CN106959318A - A kind of method for determining full content of Sulphur in coal - Google Patents
A kind of method for determining full content of Sulphur in coal Download PDFInfo
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- CN106959318A CN106959318A CN201710353711.0A CN201710353711A CN106959318A CN 106959318 A CN106959318 A CN 106959318A CN 201710353711 A CN201710353711 A CN 201710353711A CN 106959318 A CN106959318 A CN 106959318A
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- coal
- sample
- sulphur
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- calibration
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- 239000003245 coal Substances 0.000 title claims abstract description 63
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 title claims abstract description 45
- 239000005864 Sulphur Substances 0.000 title claims abstract description 36
- 238000000034 method Methods 0.000 title claims abstract description 30
- 238000012360 testing method Methods 0.000 claims abstract description 27
- 229910052717 sulfur Inorganic materials 0.000 claims abstract description 9
- 239000011593 sulfur Substances 0.000 claims abstract description 9
- 238000002474 experimental method Methods 0.000 claims abstract description 8
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 6
- 238000002485 combustion reaction Methods 0.000 claims abstract description 6
- 238000001514 detection method Methods 0.000 claims abstract description 6
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 6
- 239000001301 oxygen Substances 0.000 claims abstract description 6
- 230000003750 conditioning effect Effects 0.000 claims abstract description 4
- 239000000126 substance Substances 0.000 claims description 25
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 12
- 238000005259 measurement Methods 0.000 claims description 9
- 238000007689 inspection Methods 0.000 claims description 8
- 239000000463 material Substances 0.000 claims description 8
- 229910052757 nitrogen Inorganic materials 0.000 claims description 6
- 239000003153 chemical reaction reagent Substances 0.000 claims description 5
- CMPGARWFYBADJI-UHFFFAOYSA-L tungstic acid Chemical compound O[W](O)(=O)=O CMPGARWFYBADJI-UHFFFAOYSA-L 0.000 claims description 4
- 238000011088 calibration curve Methods 0.000 claims description 3
- 239000012159 carrier gas Substances 0.000 claims description 3
- 239000003054 catalyst Substances 0.000 claims description 3
- 238000012937 correction Methods 0.000 claims description 3
- 239000011888 foil Substances 0.000 claims description 3
- 239000007789 gas Substances 0.000 claims description 3
- 230000000873 masking effect Effects 0.000 claims description 3
- 230000010076 replication Effects 0.000 claims description 3
- 239000003381 stabilizer Substances 0.000 claims description 3
- ZNOKGRXACCSDPY-UHFFFAOYSA-N tungsten trioxide Chemical compound O=[W](=O)=O ZNOKGRXACCSDPY-UHFFFAOYSA-N 0.000 claims description 3
- 238000005303 weighing Methods 0.000 claims description 3
- RAHZWNYVWXNFOC-UHFFFAOYSA-N Sulphur dioxide Chemical compound O=S=O RAHZWNYVWXNFOC-UHFFFAOYSA-N 0.000 abstract description 20
- AKEJUJNQAAGONA-UHFFFAOYSA-N sulfur trioxide Chemical compound O=S(=O)=O AKEJUJNQAAGONA-UHFFFAOYSA-N 0.000 abstract description 12
- 235000010269 sulphur dioxide Nutrition 0.000 abstract description 10
- 238000004458 analytical method Methods 0.000 abstract description 5
- 239000000203 mixture Substances 0.000 abstract description 4
- 239000004291 sulphur dioxide Substances 0.000 abstract description 3
- 238000012545 processing Methods 0.000 abstract description 2
- 238000005516 engineering process Methods 0.000 description 3
- 238000003556 assay Methods 0.000 description 2
- 238000005070 sampling Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- TXKMVPPZCYKFAC-UHFFFAOYSA-N disulfur monoxide Inorganic materials O=S=S TXKMVPPZCYKFAC-UHFFFAOYSA-N 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 125000001741 organic sulfur group Chemical group 0.000 description 1
- 238000010248 power generation Methods 0.000 description 1
- 238000004445 quantitative analysis Methods 0.000 description 1
- 238000011895 specific detection Methods 0.000 description 1
- XTQHKBHJIVJGKJ-UHFFFAOYSA-N sulfur monoxide Chemical compound S=O XTQHKBHJIVJGKJ-UHFFFAOYSA-N 0.000 description 1
- 239000013589 supplement Substances 0.000 description 1
- 230000009897 systematic effect Effects 0.000 description 1
Classifications
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N25/00—Investigating or analyzing materials by the use of thermal means
- G01N25/20—Investigating or analyzing materials by the use of thermal means by investigating the development of heat, i.e. calorimetry, e.g. by measuring specific heat, by measuring thermal conductivity
