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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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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Cited By (4)
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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 |
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| 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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