CN101694430B - Method for detecting raw coal - Google Patents
Method for detecting raw coal Download PDFInfo
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- CN101694430B CN101694430B CN200910235721XA CN200910235721A CN101694430B CN 101694430 B CN101694430 B CN 101694430B CN 200910235721X A CN200910235721X A CN 200910235721XA CN 200910235721 A CN200910235721 A CN 200910235721A CN 101694430 B CN101694430 B CN 101694430B
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Abstract
The invention relates to a method for detecting raw coal, which comprises steps as follows: firstly preparing a group of standard samples with given element content concentrations; secondarily, inputting chemical concentration of each standard sample, diluting and drying each standard sample, manufacturing analyzing sample wafers via the melting method, determining fluorescence intensity of each element in each analyzing sample wafer on a fluorescence analyzer, and building a standard curve between the chemical concentration of each element oxide and the fluorescence intensity on a computer; thirdly, using coal powder to manufacture standard performing, placing the standard performing on the fluorescence analyzer which displays fluorescence intensity of each element, obtaining corresponding percentage composition of each element oxide according to the standard curve, and finally adding the percentage compositions/dilution proportions of all element oxide together to obtain a sum, namely the ash content in coal powder. The method for detecting raw coal is short in used time and simple in operation, is convenient and timely and has great practical value on guiding coal usage in actual production.
Description
Technical field
The present invention relates to a kind of detection method of raw coal, be meant a kind of method of utilizing fluorescence analyser the ash content of raw coal to be carried out fast detecting especially.
Background technology
The detection method of traditional raw coal will be at the coal dust sampling back high-temp combustion in high temperature furnace of weighing, becoming oxide after the element oxidations such as the C in the coal dust, H, N, S runs away with gas form, weigh after the remaining material cooling and can obtain the content of ash content, total time spent measured about 70 minutes.The shortcoming of this method is: length consuming time, workload is big, process is loaded down with trivial details, untimely.
Summary of the invention
At above-mentioned defective, the object of the present invention is to provide a kind of multielement fluorescence analyser that utilizes that the percentage composition of each oxide in the raw coal is accurately detected, under the situation of not destroying former texture of coal, finish the fast detecting of ash content, data are accurate, the detection method of also simple timesaving coal ash.
The objective of the invention is to realize that by following technical scheme it may further comprise the steps:
One, set up typical curve:
1, prepares sample
At first prepare the standard model of one group of known each element (the various elements in the ash content) content concn, standard model quantity must not be lower than 12, and sample size is many more, and typical curve is accurate more; The chemical concentrations of each standard model is imported computing machine earlier, and each the constituent content concentration in each standard model is all different, just can make the typical curve of each element;
2, preparation sample
(1) determine dilution ratio then, the dilution ratio of the standard model of getting and flux be controlled between 1: 3～1: 10;
(2) dry behind the standard model mixing after will diluting, need do the detection of loss on ignition for standard model, number percent according to the loss on ignition loss should be carried out data recording, the amount of loss should be given polishing according to number percent in flux when doing melting experiment in next step;
(3) above-mentioned each standard model of difference fusion, melt temperature is controlled between 850～1250 ℃, and the time is 2～15 minutes;
3, analytic sample, set up typical curve
Above-mentioned standard model is made glass analysis print with fusion method, on fluorescence analyser, each each element of analyzing in the print is carried out fluorescent strength determining, and by setting up the chemical concentrations of every kind of element oxide and the typical curve between the fluorescence intensity on the computing machine that links to each other, this curve can use for a long time as the typical curve of coal powder fraction analysis;
Two, detect the content of ash content in the coal dust:
4, get coal dust and carry out film-making, make the standard compressing tablet that is fit to the fluorescence analyser analysis;
5, the standard compressing tablet is put in the fluorescence analyser, demonstrates the fluorescence intensity of each element (the various elements in the ash content) on the fluorescence analyser, detect according to above-mentioned typical curve again, draw the chemical concentrations (percentage composition) of each corresponding element oxide;
6, the percentage composition of each element oxide of testing result/dilution ratio sum, the summation that addition obtains is the content of coal powder fraction; But the content of oxide does not comprise carbon, hydrogen, nitrogen, sulfur oxide, and can detect coal dust SO simultaneously yet
3Content.