- G01N25/22—Investigating or analyzing materials by the use of thermal means by investigating the development of heat, i.e. calorimetry, e.g. by measuring specific heat, by measuring thermal conductivity on combustion or catalytic oxidation, e.g. of components of gas mixtures
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Combustion & Propulsion (AREA)
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Investigating Or Analyzing Materials Using Thermal Means (AREA)
Abstract
The invention belongs to coal analysis detection technique field, a kind of method for determining full content of Sulphur in coal is refered in particular to；Comprise the following steps：S1, weigh sample；S2, equipment debugging；S3, blank test；S4, conditioning experiment；S5, demarcation；S6, measure；The present invention determines full content of Sulphur in coal using high-temp combustion thermal conductivity method, is that the general analysis experiment coal sample of known quality is fully burnt in high temperature and oxygen stream, the sulphur in coal burns completely generates sulfur dioxide, sulfur trioxide mixture.Filtered by specific processing system to determining noisy influence factor, and be sulfur dioxide by sulfur trioxide Restore All.Sulfur content in coal is quantitative determined by thermal conductivity cell detector in the form of sulphur dioxide, with easy to operate, determines that the cycle is short, and testing result is accurate, simplifies cumbersome intermediate steps.
Description
Technical field
The invention belongs to coal analysis detection technique field, a kind of method for determining full content of Sulphur in coal is refered in particular to.
Background technology
Coal resources are the first big energy of China, are the basic energy resource materials needed for industrial development.Coal resources in China
Enrich very much, account for 70% or so of China's total energy.
Sulphur in coal is harmful element, and the sulfur dioxide and sulfur trioxide converted in burning can be caused to atmospheric environment
Sulphur can also shorten the low-temperature pre-heater life-span, cause boiler scaling etc. in pollution, coal, and power generation is caused harm, therefore, determine
Sulphur has turned into the Ordinary fruit quality project that coal is examined of importing and exporting in coal.But, current assay method has operating process more numerous
The defects such as trivial, measure cycle length.
The content of the invention
There is provided one kind is easy to operate, the measure cycle is short, detection for the above mentioned problem existed the present invention be directed to existing technology
As a result the method for accurately determining full content of Sulphur in coal.
The purpose of the present invention can be realized by following technical proposal：
A kind of method for determining full content of Sulphur in coal, comprises the following steps：
S1, weigh sample
More than 80mg sample is weighed from coal sample, 0.1mg is accurate to；
Sample is put into masking foil, and catalyst tungstic oxide is added by instrument requirements, is wrapped up tight, it is desirable to every part of examination
Material adds more than 3 parts of tungstic acid；
The sample for weighing more than two parts carries out parallel determination, as a result takes its average value；
S2, equipment debugging
Open and adjusting instrument, the instrument is thermal conductivity cell detector, whether inspection apparatus parameters meet detection needs,
And inspection apparatus combustion system and the air-tightness of carrier gas system；Oxygen-supply quantity and logical oxygen time are adjusted, to ensure that coal sample is burnt completely；
S3, blank test
Enter instrument Nitrogen response value when nitrogen content should not exceed calibration substance minimum in line blank test, gas to instrument
1%；When having changed reagent or material in process of the test, blank test should be re-started；
S4, conditioning experiment
A kind of parallel determination that close coal sample is constituted with sample element to be measured, at least 4 times are carried out to the coal sample of selection, house
First time measurement result is gone, remaining three measurement results are judged, when the maximum deflection difference value of sulphur is in 1.2 times of repeatability limits
It is interior, show the instrument stabilizer；Otherwise, reason should be searched, problem is solved；
S5, demarcation
Demarcated from one or more calibration substances, if wherein using a calibration substance, being calibrated by changing
The sample weighting amount of material is demarcated, and the measurement range of the calibration curve demarcated should be able to cover containing for sulphur in all tested coal samples
Measure scope；
S6, measure
Sample is placed in instrument, is measured according to the program that instrument is pre-set.
