CN104215651B - Method for measuring content of sulfur in coal by utilizing energy chromatic dispersion X-ray fluorescence analysis - Google Patents
Method for measuring content of sulfur in coal by utilizing energy chromatic dispersion X-ray fluorescence analysis Download PDFInfo
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- CN104215651B CN104215651B CN201410436468.5A CN201410436468A CN104215651B CN 104215651 B CN104215651 B CN 104215651B CN 201410436468 A CN201410436468 A CN 201410436468A CN 104215651 B CN104215651 B CN 104215651B
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Abstract
The invention relates to a method for measuring the content of sulfur in coal by utilizing energy chromatic dispersion X-ray fluorescence analysis, and mainly solves the problem that the sensitivity and the efficiency for detecting a sulfur element in the coal are low in the prior art. The method comprises the following steps of firstly pre-treating a coal sample, and preparing a standard sample and a test sample; measuring a barium element in the test sample by utilizing an energy chromatic dispersion X-ray fluorescence analyzer, detecting the fluorescent number of the barium element, and substituting the detected fluorescent number of the barium element in a calibration curve to obtain the percentage composition of the barium element in the test sample; and calculating the percentage composition of the sulfur element in the coal sample according to a chemical number relation between the sulfur and barium in the sample. The measurement of the sulfur content in the coal is realized by adopting an indirect measuring method. The method has characteristics of rapidness in measurement and easiness in operation.
Description
Technical field
The present invention relates to a kind of method that applied energy dispersive x-ray fluorescence analysiss measure sulfur content of coal, belong to analysis
Detection technique field.
Background technology
At present, the method for light element content detection in material mainly has chemical analysis and instrumental method two big
Class.Chemical analysis be directed to different elements and sample type can be divided into Ignition Lamp Method, tube oven method, gravimetric method, neutralization titration,
The concrete measuring method such as colorimetry and volumetric method.Relatively accurately light element can be carried out using common chemical method merely
Quantitative analyses, but complex steps, take longer, and need operator to have compared with the chemical knowledge of horn of plenty and higher
Experiment attainment, this allow for instrument analytical method increasingly by analysis user favored.At present, instrument research method includes
Emission spectrometry, atomic absorption spectrum (aas) analysis, x-ray fluorescence analysiss (xrf) and plasma emlssion spectrometry etc..Its
Middle energy dispersive x ray fluorescence analysis measurement is the excitation apparatus by the use of x-ray tube as simple spectral line, and x-ray tube sends
Primary X roentgenization, in coal sample, makes the object element in sample be excited, and produces x-ray fluorescence, and x-ray fluorescence is detected
Device receives, and detects the energy value of object element, and the calibration curve contrast making with according to standard sample, and Inversion Calculation goes out sample
The content of object element in product, completes the quantitative analyses of element.Although xrf analytic process has, analyze speed is fast, analyst coverage is wide,
Sample preparation requires the advantages of low, analysis precision is high so that the method has more certain advantage compared with other instruments analysis method.But by
In some limitation of element sulphur itself, the x-ray fluorescent yield of such as element sulphur is low, launching efficiency is low, signature x-ray energy
The features such as impact of low and matrix effect is extremely serious is so that energy dispersive x ray fluorescence analysis (edxrf) technology is to sulfur unit
The sensitivity of the light elements such as element measurement is relatively low.
Content of the invention
Based on deficiency in terms of element sulphur measurement for the above-mentioned energy dispersive x ray fluorescence analytical technology, it is directed to application energy
Chromatic dispersion quantity x-ray fluorescent spectrometry detects the low problem of element sulphur sensitivity, and the present invention provides a kind of reasonable and effective energy
Dispersive x-ray fluorescence analysiss are applied to the measuring method of sulfur content.