Come out time spent＜5 minute of above sample (coal dust standard compressing tablet) testing result.
Described flux is lithium tetraborate (Li
2B
4O
7).
Standard model bake out temperature after the described dilution is controlled at 120 ℃.
Inventive principle:
Coal dust is the process that element oxidation change oxides such as the C in the coal dust, H, N, S are run away with gas form in the process of high temperature furnace internal combustion, and remaining material is called ash content, and weighing after cooling obtains the content of coal powder fraction.Contained element is generally Si, Al, Fe, Ca, Mg, K, Ti etc. in the ash content (calcination base), exists with oxide form.And the characteristics of fluorescence analyser are under the situation of not destroying coal dust form and structure, can from coal dust, directly detect the percentage composition of each element oxide, percentage composition addition with each oxide, the summation that obtains promptly is the content of ash content in the coal dust, verify through practical application, this method and traditional ashing method compare, as a result the height unanimity.Can be used as the alternative method that coal powder fraction is measured, for instructing actual production to have high practical value with coal.
Innovative idea: new notion of this method proposition is that the ash content in the coal dust is actually each not volatilizable in coal dust element oxide content summation, therefore, coal dust is not carried out the calcination ashing,, can draw ash content yet as long as can directly detect each oxide content;
Innovative approach: all appts quantitative test all needs to set up working curve, at each material, prepare the standard model of one group of known each constituent content concentration, the chemical concentrations of standard model is imported computing machine earlier, again each element in each sample is carried out fluorescent strength determining, set up the chemical concentrations and the linear equation between the fluorescence intensity (y=ax+b, y are fluorescence intensity, and x is a chemical concentrations) of each element on computers--be called working curve.Generally speaking, different types of material can not shared one group of working curve.The innovative point of this method does not adopt the coal dust standard specimen when being to detect the ash content of coal dust, need not set up special-purpose coal dust analytical work curve yet, but use the working curve of other material fusion sample preparation analytical approach.When detecting various silicate starting materials, adopted melting method: with lithium tetraborate (Li
2B
4O
7) as flux, sample and flux are pressed weighing in 1: 4, glassy print is made in fusion at high temperature behind the mixing, analyzes on luminoscope then, can obtain very high analysis precision.The working curve of Jian Liing can be analyzed at any material like this.Coal dust is pressed into sheet, on instrument, uses above-mentioned working curve, each element oxide content in the coal dust accurately can be detected, each element oxide content addition is just obtained coal powder fraction.Principle-main substance the C in the coal dust, H, O are considered as " flux ", ash content is considered as being evenly distributed on the mineral matter sample in " flux ", compares with the Li2B4O7 antiflux, and its mean molecular weight is suitable substantially, the matrix effect unanimity is not so have big error.
Advantage of the present invention is: the time spent is short, simple, convenient in time, for instructing actual production to have high practical value with coal.
Description of drawings
Fig. 1 is SiO
2Fluorescence intensity and the typical curve of chemical concentrations
Fig. 2 is Al
2O
3Fluorescence intensity and the typical curve of chemical concentrations
Fig. 3 is Fe
2O
3Fluorescence intensity and the typical curve of chemical concentrations
Fig. 4 is the fluorescence intensity of CaO and the typical curve of chemical concentrations
Fig. 5 is the fluorescence intensity of MgO and the typical curve of chemical concentrations
Fig. 6 is K
2The fluorescence intensity of O and the typical curve of chemical concentrations
Fig. 7 is Na
2The fluorescence intensity of O and the typical curve of chemical concentrations
Fig. 8 is SO
3Fluorescence intensity and the typical curve of chemical concentrations
Among the figure: ordinate is a fluorescence intensity, and horizontal ordinate is chemical concentrations (an oxide percentage composition).
Embodiment
The detection method of the described a kind of raw coal of present embodiment, it may further comprise the steps:
One, set up typical curve:
1, prepares sample
At first prepare the standard model of one group of known each element (the various elements in the ash content) content concn, standard model quantity must not be lower than 12, and sample size is many more, and typical curve is accurate more; The chemical concentrations of each standard model is imported computing machine earlier, and each the constituent content concentration in the standard model is all different, just can make the typical curve of each element; Standard model quantity in the present embodiment is 20.
