CN105928963A - Method for detecting quality of raw coal - Google Patents

Abstract

The invention discloses a method for detecting the quality of raw coal, and aims to provide a method, which can quickly and accurately measure the whole sulfur content of raw coal. The method comprises the following steps: (1) adding 30 grams of sample to be detected into a fluorescent analyzer, grinding the sample for 120 seconds, setting the pressure of a tablet press at 35 MPa, keeping the pressure for 120 seconds, analyzing the sample for 120 seconds, and measuring the cps strength of the sample; (2) choosing sulfur standards with a concentration of 0.09 to 6.11%, adding the chosen standards into a X fluorescent analyzer in sequence, detecting the standards according to the operation of step (1), recording the measured concentration values of the standards, and calculating the data by a computer to obtain a calculating equation of S concentration and cps strength: Y=0.473X-0.254, and related coefficient (r)=0.9998; (3) performing comparison validation. The invention belongs to the technical field of chemical detection.

Description

A kind of method detecting raw coal quality

Technical field

The present invention relates to a kind of quality determining method, specifically, be a kind of method detecting raw coal quality, Belong to technical field of chemical detection.

Background technology

In the planned economy era, the price of coal product depends on coal index, and this just makes the yield of coal become In order to affect the single factor of the performance of enterprises, what coal enterprise the most at that time was pursued is exactly coal production. And in market economy times, can the price of coal product depend on reaching contracted quality standard, because of The quality of this coal product is increasingly becoming the first place that coal enterprise manages.Especially for coal preparation plant, although it Great majority in all serve colliery, but it is selected to reach to guarantee also to realize controlling raw coal quality, homogenizing The purpose of product quality.

Owing to being affected by coal mining condition and coal field geology condition, coal enterprise is when different mines and difference The raw coal that phase is produced, quality all also exists certain difference.Raw coal sulfur, ash, carbon is all important coal One of matter index, the productivity of cleaned coal and quality all with raw coal sulfur, ash, the height of carbon also exists directly pass System, even if being identical sulfur, ash, the raw coal of carbon, its washability is also possible to difference, raw coal thus Quality be uncertain, need periodically to test.

Benefit is the pursuit of enterprise, and quality is the life of enterprise, and coal enterprise wants to ensure the warp of enterprise simultaneously Ji benefit and product quality, being necessary for will be putting the Quality inspection of raw coal in the first place of routine work. If this work is paid little attention to, neither control, do not check, then when the quality of raw coal changes Time, just influence whether the product quality of coal enterprise, cause the loss of cleaned coal and the waste of the energy, finally make Become the loss of enterprise.

Summary of the invention

For the problems referred to above, the purpose that the present invention provides is to provide one accurately and rapidly to former full content of Sulphur in coal The method that is measured of content.

For solving above-mentioned technical problem, the technical scheme that the present invention provides is such that

A kind of method detecting raw coal quality, comprises the steps: successively

1) add detected sample 30 grams to fluorescence analyser, measure by following operation sequence: grinding 120 Second, tablet machine pressure 35Mpa, pressure continue 120 seconds, 120 seconds analysis times, measure the cps of sample Intensity；

2) select element sulphur at 0.09-6.11% concentration standards, selected standard sample is sequentially placed into X glimmering In light analyser, as step 1) described in operation sequence detect, and fill according to the measurement data of instrument The concentration value of standard sample, by the calculating of computer, draws S concentration of element and the accounting equation of cps intensity: Y=0.473X-0.254, correlation coefficient r=0.9998；

3) contrast verification.

Compared with prior art, the technical scheme that the present invention provides is by detecting raw coal matter to xrf analysis instrument Quantitative analysis is it can be seen that the content of former full content of Sulphur in coal can be carried out by this kind of check system accurately and rapidly Measuring, the accuracy of testing result is higher, can be that coal enterprise controls to produce the strong foundation of offer.

Detailed description of the invention

Below in conjunction with detailed description of the invention, the claim of the present invention is described in further detail, but not Constitute any limitation of the invention, any limited number of time done in the claims in the present invention protection domain Amendment, still within the claims of the present invention.

Embodiment 1

To the analysis utilizing xrf analysis instrument detection raw coal quality

The configuration of 1.1 detecting instruments

When this time detecting, the analytical tool of employing is the VENUS200 that Phillips of Holland produces Type multichannel fluorescence analyser, analyser is configured with crystal roundabout lane, scanning road and fixing road, Ke Yishi The now detection to nine kinds of elements of Al, Si, Ca, Fe, Na, Mg, P, S, K contained in raw coal；Use Sample preparation instrument be Shanghai Sheng Li company produce the sealed vibromill of SL301 and the semi-automatic pressure of SL201 type Model machine.