In a kind of method of above-mentioned measure full content of Sulphur in coal, when instrument is needed by determining calibration factor come correction test
During the testing result of coal sample, the calibration substance close with sample sulfur content or coal standard substance should be used to calculate calibration system
Number, each calibration point answers replication at least 4 times.
In a kind of method of above-mentioned measure full content of Sulphur in coal, during sample is determined, also include demarcation and check：Use
1~2 calibration substance or coal standard substance determine its sulfur content, if the difference of measured value and standard value is in the uncertainty of standard value
In the range of, illustrate that demarcation is effective, otherwise should ascertain the reason, re-scale；Instrument is re-scaled by S5 if necessary, and to checking
The result of the test of preceding completion is redeterminated.
In a kind of method of above-mentioned measure full content of Sulphur in coal, demarcation is checked at the beginning and end of every batch of sampling test
Carry out.
In a kind of method of above-mentioned measure full content of Sulphur in coal, often carrying out to carry out after 10 samples are determined during determining
Demarcation is checked.
Compared with prior art, the present invention has advantages below：
The present invention determines full content of Sulphur in coal using high-temp combustion thermal conductivity method, is that the general analysis experiment coal sample of known quality exists
Fully burnt in high temperature and oxygen stream, the sulphur in coal burns completely generates sulfur dioxide, sulfur trioxide mixture.By specifically
Reason system is filtered to determining noisy influence factor, and is sulfur dioxide by sulfur trioxide Restore All.Sulfur content in coal
Quantitative determined in the form of sulphur dioxide by thermal conductivity cell detector, with easy to operate, determine that the cycle is short, testing result is accurate
Really, cumbersome intermediate steps are simplified.
Brief description of the drawings
Fig. 1 is the FB(flow block) of the present invention.
Embodiment
The following is specific embodiment of the invention and with reference to accompanying drawing, technical scheme is further described,
But the present invention is not limited to these embodiments.
As shown in Figure 1.The present invention provides a kind of method for determining full content of Sulphur in coal, is determined using high-temp combustion thermal conductivity method in coal
Full sulphur, wherein full sulphur refers to all sulphur in coal, including organic sulfur, inorganic sulfur.Specific detection method is as follows：
S1, weigh sample
More than 80mg sample is weighed from coal sample, 0.1mg is accurate to；The weight of sample can appoint in 80-120mg intervals
Meaning value.Such as 80mg, 100mg etc..
Sample is put into masking foil, and catalyst tungstic oxide is added by instrument requirements, is wrapped up tight, it is desirable to every part of examination
Material adds more than 3 parts of tungstic acid.Percentage by weight such as sample and tungstic acid is 1:3；Or 1:4 etc..
The sample for weighing more than two parts carries out parallel determination, as a result takes its average value；The present embodiment weighs two parts, certainly
It can be many parts.
Wherein, parallel determination refers to take several parts of same samples, and they are measured under the same operating conditions.
S2, equipment debugging
Open and adjusting instrument, the instrument is thermal conductivity cell detector, whether inspection apparatus parameters meet detection needs,
And inspection apparatus combustion system and the air-tightness of carrier gas system；Oxygen-supply quantity and logical oxygen time are adjusted according to the specification of instrument, with
Ensure that coal sample is burnt completely.
