CN109991210A - Test methods of sulphur contents in coal ash - Google Patents
Test methods of sulphur contents in coal ash Download PDFInfo
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- CN109991210A CN109991210A CN201910319337.1A CN201910319337A CN109991210A CN 109991210 A CN109991210 A CN 109991210A CN 201910319337 A CN201910319337 A CN 201910319337A CN 109991210 A CN109991210 A CN 109991210A
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- coal ash
- sulfur content
- kappa number
- low
- sulphur
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- 239000010883 coal ash Substances 0.000 title claims abstract description 164
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 title claims abstract description 137
- 239000005864 Sulphur Substances 0.000 title claims abstract description 65
- 238000010998 test method Methods 0.000 title claims abstract description 29
- 238000000034 method Methods 0.000 claims abstract description 77
- 239000011593 sulfur Substances 0.000 claims abstract description 72
- 229910052717 sulfur Inorganic materials 0.000 claims abstract description 72
- 238000002354 inductively-coupled plasma atomic emission spectroscopy Methods 0.000 claims abstract description 44
- 238000005259 measurement Methods 0.000 claims abstract description 39
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 72
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 62
- VLTRZXGMWDSKGL-UHFFFAOYSA-N perchloric acid Chemical compound OCl(=O)(=O)=O VLTRZXGMWDSKGL-UHFFFAOYSA-N 0.000 claims description 62
- 150000003839 salts Chemical class 0.000 claims description 37
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 29
- 238000009616 inductively coupled plasma Methods 0.000 claims description 27
- 239000000126 substance Substances 0.000 claims description 27
- 239000000243 solution Substances 0.000 claims description 24
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 20
- 239000007789 gas Substances 0.000 claims description 20
- 239000012086 standard solution Substances 0.000 claims description 18
- 238000001514 detection method Methods 0.000 claims description 17
- 238000010926 purge Methods 0.000 claims description 17
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 14
- 239000007788 liquid Substances 0.000 claims description 13
- 238000001816 cooling Methods 0.000 claims description 12
- 238000001914 filtration Methods 0.000 claims description 12
- 239000000203 mixture Substances 0.000 claims description 12
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 12
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 12
- 229910052760 oxygen Inorganic materials 0.000 claims description 11
- 239000001301 oxygen Substances 0.000 claims description 11
- 229910052786 argon Inorganic materials 0.000 claims description 10
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 10
- 239000003381 stabilizer Substances 0.000 claims description 10
- 238000010792 warming Methods 0.000 claims description 10
- 238000002485 combustion reaction Methods 0.000 claims description 9
- 239000000377 silicon dioxide Substances 0.000 claims description 7
- 239000002253 acid Substances 0.000 claims description 6
- -1 polytetrafluoroethylene Polymers 0.000 claims description 6
- 238000010521 absorption reaction Methods 0.000 claims description 4
- 239000011505 plaster Substances 0.000 claims description 4
- 238000001637 plasma atomic emission spectroscopy Methods 0.000 claims description 3
- 238000000746 purification Methods 0.000 claims description 3
- 235000012239 silicon dioxide Nutrition 0.000 claims description 3
- 238000001228 spectrum Methods 0.000 claims description 3
- 238000012360 testing method Methods 0.000 abstract description 22
- TZCXTZWJZNENPQ-UHFFFAOYSA-L barium sulfate Chemical compound [Ba+2].[O-]S([O-])(=O)=O TZCXTZWJZNENPQ-UHFFFAOYSA-L 0.000 abstract description 10
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 abstract description 8
- 229910052742 iron Inorganic materials 0.000 abstract description 4
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 abstract description 3
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 abstract description 3
- 238000003912 environmental pollution Methods 0.000 abstract description 3
- 239000011591 potassium Substances 0.000 abstract description 3
- 229910052700 potassium Inorganic materials 0.000 abstract description 3
- 239000011734 sodium Substances 0.000 abstract description 3
- 229910052708 sodium Inorganic materials 0.000 abstract description 3
- 239000000470 constituent Substances 0.000 abstract description 2
- 238000007781 pre-processing Methods 0.000 abstract description 2
- 238000011084 recovery Methods 0.000 description 14
- 238000000295 emission spectrum Methods 0.000 description 10
- 239000002956 ash Substances 0.000 description 8
- 239000003245 coal Substances 0.000 description 6
- AKEJUJNQAAGONA-UHFFFAOYSA-N sulfur trioxide Chemical compound O=S(=O)=O AKEJUJNQAAGONA-UHFFFAOYSA-N 0.000 description 6
- 230000010076 replication Effects 0.000 description 4
- 238000009736 wetting Methods 0.000 description 4
- 230000008878 coupling Effects 0.000 description 3
- 238000010168 coupling process Methods 0.000 description 3
- 238000005859 coupling reaction Methods 0.000 description 3
- 239000000706 filtrate Substances 0.000 description 3
- 239000010881 fly ash Substances 0.000 description 3
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 2
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 2
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 2
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 2
- 239000004411 aluminium Substances 0.000 description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- 239000011575 calcium Substances 0.000 description 2
- 229910052791 calcium Inorganic materials 0.000 description 2
- OSGAYBCDTDRGGQ-UHFFFAOYSA-L calcium sulfate Chemical compound [Ca+2].[O-]S([O-])(=O)=O OSGAYBCDTDRGGQ-UHFFFAOYSA-L 0.000 description 2
- 238000005443 coulometric titration Methods 0.000 description 2
- 230000005611 electricity Effects 0.000 description 2
- 230000001939 inductive effect Effects 0.000 description 2
- 239000004615 ingredient Substances 0.000 description 2
- 239000011777 magnesium Substances 0.000 description 2
- 229910052749 magnesium Inorganic materials 0.000 description 2
- 238000006386 neutralization reaction Methods 0.000 description 2
- 239000011574 phosphorus Substances 0.000 description 2
- 229910052698 phosphorus Inorganic materials 0.000 description 2
- 238000004611 spectroscopical analysis Methods 0.000 description 2
