CN101907570A - Multi-component spectrometric method for desulphurization gypsum - Google Patents
Multi-component spectrometric method for desulphurization gypsum Download PDFInfo
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- 229910052602 gypsum Inorganic materials 0.000 title claims abstract description 21
- 239000010440 gypsum Substances 0.000 title claims abstract description 21
- 238000004611 spectroscopical analysis Methods 0.000 title claims abstract description 6
- 238000000034 method Methods 0.000 claims abstract description 29
- 238000000120 microwave digestion Methods 0.000 claims abstract description 19
- 238000004458 analytical method Methods 0.000 claims abstract description 8
- 239000000523 sample Substances 0.000 claims description 46
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 24
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 22
- 239000011505 plaster Substances 0.000 claims description 13
- 239000004809 Teflon Substances 0.000 claims description 11
- 229920006362 Teflon® Polymers 0.000 claims description 11
- 239000012496 blank sample Substances 0.000 claims description 10
- 239000007789 gas Substances 0.000 claims description 8
- 238000005303 weighing Methods 0.000 claims description 8
- 238000001816 cooling Methods 0.000 claims description 7
- 238000001228 spectrum Methods 0.000 claims description 6
- 239000004743 Polypropylene Substances 0.000 claims description 5
- 239000012159 carrier gas Substances 0.000 claims description 5
- 230000014759 maintenance of location Effects 0.000 claims description 5
- 230000002572 peristaltic effect Effects 0.000 claims description 5
- -1 polypropylene Polymers 0.000 claims description 5
- 229920001155 polypropylene Polymers 0.000 claims description 5
- 238000002360 preparation method Methods 0.000 claims description 5
- 230000004907 flux Effects 0.000 claims description 2
- 238000005259 measurement Methods 0.000 abstract description 9
- 238000005516 engineering process Methods 0.000 abstract description 7
- 239000003153 chemical reaction reagent Substances 0.000 abstract description 3
- 238000001637 plasma atomic emission spectroscopy Methods 0.000 abstract description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 7
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 6
- 238000002474 experimental method Methods 0.000 description 6
- 239000011734 sodium Substances 0.000 description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 4
- 238000003556 assay Methods 0.000 description 4
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 3
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 3
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 3
- 229910004298 SiO 2 Inorganic materials 0.000 description 3
- 229910010413 TiO 2 Inorganic materials 0.000 description 3
- 239000002253 acid Substances 0.000 description 3
- 239000000654 additive Substances 0.000 description 3
- 230000000996 additive effect Effects 0.000 description 3
- 239000004411 aluminium Substances 0.000 description 3
- 229910052782 aluminium Inorganic materials 0.000 description 3
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 3
- 238000000889 atomisation Methods 0.000 description 3
- 239000011575 calcium Substances 0.000 description 3
- 229910052791 calcium Inorganic materials 0.000 description 3
- 238000011010 flushing procedure Methods 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 229910001385 heavy metal Inorganic materials 0.000 description 3
- 239000011777 magnesium Substances 0.000 description 3
- 229910052749 magnesium Inorganic materials 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 238000012544 monitoring process Methods 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- 239000012498 ultrapure water Substances 0.000 description 3
- 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 description 2
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 2
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 description 2
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 2
- 239000003513 alkali Substances 0.000 description 2
- TZCXTZWJZNENPQ-UHFFFAOYSA-L barium sulfate Chemical compound [Ba+2].[O-]S([O-])(=O)=O TZCXTZWJZNENPQ-UHFFFAOYSA-L 0.000 description 2
- 238000006477 desulfuration reaction Methods 0.000 description 2
- 230000023556 desulfurization Effects 0.000 description 2
- 239000000706 filtrate Substances 0.000 description 2
- 230000004927 fusion Effects 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- 229910017604 nitric acid Inorganic materials 0.000 description 2
- 238000007500 overflow downdraw method Methods 0.000 description 2
- 229910052573 porcelain Inorganic materials 0.000 description 2
- 239000011591 potassium Substances 0.000 description 2
- 229910052700 potassium Inorganic materials 0.000 description 2
- NROKBHXJSPEDAR-UHFFFAOYSA-M potassium fluoride Chemical compound [F-].[K+] NROKBHXJSPEDAR-UHFFFAOYSA-M 0.000 description 2
- 239000000377 silicon dioxide Substances 0.000 description 2
- 229910052708 sodium Inorganic materials 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000011593 sulfur Substances 0.000 description 2