2, preparation sample
(1) determine dilution ratio then, the dilution ratio of the standard model of getting and flux be controlled between 1: 3～1: 10; Flux in the present embodiment is lithium tetraborate (Li
2B
4O
7), the dilution ratio of standard model and flux was controlled at 1: 4.
(2) dry behind the standard model mixing after will diluting, bake out temperature is 120 ℃.Need do the detection of loss on ignition for standard model, should carry out data recording, the amount of loss should be given polishing according to number percent in flux when in next step, doing melting experiment according to the number percent of loss on ignition loss; Standard model is 2 grams in the present embodiment, flux lithium tetraborate (Li
2B
4O
7) be 8 grams, the standard model loss on ignition is 1 gram, loss on ignition is 50% (burn the just moisture that loses, essence and do not become, and does not influence dilution ratio), loss amount 1 gram should be given polishing according to number percent in flux when doing melting experiment in next step.
(3) above-mentioned each standard model of difference fusion, melt temperature is controlled between 850～1250 ℃, and the time is 2～15 minutes.
3, analytic sample, set up typical curve
Above-mentioned standard model is made glass analysis print with fusion method, on fluorescence analyser, each each element of analyzing in the print is carried out fluorescent strength determining, and by setting up the chemical concentrations of every kind of element oxide and the typical curve between the fluorescence intensity on the computing machine that links to each other, as Fig. 1～shown in Figure 8, these curves can use for a long time as the typical curve of coal powder fraction analysis.
Two, detect the content of ash content in the coal dust:
4, get coal dust and carry out film-making, make the standard compressing tablet that is fit to the fluorescence analyser analysis; The surface requirements of coal dust standard compressing tablet is smooth, pollution-free.
5, the standard compressing tablet is put in the fluorescence analyser, demonstrates the fluorescence intensity of each element (the various elements in the ash content) on the fluorescence analyser, detect according to above-mentioned typical curve again, draw the chemical concentrations (percentage composition) of each corresponding element oxide.
6, the percentage composition/1+4 of each element oxide of testing result, the summation that addition obtains is the content of coal powder fraction; But the content of oxide does not comprise carbon, hydrogen, nitrogen, sulfur oxide, and can detect coal dust SO simultaneously yet
3Content.
In the present embodiment, coal dust standard compressing tablet is put in the fluorescence analyser, the fluorescence intensity that demonstrates each element (the various elements in the ash content) on the fluorescence analyser is as follows:
Element (under the oxide system) fluorescence intensity (kcps)
Fe 122.4495
Ca 78.8364
K 2.9854
S 28.4502
Si 41.9553
Al 18.8050
Mg 3.9139
Na 1.5218
Detect according to above-mentioned typical curve again, draw the percentage composition value of each corresponding element oxide:
Oxide percentage composition percentage composition/1+4
SiO
2 16.719％ 3.344％
Al
2O
3 7.130％ 1.426％
Fe
2O
3 7.415％ 1.483％
CaO 15.871％ 3.174％
MgO 1.041％ 0.208％
K
2O 0.667％ 0.133％
Na
2O 0.925％ 0.185％
SO
34.094% (not in the addition scope)
Analysis result addition summation 49.768% 9.953%
Coal powder fraction content is 9.953%
Coal dust-SO
3(4.094%/1+4) 0.819%
Percentage composition among the present invention all refers to weight percentage.
