 1, it is characterized in that the melt temperature described in operation A is 850 DEG C, the melting time is 15min.
7. sample processing method according to claim 1, is characterized in that the consumption of the dilute hydrochloric acid solution described in process B is 100ml.
8. the sample processing method according to claim 1 or 7, is characterized in that the temperature of the dilute hydrochloric acid solution described in process B is 50 ~ 60 DEG C.
9. sample processing method according to claim 1, is characterized in that the room temperature described in operation C is 18 ~ 26 DEG C.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201410707207.2A CN104502179A (en) | 2014-12-01 | 2014-12-01 | Test sample treatment method for simultaneously measuring content of silicon and phosphor in silicon-manganese alloy by ICP |
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| CN201410707207.2A CN104502179A (en) | 2014-12-01 | 2014-12-01 | Test sample treatment method for simultaneously measuring content of silicon and phosphor in silicon-manganese alloy by ICP |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106596522A (en) * | 2017-02-28 | 2017-04-26 | 武钢集团昆明钢铁股份有限公司 | Determination method for contents of silicon, manganese and phosphorus in natural microalloy iron powder |
| CN106814062A (en) * | 2015-11-27 | 2017-06-09 | 中冶建筑研究总院有限公司 | The method for determining various chemical element contents in slag simultaneously |
| CN107505275A (en) * | 2017-10-17 | 2017-12-22 | 浙江中煤检测有限公司 | The assay method of silicon in a kind of soils and sediments |
| CN107764801A (en) * | 2016-08-20 | 2018-03-06 | 江西三和金业有限公司 | A kind of method that stable measure scraps graphite crucible residue gold |
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Application publication date: 20150408 |
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