CN103344626A - Rapid analysis method for component of coal ash - Google Patents
Rapid analysis method for component of coal ash Download PDFInfo
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- CN103344626A CN103344626A CN2013102442026A CN201310244202A CN103344626A CN 103344626 A CN103344626 A CN 103344626A CN 2013102442026 A CN2013102442026 A CN 2013102442026A CN 201310244202 A CN201310244202 A CN 201310244202A CN 103344626 A CN103344626 A CN 103344626A
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Abstract
The invention discloses a rapid analysis method for components of coal ash. The rapid analysis method comprises the following steps of weighing a proper amount of a sample; sealing a digestion tank with a cover; digesting the sample; then adding 4% boric acid, sealing the digestion tank with the cover; digesting; diluting to a constant volume scale; preparing a blank solution; preparing a mixed standard solution; zero setting an ICP-OES spectrometer by using the blank solution; conversing into percentages of each component of the coal ash. The rapid analysis method is characterized in that the coal ash sample is firstly subjected to the digestion and then analyzed by using an ICP-OES method after the coal ash sample is prepared, all results of total analysis for the components of the coal ash can be obtained within four hours analysis time. A standard coal ash sample is used to prepare the standard solution, so that perfect matching of the standard solution and the sample solution is realized easily and various complex procedures and a lot of work for preparing a plurality of standard solutions in chemical analysis of a national standard method, thereby greatly saving time, cost and manpower, increasing analysis efficiency and shortening analysis period.
Description
Technical field
The present invention relates to the components of coal ash rapid analysis, belong to the analysis test method technical field.
Background technology
Coal evaporates moisture through perfect combustion, discharges heat, and the organism that remaining inorganic mineral and some contain metal just forms residue, and these residues are exactly ash content.Components of coal ash is very complicated, mainly is made up of oxide and the salt of elements such as silicon, aluminium, iron, calcium, magnesium, titanium, sulphur, potassium, sodium, phosphorus, manganese.Along with development of science and technology, the introduction of advanced technology, each pulls up Coal Chemical Industry horizontally in China, becomes the fresh combatants of chemical enterprise rapidly, has promoted China's economic development.This makes that also the consumption of coal is huge day by day, and the discharging of coal ash also increases day by day, and the constituent analysis of coal ash also seems particularly important under this megatrend.The constituent analysis of coal ash can not only be instructed explained hereafter coal blending ratio, prevents coal ash fouling, etching apparatus pipeline, can also turn waste into wealth coal ash according to the content of components of coal ash, and many-sided the utilization reduced environmental pollution.Have so a kind of fast, simply, the coal ash analysis method just becomes at the moment the task of top priority accurately.
In existing national standard coal ash analysis method, the coal ash sample needs 10 analysts at least, just can make through fusing sample more than three times can be for the solution of analyzing, analyze 8 hours through methods such as gravimetric method, volumetric method, compleximetry, spectrophotometric method, flame photometry, coulometric titrations again and just can obtain final result, wherein also need prepare the standard solution of various compositions, extensive works such as production standard curve.This process is length consuming time not only, and efficient is low, and running program is various, and the error probability is bigger, has been difficult to satisfy modern production technology to accurate express-analysis result's needs.
Summary of the invention
The object of the present invention is to provide that a kind of analysis speed is fast, result's coal ash analysis method accurately, can save time, cost and manpower, improve analysis efficiency, shorten analytical cycle.
The objective of the invention is to be achieved through the following technical solutions: the components of coal ash rapid analysis, it comprises following steps:
(1), preparation coal ash sample: place the muffle furnace calcination to constant weight the pulverized coal sample of grain size 0.1-0.3mm, heating-up temperature 800-900 ℃, obtain the coal ash sample, take out that to be cooled to the room temperature pack standby;
(2), take by weighing coal ash sample 0.08g-0.1g and put into the teflon counteracting tank;
(3), in counteracting tank, add 3-10ml red fuming nitric acid (RFNA), 1-2ml hydrofluorite, 1-3ml hydrogen peroxide successively;
(4), seal counteracting tank, in microwave dissolver, cleared up 15～30 minutes in 150-200 ℃;
(5), then after being cooled to the counteracting tank taking-up below 80 ℃, opening gland bonnet and add 10-20ml4% boric acid again;
(6), again seal counteracting tank, in microwave dissolver, continued to clear up 15～30 minutes in 120-180 ℃;
(7), go out counteracting tank and be cooled to below 80 ℃ after, uncap and transfer in the 250ml capacity, be settled to scale;
(8), the preparation of blank solution: use high purity water as analysis margin solution;
(9), the preparation of mixed standard solution: mixed standard solution obtains after by above-mentioned (3)～(7) step process for the standard coal equivalent ash sample that accurately takes by weighing identical weight;
(10), on the ICP-OES spectrometer with blank solution zeroing, with mixed standard solution production standard curve, measure the content of various compositions in the ash sample solution by typical curve, and be scaled the percentage composition of each composition in the coal ash.
