CN103884674A - Method for measuring carbon content in fly ash by using high frequency burning infrared absorption spectrum - Google Patents
Method for measuring carbon content in fly ash by using high frequency burning infrared absorption spectrum Download PDFInfo
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- CN103884674A CN103884674A CN201410074008.2A CN201410074008A CN103884674A CN 103884674 A CN103884674 A CN 103884674A CN 201410074008 A CN201410074008 A CN 201410074008A CN 103884674 A CN103884674 A CN 103884674A
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Abstract
The invention discloses a method for measuring carbon content in fly ash by using a high frequency burning infrared absorption spectrum, and belongs to the field of detection of raw materials and finished products. The method provided by the invention comprises the following steps of adding different quantities of standard lithium carbonate, wherein the addition amounts of the standard lithium carbonate, based on the content of carbon, need to cover 10%-40% of a measurement area; measuring infrared absorption energy of the standard lithium carbonate; and drawing a calibration curve by adopting a multi-point correcting manner. The method provided by the invention has the advantages that the operation is simple and convenient, the result is accurate, and a problem that a fly ash standard sample is not available is solved.
Description
Technical field
The invention belongs to the detection method of starting material and finished product, particularly a kind of assay method of high-frequency combustion infrared absorption spectrum to carbon content in dedusting ash of using.
Background technology
In recent years, along with the continuous minimizing of iron ore deposit, iron ore price is constantly soaring, iron and steel enterprise is under the pressure of cost pressure, one after another the material dedusting ash of coming out of the stove is carried out to secondary utilization, common way is first dedusting ash to be carried out to harmful element processing, process qualified after by it with addition of in sintering deposit.But the maximization of blast furnace is higher to the requirement of raw material and fuel quality, this has just caused raw material and fuel quality to decline and the contradiction of blast furnace maximization, and how Shoudu Iron and Steel Co safely and reasonably utilizes aspect dedusting ash has accumulated certain experiences.
Each component to dedusting ash is carried out Accurate Determining, is the basis that effectively utilizes dedusting ash.Dedusting ash mainly comprises four kinds of gravitational dust collection ashes, dry method dust ash, cyclone dust removal ash, stokehold dedusting ash.The principal ingredient of dedusting ash is iron and carbon, and wherein the content range of carbon is many measures carbon content exactly 10%～40%, and tool is of great significance undoubtedly.
For the mensuration of carbon, main analytical approach has gravimetric method, gas volumetric method, infrared absorption method etc. at present.Wherein gravimetric method is classical chemical analysis method, has advantages of that accuracy is high, traceability good, and shortcoming is that analytic process is tediously long, can not meet the demand of modern scientific research and production on the time; Gas volumetric method will be used high temperature process furnances, and this equipment is applied in small enterprise mostly; Most unit all adopts high-frequency combustion Carbon Content By Infra-red Absorption Method, and the method has the features such as accuracy is high, easy to operate, analysis speed is fast.In dedusting ash, carbon content is generally between 10%～40%, high-frequency combustion infrared absorption method is a kind of relative analytical approach, the method need to be proofreaied and correct result with suitable standard model, otherwise can make measurement result produce very large deviation, there is no in the market the standard model of dedusting ash at all.Therefore need to find out a kind of applicable assay method of high-frequency combustion infrared absorption spectrum to carbon content in dedusting ash that utilize for this problem, guarantee measurement result accurately and reliably.
Summary of the invention
The object of the present invention is to provide a kind of assay method of high-frequency combustion infrared absorption spectrum to carbon content in dedusting ash of using.
The present invention adopts the benchmark lithium carbonate that adds different amounts, and its addition is converted on carbon, should be able to cover 10%～40% scope, measures their infrared absorption energy, adopts Supplements mode to draw calibration curve.Concrete steps are as follows:
Bug check instrument, makes instrument in normal steady state (SS), and be chosen as to 40 seconds the analysis time of instrument, and comparison level is set as 1.
Take primary standard substance lithium carbonate by table 1, be accurate to 0.0002g, be placed in the crucible of anticipating and be covered with 0.6g pure iron, then cover 0.2g glass putty and 1.3g tungsten powder as carbon standard series.
