CN103278553A - Method for determination of volatile element mercury in fire coal product - Google Patents
Method for determination of volatile element mercury in fire coal product Download PDFInfo
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- CN103278553A CN103278553A CN2013101522926A CN201310152292A CN103278553A CN 103278553 A CN103278553 A CN 103278553A CN 2013101522926 A CN2013101522926 A CN 2013101522926A CN 201310152292 A CN201310152292 A CN 201310152292A CN 103278553 A CN103278553 A CN 103278553A
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Abstract
The invention discloses a method for determination of volatile element mercury in a fire coal product. The method comprises the following steps of carrying out microwave digestion of a sample and third-level analytically-pure nitric acid, adding deionized water into the digestion product to obtain a solution having a constant volume of 100ml, and carrying out quantitative determination by an inductively coupled plasma mass spectrometer. The method can solve the problem that in pretreatment, Hg volatilizes easily so that sample treatment time is long and a detection limit of a quantitative analysis apparatus is not enough accurate. The method is a novel method having high selectivity, simple processes, a fast determination rate and a high determination result precision.
Description
Technical field
The present invention relates to the analytical chemistry field, more particularly, belong to volatile trace element quantitative analysis method.
Background technology
Hg is a kind of poisonous silvery white heavy metal element, and it is liquid metals unique under the normal temperature, and element Hg can be converted into the stronger methyl mercury of toxicity under the synthetic bacterial action of anaerobic methane.Hg can be combined with plasma proteins after entering blood, the damage red blood cell.Hg also can act on cell membrane, change function of plasma membrane, and then influence cell function, so the fast quantification of Hg detects significant.National standard (Hg:GB/T 16659-2008) is comparatively loaded down with trivial details for the pre-treatment step of the quantitative detection of Hg, need be with target substance and reagent mixing calcination, and object element need change it into test substance through a series of redox reactions.Wherein to the calcination of target substance, the volatilization loss that reduction process can cause element; Adopt quantitative test instrument cold atomic absorption spectrometry and cold atom absorptiometry simultaneously, the instrument detection limit is big, detection for trace element may not reach enough accuracy, and equipment debugging is comparatively loaded down with trivial details, needs the laboratory technician to have abundant analysis experience and skill.For the effumability element, in the preparation process of sample, element volatilizees easily, and detected value is on the low side, and measurement effect does not reach standard.Handle the early stage of selecting micro-wave digestion to carry out sample, can effectively guarantee to survey the reduction of detection elements loss.Hg belongs to trace element, and the content in coal-fired product is very low, and icp ms is highly sensitive, and detectability is low, can satisfy now for volatile trace element Study on Distribution Law in coal-fired product; The process of whole mensuration is quick, and is accurately easy and simple to handle, saved a large amount of time, human and material resources.
Summary of the invention
The object of the invention is to overcome the deficiencies in the prior art, provides a kind of and can overcome Hg volatile loss in the pre-treatment process, and the processing sample time is long, drawbacks such as quantitative test instrument detectability is not accurate enough, and have high selectivity, easy and simple to handle, fast, the high new method of measurement result precision.
Technical purpose of the present invention is achieved by following technical proposals:
A kind of method of measuring Volatile Elements mercury in the coal-fired product, carry out according to following step:
(1) takes by weighing 0.1g sample and 9mLHNO
3Carry out micro-wave digestion; Described HNO
3Use three grades of analytically pure nitric acid (BV-III level, quality percentage composition are 65%), described micro-wave digestion carries out in counteracting tank, and microwave power is 1600W, and temperature is 100 ℃-210 ℃, preferred 160 ℃; Begin to heat up from room temperature (25 ℃), wherein the heating-up time is 20 minutes, keeps predetermined temperature 30 minutes, is cooled to room temperature (25 ℃) and takes out counteracting tank from microwave dissolver;
(2) liquid in the counteracting tank is filtered, the filtering solid residue, the liquid that filtration is obtained uses deionized water to be settled to 100mL
(3) then the solution to be measured behind the constant volume is quantitatively detected by icp ms (Agilent 7700x), the quantitative test time is 30min.
Compared with prior art, meaning of the present invention has been to provide a kind of quantitative detecting method at Volatile Elements Hg in the coal combustion product, it is advantageous that:
(1) adopts microwave digestion technology to carry out the pre-treatment of sample, reduce the volatilization loss of sample in the pre-treatment process;
(2) adopt microwave digestion technology to carry out the pre-treatment of sample, at utmost reduce the pretreated time, the whole process of micro-wave digestion is from being heated to insulation, to being cooled to the room temperature constant volume at last, whole process needs 1 hour approximately, and traditional pre-service needs several hours even 1 day;
(3) adopt icp ms to carry out the quantitative detection of element, detectability is low, fast.
Embodiment
Further specify technical scheme of the present invention below in conjunction with specific embodiment.
Use coal fly ash constituent analysis standard substance (GBW08401), use three grades of analytically pure nitric acid (BV-III levels, the quality percentage composition is 65%) carry out micro-wave digestion and carry out pre-treatment, being about to coal fly ash constituent analysis standard substance and three grades of analytically pure nitric acid mixes in counteracting tank, put into microwave dissolver then and carry out micro-wave digestion (U.S. CE M counteract appearance, can realize that pressure controls automatically), microwave power is 1600W.