For achieving the above object, present invention employs one kind indirectly measuring method it is achieved that application edxrf method in coal
The quantitative analyses of element sulphur.The method measures front pretreatment first to coal sample, by coal sample and the Emhorn card having sulfur fixation
Reagent (by the 2 parts of light magnesium oxides and 1 part of natrium carbonicum calcinatum synthesis) mixing of 1:2 in mass ratio, with Muffle furnace at 800-850 DEG C
Slow calcination 2 hours under high temperature.Organic sulfur in coal, sulfide sulfur and sulfate sulfur are all oxidized to oxysulfide, and through Chinese mugwort
The fixation of family name's card reagent changes into the sulfate (mgso of solubility4And na2so4).The Deca in the mixed liquor with calcination thing for this solution
bacl2Solution, makes sulfate ion be completely converted into baso4Precipitation.Filter, dry.
In order to ensure the physical aspect of standard specimen and sample and the concordance of chemical composition, make one group of standard sample by oneself.Standard
Simply it is added without barium chloride solution during sample making, directly filtered, remaining same coal sample pretreatment.Sulphuric acid after filtration
Root is filtered out completely, comprises the noncombustibles of coal and the component magnesium oxide of Eschka reagent in precipitate.So far, in precipitate
Composition remove without baso4Outside, other compositions are all identical with sample.By this calcination thing precipitation having filtered sulfate radical
With baso4Powder is mixed in the ratio that barium content becomes a graded, and powder pressing method makes sample.Use energy dispersion x-ray
Fluorescence analyser measures the standard sample that above-mentioned preparation completes, and the fluorescence recording barium element in each standard specimen counts.With barium element
Percentage composition be abscissa, with the fluorescence of barium element be counted as vertical coordinate draw calibration curve.
Test sample is made using the method for coal sample pretreatment, equally uses energy dispersive x ray fluorescence analyser to sample
In barium element measure, detect barium element fluorescence count, substituted into calibration curve, tried to achieve barium element in sample
Percentage composition.Further according to the stoichiometric relation of sulfur in sample and barium, it is calculated the percentage composition of element sulphur in coal sample.
Beneficial effects of the present invention and feature: can not will directly and accurately use energy dispersive x ray fluorescence analysis measurement
Element sulphur in coal be converted into can barium element measured directly, go out element sulphur further according to chemical equation relation Inversion Calculation and contain
Amount is it is achieved that the measurement to sulfur content of coal for the applied energy dispersive x-ray fluorescence analysiss measurement method.
The present invention is quick, easy to operate for the measurement of sulfur content, and with dividing from the wavelength dispersion x-ray fluorescence of external import
Relatively inexpensive, saving cost is compared in analyzer measurement, overcomes time-consuming longer, complex operation the disadvantage of chemical method that tradition is used
End.The quantitative analyses to element sulphur in coal using energy dispersive x ray fluorescence analyser can be effectively realized.
In order to be illustrated more clearly that the present invention, below the accompanying drawing of use required in the description of this invention is made simply
Introduce it should be apparent that, drawings in the following description are only some embodiments of the present invention, for ordinary skill people
For member, on the premise of not paying creative work, other accompanying drawings can also be obtained according to these accompanying drawings.
Brief description
Fig. 1 is coal sample pretreatment flow chart.
Fig. 2 is the preparation flow figure of standard sample.
Fig. 3 is energy dispersive x ray fluorescence analytic process measured value and certificate value results contrast figure.