- 239000010936 titanium Substances 0.000 description 2
- 229910052719 titanium Inorganic materials 0.000 description 2
- 238000004566 IR spectroscopy Methods 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 238000001636 atomic emission spectroscopy Methods 0.000 description 1
- 229910052788 barium Inorganic materials 0.000 description 1
- DSAJWYNOEDNPEQ-UHFFFAOYSA-N barium atom Chemical compound [Ba] DSAJWYNOEDNPEQ-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000004566 building material Substances 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- GJYLKIZKRHDRER-UHFFFAOYSA-N calcium;sulfuric acid Chemical compound [Ca].OS(O)(=O)=O GJYLKIZKRHDRER-UHFFFAOYSA-N 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000003610 charcoal Substances 0.000 description 1
- 238000005660 chlorination reaction Methods 0.000 description 1
- 239000000571 coke Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- UZUODNWWWUQRIR-UHFFFAOYSA-L disodium;3-aminonaphthalene-1,5-disulfonate Chemical compound [Na+].[Na+].C1=CC=C(S([O-])(=O)=O)C2=CC(N)=CC(S([O-])(=O)=O)=C21 UZUODNWWWUQRIR-UHFFFAOYSA-L 0.000 description 1
- 229910052571 earthenware Inorganic materials 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 238000004993 emission spectroscopy Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 230000004927 fusion Effects 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 1
- HZRMTWQRDMYLNW-UHFFFAOYSA-N lithium metaborate Chemical compound [Li+].[O-]B=O HZRMTWQRDMYLNW-UHFFFAOYSA-N 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- NICDRCVJGXLKSF-UHFFFAOYSA-N nitric acid;trihydrochloride Chemical compound Cl.Cl.Cl.O[N+]([O-])=O NICDRCVJGXLKSF-UHFFFAOYSA-N 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- CMPGARWFYBADJI-UHFFFAOYSA-L tungstic acid Chemical compound O[W](O)(=O)=O CMPGARWFYBADJI-UHFFFAOYSA-L 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/35—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
- G01N21/3504—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light for analysing gases, e.g. multi-gas analysis
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/71—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light thermally excited
- G01N21/73—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light thermally excited using plasma burners or torches
Landscapes
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Pathology (AREA)
- General Health & Medical Sciences (AREA)
- Immunology (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Physics & Mathematics (AREA)
- Spectroscopy & Molecular Physics (AREA)
- Plasma & Fusion (AREA)
- Nuclear Medicine, Radiotherapy & Molecular Imaging (AREA)
- Engineering & Computer Science (AREA)
- Investigating, Analyzing Materials By Fluorescence Or Luminescence (AREA)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
The invention discloses test methods of sulphur contents in a kind of coal ash, belong to coal ash constituent determination techniques field.The measurement that sulfur content is carried out using low-kappa number combination inductively coupled plasma atomic emission spectrometry of the invention, specific steps are as follows: (1) coal ash sample to be determined is subjected to low-kappa number；(2) standard curve is established；(3) measurement of sulfur content is carried out to the coal ash sample after low-kappa number using inductively coupled plasma atomic emission spectrometry.Of the invention uses sulfur content in infrared spectroscopic determination coal ash, specific steps are as follows: (1) establish standard curve；(2) using sulfur content in infrared spectroscopic determination coal ash.The present invention considerably reduces the factor that may influence test result compared with traditional barium sulfate mass method, has preprocessing process simple, environmental pollution is small, the high advantage of measurement accuracy.When using sulfur content in infrared spectroscopic determination coal ash, the elements such as potassium, sodium, the iron in coal ash can also be measured simultaneously.
Description
Technical field
The present invention relates to coal ash constituent determination techniques fields, and in particular to test methods of sulphur contents in a kind of coal ash.
Background technique
China is a big coal country, can all discharge a large amount of flyash every year, flyash is building work, building materials, water conservancy at present
It has been widely used etc. each field, but sulfur content is excessively high in flyash will affect its application, therefore has measured coal ash group its use in pairs
There is directive significance on way.The measurement of sulfur content mainly has barium sulfate mass method, burning neutralisation and coulometric titration at present in coal ash.
Barium sulfate mass method is as a kind of chemistry in detecting, and the scope of application is wide and at low cost, but operating process is comparatively laborious, and measures
The excess chlorination barium being added in the process easily causes environmental pollution；Neutralisation of burning operation is fairly simple, but when single sample test
Between it is long, be not suitable for carry out batch testing；Coulometric titration is easy to operate quickly, cost is relatively low, but test temperature is lower, test temperature
Degree is 1150 DEG C, and tungstic acid need to be added and make catalyst, and the single sample testing time is long.
Inductively coupled plasma atomic emission spectrometry (ICP-AES) is using inductively coupled plasma square as exciting light
The spectroscopic analysis methods in source, with accuracy height and precision are high, detection limit is low, measurement is quick, the range of linearity is wide, can survey simultaneously
The advantages that determining multiple element, is widely used in the measurement of tens of kinds of elements in the samples such as environmental sample and geology, material, but is used for
The measurement of sulfur content is relatively fewer in ash, and Liu Hua etc. melts coal ash and tabletting with lithium metaborate, dissolves in chloroazotic acid, in inductance coupling
It closes plasma emlssion spectrometry and measures sulfur trioxide content at 180.7nm.Zhang Di etc. is existed using inductive coupling emission spectrum
The sulfur trioxide in sample after coal ash alkali fusion is measured at 182.0nm, two researchers use a kind of high temperature melting
The mode melted handles coal ash sample.