Claims (3)
1. the detection method of a raw coal is characterized in that may further comprise the steps:
One, set up typical curve:
(1) prepares sample
At first prepare the standard model of the various constituent content concentration in one group of known ash content, standard model quantity must not be lower than 12, and sample size is many more, and typical curve is accurate more; The chemical concentrations of each standard model is imported computing machine earlier, and each the constituent content concentration in each standard model is all different, just can make the typical curve of each element;
(2) preparation sample
1. determine dilution ratio then, the dilution ratio of the standard model of getting and flux be controlled between 1: 3～1: 10;
2. dry behind the standard model mixing after will diluting, need do the detection of loss on ignition for standard model, number percent according to the loss on ignition loss should be carried out data recording, the amount of loss should be given polishing according to number percent in flux when doing melting experiment in next step;
3. distinguish above-mentioned each standard model of fusion, melt temperature is controlled between 850～1250 ℃, and the time is 2～15 minutes;
(3) analytic sample, set up typical curve
Above-mentioned standard model is made glass analysis print with fusion method, on fluorescence analyser, each each element of analyzing in the print is carried out fluorescent strength determining, and by setting up the chemical concentrations of every kind of element oxide and the typical curve between the fluorescence intensity on the computing machine that links to each other, this curve can use for a long time as the typical curve of coal powder fraction analysis;
Two, detect the content of ash content in the coal dust:
(4) get coal dust and carry out film-making, make the standard compressing tablet that is fit to the fluorescence analyser analysis;
(5) the standard compressing tablet is put in the fluorescence analyser, demonstrates the fluorescence intensity of each element on the fluorescence analyser, detect according to above-mentioned typical curve again, draw the chemical concentrations of each corresponding element oxide, i.e. percentage composition;
(6) the percentage composition of each element oxide of testing result/dilution ratio sum, the summation that addition obtains is the content of coal powder fraction; And also can detect coal dust SO simultaneously
3Content.
2. the detection method of a kind of raw coal as claimed in claim 1, it is characterized in that: described flux is lithium tetraborate.
3. the detection method of a kind of raw coal as claimed in claim 1, it is characterized in that: the standard model bake out temperature after the described dilution is controlled at 120 ℃.
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| CN103728285A (en) * | 2013-12-20 | 2014-04-16 | 吴江市震宇缝制设备有限公司 | Calibration curve making and calibration method for fluorescence analyzer |
| CN104330389A (en) * | 2013-12-31 | 2015-02-04 | 东旭集团有限公司 | Method for detecting content of various components in stannic oxide electrode block |
| CN112161894A (en) * | 2020-09-10 | 2021-01-01 | 北京沄汇智能科技有限公司 | Material component measuring system and method |
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| CN1328639A (en) * | 1998-09-17 | 2001-12-26 | 程序控制公司 | X-ray fluorescence element analyzer |
| JP2003227795A (en) * | 2002-02-05 | 2003-08-15 | Tohoku Electric Power Co Inc | Measuring apparatus of unburned content in ash |
| JP2004245702A (en) * | 2003-02-14 | 2004-09-02 | Tohoku Electric Power Co Inc | In-ash unburnt combustible content measuring system |
| CN1912588A (en) * | 2006-08-23 | 2007-02-14 | 太原市海通自动化技术有限公司 | Coal on-line analyse equipment based on laser induced spectral and nerve network technology |
| CN101206186A (en) * | 2007-11-27 | 2008-06-25 | 南京国晟科技有限公司 | Device for analyzing and detecting coal constituent rapidly |
-
2009
- 2009-10-13 CN CN200910235721XA patent/CN101694430B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1328639A (en) * | 1998-09-17 | 2001-12-26 | 程序控制公司 | X-ray fluorescence element analyzer |
| JP2003227795A (en) * | 2002-02-05 | 2003-08-15 | Tohoku Electric Power Co Inc | Measuring apparatus of unburned content in ash |
| JP2004245702A (en) * | 2003-02-14 | 2004-09-02 | Tohoku Electric Power Co Inc | In-ash unburnt combustible content measuring system |
| CN1912588A (en) * | 2006-08-23 | 2007-02-14 | 太原市海通自动化技术有限公司 | Coal on-line analyse equipment based on laser induced spectral and nerve network technology |
| CN101206186A (en) * | 2007-11-27 | 2008-06-25 | 南京国晟科技有限公司 | Device for analyzing and detecting coal constituent rapidly |
Non-Patent Citations (2)
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| 刘尚华 等.X射线荧光光谱分析中的粉末压片制样法.《光谱试验室》.1998,第15卷(第6期),9-15. * |
| 徐强 等.巧用X射线荧光分析仪快速分析原煤灰分.《水泥》.2008,(第1期),43. * |
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Assignee: Beijing Building Material Inspection Center Co Ltd Assignor: Beijing Jinyu Hongshulin Environment Protecting Techn Co., Ltd. Contract record no.: 2012110000108 Denomination of invention: Method for detecting raw coal Granted publication date: 20110824 License type: Exclusive License Open date: 20100414 Record date: 20120611 |
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