- 229910052717 sulfur Inorganic materials 0.000 description 2
- 238000004448 titration Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 1
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 241001397173 Kali <angiosperm> Species 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- PRKQVKDSMLBJBJ-UHFFFAOYSA-N ammonium carbonate Chemical compound N.N.OC(O)=O PRKQVKDSMLBJBJ-UHFFFAOYSA-N 0.000 description 1
- 235000012501 ammonium carbonate Nutrition 0.000 description 1
- 235000011114 ammonium hydroxide Nutrition 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 230000003009 desulfurizing effect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000000921 elemental analysis Methods 0.000 description 1
- 238000000295 emission spectrum Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000003546 flue gas Substances 0.000 description 1
- 239000008236 heating water Substances 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 238000002386 leaching Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- JKQOBWVOAYFWKG-UHFFFAOYSA-N molybdenum trioxide Chemical compound O=[Mo](=O)=O JKQOBWVOAYFWKG-UHFFFAOYSA-N 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000001103 potassium chloride Substances 0.000 description 1
- 235000011164 potassium chloride Nutrition 0.000 description 1
- 239000011698 potassium fluoride Substances 0.000 description 1
- 235000003270 potassium fluoride Nutrition 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- KKCBUQHMOMHUOY-UHFFFAOYSA-N sodium oxide Chemical compound [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 description 1
- 229910001948 sodium oxide Inorganic materials 0.000 description 1
- 238000002798 spectrophotometry method Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 238000003809 water extraction Methods 0.000 description 1
Landscapes
- Investigating, Analyzing Materials By Fluorescence Or Luminescence (AREA)
Abstract
The invention relates to a multi-component spectrometric method for desulphurization gypsum. A microwave digestion method is adopted for pretreating gypsum, and the element measurement adopts high-precision wide-measurement range plasma-atomic emission spectrometry. Therefore, the multi-component spectrometric method has the characteristics of short measurement time, a few instruments, simple process and technology, low sample demand, and the like. The microwave digestion technology makes the pretreatment time and element analysis and measurement time of the gypsum sample shortened by 90 percent and makes the reagent dosage reduced by 95 percent. The microwave digestion method is implemented under the sealed condition, so the laboratory pollution is reduced to the greatest degree. By measuring various elements by the plasma-atomic emission spectrometry technology, multiple element kinds are measured, the range of the measured elements is multiplied, and the element concentration can be measured at one time from ppm to percentage content.
Description
Technical field
Patent of the present invention relates to a kind of multi-component spectrometric method of desulfurated plaster.
Background technology
The chemical composition of gypsum is measured the conventional GB/T5484-2000 of employing, and the sample pretreatment of this method is measured element according to difference and adopted multiple different disposal method respectively, adopts hydrochloric acid heating for dissolving, barium sulfate precipitate gravimetric determination as elementary sulfur.Several elements such as calcium, magnesium and aluminium will adopt muffle furnace high temperature hydrogen sodium oxide molybdena alkali fusion method, be that sample adds behind the NaOH high-temperature fusion in muffle furnace, leach with boiling water, add hydrochloric acid and nitric acid heating for dissolving sample under constantly stirring again, measure calcium, magnesium and aluminium respectively with the EDTA titrimetry, with spectrophotometry elemental iron, titanium and phosphorus.The mensuration of elemental silicon also needs the individual processing sample, need to adopt muffle furnace high temperature hydrogen kali alkali fusion method, be that sample adds behind the potassium hydroxide high-temperature fusion in muffle furnace, the heating water extraction, add nitric acid, potassium fluoride and potassium chloride, through precipitation, filtration, filtrate is obtained the content of silicon dioxide with the NaOH titration.The mensuration of element potassium and sodium also is that more complicated and error are bigger, promptly sample through hydrofluorite-sulfuric acid evaporation silica removal after with the hot water leaching, to filter behind ammoniacal liquor and hartshorn salt separation of iron, aluminium, calcium, the magnesium, with potassium and the sodium in the flame spectrophotometer measuring filtrate.The process of above assay method is very loaded down with trivial details, and analytical cycle is long, and the instrument and the reagent that need are a lot, and error at measurment is bigger, usually can not satisfy on-the-spot real work requirement.