Beneficial effect of the present invention is: after the coal ash specimen preparation is good, clear up earlier and use the analysis of ICP-OES method again, 1 people can obtain all results of components of coal ash total analysis in 4 hour analysis time, with standard coal equivalent ash sample production standard solution, easily realize the perfect coupling of standard solution and sample solution, the extensive work that has saved chemico-analytic various numerous and diverse formalities and preparation multiple standards solution in the national standard method, time, cost and manpower have been saved greatly, improve analysis efficiency, shortened analytical cycle.
Embodiment
Further describe technical scheme of the present invention below in conjunction with embodiment, but that claimed scope is not limited to is described.
Embodiment 1
The components of coal ash rapid analysis, it comprises following steps:
(1), preparation coal ash sample: place the muffle furnace calcination to constant weight the pulverized coal sample of grain size 0.2mm, 815 ℃ of heating-up temperatures obtain the coal ash sample, and it is standby that taking-up is cooled to the room temperature pack;
(2), take by weighing coal ash sample 0.091g and put into the teflon counteracting tank;
(3), in counteracting tank, add 5ml red fuming nitric acid (RFNA), 1.2ml hydrofluorite, 2ml hydrogen peroxide successively;
(4), seal counteracting tank, in microwave dissolver, cleared up 15 minutes in 170 ℃;
(5), then after the counteracting tank taking-up being cooled to 70 ℃, opening gland bonnet and add 15ml4% boric acid again;
(6), again seal counteracting tank, in microwave dissolver, continued to clear up under 150 ℃ 15 minutes;
(7), go out counteracting tank and be cooled to 70 ℃, uncap and transfer in the 250ml capacity, be settled to scale;
(8), the preparation of blank solution: use high purity water as analysis margin solution;
(9), the preparation of mixed standard solution: mixed standard solution obtains after by above-mentioned (3)～(7) step process for the standard coal equivalent ash sample that accurately takes by weighing identical weight;
(10), on the ICP-OES spectrometer with blank solution zeroing, with mixed standard solution production standard curve, measure the content of various compositions in the ash sample solution by typical curve, and be scaled the percentage composition of each composition in the coal ash, its analysis result sees Table one.
Table one ICP-OES method ash sample is analyzed comparing result one
Embodiment 2
The components of coal ash rapid analysis, it comprises following steps:
(1), preparation coal ash sample: place the muffle furnace calcination to constant weight the pulverized coal sample of grain size 0.2mm, 815 ℃ of heating-up temperatures obtain the coal ash sample, and it is standby that taking-up is cooled to the room temperature pack;
(2), take by weighing coal ash sample 0.092g and put into the teflon counteracting tank;
(3), in counteracting tank, add 5ml red fuming nitric acid (RFNA), 1.4ml hydrofluorite, 2ml hydrogen peroxide successively;
(4), seal counteracting tank, in microwave dissolver, cleared up 15 minutes in 170 ℃;
(5), then after the counteracting tank taking-up being cooled to 80 ℃, opening gland bonnet and add 15ml4% boric acid again;
(6), again seal counteracting tank, 150 ℃ were continued to clear up 15 minutes in microwave dissolver;
(7), go out counteracting tank and be cooled to 80 ℃, uncap and transfer in the 250ml capacity, be settled to scale;
(8), the preparation of blank solution: use high purity water as analysis margin solution;
(9), the preparation of mixed standard solution: mixed standard solution obtains after by above-mentioned (3)～(7) step process for the standard coal equivalent ash sample that accurately takes by weighing identical weight;
(10), on the ICP-OES spectrometer with blank solution zeroing, with mixed standard solution production standard curve, measure the content of various compositions in the ash sample solution by typical curve, and be scaled the percentage composition of each composition in the coal ash, its analysis result sees Table two.
Table two ICP-OES method ash sample is analyzed comparing result two
Embodiment 3
The components of coal ash rapid analysis, it comprises following steps:
(1), preparation coal ash sample: place the muffle furnace calcination to constant weight the pulverized coal sample of grain size 0.2mm, 815 ℃ of heating-up temperatures obtain the coal ash sample, and it is standby that taking-up is cooled to the room temperature pack;
(2), take by weighing coal ash sample 0.093g and put into the teflon counteracting tank;
(3), in counteracting tank, add 5ml red fuming nitric acid (RFNA), 1.3ml hydrofluorite, 2ml hydrogen peroxide successively;
(4), seal counteracting tank, in microwave dissolver, cleared up 15 minutes in 180 ℃;
(5), then after the counteracting tank taking-up being cooled to 75 ℃, opening gland bonnet and add 15ml4% boric acid again;
(6), again seal counteracting tank, in microwave dissolver, continued to clear up under 150 ℃ 15 minutes;
(7), go out counteracting tank and be cooled to 75 ℃, uncap and transfer in the 250ml capacity, be settled to scale;
(8), the preparation of blank solution: use high purity water as analysis margin solution;
(9), the preparation of mixed standard solution: mixed standard solution obtains after by above-mentioned (3)～(7) step process for the standard coal equivalent ash sample that accurately takes by weighing identical weight;
(10), on the ICP-OES spectrometer with blank solution zeroing, with mixed standard solution production standard curve, measure the content of various compositions in the ash sample solution by typical curve, and be scaled the percentage composition of each composition in the coal ash, its analysis result sees Table three.
