CN110487758A - A method of arsenic, selenium, lead in measurement coal-burning power plant's coal and its combustion by-products - Google Patents
A method of arsenic, selenium, lead in measurement coal-burning power plant's coal and its combustion by-products Download PDFInfo
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- CN110487758A CN110487758A CN201910753128.8A CN201910753128A CN110487758A CN 110487758 A CN110487758 A CN 110487758A CN 201910753128 A CN201910753128 A CN 201910753128A CN 110487758 A CN110487758 A CN 110487758A
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- 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
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- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
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Abstract
The invention discloses a kind of method of arsenic, selenium, lead in measurement coal-burning power plant's coal and its combustion by-products, this method weighs sample in counteracting tank first, sequentially adds appropriate nitric acid, hydrochloric acid and hydrofluoric acid, carries out micro-wave digestion after closed；It carries out catching up with sour processing after resolution；Then testing liquid is configured；Configure corresponding current-carrying, reducing agent and standard serial solution；Make standard series curve, the test sample data arsenic obtained in sample corresponding with standard curve, selenium and lead content.Coal-burning power plant's coal and its combustion by-products are arranged by effectively pretreatment, reasonable reagent proportion and instrument parameter for this method, overcome the defect of traditional arsenic, selenium and Determination of Pb method, it can stablize and clear up and sufficiently extract arsenic, selenium and lead in sample, coal quality complexity and residual acid are solved to the interference problem of measurement result, can accurately measure the content of arsenic, selenium and lead in coal-burning power plant's coal and its production of combustion.
Description
Technical field
The present invention relates to a kind of methods of arsenic, selenium, lead in measurement coal-burning power plant's coal and its combustion by-products, belong to detection skill
Art field.
Background technique
Arsenic, selenium and lead are to common are malicious trace element in coal, pass through the modes such as breathing, skin adsorption or food intake
Into human body, human central nervous and a variety of organs are damaged, while three is savings property element, long-term chronic poisoning
It can be carcinogenic.The percentage of total amount is accounted for each discharge of pollutant sources heavy metal in the estimation whole world according to statistics, wherein the arsenic of 2-6%, 6-
13% selenium and the lead of 0.2-1.2% come from coal-burning power plant.
Arsenic, selenium and lead in as-fired coal used in coal-burning power plant is with its whole process, and usually there are three whereabouts: first is that being present in
In the flying dust that bottom ash and flue gas after coal combustion are trapped through deduster；Second is that flue gas is present in desulfurized gypsum after desulfurizing tower；
Atmosphere is discharged into flue gas third is that finally remaining in.Studies have shown that trace element has largely all been enriched in flying dust and desulfurization in coal
In gypsum.Desulfurized gypsum and flying dust are the most important solid waste in coal-burning power plant, are the main sources of China's solid waste
One of.It takes up a large area, and human cost is high, and since wherein trace element deposits environment there are the potentiality of secondary release
In biggish harm.Therefore accurate to grasp arsenic, selenium and lead content in measurement coal-burning power plant's coal and its combustion by-products, it can be coal
The offers such as the recycling of the pre-processing, the control of coal-burning power plant's trace element exhaust emission and the solid waste of fuel coal that utilize refer to
It leads.
In recent years, some analysis and detecting instruments are used for the detection of arsenic, selenium and lead, such as X-ray absorption fine structure spectroscopy
Corresponding spectral signature can be generated to heavy metal element with x ray absorption near edge structure, but both technologies are for sample
Detection limit it is higher, be only applicable to the sample analysis of high constituent content, and in coal and its production of combustion trace element arsenic,
Selenium and lead then and are not suitable for.Graphite furnace atomic absorption spectrometry and Inductive coupling plasma-atomic emission spectrometry can be same
When measure detection device for multi metallic elements, but it needs more complicated pre-treatment step, and detection sensitivity is relatively low, detection limit
It is higher.The advantages such as Hydride Generation-atomic Fluorescence Spectrometry has high sensitivity, and detection limit is low are suitable for coal and its burning by-product
The lower arsenic of concentration, selenium and lead detection in object.