Specific embodiment
Experiment is with reference to the assorted block-regulations of Chinese mugwort in national standard gb/t 214 2007 " assay method of full content of Sulphur in coal " to coal sample
Carry out pretreatment, be embodied as flow process as shown in Figure 1:
1. weigh in the dry pot of 30ml porcelain that particle diameter is less than 0.2mm is dried coal sample 1g and Ai Shika reagent (magnesium oxide and no
Aqueous sodium carbonate 2:1 in mass ratio mixes) 2g mix homogeneously, then covered on coal sample with 1g Ai Shika reagent;
2. the dry pot that will be equipped with coal sample moves in draughty Muffle furnace, is progressively heated at from room temperature with the time of 1.5h
840 DEG C, in order that the oxysulfide that coal sample calcination generates is with Ai Shika reagent reacting completely, 2h must be kept at such a temperature.Profit
With the temperature programming control device of Muffle furnace, during 1.5h, the temperature from ambient of Muffle furnace is made to be to slowly warm up to 840
℃.Sample calcination in Muffle furnace, its reaction equation mainly has:
2so2+o2+2na2co3=2na2so4+2co2↑
so3+na2co3=na2so4+co2↑
2mgo+2so2+o2=2mgso4
meso4+na2co3=na2so4+meco3;
3. dry pot is taken out from Muffle furnace, be cooled to room temperature.Now the calcination thing in dry pot include coal non-combustibles,
Magnesium oxide and powdered sodium carbonate.With Glass rod, the calcination thing in dry pot is carefully stirred pine, smashs to pieces, then calcination thing is transferred to burning
In cup.With hot water injection's dry pot inwall, washing liquid is taken in beaker.Add distilled water, be sufficiently stirred for, make in calcination thing mixed liquor
Soluble substance can be completely dissolved;
4. add dilute hydrochloric acid solution in washing liquid, in order to remove the carbonate in mixture solution it is therefore an objective to prevent carbonic acid
Root reacts generation barium carbonate sediment with the follow-up barium chloride solution adding, thus increasing the content of barium element in mixture, increases
Experimental error.During salt adding acid solution, until mixed liquor be in acid (ph=2) it was demonstrated that carbonate in mixture solution from
Son is completely removed, and now added hydrochloric acid solution is about 20ml;
5. by solution heated and boiled.The carbon dioxide gass that previous step reaction can be generated by solution are boiled in sour environment
Body is completely exhausted out.It is slowly added dropwise barium chloride solution 10ml so as to generate with the sulphuric acid reactant salt in mixed liquor under being stirred continuously
Barium sulfate precipitate.Its ion-reaction equation is:
6. mixed liquor cools down at room temperature, stands 2h.Mixed liquor is stood, the barium sulfate precipitate generating can have been settled
Entirely.Filtered with fine and close ashless quantitative filter paper, then dried with drying baker, wait tabletting to produce sample.
Below in conjunction with the accompanying drawing 2 of the present invention, to the standard sample preparation method in the embodiment of the present invention and test sample
Preparation method carry out clearly, be fully described by.
As shown in Figure 2: for the physical aspect of standard sample and test sample and the concordance of chemical composition, to make one group by oneself
Standard sample.The manufacturing process of standard sample 1.~4. step identical with the pre-treatment step of coal sample, be added without in the 5. step
Barium chloride solution, is directly filtered.Now sulfate radical is filtered to remove completely, comprises coal in the precipitate after filtration
The component magnesium oxide of noncombustibles and Ai Shika reagent.By this calcination thing precipitation having filtered sulfate radical and baso4Powder is pressed
Barium content is mixed into 6 parts from the ratio of 1.76~4.70% one-tenth graded, makes the quality of every part of sample be about 1g.Pressed powder
Legal system makees print.
Equally take several pieces coal sample, carry out sample determination pre-treatment according to above-mentioned coal sample processing method.When sample is in Muffle
In stove during calcination, in coal matrix, all of carbon is all removed with the gas form of oxycarbide.Therefore, take out from Muffle furnace
Calcination amount of substance be less than put it in stove before quality.Additionally, 4. in coal sample pretreatment the walk, add dilute hydrochloric acid,
Eliminate the component sodium carbonate of the Ai Shika reagent being present in mixture solution.5. Deca barium chloride solution during walking the
Sulfate radical is precipitated into completely barium sulfate.After filtering, drying, the sample quality obtaining will certainly be different from coal sample pretreatment
The quality of front sample.Weigh the sample obtaining after processing through coal sample with electronic balance successively, its quality is respectively mi.In order to be suitable for
The size of tabletting grinding tool, takes off a part respectively from the sample of these known quality, makes test sample with powder pressing method,
Wait dispersive x-ray fluorescence analyser that it is tested.