Each sampling amount is 0.1g, 9mLHNO
3Carry out micro-wave digestion, select 100 ℃, 130 ℃, 160 ℃, 190 ℃, 210 ℃ as experimental temperature, begin to heat up from room temperature (25 ℃), wherein the heating-up time is 20 minutes, kept predetermined temperature 30 minutes, and be cooled to room temperature (25 ℃) and from microwave dissolver, take out.Liquid in the counteracting tank is filtered, the filtering solid residue, the liquid that filtration is obtained uses deionized water to be settled to 100mL.Then the solution to be measured behind the constant volume is quantitatively detected by icp ms (Agilent 7700x), the quantitative test time is 30min.Net result is the mean value of the parallel sample of many groups, and is as shown in the table:
Table 1Hg clears up condition in difference and detects mean value and the recovery
The best application of the present invention is burning of coal product flying dust, bottom ash.The microwave digestion technology of using is a kind of pre-treatment mode of newer solid sample, this technology places counteracting tank with sample, under the acid reagent condition, the sealing High Temperature High Pressure is cleared up, reach clearing up fast of solid sample, reduce the loss of Volatile Elements in the pre-treatment process simultaneously to greatest extent.Icp ms is one of the highest instrument of present quantitative measurement precision, almost can measure the most elements and the detection limit low (Hg ≈ 0.3000ng/g) that cover in the periodic table of elements, detects fast.Test result shows, the numerical value that the process icp ms detects is all in the scope of sample standard value, and can obtain the higher recovery for volatile element, whole 2.5 hours quantitative process times spent of single-element, top condition is for carrying out micro-wave digestion under 160 ℃.
More than the present invention has been done exemplary description; should be noted that; under the situation that does not break away from core of the present invention, the replacement that is equal to that any simple distortion, modification or other those skilled in the art can not spend creative work all falls into protection scope of the present invention.
Claims (3)
1. a method of measuring Volatile Elements mercury in the coal-fired product is characterized in that, carries out according to following step:
(1) takes by weighing 0.1g sample and 9mLHNO
3Carry out micro-wave digestion; Described HNO
3Use three grades of analytically pure nitric acid, the quality percentage composition is 65%, and described micro-wave digestion carries out in counteracting tank, and microwave power is 1600W, and temperature is 100 ℃-210 ℃; Begin to heat up from 25 ℃ of room temperatures, wherein the heating-up time is 20 minutes, keeps predetermined temperature 30 minutes, is cooled to room temperature and takes out counteracting tank for 25 ℃ from microwave dissolver;
(2) liquid in the counteracting tank is filtered, the filtering solid residue, the liquid that filtration is obtained uses deionized water to be settled to 100mL;
(3) then the solution to be measured behind the constant volume is quantitatively detected by icp ms, the quantitative test time is 30min.
2. a kind of method of measuring Volatile Elements mercury in the coal-fired product according to claim 1 is characterized in that, preferred 160 ℃ of the temperature of described micro-wave digestion.
3. a kind of method of measuring Volatile Elements mercury in the coal-fired product according to claim 1 is characterized in that, whole 2.5 hours quantitative process times spent.
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| CN2013101522926A CN103278553A (en) | 2013-04-27 | 2013-04-27 | Method for determination of volatile element mercury in fire coal product |
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| CN2013101522926A CN103278553A (en) | 2013-04-27 | 2013-04-27 | Method for determination of volatile element mercury in fire coal product |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104849341A (en) * | 2015-04-22 | 2015-08-19 | 北京大学 | Method for measuring mercury element content of gangue or fly ash |
| CN111879873A (en) * | 2020-08-03 | 2020-11-03 | 国家煤化工产品质量监督检验中心（安徽）（淮南市产品质量监督检验所） | Method for detecting arsenic and mercury occurrence form of coal |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CA2111383C (en) * | 1992-12-31 | 2005-04-12 | Brian W. Renoe | Control of continuous microwave digestion process |
| EP1196764B1 (en) * | 1999-07-23 | 2007-10-17 | Efthimion Emerging Industries, LLC | A continuous emissions monitor of multiple metal species in harsh environments |
| CN101196448A (en) * | 2007-12-22 | 2008-06-11 | 河南理工大学 | Sampling method for measuring coal gangue component by ICP-MS |
| CN101839900A (en) * | 2010-05-19 | 2010-09-22 | 重庆大学 | Detection method of mercury content in burning coal |
-
2013
- 2013-04-27 CN CN2013101522926A patent/CN103278553A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CA2111383C (en) * | 1992-12-31 | 2005-04-12 | Brian W. Renoe | Control of continuous microwave digestion process |
| EP1196764B1 (en) * | 1999-07-23 | 2007-10-17 | Efthimion Emerging Industries, LLC | A continuous emissions monitor of multiple metal species in harsh environments |
| CN101196448A (en) * | 2007-12-22 | 2008-06-11 | 河南理工大学 | Sampling method for measuring coal gangue component by ICP-MS |
| CN101839900A (en) * | 2010-05-19 | 2010-09-22 | 重庆大学 | Detection method of mercury content in burning coal |
Non-Patent Citations (2)
| Title |
|---|
| 王晖等: "ICP-OES/ICP-MS测定煤中多种元素的微波消解方法研究", 《光谱学与光谱分析》, vol. 32, no. 6, 30 June 2012 (2012-06-30) * |
| 麻银娟: "煤中挥发性微量元素Hg、As、Pb燃烧固化的热力学模拟和实验研究", 《中国优秀硕士学位论文全文数据库 基础科学辑》, no. 10, 15 October 2011 (2011-10-15) * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104849341A (en) * | 2015-04-22 | 2015-08-19 | 北京大学 | Method for measuring mercury element content of gangue or fly ash |
| CN104849341B (en) * | 2015-04-22 | 2017-08-18 | 北京大学 | The measuring method of mercury element content in a kind of gangue or flyash |
| CN111879873A (en) * | 2020-08-03 | 2020-11-03 | 国家煤化工产品质量监督检验中心（安徽）（淮南市产品质量监督检验所） | Method for detecting arsenic and mercury occurrence form of coal |
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Application publication date: 20130904 |