In terms of sample pre-treatments, some researchers are by sample and Eschka reagent mixing calcining method and As-molybdenum blue light splitting degree
Method, longer the time required to both methods, Eschka reagent burns at least at five hours or more, along with processing later,
Entire at least two days experimental period.Microwave Digestion of pressurizeing is because of its airtightness, high efficiency, stability and to introduce pollution small etc. excellent
Point becomes relatively broad sample-pretreating method, and many research institutions are directed to different sample types, have formulated different resolutions
Program and digestive reagent.But the component accounting of the complicated component of coal, different rank coal differs greatly, and existing digestion procedure is not
All coals can be cleared up completely.And catch up with sour process also particularly critical after micro-wave digestion, and if acid is caught up with to be not thorough, remaining nitre
Element oxide to be measured to higher valence state can be generated liquid phase interference, and also have certain heavy metal in acid by the acid with strong oxidizing property such as acid,
Certain error can be caused to measurement result.
It extracts and accurately measures in coal-burning power plant's coal and its combustion by-products it is therefore proposed that one kind can stablize resolution
The method of arsenic, selenium and lead, it is special to arsenic, the Transport And Transformation of selenium and lead and distribution in solid waste after coal-burning power plant's coal and its burning
Property and its caused secondary release problem, are of great practical significance.
Summary of the invention
To solve the above-mentioned problems of the prior art, the purpose of the present invention is to provide a kind of measurement coal-burning power plant's coal and
The method of arsenic, selenium, lead in its combustion by-products.
In order to achieve the above objectives, the technical solution of the present invention is as follows: in a kind of measurement coal-burning power plant's coal and its combustion by-products
The method of arsenic, selenium, lead.The following steps are included:
(1) micro-wave digestion: weighing 0.1-1g coal, bottom ash, flying dust or gypsum, is placed in Teflon counteracting tank, is added mixed
Sealed digestion tank after acid is started to warm up from room temperature to 220 DEG C, and different stalls timing gradient increased temperature pressurization resolution, heating pressurization disappears
The temperature range of solution is 120 DEG C -220 DEG C, pressure range 5-3MPa, and time 3-20min is cooled to 80 DEG C or less after resolution
Afterwards from taking-up counteracting tank in microwave dissolver and as in draught cupboard；
(2) acid is caught up with to digestion solution: the liquid wash in counteracting tank is transferred in polytetrafluoroethylene beaker with deionized water,
Polytetrafluoroethylene beaker is caught up with into acid as heating is carried out on electric boiling plate, electric boiling plate set temperature is 110-140 DEG C；To poly- four
Appropriate amount of deionized water is added when liquid is closely dry in vinyl fluoride beaker, progress is secondary to catch up with acid, to second of polytetrafluoroethylene beaker
Stop catching up with acid when middle liquid is closely dry；
(3) it prepares solution to be measured: the liquid in step 2 in polytetrafluoroethylene beaker being moved into 100ml volumetric flask, is spent
Ionized water flushes three times and flushing liquor is transferred together into volumetric flask, and hydrochloric acid constant volume is added；
(4) configure atomic fluorescence agents useful for same: current-carrying used in measurement element is the hydrochloric acid solution of fixed volume ratio, is added
Reducing agent；
(5) drafting of standard curve: accurate configuration 10ml concentration is the standard solution of 50ppb concentration, wherein using respectively
Volume ratio be 3%, 10% and 1% hydrochloric acid solution, using atomic fluorescence-automatic dilution method configuration standard curve, obtain by
The standard curve that 10ppb, 20ppb, 30ppb, 40ppb and 50ppb standard series are constituted, it is desirable that each standard curve degree of correlation R2 >
0.9997；
(6) made solution to be measured is measured: made to step 3 with hollow cathode lamp using Atomic Fluorescence Spectrometer
Solution to be measured measures, and obtains its fluorescence intensity, compares with standard curve is obtained in step 5, obtains corresponding concentration of element；
(7) measurement of blank sample: separately setting blank group, solid sample be not added, and grasps simultaneously by step (1)-(6) with sample to be tested
Make, content of the measured value as blank corresponding element；
Preferably, when the measurement element is arsenic, after 3ml hydrochloric acid and 3-5g thiocarbamide is added in volumetric flask described in step 3
Constant volume shakes up, cooling and standings after 50 DEG C of water bath with thermostatic control heating 30min, the solution to be measured as arsenic element；It is measured described in step 4
Element is arsenic element, and current-carrying used is the hydrochloric acid solution of volume ratio 3%, and reducing agent used is 0.5% potassium hydroxide and 1% boron hydrogen
Change potassium mixed solution；Standard solution described in step 5 is arsenic, and 0.3-0.5g thiocarbamide is added in standard solution；Described in step 6
Hollow cathode lamp is as hollow cathode lamp, obtains corresponding arsenic concentration；Step 7 blank corresponding element is arsenic element.