In order to verify the accuracy of the method, using the method to gbw11101t, gbw11104h, gbw11104h,
Five kinds of national standard coal samples of gbw11108j and gbw11113e measure, and every kind of standard sample respectively makes some parallel sample,
It is measured, and measurement result is averaged, then contrasted with the method for matched curve with GB coal sample certificate value,
Comparing result is as shown in Figure 3.From figure 3, it can be seen that the method is consistent with certificate value to the measurement result of sulfur content of coal, card
Bright the method can be to reliably applied to the measurement of sulfur content of coal.
Described above to the disclosed embodiments, makes professional and technical personnel in the field be capable of or uses the present invention.
Multiple modifications to these embodiments will be apparent from for those skilled in the art, as defined herein
Conventional method can be realized in the case of the marrow without departing from invention or scope in other embodiments.Therefore, the present invention will
Will not be intended to be limited to the embodiments shown herein, and be intended to accord with method disclosed herein and features of novelty is consistent
Scope the widest.
Claims (2)
1. a kind of method that applied energy dispersive x-ray fluorescence analysiss measure sulfur content of coal, the process employs a kind of indirect
Measuring method realizing the quantitative analyses to element sulphur in coal, implementation step:
(1) first coal sample is measured with front pretreatment, by coal sample and the Eschka reagent 1:2 in mass ratio having sulfur fixation
Mixing, with Muffle furnace under 800-850 DEG C of high temperature slow calcination 2 hours, organic sulfur in coal, sulfide sulfur and sulfate sulfur
All it is oxidized to oxysulfide, and through the fixing sulfate changing into solubility of Eschka reagent, to this solution and calcination thing
Deca bacl in mixed liquor2Solution, makes sulfate ion be completely converted into baso4Precipitation, filters, dries;
(2) in order to ensure the physical aspect of standard specimen and sample and the concordance of chemical composition, make one group of standard sample by oneself;Standard sample
Simply it is added without barium chloride solution in product manufacturing process, directly filtered, coal sample pretreatment in remaining same step (1), filters
Sulfate radical is filtered out completely afterwards, comprises the noncombustibles of coal and the component magnesium oxide of Eschka reagent in precipitate, so far,
Composition in precipitate removes without baso4Outside, other compositions are all identical with sample, filtered burning of sulfate radical by this
Burn thing precipitation and baso4Powder is mixed in the ratio that barium content becomes a graded, makes sample using powder pressing method, with energy
Chromatic dispersion quantity x-ray fluorescence analyser measures the standard sample that above-mentioned preparation completes, and records the exometer of barium element in each standard specimen
Number, with the percentage composition of barium element as abscissa, is counted as vertical coordinate with the fluorescence of barium element and draws calibration curve;
(3) method adopting coal sample pretreatment makes test sample, equally uses energy dispersive x ray fluorescence analyser in sample
Barium element measure, detect barium element fluorescence count, substituted into calibration curve, tried to achieve hundred of barium element in sample
Divide content, further according to the stoichiometric relation of sulfur in sample and barium, be calculated the percentage composition of element sulphur in coal sample.