Infra-red sepectrometry is a kind of measuring method of fast and accurately full content of Sulphur in coal content, but is only applicable to coal and coke at present
Charcoal is not applied to the measurement of sulfur content in coal ash.
Summary of the invention
The technical problem to be solved by the present invention is to overcome above-mentioned deficiency, inductance can be combined using acid processing by providing one kind
The method of sulphur in coupled plasma-atomic emission spectrometry ICP-AES rapid and accurate determination coal ash, and utilize infrared spectroscopy
The content of sulphur in method rapid and accurate determination coal ash.
Technical scheme is as follows:
Test methods of sulphur contents in a kind of coal ash, utilizes low-kappa number combination inductively coupled plasma atomic emission spectrum
Method carries out the measurement of sulfur content in coal ash, the specific steps are as follows:
(1) coal ash sample is subjected to low-kappa number；
(2) standard curve is established；
(3) sulfur content is carried out to the coal ash sample after low-kappa number using inductively coupled plasma atomic emission spectrometry
Measurement.
Further, coal ash sample is carried out low-kappa number by the step (1)；The low-kappa number refers to that hydrochloric acid is located in advance
Reason or perchloric acid/hydrofluoric acid/salt low-kappa number.
Still further, the pretreated method of hydrochloric acid are as follows:
0.2~0.5g of coal ash sample is weighed in beaker, the hydrochloric acid solution 50-100mL that volume ratio is (1+3), lid is added
Upper surface ware is heated to removing after 20min occurs in bubble on electric hot plate, with filter paper filtering in beaker, with 60-100 DEG C
Hot water washs at least 5 times, and liquid to be filtered uses volumetric flask constant volume after being cooled to room temperature.This method can guarantee that the sulphur in coal ash can be all molten
It solves, be fully converted to solution state.
Further, the perchloric acid/pretreated method of hydrofluoric acid/hydrochloric acid are as follows: weighed coal ash 0.09-0.12g
In polytetrafluoroethylene (PTFE) crucible, 2mL perchloric acid and 10mL hydrofluoric acid are added after being soaked with water, is heated to solution and steams to dry but not
It is burned black, after removing natural cooling at least 1min, 5mL hydrochloric acid and 15mL water is added, is again heated to bubble and occurs and keep the temperature 2-5min,
Solution is transferred in volumetric flask with water after removing natural cooling at least 1min, is cooled to room temperature rear constant volume.This method can guarantee coal
Sulphur in ash can all dissolve, be fully converted to solution state.ICP-AES can use by the solution that this method obtains simultaneously
Potassium, sodium, iron, calcium, magnesium, aluminium, phosphorus, titanium elements are measured, visible utilization preprocess method of content of respective element in coal ash is obtained
The purpose for measuring nine kinds of ingredients to coal ash single treatment, simultaneously can be achieved, greatly reduce using other methods institute with come
Workload.
Further, the standard curve method for building up of the inductively coupled plasma atomic emission spectrometry are as follows: adopt
With having, card coal ash standard substance is acid treated to obtain solution single-point or multi-point calibration, or use sulphur standard solution preparation at least 3
A sulfur content be 0-30mg/L series standard solution, inductively coupled plasma atomic emission spectrometer after argon purge,
Standard curve is established at 182.03nm or 180.73nm analytical line under instrument optimum condition.Have in card coal ash standard substance
Sulfur content establishes standard song according to certificate calibration value it is known that can be used after treatment process identical with coal ash to be measured obtains solution
Line can also prepare series standard solution using sulphur standard solution and establish standard curve, can flexibly implement according to the actual situation.
Further, the step (3) using inductively coupled plasma atomic emission spectrometry to low-kappa number after
Coal ash sample carry out sulfur content measurement, refer to after salt low-kappa number or perchloric acid/hydrofluoric acid/salt low-kappa number constant volume
Coal ash sample measures sulfur content in 182.03nm or 180.73nm wavelength with inductively coupled plasma atomic emission spectrometry.
This method directly measures the solution that acid processing obtains through inductively coupled plasma atomic emission spectrometry, avoids other steps
Rapid introduced error, it is simple accurate.
Further, in the pretreated method of the hydrochloric acid, 0.2~0.5g of coal ash sample is weighed in beaker, is added
Volume ratio is the hydrochloric acid solution 50-100mL of (1+3), and cap upper surface ware is heated to taking after 20min occurs in bubble on electric hot plate
Under, with filter paper filtering in beaker, washed at least 5 times with 60-100 DEG C of hot water, liquid to be filtered uses volumetric flask after being cooled to room temperature
Constant volume；Filter paper therein is that middling speed is qualitative or middling speed quantitative filter paper.This method fully enters the sulphur in acid treated coal ash
In filtrate.
In the pretreated method of hydrochloric acid, coal ash sample 0.2-0.5g is weighed in beaker, and it is (1+3) that volume ratio, which is added,
Hydrochloric acid solution 50-100mL, cap upper surface ware is heated to removing after 20min occurs in bubble on electric hot plate, be filtered with filter paper
In beaker, washed at least 5 times with 60-100 DEG C of hot water, liquid to be filtered uses volumetric flask constant volume after being cooled to room temperature；Filter therein
Paper is that middling speed is qualitative or middling speed quantitative filter paper.
Test methods of sulphur contents is included the following steps: using sulfur content in infrared spectroscopic determination coal ash in a kind of coal ash
(1) standard curve is established；
(2) using sulfur content in infrared spectroscopic determination coal ash.