S3, blank test
Enter instrument Nitrogen response value when nitrogen content should not exceed calibration substance minimum in line blank test, gas to instrument
1%；When having changed reagent or material in process of the test, blank test should be re-started；Wherein, blank assay is to be not added with coal sample
In the case of, quantitative analysis is carried out with determination sample identical method, step, using acquired results as blank value, from sample
Deducted in analysis result.Can so eliminate due to reagent is impure or reagent interference etc. caused by systematic error.
S4, conditioning experiment
A kind of parallel determination that close coal sample is constituted with sample element sulphur to be measured, at least 4 times are carried out to the coal sample of selection,
Cast out first time measurement result, remaining three measurement results are judged, when the maximum deflection difference value of sulphur is in 1.2 times of repeatability
In limit, show the instrument stabilizer；Otherwise, reason should be searched, problem is solved.
S5, demarcation
Demarcated from one or more calibration substances, if wherein using a calibration substance, being calibrated by changing
The sample weighting amount of material is demarcated, and the measurement range of the calibration curve demarcated should be able to cover containing for sulphur in all tested coal samples
Measure scope.
Currently preferred instrumental calibration method is as follows：
1st, calibrating procedure
According to determination step, use Instrument measuring calibration substance (being shown in Table 2).By the sulphur measured value and standard of calibration substance
Value input instrument (or instrument is read automatically), generates standard curve.
If above-mentioned all approximating methods are applied in the demarcation of instrument, the calibration point of more than 10 is selected
Number.
The minimum demarcation points that the present invention recommends are shown in Table 1.
The minimum demarcation points that table 1 is recommended
| Curve-fitting method | Calibration points |
| Linearly | 6 |
| It is secondary | 7 |
| Power | 7 |
| Three times | 8 |
2nd, scalar quantity
As shown in table 2, list when testing coal sample and being 100mg, it is necessary to the amount for the calibration substance demarcated.
The percentage composition of equivalent sulphur in the experiment coal sample of table 2
S6, measure
Sample is placed in instrument, is measured according to the program that instrument is pre-set.
The present invention fully burns sample in high temperature and oxygen stream, and the sulphur in coal burns completely generates sulfur dioxide, three
Sulfur oxide mixture.Filtered by specific processing system to determining noisy influence factor, and by sulfur trioxide Restore All
For sulfur dioxide.Sulfur content in coal is quantitative determined by thermal conductivity cell detector in the form of sulphur dioxide.
When instrument need by determine calibration factor come correction test coal sample testing result when, should use and sample element
The close calibration substance of content or coal standard substance calculate calibration factor, and each calibration point answers replication at least 4 times.
In addition, during sample is determined, demarcation inspection should be carried out.Demarcate the detailed process checked as follows：Use 1~2
Individual calibration substance or coal standard substance determines its sulfur content, if the difference of measured value and standard value is in the range of uncertainty of standard value
It is interior, illustrate that demarcation is effective, otherwise should ascertain the reason, re-scale；Instrument is re-scaled by S5 if necessary, and it is preceding complete to checking
Into result of the test redeterminate.
Demarcation of the present invention, which is checked, to be recommended to carry out at the beginning and end of every batch of sampling test；It is every during determining
Carry out that after 10 samples are determined demarcation inspection should be carried out.
Specific embodiment described herein is only to spirit explanation for example of the invention.Technology neck belonging to of the invention
The technical staff in domain can be made various modifications or supplement to described specific embodiment or be replaced using similar mode
Generation, but without departing from the spiritual of the present invention or surmount scope defined in appended claims.