Table three ICP-OES method ash sample is analyzed comparing result three
Embodiment 4
The components of coal ash rapid analysis, it comprises following steps:
(1), preparation coal ash sample: place the muffle furnace calcination to constant weight the pulverized coal sample of grain size 0.1mm, 800 ℃ of heating-up temperatures obtain the coal ash sample, and it is standby that taking-up is cooled to the room temperature pack;
(2), take by weighing coal ash sample 0.08g and put into the teflon counteracting tank;
(3), in counteracting tank, add 3ml red fuming nitric acid (RFNA), 1ml hydrofluorite, 1ml hydrogen peroxide successively;
(4), seal counteracting tank, in microwave dissolver, cleared up 30 minutes in 150 ℃;
(5), then counteracting tank is taken out and be cooled to 65 ℃, open gland bonnet and add 10ml4% boric acid again;
(6), again seal counteracting tank, in microwave dissolver, continued to clear up under 120 ℃ 30 minutes;
(7), go out counteracting tank and be cooled to 65 ℃, uncap and transfer in the 250ml capacity, be settled to scale;
(8), the preparation of blank solution: use high purity water as analysis margin solution;
(9), the preparation of mixed standard solution: mixed standard solution obtains after by above-mentioned (3)～(7) step process for the standard coal equivalent ash sample that accurately takes by weighing identical weight;
(10), on the ICP-OES spectrometer with blank solution zeroing, with mixed standard solution production standard curve, measure the content of various compositions in the ash sample solution by typical curve, and be scaled the percentage composition of each composition in the coal ash.
Embodiment 5
The components of coal ash rapid analysis, it comprises following steps:
(1), preparation coal ash sample: place the muffle furnace calcination to constant weight the pulverized coal sample of grain size 0.3mm, 900 ℃ of heating-up temperatures obtain the coal ash sample, and it is standby that taking-up is cooled to the room temperature pack;
(2), take by weighing coal ash sample 0.1g and put into the teflon counteracting tank;
(3), in counteracting tank, add 6ml red fuming nitric acid (RFNA), 2ml hydrofluorite, 3ml hydrogen peroxide successively;
(4), seal counteracting tank, in microwave dissolver, cleared up 20 minutes in 200 ℃;
(5), then counteracting tank is taken out and be cooled to 65 ℃, open gland bonnet and add 20ml4% boric acid again;
(6), again seal counteracting tank, in microwave dissolver, continued to clear up under 150 ℃ 20 minutes;
(7), go out counteracting tank and be cooled to 65 ℃, uncap and transfer in the 250ml capacity, be settled to scale;
(8), the preparation of blank solution: use high purity water as analysis margin solution;
(9), the preparation of mixed standard solution: mixed standard solution obtains after by above-mentioned (3)～(7) step process for the standard coal equivalent ash sample that accurately takes by weighing identical weight;
(10), on the ICP-OES spectrometer with blank solution zeroing, with mixed standard solution production standard curve, measure the content of various compositions in the ash sample solution by typical curve, and be scaled the percentage composition of each composition in the coal ash.
Embodiment 6
The components of coal ash rapid analysis, it comprises following steps:
(1), preparation coal ash sample: place the muffle furnace calcination to constant weight the pulverized coal sample of grain size 0.2mm, 850 ℃ of heating-up temperatures obtain the coal ash sample, and it is standby that taking-up is cooled to the room temperature pack;
(2), take by weighing coal ash sample 0.083g and put into the teflon counteracting tank;
(3), in counteracting tank, add 10ml red fuming nitric acid (RFNA), 1.5ml hydrofluorite, 2ml hydrogen peroxide successively;
(4), seal counteracting tank, in microwave dissolver, cleared up 20 minutes in 190 ℃;
(5), then counteracting tank is taken out and be cooled to 75 ℃, open gland bonnet and add 20ml4% boric acid again;
(6), again seal counteracting tank, in microwave dissolver, continued to clear up under 180 ℃ 25 minutes;
(7), go out counteracting tank and be cooled to 65 ℃, uncap and transfer in the 250ml capacity, be settled to scale;
(8), the preparation of blank solution: use high purity water as analysis margin solution;
(9), the preparation of mixed standard solution: mixed standard solution obtains after by above-mentioned (3)～(7) step process for the standard coal equivalent ash sample that accurately takes by weighing identical weight;
(10), on the ICP-OES spectrometer with blank solution zeroing, with mixed standard solution production standard curve, measure the content of various compositions in the ash sample solution by typical curve, and be scaled the percentage composition of each composition in the coal ash.