Further, step (1) establishes standard curve, and specially using has card coal ash standard substance single-point or multiple spot mark
It is fixed, or dead plaster and silica is used to prepare sulfur content respectively as the correct mixture of 0.00%-12.00%, wherein
0.00% mixture available spectrum pure silicon dioxide, each coal ash standard substance or correct mixture are enterprising in infrared constant sulphur appliance
Row is measured in parallel at least twice, specially infrared constant sulphur appliance is warming up to not less than 1300 DEG C, after instrument stabilizer, with 2.8-
3.5L/min is passed through the oxygen that purity is greater than 99.5%, by the earthenware equipped with 0.08-0.12g coal ash standard substance or correct mixture
Crucible is pushed into combustion tube flat-temperature zone, and the gas after burning enters infrared detection system through gas purge system, it is strong to obtain infrared absorption
The relation curve of degree and sulfur content.There is the sulfur content in card coal ash standard substance it is known that having card coal ash standard substance through infrared
Spectrographic determination can also can have card coal using multiple with individually there is the asserting value of card coal ash standard substance to carry out single-point calibration
The asserting value of grey standard substance establishes standard curve, and dead plaster also can be used and silica prepares different sulfur contents
Mixture establishes standard curve through infrared spectroscopic determination as standard substance.Can flexibly it implement according to the actual situation.
Still further, the step (2) is using sulfur content in infrared spectroscopic determination coal ash；Specially sulphur is determined by infrared
Instrument is warming up to not less than 1300 DEG C, after instrument stabilizer, is passed through the oxygen that purity is greater than 99.5% with 2.8-3.5L/min, will be filled
There is the crucible push-in combustion tube flat-temperature zone of 0.08-0.12g coal ash, the gas after burning enters infrared detection through gas purge system
System obtains the sulfur content in coal ash.
Compared with prior art, the invention has the following beneficial effects:
1, traditional barium sulfate mass method test process is cumbersome, some ash samples can generate more hydrogen-oxygen during the test
Change iron precipitating, filtrate caused to be difficult to the step for filtering, being washed repeatedly with hot water time-consuming several days, will lead to test result error compared with
Greatly.Compared with barium sulfate mass method result, salt low-kappa number hydrochloric acid of the invention disappears boil ash sample, filtering after constant volume use
Inductively coupled plasma atomic emission spectrometry ICP-AES is detected, instead of tune acidity-precipitating hydroxide in gravimetric method
This series of steps of iron-filtration washing-filtrate tune acidity-blanc fixe-filtration washing-calcination greatly reduces test knot
The influence factor of fruit has preprocessing process simple, and environmental pollution is small, and the high advantage of measurement accuracy can survey sulfur content in ash
Lower limit is 0.008%.
2, perchloric acid/hydrofluoric acid/salt low-kappa number is in conjunction with inductively coupled plasma atomic emission spectrometry ICP-AES
Measuring method, inductively coupled plasma atomic emission spectrometry ICP-AES is used to be examined with constant volume after the molten ash sample of acid
It surveys, potassium, sodium, iron, calcium, magnesium, aluminium, phosphorus, the titanium elements in coal ash can also be measured while testing sulfur content, are obtained in coal ash
The content of respective element.Therefore the mesh of nine kinds of ingredients can be realized to coal ash single treatment while measured using method of the invention
's.The lower limit that sulfur content in ash can be surveyed is 0.023%.
3, have the advantages that quick and precisely Determination Limit is using the method for sulfur content in infrared spectroscopic determination coal ash
0.041%.
4, perchloric acid/hydrofluoric acid/salt low-kappa number is in conjunction with inductively coupled plasma atomic emission spectrometry ICP-AES
The measuring method rate of recovery reach 98%-103%, salt low-kappa number and inductively coupled plasma atomic emission spectrometry ICP-
The measuring method rate of recovery that AES is combined reaches 98%-101%, using test methods of sulphur contents in infrared spectroscopic determination coal ash
The rate of recovery reach 100.24%-103.59%, the accuracy of three kinds of methods is all very high.
Specific embodiment
The present invention is described in detail below with reference to embodiment.
Embodiment 1
Test methods of sulphur contents in a kind of coal ash, utilizes low-kappa number combination inductively coupled plasma atomic emission spectrum
The measurement of method progress sulfur content, the specific steps are as follows:
(1) coal ash sample is subjected to low-kappa number；Coal ash sample is specifically subjected to salt low-kappa number.The hydrochloric acid is located in advance
The method of reason are as follows: weigh coal ash sample 0.2000g in beaker, the hydrochloric acid solution 100mL that volume ratio is (1+3) is added, covers
Surface plate is heated to removing after 20min occurs in bubble on electric hot plate, with the filtering of middling speed qualitative filter paper in beaker, with 80 DEG C
Hot water wash 5 times, liquid to be filtered uses volumetric flask constant volume after being cooled to room temperature.
(2) standard curve is established；7 series standard solution: 0,2mg/L, 4mg/L, 8mg/ are prepared using sulphur standard solution
L, 10mg/L, 20mg/L, 30mg/L, inductively coupled plasma atomic emission spectrometer are best in instrument after argon purge
Under the conditions of establish standard curve at 182.03nm analytical line.
(3) sulfur content is carried out to the coal ash sample after low-kappa number using inductively coupled plasma atomic emission spectrometry
Measurement.Coal ash sample after salt low-kappa number constant volume, with inductively coupled plasma atomic emission spectrometry in
182.03nm wavelength measures sulfur content.