Claims (5)
1. a kind of method for determining full content of Sulphur in coal, it is characterised in that：Comprise the following steps：
S1, weigh sample
More than 80mg sample is weighed from coal sample, 0.1mg is accurate to；
Sample is put into masking foil, and catalyst tungstic oxide is added by instrument requirements, is wrapped up tight, it is desirable to which every part of sample adds
Enter more than 3 parts of tungstic acid；
The sample for weighing more than two parts carries out parallel determination, as a result takes its average value；
S2, equipment debugging
Open and adjusting instrument, the instrument is thermal conductivity detector (TCD), and whether inspection apparatus parameters meet detection needs, and check
The air-tightness of instrument combustion system and carrier gas system；Oxygen-supply quantity and logical oxygen time are adjusted, to ensure that coal sample is burnt completely；
S3, blank test
Enter 1% of instrument Nitrogen response value when nitrogen content should not exceed calibration substance minimum in line blank test, gas to instrument；
When having changed reagent or material in process of the test, blank test should be re-started；
S4, conditioning experiment
A kind of parallel determination that close coal sample is constituted with sample element to be measured, at least 4 times are carried out to the coal sample of selection, casts out the
Measurement result, judges remaining three measurement results, when the maximum deflection difference value of sulphur is in 1.2 times of repeatability limits,
Show the instrument stabilizer；Otherwise, reason should be searched, problem is solved；
S5, demarcation
Demarcated from one or more calibration substances, if wherein using a calibration substance, by changing calibration substance
Sample weighting amount demarcated, the measurement range for the calibration curve demarcated should be able to cover the content models of sulphur in all tested coal samples
Enclose；
S6, measure
Sample is placed in instrument, is measured according to the program that instrument is pre-set.
2. a kind of method for determining full content of Sulphur in coal according to claim 1, it is characterised in that：When instrument is needed by determining
When calibration factor carrys out the testing result of correction test coal sample, the calibration substance or coal close with the sulfur content of sample should be used
Standard substance calculates calibration factor, and each calibration point answers replication at least 4 times.
3. a kind of method for determining full content of Sulphur in coal according to claim 1, it is characterised in that：During sample is determined, also
Include demarcation to check：Determine its sulfur content using 1~2 calibration substance or coal standard substance, if measured value and standard value it
Difference illustrates that demarcation is effective, otherwise should ascertain the reason, re-scale in the range of uncertainty of standard value；If necessary by S5 weights
New calibrating instrument, and the result of the test completed before checking is redeterminated.
4. a kind of method for determining full content of Sulphur in coal according to claim 3, it is characterised in that：Demarcation is checked in every batch of sample
Carried out at the beginning and end of experiment.
5. a kind of method of measure full content of Sulphur in coal according to claim 3 or 4, it is characterised in that：Often enter during determining
10 samples of row should carry out demarcation inspection after determining.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710353711.0A CN106959318A (en) | 2017-05-18 | 2017-05-18 | A kind of method for determining full content of Sulphur in coal |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710353711.0A CN106959318A (en) | 2017-05-18 | 2017-05-18 | A kind of method for determining full content of Sulphur in coal |
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| Publication Number | Publication Date |
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| CN106959318A true CN106959318A (en) | 2017-07-18 |
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| CN201710353711.0A Pending CN106959318A (en) | 2017-05-18 | 2017-05-18 | A kind of method for determining full content of Sulphur in coal |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109283313A (en) * | 2018-11-12 | 2019-01-29 | 力鸿智信（北京）科技有限公司 | A kind of carbon content in coal hydrogen nitrogen intelligent detection device and coal property test system |
| CN112461911A (en) * | 2020-11-16 | 2021-03-09 | 包头钢铁（集团）有限责任公司 | Method for rapidly and economically detecting purity of sulfur paste |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109283313A (en) * | 2018-11-12 | 2019-01-29 | 力鸿智信（北京）科技有限公司 | A kind of carbon content in coal hydrogen nitrogen intelligent detection device and coal property test system |
| CN112461911A (en) * | 2020-11-16 | 2021-03-09 | 包头钢铁（集团）有限责任公司 | Method for rapidly and economically detecting purity of sulfur paste |
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