Preferably, when the measurement element is selenium, be added in volumetric flask described in step 3 constant volume after 10ml hydrochloric acid shake up it is quiet
It sets, the solution to be measured as selenium element；Measurement element described in step 4 is selenium element, and measuring current-carrying used in selenium element is volume ratio
10% hydrochloric acid solution, reducing agent used are+1% potassium borohydride mixed solution of 0.2% potassium hydroxide；Standard described in step 5 makes
It is selenium with liquid；Hollow cathode lamp is selenium hollow cathode lamp in step 6, obtains corresponding selenium concentration；Step 7 corresponds to space element
Selenium element.
Preferably, when the measurement element is lead, be added in volumetric flask described in step 3 constant volume after 1ml hydrochloric acid shake up it is quiet
It sets, the solution to be measured as lead element；Measurement element described in step 4 is lead element, and measuring current-carrying used in lead element is volume ratio
1% hydrochloric acid solution, reducing agent used are+1% potassium ferricyanide mixed solution of+1% potassium borohydride of 1% potassium hydroxide；In step 5
The standard solution is lead；Hollow cathode lamp is lead hollow cathode lamp in step 6, obtains corresponding lead concentration；Step 7 is corresponding
Space element is lead element.
Preferably, the group of step 1 mixed acid solution becomes 6mlHNO3,2mlHCl and 2mlHF.
Preferably, in the step 1, microwave dissolver gradient increased temperature pressurization first- to six-speed step are as follows: 120 DEG C, 5MPa,
3min；150 DEG C, 10MPa, 3min；170 DEG C, 15MPa, 3min；190 DEG C, 20MPa, 3min；210 DEG C, 25MPa, 20min；220
DEG C, 30MPa, 20min.
Preferably, the reducing agent is first to be added after potassium hydroxide is completely dissolved, and adds potassium borohydride.
Preferably, reducing agent used in lead element should first be added after potassium hydroxide is completely dissolved, and add potassium borohydride, finally
The potassium ferricyanide is added.
Preferably, in the step 5 and step 6, Atomic Fluorescence Spectrometer is carrier gas using high-purity argon gas, and operating condition is set
Be set to: lamp current 55-70mA, negative high voltage 250-270V, atomizer height be 7.5-8.0mm, carrier gas flux 380-
420ml/min, delay time 0.5-1.0s, reading duration 7-10s.
Compared with the existing technology, the invention has the benefit that 1, this method is to coal-burning power plant's coal and its combustion by-products
By effectively pre-processing, reasonable reagent matches and instrument parameter setting, overcomes traditional arsenic, selenium and Determination of Pb side
The defect of method can be stablized and clear up and sufficiently extract arsenic, selenium and lead in sample, solve coal quality complexity and residual acid to survey
The interference problem for measuring result, can accurately measure the content of arsenic, selenium and lead in coal-burning power plant's coal and its production of combustion.2, microwave disappears
Solution scheme, which can be stablized, to be cleared up and sufficiently extracts arsenic, selenium and lead in coal and its combustion by-products, catches up with sour process that can sufficiently eliminate
The influence of residual acid in liquid is solved, atomic fluorescence spectrometry can accurately measure arsenic, selenium in the digestion solution obtained after pre-treatment
And lead concentration.