Embodiment 2
Test methods of sulphur contents in a kind of coal ash, utilizes low-kappa number combination inductively coupled plasma atomic emission spectrum
The measurement of method progress sulfur content, the specific steps are as follows:
(1) coal ash sample is subjected to low-kappa number；Coal ash sample is specifically subjected to salt low-kappa number.The hydrochloric acid is located in advance
The method of reason are as follows: weigh coal ash sample 0.3515g in beaker, the hydrochloric acid solution 75mL that volume ratio is (1+3) is added, covers table
Face ware is heated to removing after 20min occurs in bubble on electric hot plate, with the filtering of middling speed quantitative filter paper in beaker, with 100 DEG C
Hot water washs 8 times, and liquid to be filtered uses volumetric flask constant volume after being cooled to room temperature.
(2) standard curve is established；Using coal ash standard substance GBW11131a, GBW11128a and GBW11132a pass through with
The identical salt low-kappa number of step (1) obtains standard solution, and inductively coupled plasma atomic emission spectrometer is through argon purge
Afterwards, standard curve is established at 180.73nm analytical line under instrument optimum condition.
(3) sulfur content is carried out to the coal ash sample after low-kappa number using inductively coupled plasma atomic emission spectrometry
Measurement.Coal ash sample after salt low-kappa number constant volume, with inductively coupled plasma atomic emission spectrometry in
180.73nm wavelength measures sulfur content.
Embodiment 3
Test methods of sulphur contents in a kind of coal ash, utilizes low-kappa number combination inductively coupled plasma atomic emission spectrum
The measurement of method progress sulfur content, the specific steps are as follows:
(1) coal ash sample is subjected to low-kappa number；Coal ash sample is specifically subjected to salt low-kappa number.The hydrochloric acid is located in advance
The method of reason are as follows: weigh coal ash sample 0.5000g in beaker, the hydrochloric acid solution 50mL that volume ratio is (1+3) is added, covers table
Face ware is heated to removing after 20min occurs in bubble on electric hot plate, with the filtering of middling speed quantitative filter paper in beaker, with 60 DEG C
Hot water washs 6 times, and liquid to be filtered uses volumetric flask constant volume after being cooled to room temperature.
(2) standard curve is established；Salt low-kappa number identical as step (1) is passed through using coal ash standard substance GBW11128a
Obtain standard solution, inductively coupled plasma atomic emission spectrometer after argon purge, under instrument optimum condition in
182.03nm establishing standard curve at analytical line.
(3) sulfur content is carried out to the coal ash sample after low-kappa number using inductively coupled plasma atomic emission spectrometry
Measurement.Coal ash sample after salt low-kappa number constant volume, with inductively coupled plasma atomic emission spectrometry in
182.03nm wavelength measures sulfur content.
Embodiment 4
Test methods of sulphur contents in a kind of coal ash, utilizes low-kappa number combination inductively coupled plasma atomic emission spectrum
The measurement of method progress sulfur content, the specific steps are as follows:
(1) coal ash sample is subjected to low-kappa number；Coal ash sample is specifically subjected to salt low-kappa number.The hydrochloric acid is located in advance
The method of reason are as follows: weigh coal ash sample 0.2000g in beaker, the hydrochloric acid solution 100mL that volume ratio is (1+3) is added, covers
Surface plate is heated to removing after 20min occurs in bubble on electric hot plate, with the filtering of middling speed qualitative filter paper in beaker, with 80 DEG C
Hot water wash 5 times, liquid to be filtered uses volumetric flask constant volume after being cooled to room temperature.
(2) standard curve is established；3 series standard solution: 0,15mg/L, 30mg/L, electricity are prepared using sulphur standard solution
Coupled plasma-atomic emission spectrometer is felt after argon purge, is built at 182.03nm analytical line under instrument optimum condition
Day-mark directrix curve.
(3) sulfur content is carried out to the coal ash sample after low-kappa number using inductively coupled plasma atomic emission spectrometry
Measurement.Coal ash sample after salt low-kappa number constant volume, with inductively coupled plasma atomic emission spectrometry in
182.03nm wavelength measures sulfur content.
Embodiment 5
Test methods of sulphur contents in a kind of coal ash, utilizes low-kappa number combination inductively coupled plasma atomic emission spectrum
The measurement of method progress sulfur content, the specific steps are as follows:
(1) coal ash sample is subjected to low-kappa number；Specifically coal ash sample progress perchloric acid/hydrofluoric acid/hydrochloric acid is located in advance
Reason, the perchloric acid/pretreated method of hydrofluoric acid/hydrochloric acid are as follows: weigh coal ash 0.1023g in polytetrafluoroethylene (PTFE) crucible, use
2mL perchloric acid and 10mL hydrofluoric acid is added after water wetting, is heated to solution and steams to dry but not burned black, remove natural cooling 5min
Afterwards, 5mL hydrochloric acid and 15mL water is added, is again heated to bubble and occurs and keep the temperature 2min, removing will be molten with water after natural cooling 1min
Liquid is transferred in volumetric flask, is cooled to room temperature rear constant volume.
(2) standard curve is established；Using coal ash standard substance GBW11131a, GBW11128a and GBW11132a pass through with
The identical salt low-kappa number of step (1) obtains standard solution, inductively coupled plasma atomic emission spectrometer after argon purge,
Standard curve is established at 182.03nm analytical line under instrument optimum condition.
(3) sulfur content is carried out to the coal ash sample after low-kappa number using inductively coupled plasma atomic emission spectrometry
Measurement.Coal ash sample after perchloric acid/hydrofluoric acid/salt low-kappa number constant volume, with inductively coupled plasma body atomic emissions
Spectroscopic methodology measures sulfur content in 182.03nm wavelength.