Along with the fast development of coal-fired plant flue gas desulfurization industry, as the quality of the gypsum of desulfurizing byproduct and economy, society and the environmental benefit that output will directly influence power plant.Power plant is a desulfurated plaster through the accessory substance that produces after the desulfurization, its physicochemical characteristics is compared with common gypsum bigger variation, the change of component of desulfurated plaster and the sulfur removal technology of power plant, operational factor control have direct confidential relation, therefore, the product gypsum under different operational systems, the different operational factor has characteristic inequality.Timely Adjustment System operation conditions and parameter are convenient in the various elementary compositions of assay determination desulfurated plaster rapidly and accurately, can guarantee the high-quality of gypsum to greatest extent, strive for economic benefit to greatest extent.
But at present not at the examination criteria of desulfurated plaster, in the work all the method with reference to common gypsum carry out, and the assay method of employing common gypsum, the mensuration cycle is long, process is loaded down with trivial details, can not satisfy the production actual needs.
Summary of the invention
Technical matters to be solved by this invention provides a kind of method of spectroscopic methodology fast measuring gypsum component.
The technical solution used in the present invention is that the optical spectrum rapid measuring method of gypsum component comprises the steps:
The present invention adopts following method step:
(1) gets 3-5g gypsum to be measured, heat 60min down, accurately take by weighing 0.0500g～0.1000g after the cooling as analytic sample at 230 ℃～235 ℃;
(2) analytic sample is positioned in the teflon of counteracting tank in the pipe, add concentrated hydrochloric acid 1.9～2.1ml, shake up the back and add red fuming nitric acid (RFNA) 3.9～4.1ml, add hydrofluorite 0.4～0.6ml at last, in temperature is 210 ℃～230 ℃, pressure is under 6000kPa～8000kPa and the airtight situation analytic sample to be carried out micro-wave digestion, micro-wave digestion adopts the power gradient method, the condition of clearing up is 10～15 minutes gradient time, 30～45 minutes retention times, force 10～15 minutes cool times, microwave power is 800W～1000W, the rate of rise is 20kPa/s～30kPa/s, and the highest pressure limiting is 6000kPa～8000kPa, naturally cools to room temperature after clearing up fully, obtain clearing up sample, described concentrated hydrochloric acid, red fuming nitric acid (RFNA), hydrofluorite is to be analyzed pure or top grade is pure;
(3) adopting massfraction is that 2%～3% salpeter solution will above-mentionedly be cleared up in the polypropylene volumetric flask that sample all is transferred to 25ml or 50ml, and accurate constant volume gets analytical solution;
(4) a omnidistance preface blank sample solution of preparation, promptly adopt above-mentioned (2), (3) step method is except sample without analyse, other step method all and (2), (3) the identical and solution that obtains, with blank sample solution serves as that each components contents in the full spectrum direct-reading plasma emission spectrometer determination and analysis solution is adopted in contrast, condition determination is: echelle grating, the pouring-in monitor of CID electric charge, radio-frequency generator operating power 1150W, the ICP frequency is 27.12MHZ, carrier gas flux 0.9L/min～1.1L/min, secondary air amount 0.9L/min～1.1L/min, plasma gas flow rate 0.9L/min～1.1L/min, sample size 1.80ml/min～1.90ml/min, atomizer pressure are 187kPa～199kPa, peristaltic pump rotating speed 129r/min～131r/min.