2. a kind of method that applied energy dispersive x-ray fluorescence analysiss measure sulfur content of coal as claimed in claim 1, the party
The concrete steps that method is realized:
(1) coal sample measures front pretreatment
1. weigh in the dry pot of 30ml porcelain that particle diameter is less than 0.2mm is dried coal sample 1g and Ai Shika reagent 2g mix homogeneously, then uses
1g Ai Shika reagent covers on coal sample, and described Ai Shika reagent is to be mixed by magnesium oxide and natrium carbonicum calcinatum 2:1 in mass ratio
Conjunction forms;
2. the dry pot that will be equipped with coal sample moves in draughty Muffle furnace, is progressively heated at 840 with the time of 1.5h from room temperature
DEG C, in order that the oxysulfide that coal sample calcination generates is with Ai Shika reagent reacting completely, 2h must be kept at such a temperature, using horse
The not temperature programming control device of stove, during 1.5h, makes the temperature from ambient of Muffle furnace be to slowly warm up to 840 DEG C, sample
Product calcination in Muffle furnace, its reaction equation mainly has:
2so2+o2+2na2co3=2na2so4+2co2↑
so3+na2co3=na2so4+co2↑
2mgo+2so2+o2=2mgso4
meso4+na2co3=na2so4+meco3;
3. dry pot is taken out from Muffle furnace, be cooled to room temperature, now the calcination thing in dry pot includes coal non-combustibles, oxidation
Calcination thing in dry pot is carefully stirred pine, smashs to pieces with Glass rod, then calcination thing transferred to beaker by magnesium and powdered sodium carbonate
In, with hot water injection's dry pot inwall, washing liquid is taken in beaker, adds distilled water, be sufficiently stirred for, make in calcination thing mixed liquor
Soluble substance can be completely dissolved;
4. in washing liquid add dilute hydrochloric acid solution, in order to remove the carbonate in mixture solution it is therefore an objective to prevent carbonate with
The follow-up barium chloride solution reaction adding generates barium carbonate sediment, thus increasing the content of barium element in mixture, increases experiment
Error;During salt adding acid solution, until mixed liquor is in acid ph=2 it was demonstrated that the carbanion in mixture solution is complete
Full removing, now added hydrochloric acid solution is about 20ml;
5. by solution heated and boiled, boil in sour environment solution can will previous step reaction generate carbon dioxide complete
Full discharge, is slowly added dropwise barium chloride solution 10ml so as to generate sulphuric acid with the sulphuric acid reactant salt in mixed liquor under being stirred continuously
Precipitated barium, its ion-reaction equation is:
6. mixed liquor cools down at room temperature, stands 2h, and mixed liquor is stood, and the barium sulfate precipitate that can generate settles completely,
Filtered with fine and close ashless quantitative filter paper, then dried with drying baker, wait tabletting to produce sample;
(2) standard sample and test sample preparation
The manufacturing process of standard sample 1.~4. step identical with the pre-treatment step of coal sample, be added without barium chloride in the 5. step
Solution, is directly filtered, and now sulfate radical is filtered to remove completely, comprises the non-combustible of coal in the precipitate after filtration
The component magnesium oxide of thing and Ai Shika reagent, by this calcination thing precipitation having filtered sulfate radical and baso4Powder presses barium content
It is mixed into 6 parts from the ratio of 1.76~4.70% one-tenth graded, make the quality of every part of sample be about 1g, powder pressing method makes
Print, equally takes several pieces coal sample, carries out sample determination pre-treatment according to above-mentioned coal sample processing method, when sample is in Muffle furnace
During calcination, in coal matrix, all of carbon is all removed with the gas form of oxycarbide, and therefore, that takes out from Muffle furnace burns
Burn amount of substance and be less than quality before putting it in stove, additionally, 4. the in coal sample pretreatment walk, add dilute hydrochloric acid, remove
It is present in the component sodium carbonate of the Ai Shika reagent in mixture solution, during 5. walking the, Deca barium chloride solution is by sulfur
Acid group precipitates into barium sulfate completely, and after filtering, drying, the sample quality obtaining will certainly be different from sample before coal sample pretreatment
The quality of product, weighs the sample obtaining after processing through coal sample successively with electronic balance, and its quality is respectively mi, in order to be suitable for tabletting
The size of grinding tool, takes off a part from the sample of these known quality respectively, makes test sample with powder pressing method, waits
Dispersive x-ray fluorescence analyser is tested to it, in order to verify the accuracy of the method, using the method to gbw11101t,
Five kinds of national standard coal samples of gbw11104h, gbw11104h, gbw11108j and gbw11113e measure, every kind of standard sample
Respectively make some parallel sample, it measured, and measurement result is averaged, then with GB coal sample certificate value matching
The method of curve is contrasted.
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