Embodiment 6
Test methods of sulphur contents in a kind of coal ash, utilizes low-kappa number combination inductively coupled plasma atomic emission spectrum
The measurement of method progress sulfur content, the specific steps are as follows:
(1) coal ash sample is subjected to low-kappa number；Specifically coal ash sample progress perchloric acid/hydrofluoric acid/hydrochloric acid is located in advance
Reason, the perchloric acid/pretreated method of hydrofluoric acid/hydrochloric acid are as follows: weigh coal ash 0.1200g in polytetrafluoroethylene (PTFE) crucible, use
2mL perchloric acid and 10mL hydrofluoric acid is added after water wetting, is heated to solution and steams to dry but not burned black, remove natural cooling 1min
Afterwards, 5mL hydrochloric acid and 15mL water is added, is again heated to bubble and occurs and keep the temperature 4min, removing will be molten with water after natural cooling 2min
Liquid is transferred in volumetric flask, is cooled to room temperature rear constant volume.
(2) standard curve is established；7 series standard solution: 0,2mg/L, 4mg/L, 8mg/ are prepared using sulphur standard solution
L, 10mg/L, 20mg/L, 30mg/L, inductively coupled plasma atomic emission spectrometer are best in instrument after argon purge
Under the conditions of establish standard curve at 180.73nm analytical line.
(3) sulfur content is carried out to the coal ash sample after low-kappa number using inductively coupled plasma atomic emission spectrometry
Measurement.Coal ash sample after perchloric acid/hydrofluoric acid/salt low-kappa number constant volume, with inductively coupled plasma body atomic emissions
Spectroscopic methodology measures sulfur content in 180.73nm wavelength.
Embodiment 7
Test methods of sulphur contents in a kind of coal ash, utilizes low-kappa number combination inductively coupled plasma atomic emission spectrum
The measurement of method progress sulfur content, the specific steps are as follows:
(1) coal ash sample is subjected to low-kappa number；Specifically coal ash sample progress perchloric acid/hydrofluoric acid/hydrochloric acid is located in advance
Reason, the perchloric acid/pretreated method of hydrofluoric acid/hydrochloric acid are as follows: weigh coal ash 0.0900g in polytetrafluoroethylene (PTFE) crucible, use
2mL perchloric acid and 10mL hydrofluoric acid is added after water wetting, is heated to solution and steams to dry but not burned black, remove natural cooling 3min
Afterwards, 5mL hydrochloric acid and 15mL water is added, is again heated to bubble and occurs and keep the temperature 20min, removing will be molten with water after natural cooling 5min
Liquid is transferred in volumetric flask, is cooled to room temperature rear constant volume.
(2) standard curve is established；Salt low-kappa number identical as step (1) is passed through using coal ash standard substance GBW11128a
Obtain standard solution, inductively coupled plasma atomic emission spectrometer after argon purge, under instrument optimum condition in
180.73nm establishing standard curve at analytical line.
(3) sulfur content is carried out to the coal ash sample after low-kappa number using inductively coupled plasma atomic emission spectrometry
Measurement.Coal ash sample after perchloric acid/hydrofluoric acid/salt low-kappa number constant volume, with inductively coupled plasma body atomic emissions
Spectroscopic methodology measures sulfur content in 180.73nm wavelength.
Embodiment 8
Test methods of sulphur contents in a kind of coal ash, utilizes low-kappa number combination inductively coupled plasma atomic emission spectrum
The measurement of method progress sulfur content, the specific steps are as follows:
(1) coal ash sample is subjected to low-kappa number；Specifically coal ash sample progress perchloric acid/hydrofluoric acid/hydrochloric acid is located in advance
Reason, the perchloric acid/pretreated method of hydrofluoric acid/hydrochloric acid are as follows: weigh coal ash 0.1200g in polytetrafluoroethylene (PTFE) crucible, use
2mL perchloric acid and 10mL hydrofluoric acid is added after water wetting, is heated to solution and steams to dry but not burned black, remove natural cooling 1min
Afterwards, 5mL hydrochloric acid and 15mL water is added, is again heated to bubble and occurs and keep the temperature 4min, removing will be molten with water after natural cooling 2min
Liquid is transferred in volumetric flask, is cooled to room temperature rear constant volume.
(2) standard curve is established；3 series standard solution: 0,15mg/L, 30mg/L, electricity are prepared using sulphur standard solution
Coupled plasma-atomic emission spectrometer is felt after argon purge, is built at 180.73nm analytical line under instrument optimum condition
Day-mark directrix curve.
(3) sulfur content is carried out to the coal ash sample after low-kappa number using inductively coupled plasma atomic emission spectrometry
Measurement.Coal ash sample after perchloric acid/hydrofluoric acid/salt low-kappa number constant volume, with inductively coupled plasma body atomic emissions
Spectroscopic methodology measures sulfur content in 180.73nm wavelength.
Embodiment 9
Test methods of sulphur contents in coal ash is included the following steps: using sulphur content determination in infrared spectroscopic determination coal ash
(1) establish standard curve: method is using coal ash standard substance GBW11128a single-point calibration, by infrared constant sulphur appliance
1300 DEG C are warming up to, after instrument stabilizer, the oxygen that purity is greater than 99.5% is passed through with 2.8L/min, 0.1200g coal will be housed
The crucible of grey standard substance GBW11128a is pushed into combustion tube flat-temperature zone, and the gas after burning enters infrared through gas purge system
Detection system, coal ash standard substance are measured in parallel twice on infrared constant sulphur appliance, obtain ratio of infrared absorption intensity and sulfur content
Relation curve.
(2) using sulphur content determination in infrared spectroscopic determination coal ash: it is specially that infrared constant sulphur appliance is warming up to 1300 DEG C,
After instrument stabilizer, the oxygen that purity is greater than 99.5% is passed through with 2.8L/min, the crucible equipped with 0.0800g coal ash is pushed into combustion
Pipe flat-temperature zone is burnt, the gas after burning enters infrared detection system through gas purge system, obtains the sulfur content in coal ash.