Employing the invention has the beneficial effects as follows: the present invention has adopted Microwave Digestion for the pre-service of gypsum, high precision, measurement range plasma emission spectrometry has widely been adopted in element determination, thereby it is short to have had a minute, characteristics such as used instrument and equipment is few, and process and technology are simple, the sample requirement is few.Microwave digestion technology of the present invention makes the pretreatment time of gypsum samples and determination of elemental analysis time all shorten 90%, and reagent dosage has reduced 95%.Because the Microwave Digestion that the present invention adopts is carried out in confined conditions, thus farthest reduced breadboard pollution, concerning laboratory environment and experimenter, all be ten parts useful.The various elements of plasma emission spectrum technical measurement that the present invention adopts, not only the element kind of Ce Dinging is many, and the scope of mensuration element also enlarged several times, and the concentration of element all can once be measured from ppm to the percentage composition and finish.Therefore adopt the inventive method can rapid and accurate determination to go out the content of multiple metal, nonmetalloid in desulfurated plaster or the common gypsum.
Assay method of the present invention both had been applicable to desulfurated plaster, also was applicable to have enlarged range of application by common gypsum.
Embodiment
Embodiment 1
Method step of the present invention is:
At first before the experiment beginning, all vessel of using all soaked 24 hours with high purity water, and dry back is standby.
(1) takes by weighing through 230 ℃～235 ℃ following heating 60min, cooled common gypsum sample 0.0500g (being accurate to 0.0001g) as analytic sample.
(2) the 0.0500g analytic sample that takes by weighing carefully is positioned in the teflon of counteracting tank in the pipe, carefully adds concentrated hydrochloric acid 2.0ml, red fuming nitric acid (RFNA) 4.0ml, dense hydrofluorite 0.4ml successively, note: will shake up gently after a kind of acid of every adding along tube wall; Add fashionable will solid sample the flushing in the solution along tube wall, employed concentrated hydrochloric acid, red fuming nitric acid (RFNA), dense hydrofluorite are to be analyzed pure or top grade is pure; Pipe in the teflon is put into the micro-wave digestion device, setting the highest monitoring temperature and be 210 ℃, maximum controlled pressure pressure is under the condition of 6000kPa, under airtight situation analytic sample is carried out micro-wave digestion, and micro-wave digestion adopts the power gradient method, the condition of clearing up is 15 minutes gradient time, 30 minutes retention times, force cooling 15 minutes, microwave power is 1000W, the rate of rise is 20kPa/s, the highest pressure limiting is 6000kPa, naturally cools to room temperature after clearing up fully, obtains clearing up sample;
(3) to adopt massfraction be 2% salpeter solution with in the pipe in the teflon clear up sample comprise drop in the lid to all be transferred in the polypropylene volumetric flask of 25ml and accurately constant volume get analytical solution;
To prepare a omnidistance preface blank sample solution in the time of specimen preparation, promptly except sample without analyse, all identical and solution that obtains of additive method step with above-mentioned (2), (3).
With the solution behind the constant volume according to the instrument parameter of the best and experiment condition and blank sample solution to impinging upon the mensuration of carrying out various components on the full spectrum direct-reading plasma emission spectrometer.Each parameter of instrument is: echelle grating, the pouring-in monitor of CID electric charge, radio-frequency generator operating power 1150W, the ICP frequency is 27.12MHZ, carrier gas (atomization gas) flow 0.9L/min, secondary air amount 1.1L/min, plasma gas flow rate 0.9L/min, sample size 1.80ml/min, atomizer pressure are 199Kpa, peristaltic pump rotating speed 131r/min.
Each element determination result is as follows:
The measurement result of each element of common gypsum (mg/g)
| Macroelement | Measured value of the present invention | Heavy metal element | Measured value of the present invention |
| K 2O | 0.078 | SiO 2 | 4.372 |
| Na 2O | 0.019 | AL 2O 3 | 0.418 |
| CaO | 36.60 | TiO 2 | 0.105 |
| MgO | 0.079 | SO 3 | 56.24 |
| Fe 2O 3 | 1.156 |
Embodiment 2
Method step of the present invention is:
At first before the experiment beginning, all vessel of using all soaked 24 hours with high purity water, and dry back is standby.
(1) desulfurated plaster is got 5g and placed porcelain boat to heat 60min down, take by weighing 0.1000g (being accurate to 0.0001g) after the cooling as analytic sample at 230 ℃～235 ℃.