Claims (1)
1. components of coal ash rapid analysis, it is characterized in that: it comprises following steps:
(1), preparation coal ash sample: place the muffle furnace calcination to constant weight the pulverized coal sample of grain size 0.1-0.3mm, heating-up temperature 800-900 ℃, obtain the coal ash sample, take out that to be cooled to the room temperature pack standby;
(2), take by weighing coal ash sample 0.08g-0.1g and put into the teflon counteracting tank;
(3), in counteracting tank, add 3-10ml red fuming nitric acid (RFNA), 1-2ml hydrofluorite, 1-3ml hydrogen peroxide successively;
(4), seal counteracting tank, in microwave dissolver, cleared up 15～30 minutes in 150-200 ℃;
(5), then after being cooled to the counteracting tank taking-up below 80 ℃, opening gland bonnet and add 10-20ml4% boric acid again;
(6), again seal counteracting tank, in microwave dissolver, continued to clear up 15～30 minutes in 120-180 ℃;
(7), go out counteracting tank and be cooled to below 80 ℃ after, uncap and transfer in the 250ml capacity, be settled to scale;
(8), the preparation of blank solution: use high purity water as analysis margin solution;
(9), the preparation of mixed standard solution: mixed standard solution obtains after by above-mentioned (3)～(7) step process for the standard coal equivalent ash sample that accurately takes by weighing identical weight;
(10), on the ICP-OES spectrometer with blank solution zeroing, with mixed standard solution production standard curve, measure the content of various compositions in the ash sample solution by typical curve, and be scaled the percentage composition of each composition in the coal ash.
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Cited By (7)
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| CN104914090A (en) * | 2015-05-08 | 2015-09-16 | 广东省矿产应用研究所 | Detection method for continuously measuring Ga, In and Ge In lead-zinc smelting smoke dust through microwave digestion-ICP-OES |
| CN108152272A (en) * | 2017-12-28 | 2018-06-12 | 中建材蚌埠玻璃工业设计研究院有限公司 | The standard solution and its preparation method that micronutrient levels detects in quartz sand |
| CN109632770A (en) * | 2018-12-14 | 2019-04-16 | 湖北省兴发磷化工研究院有限公司 | A method of metal ion content in measurement glyphosate waste liquor |
| CN110954391A (en) * | 2019-12-24 | 2020-04-03 | 陕西华邦检测服务有限公司 | Digestion tank for monitoring pretreatment of elements in soil and application |
| CN112098394A (en) * | 2019-06-18 | 2020-12-18 | 新疆新特新能材料检测中心有限公司 | ICP-OES analysis method for determining content of metal elements in coal ash sample |
| CN112255077A (en) * | 2020-10-16 | 2021-01-22 | 中国矿业大学(北京) | Method for digesting low-quality coal |
| CN114689569A (en) * | 2022-04-02 | 2022-07-01 | 北京科技大学 | Method for testing silicon-aluminum ratio of molecular sieve |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104914090A (en) * | 2015-05-08 | 2015-09-16 | 广东省矿产应用研究所 | Detection method for continuously measuring Ga, In and Ge In lead-zinc smelting smoke dust through microwave digestion-ICP-OES |
| CN108152272A (en) * | 2017-12-28 | 2018-06-12 | 中建材蚌埠玻璃工业设计研究院有限公司 | The standard solution and its preparation method that micronutrient levels detects in quartz sand |
| CN109632770A (en) * | 2018-12-14 | 2019-04-16 | 湖北省兴发磷化工研究院有限公司 | A method of metal ion content in measurement glyphosate waste liquor |
| CN112098394A (en) * | 2019-06-18 | 2020-12-18 | 新疆新特新能材料检测中心有限公司 | ICP-OES analysis method for determining content of metal elements in coal ash sample |
| CN110954391A (en) * | 2019-12-24 | 2020-04-03 | 陕西华邦检测服务有限公司 | Digestion tank for monitoring pretreatment of elements in soil and application |
| CN112255077A (en) * | 2020-10-16 | 2021-01-22 | 中国矿业大学(北京) | Method for digesting low-quality coal |
| CN114689569A (en) * | 2022-04-02 | 2022-07-01 | 北京科技大学 | Method for testing silicon-aluminum ratio of molecular sieve |
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Application publication date: 20131009 |