Detailed description of the invention
Fig. 1 are as follows: the measured value of As in embodiment 1-3 and comparative example.
Fig. 2 are as follows: the measured value of Se in embodiment 1-3 and comparative example.
Fig. 3 are as follows: the measured value of Pb in embodiment 1-3 and comparative example.
Specific embodiment
The invention will be further described with reference to embodiments: embodiment is in addition to applying resolution nitration mixture side of the present invention
Case also has chosen other two kinds of nitration mixture schemes and conventional wet resolution method as a comparison, and concrete operations are as follows:
Embodiment 1:
Three parts of 0.1g solid sample (coal, bottom ash, flying dust or gypsum) is weighed, three Teflon counteracting tanks are respectively placed in
In, sealed digestion tank after 6mlHNO3,2mlHCl and 2mlHF is sequentially added, is cleared up in microwave dissolver, is opened from room temperature
Beginning is warming up to 220 DEG C, and from one grade to six grade (120 DEG C, 5MPa, 3min；150 DEG C, 10MPa, 3min；170 DEG C, 15MPa, 3min；
190 DEG C, 20MPa, 3min；210 DEG C, 25MPa, 20min；220 DEG C, 30MPa, 20min) the pressurization resolution of timing gradient increased temperature, disappear
From taking-up counteracting tank in microwave dissolver and as in draught cupboard after being cooled to 80 DEG C or less after solution.
The liquid in three counteracting tanks is rinsed respectively with deionized water and is transferred in three polytetrafluoroethylene beakers, will be gathered
Tetrafluoroethene beaker catches up with acid as heating is carried out on electric boiling plate, and electric boiling plate set temperature is 130 DEG C, burns to polytetrafluoroethylene (PTFE)
Appropriate amount of deionized water is added when liquid is closely dry in cup, progress is secondary to catch up with acid, close to liquid in second of polytetrafluoroethylene beaker
Stop catching up with acid when dry.
Liquid in three polytetrafluoroethylene beakers is moved into respectively in three 100ml volumetric flasks, is rinsed with deionized water
It is transferred together three times and by flushing liquor into volumetric flask, number a, b and c, 3ml hydrochloric acid and 5g thiocarbamide is wherein added in volumetric flask a
Constant volume shakes up afterwards, and cooling and standings are added in volumetric flask b as the solution to be measured of arsenic element after 50 DEG C of water bath with thermostatic control heating 30min
Constant volume shakes up standing after 10ml hydrochloric acid, as the solution to be measured of selenium element, in volumetric flask a be added 1ml hydrochloric acid after constant volume shake up it is quiet
It sets, the solution to be measured as lead element.
Atomic fluorescence agents useful for same is configured, the hydrochloric acid solution that current-carrying used in arsenic element is volume ratio 3%, reduction used are measured
Agent is to add 1% potassium borohydride mixed solution after 0.5% potassium hydroxide is completely dissolved；Measuring current-carrying used in selenium element is volume
Hydrochloric acid solution than 10%, reducing agent used adds the mixing of 1% potassium borohydride after being completely dissolved for 0.2% potassium hydroxide molten
Liquid；The hydrochloric acid solution that current-carrying used in lead element is volume ratio 1% is measured, reducing agent used is after 1% potassium hydroxide is completely dissolved
% potassium borohydride is added, 1% potassium ferricyanide mixed solution is eventually adding.
Accurate configuration 10ml concentration is arsenic, selenium and the lead standard solution of 50ppb concentration, is wherein added in arsenic standard solution
Enter 0.5g thiocarbamide, the hydrochloric acid solution for being respectively 3%, 10% and 1% with volume ratio is matched using atomic fluorescence-automatic dilution method
Standard curve is set, the standard curve being made of 10ppb, 20ppb, 30ppb, 40ppb and 50ppb standard series is obtained, it is desirable that is each
Standard curve degree of correlation R2 > 0.9997.