Embodiment 10
Test methods of sulphur contents in coal ash is included the following steps: using sulphur content determination in infrared spectroscopic determination coal ash
(1) establish standard curve: method is using coal ash standard substance GBW11131a, GBW11128a and GBW11132a
Infrared constant sulphur appliance is warming up to 1320 DEG C by multi-point calibration, after instrument stabilizer, is passed through purity with 3.0L/min and is greater than 99.5%
Crucible equipped with 0.1000g coal ash standard substance is pushed into combustion tube flat-temperature zone by oxygen, and the gas after burning is through gas purification system
System enters infrared detection system, and each coal ash standard substance carries out four parallel determinations on infrared constant sulphur appliance, obtains infrared suction
Receive the relation curve of intensity and sulfur content.
(2) using sulphur content determination in infrared spectroscopic determination coal ash: it is specially that infrared constant sulphur appliance is warming up to 1320 DEG C,
After instrument stabilizer, the oxygen that purity is greater than 99.5% is passed through with 3.0L/min, the crucible equipped with 0.0963g coal ash is pushed into combustion
Pipe flat-temperature zone is burnt, the gas after burning enters infrared detection system through gas purge system, obtains the sulfur content in coal ash.
Embodiment 11
Test methods of sulphur contents in coal ash is included the following steps: using sulphur content determination in infrared spectroscopic determination coal ash
(1) establish standard curve: method be use dead plaster and silica prepare respectively sulfur content for 0.00%,
0.37%, 0.59%, 1.13%, 2.37%, 4.72%, 7.09%, 9.43%, 12% correct mixture, wherein 0.00%
Mixture be spectrum pure silicon dioxide, each correct mixture carries out four times on infrared constant sulphur appliance and is measured in parallel, and single claims
Sample amount is 0.08g, and infrared constant sulphur appliance is warming up to 1300 DEG C, after instrument stabilizer, purity is passed through with 3.5L/min and is greater than
Crucible equipped with 0.08g coal ash standard substance is pushed into combustion tube flat-temperature zone by 99.5% oxygen, and the gas after burning is through gas
Purification system enters infrared detection system, obtains the relation curve of ratio of infrared absorption intensity and sulfur content.
(2) using sulphur content determination in infrared spectroscopic determination coal ash: it is specially that infrared constant sulphur appliance is warming up to 1300 DEG C,
After instrument stabilizer, the oxygen that purity is greater than 99.5% is passed through with 3.5L/min, the crucible equipped with 0.12g coal ash is pushed into burning
Pipe flat-temperature zone, the gas after burning enter infrared detection system through gas purge system, obtain the sulfur content in coal ash.
The method of the present invention accuracy and precision verifying:
The accuracy and essence of salt low-kappa number combination inductively coupled plasma atomic emission spectrometry detection method ICP-AES
Density verifying is as follows:
Six parts of GBW11128a, GBW11129a, GBW11132 and GBW11132a are weighed respectively according to the salt low-kappa number
Replication, six measurements knot are carried out in conjunction with the method for inductively coupled plasma atomic emission spectrometry detection method ICP-AES
Fruit is shown in Table 1, and wherein the standard value and uncertainty of sulphur are converted by sulfur trioxide standard value given in certificate and uncertainty
It arrives.Wherein RSD/% is relative standard deviation.As shown in Table 1, for measurement result deviation in range of uncertainty, it is accurate to meet
Degree measurement requires, and for relative standard deviation within 1%, measurement accuracy is high, meets precision test request.
The test of 1 precision of table
Perchloric acid/hydrofluoric acid/salt low-kappa number combination inductively coupled plasma atomic emission spectrometry detection method ICP-
The accuracy of AES and precision verifying are as follows:
Six parts of coal ash standard substance are weighed respectively according to the perchloric acid/hydrofluoric acid/salt low-kappa number combination inductive coupling
The method of plasma atomic emission spectrometry detection method ICP-AES carries out replication, and measurement result is shown in Table 2.Wherein
RSD/% is relative standard deviation.As shown in Table 2, in range of uncertainty, relative standard deviation exists the equal deviation of measurement result
Within 2%, meet veracity and precision test request.
The test of 2 precision of table
It is as follows using the accuracy of test methods of sulphur contents in infrared spectroscopic determination coal ash and precision verifying:
Six parts of coal ash standard substance are weighed respectively according to the method using sulfur content in infrared spectroscopic determination coal ash
Replication is carried out, measurement result is shown in Table 3.As seen from table, for the equal deviation of measurement result in range of uncertainty, relative standard is inclined
Difference meets veracity and precision test request within 3%.
The test of 3 precision of table
Recovery test
Utilize salt low-kappa number or perchloric acid/hydrofluoric acid/salt low-kappa number combination inductively coupled plasma body atomic emissions
The recovery test of spectroscopic methodology ICP-AES is as follows:
The calcium sulfate of different content is added into coal ash sample 1 and coal ash sample 2, according to it is above-mentioned using salt low-kappa number or
Perchloric acid/hydrofluoric acid/salt low-kappa number combination inductively coupled plasma atomic emission spectrometry carries out the measurement of sulfur content, institute
The rate of recovery of the method for survey is shown in Table 4.As seen from table, perchloric acid/hydrofluoric acid/salt low-kappa number combination inductively coupled plasma body is former
The sub- emission spectrometry ICP-AES detection method rate of recovery is between 98%-103%, salt low-kappa number combination inductively coupled plasma
For the body atomic emission spectrometry ICP-AES detection method rate of recovery between 98%-101%, two methods accuracy is very high.