1.2 analysis times and the determination of sampling

When using the inspection that powder pressing method carries out raw coal quality, the error of detection data is mainly derived from mineral Absorption-enhancement effect between effect, element and the grain effect of material.In order to make the matrix effect of detected raw coal Should reach unanimity, to use same sampling machine and specify identical sample size to be ground and phase during detection Same grinding time；In order to make the grain effect of detected raw coal reach unanimity, can proper extension grinding time, Thus eliminate mineral effect, it is thus achieved that optimal grinding effect.It addition, be also noted that when carrying out tabletting and need to make With the automatic press that pressing speed is constant, in order to eliminate packing density of particle and distribution of particles to assay Impact.

1.2.1 grinding time is selected

First, the analysis time of fluorescence analyser is set to 60 seconds, the quality treating grind away product is set to 30 grams, Ensureing that sample changes grinding time on the premise of identical, in order to measure the cps intensity (counting the most per second of sample Intensity, English full name is count per second), in order to determine optimal grinding time.That tests is relevant Data are shown in Table 1.

Table 1 same sample testing result under different grinding times

Can draw according to data above, after grinding time was more than 120 seconds, the change of S element cps intensity Change amplitude can reduce, and lies substantially in unchanged state, illustrate to be set to grinding time 120 seconds be to compare conjunction Reason.

1.2.2 select tablet machine pressure

Ensureing that sample changes tablet machine pressure and the persistent period of pressure on the premise of identical, through too much Secondary making and contrast, draw when the pressure of tablet machine is 35Mpa, when the persistent period of pressure is 120 seconds, The print flawless produced, smooth surface, moderate strength.

1.2.3 select the measurement time

After the persistent period determining grinding time, tablet machine pressure and pressure, ensureing that sample is identical On the premise of change the measurement time, draw different S element cps intensity, in order to select reasonably measure the time. The measurement time is exactly the time that fluorescence analyser carries out fluorescence irradiation, and measurement result is shown in Table 2

Table 2 same sample testing result under the different measuring time

The measurement time (second)	The cps intensity of S element
		60	7.578
90	7.582
		120	7.663
150	7.663
		180	7.665

Can draw according to data above, the measurement time more than 120 seconds after, the change of S element cps intensity Change amplitude can reduce, and lies substantially in unchanged state, illustrate to be set to the measurement time 120 seconds be to compare conjunction Reason.

By above-mentioned experimental result is considered, finally the preparation condition of coal sample is set to sample matter Measuring 30 grams, grinding time 120 seconds, tablet machine pressure 35Mpa, pressure continue 120 seconds, analysis time 120 Second.

The selection of 3.3 standard sample

The alternative condition of standard sample is the fluctuation range of element to be measured enterprise the to be covered production technology in sample And there is certain Concentraton gradient, it is also noted that simultaneously and collects the coal dust sample that some total sulphur contents are of a relatively high As high standard specimen, and according to the method for regulation in GB/T214-1996, sample being carried out accurate definite value, detection is tied Fruit is shown in Table 3.

The concentration of S element in table 3 various criterion sample

Sample number into spectrum	1	2	3	4	5	6	7	8	9	10	11	12
													Concentration %	0.09	0.16	0.24	0.32	0.86	1.23	1.85	2.17	2.85	3.26	4.93	6.11

3.4 set up working curve

Selected standard sample is sequentially placed in xrf analysis instrument and detects, and according to the measurement of instrument Data fill in the concentration value of standard sample, by the calculating of computer, draw S concentration of element and cps intensity Accounting equation:

Y=0.473X-0.254

Correlation coefficient r=0.9998

3.5 checking detection methods

In order to ensure accuracy and the reliability of raw coal quality inspection work, also to choose 8 bases The method specified in GB/T214-1996 carries out the coal dust sample of definite value and compares with national coal dust standard sample Relatively, comparative result is shown in Table 4

The testing result of table 4 fluorescence analysis detection method and the comparing result of country's coal dust standard sample

Claims (1)

1. the method detecting raw coal quality, it is characterised in that comprise the steps: successively

1) add detected sample 30 grams to fluorescence analyser, measure by following operation sequence: grinding 120 Second, tablet machine pressure 35Mpa, pressure continue 120 seconds, 120 seconds analysis times, measure the cps of sample Intensity；

2) select element sulphur at 0.09-6.11% concentration standards, selected standard sample is sequentially placed into X glimmering In light analyser, as step 1) described in operation sequence detect, and fill according to the measurement data of instrument The concentration value of standard sample, by the calculating of computer, draws S concentration of element and the accounting equation of cps intensity: Y=0.473X-0.254, correlation coefficient r=0.9998；

3) contrast verification.