Atomic Fluorescence Spectrometer parameter is set, the use of high-purity argon gas is carrier gas, operating condition setting are as follows: lamp current 55-
70mA, negative high voltage 250-270V, atomizer height be 7.5-8.0mm, carrier gas flux 380-420ml/min, delay when
Between be 0.5-1.0s, reading duration 7-10s.Made solution to be measured is measured, its fluorescence intensity is obtained, with standard curve
Comparison, obtains corresponding arsenic, selenium and lead concentration.
Blank group separately is set, solid sample is not added, is operated simultaneously by step (1)-(6) with sample to be tested, measured value is as empty
White arsenic, selenium and lead content.
Table 1 is the testing result of sample arsenic, selenium and lead:
By the above results it is found that the microwave digestion method can by the coal of different rank and its combustion by-products bottom ash,
Arsenic, selenium and lead in flying dust and desulfurized gypsum sufficiently extract, using the measurement result of Hydride Generation-atomic Fluorescence Spectrometry
For RSD within 10%, recovery of standard addition illustrates that this method measurement result is accurately credible between 80-120%.
Embodiment 2.3
Other are with embodiment 1, and nitration mixture scheme is different, wherein embodiment 1-3 nitration mixture scheme difference is as shown in table 1:
1 mixed acid system of table
| Mixed acid system | Type | Dosage (ml) |
| Embodiment 1 | HNO3-HCl-HF | 6-2-2 |
| Embodiment 2 | HNO3-HCl-H2O2 | 6-2-2 |
| Embodiment 3 | HNO3-HCl-H2SO4 | 6-2-2 |
Comparative example 1: wet resolution method
0.1g sample is weighed into polytetrafluoroethylene beaker, 6mlHNO is added3, 2mlHCl and 2mlHF, after cap upper surface ware
It is stood overnight in draught cupboard again.
Next day places the beaker is cleared up on electric boiling plate, and it is 180 DEG C that temperature, which is arranged, in electric boiling plate.When emerging in beaker
When a large amount of white dense smokes, solution colour and remaining sample color in beaker are observed, if solution becomes almost transparent, and remaining sample
When becoming canescence, assert that Specimen eliminating is completed, carry out further work after removing cooling；If solution muddiness or remaining sample
In dark brown, then need it is cooling after add appropriate mixed acid solution, be placed in and continue to clear up on electric boiling plate.
Solution in beaker after cooling is transferred in 1000ml volumetric flask, work and above-mentioned Microwave Digestion phase are post-processed
Together.
Resolution and measurement result
Using three kinds of different mixed acid systems progress micro-wave digestions and wet digestion, the results are shown in Table 3, measurement result
It is as shown in table 4:
Table 3 clears up result
4 measurement result of table (wherein nitration mixture one, two, three, respectively correspond embodiment 1-3)
As shown in Figure 1-3, according to resolution result and measurement result it is found that HNO3- HCl-HF mixed acid system and HNO3-HCl-
H2SO4Mixed acid system is preferable to the resolution effect of sample, can be complete by Specimen eliminating, and HNO3-HCl-H2O2Mixed acid system is main
For being cleared up to samples such as food, drugs, wherein H2O2Organic organization in sample can only be destroyed, and coal-fired electricity
Silicate content is higher in factory's fire coal, flying dust and bottom ash, so H2O2Poor to the resolution effect of coal-burning power plant's sample, HF is then right
Silica and silicate have good discomposing effect.
Although HNO3-HCl-H2SO4Mixed acid system can also preferably clear up sample, but its measured value is still lower, this
Be because sulfuric acid boiling point it is higher, and it is general catch up with sour process that can not drive in sulfuric acid, the measurement process pair of atomic fluorescence spectrophotometer
Acidity requirements are more stringent, and the presence of sulfuric acid has large effect to measurement result.And it observes and disappears known to the measurement result of Pb
The measurement result of Pb is extremely low in enzymatic hydrolysis system three, this is because sulfuric acid is reacted with the Pb in sample generates PbSO4Precipitating, later can not
It detected by instrument.