The standard series of table 1 carbon
| Crucible numbering | Carbon standard series | Lithium carbonate quality/g | Carbon content (massfraction) % |
| 1 | SC1 | 0.0615 | 10.00 |
| 2 | CS2 | 0.0923 | 15.00 |
| 3 | CS3 | 0.1230 | 20.00 |
| 4 | CS4 | 0.1538 | 25.00 |
| 5 | CS5 | 0.1846 | 30.00 |
| 6 | CS6 | 0.2153 | 35.00 |
| 7 | CS7 | 0.2461 | 40.00 |
Then measure the standard series of carbon of preparation, before each measurement, all will manually input the sample weighting amount of 0.1000g, check the linear relationship after calibration, if necessary, also further calibration operation curve.Then accurately take dedusting ash sample 0.100g, be accurate to 0.0001g, be placed in the crucible of anticipating and be covered with 0.6g pure iron, then cover 0.2g glass putty and 1.3g tungsten powder.Measure with identical condition, program, operation, obtain the carbon content in dedusting ash.
In dedusting ash sample, carbon content is very high, also there is no the standard model of dedusting ash on market, in order to find out a kind of applicable assay method of high-frequency combustion infrared absorption spectrum to carbon content in dedusting ash that utilize, needs select and determine following condition.
The selection of sample weighting amount: by controlling sample weighting amount, instrument is worked in measured zone.In dedusting ash, carbon content is very high, when sample weighting amount is excessive, can exceed the measured zone of instrument, and when sample weighting amount is too small, weighing error will increase, and causes accuracy greatly to reduce.Consider, adopt the sample weighting amount of 0.1g proper.
The selection of flux kind and consumption: need the flux kind of adding to have iron powder, glass putty and tungsten powder.The addition of flux is difficult for excessive, and we always wish to obtain measurement result the most accurately with less addition.
1. iron powder: do not add or consumption too small, sample cannot burn, and therefore generally add the about 0.6g of iron powder.
2. glass putty: during lower than 0.1g, the poor fluidity of sample, does not reach the object adding, during higher than 0.3g, the dust producing after glass putty burning is larger, easily splash, sample therefore generally add the about 0.2g of glass putty.3. tungsten powder: play fluxing action.When addition is too small, sample cannot be covered completely, the easy splash of sample, therefore generally adds the about 1.3g of tungsten powder.
The selection of flux and sample addition sequence: the results showed, the addition sequence the best of (pure iron+sample+glass putty+tungsten powder), not only the combustion efficiency of sample is good, and splash is very little, and the stability of measurement result is better.Because such addition sequence can make sample preferably double team in flux the inside.
The selection of analysis time: while being greater than 45 seconds analysis time, belong to invalid analysis, extended artificially analysis time; While being less than 40 seconds analysis time, for sample segment, may have certain loss, so be chosen as 40 seconds analysis time.
The selection of comparison level: the carbon content of dedusting ash is very high, even if comparison level is set as at 1 o'clock, instrument also can be identified well.
The selection of primary standard substance: the more organic stable chemical nature of inorganics, when selection reference material, generally select dead matter.When preparation C standard series, because carbon content in dedusting ash is very high, as selected BaCO
3or K
2cO
3deng material, the quality that need to take is too large, therefore select Li
2cO
3, Li
2cO3 is for C, and its mass conversion factor is 6.152, more applicable.The standard series of the carbon of preparing by measurement, has solved the difficult problem without standard model.
The invention has the advantages that, easy and simple to handle, result accurately and can solve the problem that there is no dedusting ash standard model.
Embodiment
Instrument: high-frequency combustion infrared absorption carbon sulphur instrument, balance, high temperature furnace, ceramic crucible, crucible tongs
Reagent: oxygen, power gas source (nitrogen or pressurized air), ascarite, magnesium perchlorate, glass putty, tungsten powder, pure iron, lithium carbonate (content is greater than 99.9%) etc.
Experimental procedure:
1. bug check instrument, makes instrument in normal steady state (SS), and be chosen as to 40 seconds the analysis time of instrument, and comparison level is set as 1.