(2) the 0.1000g analytic sample that takes by weighing carefully is positioned in the teflon of counteracting tank of dried and clean in the pipe, carefully add concentrated hydrochloric acid 1.9ml, red fuming nitric acid (RFNA) 4.1ml, dense hydrofluorite 0.5ml successively along tube wall, note: will shake up gently after a kind of acid of every adding; Add fashionable will solid sample the flushing in the solution along tube wall, employed concentrated hydrochloric acid, red fuming nitric acid (RFNA), dense hydrofluorite is to be analyzed pure or top grade is pure, pipe in the teflon is put into the micro-wave digestion device, setting the highest monitoring temperature is 230 ℃, maximum controlled pressure is 8000kPa and under airtight situation analytic sample is carried out micro-wave digestion, micro-wave digestion adopts the power gradient method, the condition of clearing up is 10 minutes gradient time, 45 minutes retention times, force cooling 10 minutes, microwave power is 800W, and the rate of rise is 30kPa/s, and the highest pressure limiting is 8000kPa, naturally cool to room temperature after clearing up fully, obtain clearing up sample;
(3) to adopt massfraction be 3% salpeter solution with in the pipe in the teflon clear up sample comprise drop in the lid to all be transferred in the polypropylene volumetric flask of 50ml and accurately constant volume get analytical solution;
To prepare a omnidistance preface blank sample solution in the time of specimen preparation, promptly except sample without analyse, all identical and solution that obtains of additive method step with above-mentioned (2), (3).
With the solution behind the constant volume according to the instrument parameter of the best and experiment condition and blank sample solution to impinging upon the mensuration of carrying out various components on the full spectrum direct-reading plasma emission spectrometer.Each parameter of instrument is: echelle grating, the pouring-in monitor of CID electric charge, radio-frequency generator operating power 1150W, the ICP frequency is 27.12MHZ, carrier gas (atomization gas) flow 1.1L/min, secondary air amount 0.9L/min, plasma gas flow rate 1.1L/min, sample size 1.90m l/min, atomizer pressure are 187Kpa, peristaltic pump rotating speed 129r/min.Each element determination result is as follows:
The measurement result of each element of desulfurated plaster (mg/g)
| Macroelement | Measured value of the present invention | Heavy metal element | Measured value of the present invention |
| K 2O | 0.076 | SiO 2 | 0.526 |
| Na 2O | 0.021 | AL 2O 3 | 0.268 |
| CaO | 45.61 | TiO 2 | 0.144 |
| MgO | 1.064 | SO 3 | 51.35 |
| Fe 2O 3 | 0.532 |
Embodiment 3
Step of the present invention is:
At first before the experiment beginning, all vessel of using all soaked 24 hours with high purity water, and dry back is standby.
(1) desulfurated plaster is got 5g and placed porcelain boat to heat 60min down, take by weighing 0.1000g (being accurate to 0.0001g) after the cooling as analytic sample at 230 ℃～235 ℃.
(2) the 0.1000g analytic sample that takes by weighing carefully is positioned in the teflon of counteracting tank of dried and clean in the pipe, carefully add concentrated hydrochloric acid 2.0ml, red fuming nitric acid (RFNA) 3.9ml, dense hydrofluorite 0.6ml successively along tube wall, note: will shake up gently after a kind of acid of every adding; Add fashionable will solid sample the flushing in the solution along tube wall, employed concentrated hydrochloric acid, red fuming nitric acid (RFNA), dense hydrofluorite is to be analyzed pure or top grade is pure, pipe in the teflon is put into the micro-wave digestion device, setting the highest monitoring temperature is 220 ℃, maximum controlled pressure is 7000kPa and under airtight situation analytic sample is carried out micro-wave digestion, micro-wave digestion adopts the power gradient method, the condition of clearing up is 13 minutes gradient time, 38 minutes retention times, force cooling 12 minutes, microwave power is 900W, and the rate of rise is 25kPa/s, and the highest pressure limiting is 7000kPa, naturally cool to room temperature after clearing up fully, obtain clearing up sample;
(3) to adopt massfraction be 2.5% salpeter solution with in the pipe in the teflon clear up sample comprise drop in the lid to all be transferred in the polypropylene volumetric flask of 50ml and accurately constant volume get analytical solution;
To prepare a omnidistance preface blank sample solution in the time of specimen preparation, promptly except sample without analyse, all identical and solution that obtains of additive method step with above-mentioned (2), (3).