The measurement result and HNO of wet digestion3The measurement result of-HCl-HF mixed acid system is closer to, be mainly because
For in digestion process airtightness it is poor, cause arsenic and selenium volatilization loss more, and lead element is due to least volatile, therefore measure
As a result preferably.But the shortcomings that wet digestion is that the operation cycle is long, and opening is higher to mixed acid solution heating risk.To sum up four
Kind sample digestion method, HNO3- HCl-HF mixed acid system, which carries out micro-wave digestion, has resolution complete, and the operation cycle is short, member to be measured
Element loses few advantage.
The above description is merely a specific embodiment, but scope of protection of the present invention is not limited thereto, any
The change or replacement expected without creative work, should be covered by the protection scope of the present invention.Therefore, of the invention
Protection scope should be determined by the scope of protection defined in the claims.
Claims (9)
1. a kind of method of arsenic, selenium, lead in measurement coal-burning power plant's coal and its combustion by-products, it is characterised in that: including following step
It is rapid:
(1) micro-wave digestion: weighing 0.1-1g coal, bottom ash, flying dust or gypsum, is placed in Teflon counteracting tank, after nitration mixture is added
Sealed digestion tank is started to warm up from room temperature to 220 DEG C, and different stalls timing gradient increased temperature pressurization resolution, heating pressurization is cleared up
Temperature range is 120 DEG C -220 DEG C, pressure range 5-3MPa, time 3-20min, after 80 DEG C or less are cooled to after resolution from
Counteracting tank is taken out in microwave dissolver and as in draught cupboard；
(2) acid is caught up with to digestion solution: the liquid wash in counteracting tank is transferred in polytetrafluoroethylene beaker with deionized water, will be gathered
Tetrafluoroethene beaker catches up with acid as heating is carried out on electric boiling plate, and electric boiling plate set temperature is 110-140 DEG C, to polytetrafluoroethyl-ne
Appropriate amount of deionized water is added when liquid is closely dry in alkene beaker, progress is secondary to catch up with acid, to liquid in second of polytetrafluoroethylene beaker
Stop catching up with acid when body is closely dry；
(3) it prepares solution to be measured: the liquid in step 2 in polytetrafluoroethylene beaker being moved into 100ml volumetric flask, deionization is used
Water flushes three times and flushing liquor is transferred together into volumetric flask, and hydrochloric acid constant volume is added；
(4) configure atomic fluorescence agents useful for same: current-carrying used in measurement element is the hydrochloric acid solution of fixed volume ratio, adds reduction
Agent；
(5) drafting of standard curve: accurate configuration 10ml concentration is the standard solution of 50ppb concentration, wherein using volume respectively
Than the hydrochloric acid solution for 3%, 10% and 1%, using atomic fluorescence-automatic dilution method configuration standard curve, obtain by
The standard curve that 10ppb, 20ppb, 30ppb, 40ppb and 50ppb standard series are constituted, it is desirable that each standard curve degree of correlation R2 >
0.9997；
(6) made solution to be measured is measured: made to step 3 to be measured with hollow cathode lamp using Atomic Fluorescence Spectrometer
Solution measures, and obtains its fluorescence intensity, compares with standard curve is obtained in step 5, obtains corresponding concentration of element；
(7) measurement of blank sample: separately setting blank group, solid sample be not added, and operates simultaneously by step (1)-(6) with sample to be tested,
Content of the measured value as blank corresponding element.