2. take lithium carbonate by table 1, be accurate to 0.0002g, be placed in the crucible of anticipating and be covered with 0.6g pure iron, then cover 0.2g glass putty and 1.3g tungsten powder as carbon standard series.Then measure the standard series of carbon of preparation, before each measurement, all will manually input the sample weighting amount of 0.1000g, check the linear relationship after calibration, if necessary, also further calibration operation curve.
3. accurately take dedusting ash sample 0.100g, be accurate to 0.0001g, be placed in the crucible of anticipating and be covered with 0.6g pure iron, then cover 0.2g glass putty and 1.3g tungsten powder.Measure with identical condition, program, operation, obtain the carbon content in dedusting ash.
In conjunction with application example, that the invention will be further described is as follows:
Embodiment,
Debugged after instrument, first measured the standard series of the carbon of preparation, this experiment is 10% by carbon content theoretical value; 15%; 20%; 25%; 30%; 35%; 40% the each mensuration of sample 3 times, matching is also drawn calibration curve, obtains calibration equation and is: y=0.00497078x
2+ 0.964734x-0.00187766
Its correlation coefficient r=0.9994, linear relationship is fine.
Then choose 3 representational samples, measure respectively 11 times according to definite method, the precision of investigation method, the results are shown in Table 2.
The measurement result % of table 2 carbon
The precision of method is fine.The visible assay method of high-frequency combustion infrared absorption spectrum to carbon content in dedusting ash that utilize, easy and simple to handle, result is accurate, and can solve the problem that there is no dedusting ash standard model.
Claims (3)
1. the assay method to carbon content in dedusting ash with high-frequency combustion infrared absorption spectrum, is characterized in that, processing step is:
Bug check instrument, makes instrument in normal steady state (SS), and be chosen as to 40 seconds the analysis time of instrument, and comparison level is set as 1;
Take primary standard substance lithium carbonate, be accurate to 0.0002g, flux and sample are placed in to the crucible of anticipating with certain addition and addition sequence, as carbon standard series; Then measure the carbon standard series of preparation, before each measurement, all will manually input the sample weighting amount of 0.1000g, check the linear relationship after calibration; Accurately take dedusting ash sample 0.100g, be accurate to 0.0001g, measure with identical condition, program, operation, obtain the carbon content in dedusting ash.
2. method according to claim 1, is characterized in that, the quality of primary standard substance lithium carbonate is respectively 0.0615g, 0.0923g, 0.1230g, 0.1538g, 0.1846g, 0.2153g, 0.2461g.
3. method according to claim 1, is characterized in that, the addition of flux and sample and addition sequence are 0.6g pure iron+0.1000g sample+0.2g glass putty+1.3g tungsten powder.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105651724A (en) * | 2015-12-30 | 2016-06-08 | 东旭科技集团有限公司 | Method for measuring sulfur content of glass by utilizing infrared carbon and sulfur analyzer |
| CN105806729A (en) * | 2014-12-29 | 2016-07-27 | 中核北方核燃料元件有限公司 | Method for determination of carbon and sulphur content of uranium tetrafluoride |
| CN106645000A (en) * | 2016-12-12 | 2017-05-10 | 中核北方核燃料元件有限公司 | Testing method of total carbon content in silicon carbide composite material |
| CN106932355A (en) * | 2015-12-31 | 2017-07-07 | 中核北方核燃料元件有限公司 | Carbon element content analysis method in WABA pellets |
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2014
- 2014-03-02 CN CN201410074008.2A patent/CN103884674A/en active Pending
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105806729A (en) * | 2014-12-29 | 2016-07-27 | 中核北方核燃料元件有限公司 | Method for determination of carbon and sulphur content of uranium tetrafluoride |
| CN105651724A (en) * | 2015-12-30 | 2016-06-08 | 东旭科技集团有限公司 | Method for measuring sulfur content of glass by utilizing infrared carbon and sulfur analyzer |
| CN106932355A (en) * | 2015-12-31 | 2017-07-07 | 中核北方核燃料元件有限公司 | Carbon element content analysis method in WABA pellets |
| CN106645000A (en) * | 2016-12-12 | 2017-05-10 | 中核北方核燃料元件有限公司 | Testing method of total carbon content in silicon carbide composite material |
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Application publication date: 20140625 |