With the solution behind the constant volume according to the instrument parameter of the best and experiment condition and blank sample solution to impinging upon the mensuration of carrying out various components on the full spectrum direct-reading plasma emission spectrometer.Each parameter of instrument is: echelle grating, the pouring-in monitor of CID electric charge, radio-frequency generator operating power 1150W, the ICP frequency is 27.12MHZ, carrier gas (atomization gas) flow 1.0L/min, secondary air amount 1.0L/min, plasma gas flow rate 1.0L/min, sample size 1.85m l/min, atomizer pressure are 193Kpa, peristaltic pump rotating speed 130r/min.Each element determination result is as follows:
The measurement result of each element of desulfurated plaster (mg/g)
| Macroelement | Measured value of the present invention | Heavy metal element | Measured value of the present invention |
| K 2O | 0.104 | SiO 2 | 0.871 |
| Na 2O | 0.033 | AL 2O 3 | 0.315 |
| CaO | 43.98 | TiO 2 | 0.130 |
| MgO | 1.128 | SO 3 | 52.79 |
| Fe 2O 3 | 0.565 |
Claims (1)
1. the multi-component spectrometric method of a desulfurated plaster is characterized in that it adopts following method step:
(1) gets 3-5g gypsum to be measured, heat 60min down, accurately take by weighing 0.0500g～0.1000g after the cooling as analytic sample at 230 ℃～235 ℃;
(2) analytic sample is positioned in the teflon of counteracting tank in the pipe, add concentrated hydrochloric acid 1.9～2.1ml, shake up the back and add red fuming nitric acid (RFNA) 3.9～4.1ml, add hydrofluorite 0.4～0.6ml at last, in temperature is 210 ℃～230 ℃, pressure is under 6000kPa～8000kPa and the airtight situation analytic sample to be carried out micro-wave digestion, micro-wave digestion adopts the power gradient method, the condition of clearing up is 10～15 minutes gradient time, 30～45 minutes retention times, force 10～15 minutes cool times, microwave power is 800W～1000W, the rate of rise is 20kPa/s～30kPa/s, and the highest pressure limiting is 6000kPa～8000kPa, naturally cools to room temperature after clearing up fully, obtain clearing up sample, described concentrated hydrochloric acid, red fuming nitric acid (RFNA), hydrofluorite is to be analyzed pure or top grade is pure;
(3) adopting massfraction is that 2%～3% salpeter solution will above-mentionedly be cleared up in the polypropylene volumetric flask that sample all is transferred to 25ml or 50ml, and accurate constant volume gets analytical solution;
(4) a omnidistance preface blank sample solution of preparation, promptly adopt above-mentioned (2), (3) step method is except sample without analyse, other step method all and (2), (3) the identical and solution that obtains, with blank sample solution serves as that each components contents in the full spectrum direct-reading plasma emission spectrometer determination and analysis solution is adopted in contrast, condition determination is: echelle grating, the pouring-in monitor of CID electric charge, radio-frequency generator operating power 1150W, the ICP frequency is 27.12MHZ, carrier gas flux 0.9L/min～1.1L/min, secondary air amount 0.9L/min～1.1L/min, plasma gas flow rate 0.9L/min～1.1L/min, sample size 1.80ml/min～1.90ml/min, atomizer pressure are 187kPa～199kPa, peristaltic pump rotating speed 129r/min～131r/min.
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| CN105758845A (en) * | 2016-03-03 | 2016-07-13 | 山东省第八地质矿产勘查院 | Method for determining sulfur trioxide in gypsum employing inductive coupled plasma emission spectrometer |
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| CN110487758A (en) * | 2019-08-15 | 2019-11-22 | 华北电力大学 | A method of arsenic, selenium, lead in measurement coal-burning power plant's coal and its combustion by-products |
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| CN110487758B (en) * | 2019-08-15 | 2021-05-14 | 华北电力大学 | Method for measuring arsenic, selenium and lead in coal-fired power plant coal and combustion byproducts thereof |
| CN113640399A (en) * | 2021-06-24 | 2021-11-12 | 广东一方制药有限公司 | Method for measuring element content in gypsum standard decoction |
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