2. the method for arsenic, selenium, lead in a kind of measurement coal-burning power plant's coal according to claim 1 and its combustion by-products, when
When the measurement element is arsenic, 3ml hydrochloric acid is added in volumetric flask described in step 3, constant volume shakes up after adding 3-5g thiocarbamide, and 50 DEG C
Cooling and standings after 30min, the solution to be measured as arsenic element are heated in water bath with thermostatic control；Measurement element described in step 4 is arsenic element,
Current-carrying used is the hydrochloric acid solution of volume ratio 3%, and reducing agent used is 0.5% potassium hydroxide and 1% potassium borohydride mixed solution；
Standard solution described in step 5 is arsenic, and 0.3-0.5g thiocarbamide is added in standard solution；Hollow cathode lamp described in step 6 is
As hollow cathode lamp obtains corresponding arsenic concentration；Step 7 blank corresponding element is arsenic element.
3. the method for arsenic, selenium, lead in a kind of measurement coal-burning power plant's coal according to claim 1 and its combustion by-products, when
When the measurement element is selenium, constant volume shakes up standing after 10ml hydrochloric acid is added in volumetric flask described in step 3, as selenium element to
Survey solution；Measurement element described in step 4 is selenium element, measures the hydrochloric acid solution that current-carrying used in selenium element is volume ratio 10%, institute
It is+1% potassium borohydride mixed solution of 0.2% potassium hydroxide with reducing agent；Standard solution described in step 5 is selenium；Step 6 is hollow
Heart cathode modulation is selenium hollow cathode lamp, obtains corresponding selenium concentration；The corresponding space element of step 7 is selenium element.
4. the method for arsenic, selenium, lead in a kind of measurement coal-burning power plant's coal according to claim 1 and its combustion by-products, when
When the measurement element is lead, constant volume shakes up standing after 1ml hydrochloric acid is added in volumetric flask described in step 3, as lead element to
Survey solution；Measurement element described in step 4 is lead element, measures the hydrochloric acid solution that current-carrying used in lead element is volume ratio 1%, used
Reducing agent is+1% potassium ferricyanide mixed solution of+1% potassium borohydride of 1% potassium hydroxide；Standard solution described in step 5 is
Lead；Hollow cathode lamp is lead hollow cathode lamp in step 6, obtains corresponding lead concentration；The corresponding space element of step 7 is lead member
Element.
5. the method for arsenic, selenium, lead, institute in a kind of measurement coal-burning power plant's coal according to claim 1 and its combustion by-products
The group for stating step 1 mixed acid solution becomes 6mlHNO3, 2mlHCl and 2mlHF.
6. the method for arsenic, selenium, lead, institute in a kind of measurement coal-burning power plant's coal according to claim 1 and its combustion by-products
It states in step 1, microwave dissolver gradient increased temperature pressurization first- to six-speed step are as follows: 120 DEG C, 5MPa, 3min；150 DEG C, 10MPa,
3min；170 DEG C, 15MPa, 3min；190 DEG C, 20MPa, 3min；210 DEG C, 25MPa, 20min；220 DEG C, 30MPa, 20min.
7. the method for arsenic, selenium, lead in a kind of measurement coal-burning power plant's coal according to claim 2 or 3 and its combustion by-products,
The reducing agent is first to be added after potassium hydroxide is completely dissolved, and adds potassium borohydride.
8. the method for arsenic, selenium, lead, lead in a kind of measurement coal-burning power plant's coal according to claim 4 and its combustion by-products
Reducing agent used in element should first be added after potassium hydroxide is completely dissolved, and add potassium borohydride, be eventually adding the potassium ferricyanide.
9. the method for arsenic, selenium, lead, institute in a kind of measurement coal-burning power plant's coal according to claim 1 and its combustion by-products
It states in step 5 and step 6, Atomic Fluorescence Spectrometer is carrier gas, operating condition setting are as follows: lamp current 55- using high-purity argon gas
70mA, negative high voltage 250-270V, atomizer height be 7.5-8.0mm, carrier gas flux 380-420ml/min, delay when
Between be 0.5-1.0s, reading duration 7-10s.
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| CN201910753128.8A CN110487758B (en) | 2019-08-15 | 2019-08-15 | Method for measuring arsenic, selenium and lead in coal-fired power plant coal and combustion byproducts thereof |
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