4 inductively coupled plasma atomic emission spectrometry recovery test of table
Recovery test using sulfur content method in infrared spectroscopic determination coal ash is as follows:
It selects a certain coal ash sample of sulphur to carry out recovery testu, weighs a certain amount of ash sample, be directly added into sample
Different amounts of analytical pure sulfuric acid calcium carries out 6 replications using infra-red sepectrometry, and the method rate of recovery of measuring is shown in Table 5.By measuring
As a result the rate of recovery is in 100%-104% known to.This method accuracy is high.
5 infra-red sepectrometry recovery test of table
Claims (10)
1. test methods of sulphur contents in coal ash, it is characterised in that: sent out using low-kappa number combination inductively coupled plasma body atom
Penetrate the measurement that spectroscopic methodology carries out sulfur content in coal ash, the specific steps are as follows:
(1) coal ash sample to be determined is subjected to low-kappa number；
(2) standard curve is established；
(3) survey of sulfur content is carried out to the coal ash sample after low-kappa number using inductively coupled plasma atomic emission spectrometry
It is fixed.
2. test methods of sulphur contents in coal ash according to claim 1, it is characterised in that: the step (1) is by coal ash sample
Product carry out low-kappa number；The low-kappa number refers to salt low-kappa number or perchloric acid/hydrofluoric acid/salt low-kappa number.
3. test methods of sulphur contents in coal ash according to claim 2, it is characterised in that: the pretreated method of hydrochloric acid
Are as follows: coal ash sample 0.2-0.5g is weighed in beaker, and the hydrochloric acid solution 50-100mL that volume ratio is (1+3), cap upper surface is added
Ware is heated to removing after 20min occurs in bubble on electric hot plate, with filter paper filtering in beaker, with 60-100 DEG C of hot water wash
It washs at least 5 times, liquid to be filtered uses volumetric flask constant volume after being cooled to room temperature.
4. test methods of sulphur contents in coal ash according to claim 3, it is characterised in that: the perchloric acid/hydrofluoric acid/salt
The method of low-kappa number are as follows: weigh coal ash 0.09-0.12g in polytetrafluoroethylene (PTFE) crucible, 2mL perchloric acid is added after being soaked with water
With 10mL hydrofluoric acid, be heated to solution and steam to dry but not burned black, after removing natural cooling at least 1min, be added 5mL hydrochloric acid and
15mL water is again heated to bubble and occurs and keep the temperature 2-5min, removes and solution is transferred to capacity with water after natural cooling at least 1min
In bottle, it is cooled to room temperature rear constant volume.
5. test methods of sulphur contents in coal ash according to claim 4, it is characterised in that: the step (2) establishes standard
Curve method are as follows: using has card coal ash standard substance is acid treated to obtain solution single-point or multi-point calibration, or uses sulphur standard
Solution prepares the series standard solution that at least three sulfur content is 0-30mg/L, inductively coupled plasma atomic emission spectrometer
After argon purge, standard curve is established at 182.03nm or 180.73nm analytical line under instrument optimum condition.
6. test methods of sulphur contents in coal ash according to claim 5, it is characterised in that: the step (3) uses inductance
Coupled plasma-atomic emission spectrometry carries out the measurement of sulfur content to the coal ash sample after low-kappa number, refers to pre- through hydrochloric acid
Coal ash sample to be determined after processing or perchloric acid/hydrofluoric acid/salt low-kappa number constant volume, with inductively coupled plasma body atom hair
It penetrates spectroscopic methodology and measures sulfur content in 182.03nm or 180.73nm wavelength.
7. test methods of sulphur contents in coal ash according to claim 1 to 6, it is characterised in that: the hydrochloric acid is pre-
In the method for processing, coal ash sample 0.2-0.5g is weighed in beaker, and the hydrochloric acid solution 50- that volume ratio is (1+3) is added
100mL, cap upper surface ware are heated to removing after 20min occurs in bubble on electric hot plate, with filter paper filtering in beaker, use 60-
100 DEG C of hot water washs at least 5 times, and liquid to be filtered uses volumetric flask constant volume after being cooled to room temperature；Filter paper therein be middling speed it is qualitative or
Middling speed quantitative filter paper.
8. test methods of sulphur contents in coal ash, it is characterised in that: use sulfur content in infrared spectroscopic determination coal ash, including as follows
Step:
(1) standard curve is established；
(2) using sulfur content in infrared spectroscopic determination coal ash.
9. test methods of sulphur contents in coal ash according to claim 8, it is characterised in that: the step (1) establishes standard
Curve, specially using has card coal ash standard substance single-point or multi-point calibration, or is distinguished using dead plaster and silica
The correct mixture that sulfur content is 0.00%-12.00% is prepared, wherein 0.00% mixture available spectrum pure silicon dioxide,
Each coal ash standard substance or correct mixture are measured in parallel at least twice on infrared constant sulphur appliance, specially will be infrared fixed
Sulphur instrument is warming up to not less than 1300 DEG C, after instrument stabilizer, is passed through the oxygen that purity is greater than 99.5% with 2.8-3.5L/min, will
It is pushed into combustion tube flat-temperature zone equipped with the crucible of 0.08-0.12g coal ash standard substance or correct mixture, the gas after burning is through gas
Body purification system enters infrared detection system, obtains the relation curve of ratio of infrared absorption intensity and sulfur content.
10. test methods of sulphur contents in coal ash according to claim 8 or claim 9, it is characterised in that: the step (2) uses
Infrared constant sulphur appliance is specially warming up to not less than 1300 DEG C by sulfur content in infrared spectroscopic determination coal ash, after instrument stabilizer,
It is passed through the oxygen that purity is greater than 99.5% with 2.8-3.5L/min, the crucible push-in combustion tube equipped with 0.08-0.12g coal ash is permanent
Warm area, the gas after burning enter infrared detection system through gas purge system, obtain the sulfur content in coal ash.
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