CN108535301A - A method of various heavy content in flying dust is measured using XRF instrument quantitatives - Google Patents
A method of various heavy content in flying dust is measured using XRF instrument quantitatives Download PDFInfo
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- CN108535301A CN108535301A CN201810067499.6A CN201810067499A CN108535301A CN 108535301 A CN108535301 A CN 108535301A CN 201810067499 A CN201810067499 A CN 201810067499A CN 108535301 A CN108535301 A CN 108535301A
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- 239000000428 dust Substances 0.000 title claims abstract description 113
- 238000000034 method Methods 0.000 title claims abstract description 31
- 239000011651 chromium Substances 0.000 claims abstract description 30
- 239000010949 copper Substances 0.000 claims abstract description 29
- 239000011133 lead Substances 0.000 claims abstract description 27
- 238000001514 detection method Methods 0.000 claims abstract description 26
- 229910052804 chromium Inorganic materials 0.000 claims abstract description 25
- 229910052802 copper Inorganic materials 0.000 claims abstract description 25
- 239000000758 substrate Substances 0.000 claims abstract description 24
- 229910052785 arsenic Inorganic materials 0.000 claims abstract description 22
- 229910052793 cadmium Inorganic materials 0.000 claims abstract description 21
- 239000011701 zinc Substances 0.000 claims abstract description 20
- 229910052788 barium Inorganic materials 0.000 claims abstract description 19
- 229910052725 zinc Inorganic materials 0.000 claims abstract description 19
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 claims abstract description 14
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 14
- RQNWIZPPADIBDY-UHFFFAOYSA-N arsenic atom Chemical compound [As] RQNWIZPPADIBDY-UHFFFAOYSA-N 0.000 claims abstract description 14
- DSAJWYNOEDNPEQ-UHFFFAOYSA-N barium atom Chemical compound [Ba] DSAJWYNOEDNPEQ-UHFFFAOYSA-N 0.000 claims abstract description 14
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 claims abstract description 14
- 229910052792 caesium Inorganic materials 0.000 claims abstract description 14
- TVFDJXOCXUVLDH-UHFFFAOYSA-N caesium atom Chemical compound [Cs] TVFDJXOCXUVLDH-UHFFFAOYSA-N 0.000 claims abstract description 14
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims abstract description 11
- 238000011088 calibration curve Methods 0.000 claims abstract description 6
- 238000012360 testing method Methods 0.000 claims description 21
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 19
- 238000005259 measurement Methods 0.000 claims description 12
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 claims description 11
- 238000004876 x-ray fluorescence Methods 0.000 claims description 10
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 claims description 9
- 239000000292 calcium oxide Substances 0.000 claims description 9
- 239000000377 silicon dioxide Substances 0.000 claims description 9
- 238000009472 formulation Methods 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 5
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 claims description 4
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 3
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical group [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 claims description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims 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 claims 1
- 239000000920 calcium hydroxide Substances 0.000 claims 1
- 229910001861 calcium hydroxide Inorganic materials 0.000 claims 1
- 239000000395 magnesium oxide Substances 0.000 claims 1
- 230000003647 oxidation Effects 0.000 claims 1
- 238000007254 oxidation reaction Methods 0.000 claims 1
- CHWRSCGUEQEHOH-UHFFFAOYSA-N potassium oxide Chemical compound [O-2].[K+].[K+] CHWRSCGUEQEHOH-UHFFFAOYSA-N 0.000 claims 1
- 229910001950 potassium oxide Inorganic materials 0.000 claims 1
- 229910052708 sodium Inorganic materials 0.000 claims 1
- 239000011734 sodium Substances 0.000 claims 1
- 229910052751 metal Inorganic materials 0.000 abstract description 15
- 238000002354 inductively-coupled plasma atomic emission spectroscopy Methods 0.000 abstract description 4
- 239000000523 sample Substances 0.000 description 100
- 229910001385 heavy metal Inorganic materials 0.000 description 15
- 229910052745 lead Inorganic materials 0.000 description 11
- 239000010881 fly ash Substances 0.000 description 8
- 239000010813 municipal solid waste Substances 0.000 description 7
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 5
- 238000004458 analytical method Methods 0.000 description 5
- 239000003546 flue gas Substances 0.000 description 5
- 238000000746 purification Methods 0.000 description 5
- 229920002799 BoPET Polymers 0.000 description 4
- 239000005041 Mylar™ Substances 0.000 description 4
- 238000012417 linear regression Methods 0.000 description 4
- 239000012925 reference material Substances 0.000 description 4
- 230000000087 stabilizing effect Effects 0.000 description 4
- 239000003153 chemical reaction reagent Substances 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 229910052711 selenium Inorganic materials 0.000 description 3
- 230000006641 stabilisation Effects 0.000 description 3
- 238000011105 stabilization Methods 0.000 description 3
- JBQYATWDVHIOAR-UHFFFAOYSA-N tellanylidenegermanium Chemical compound [Te]=[Ge] JBQYATWDVHIOAR-UHFFFAOYSA-N 0.000 description 3
- 238000003556 assay Methods 0.000 description 2
- 239000002738 chelating agent Substances 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000002386 leaching Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000002203 pretreatment Methods 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- KKCBUQHMOMHUOY-UHFFFAOYSA-N sodium oxide Chemical compound [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 description 2
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 230000010165 autogamy Effects 0.000 description 1
- 239000001913 cellulose Substances 0.000 description 1
- 229920002678 cellulose Polymers 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000013522 chelant Substances 0.000 description 1
- 239000013068 control sample Substances 0.000 description 1
- 230000002354 daily effect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- FZFYOUJTOSBFPQ-UHFFFAOYSA-M dipotassium;hydroxide Chemical compound [OH-].[K+].[K+] FZFYOUJTOSBFPQ-UHFFFAOYSA-M 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 230000003203 everyday effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 231100001261 hazardous Toxicity 0.000 description 1
- 239000002920 hazardous waste Substances 0.000 description 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 1
- 230000013011 mating Effects 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- JKQOBWVOAYFWKG-UHFFFAOYSA-N molybdenum trioxide Chemical compound O=[Mo](=O)=O JKQOBWVOAYFWKG-UHFFFAOYSA-N 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- VDGJOQCBCPGFFD-UHFFFAOYSA-N oxygen(2-) silicon(4+) titanium(4+) Chemical compound [Si+4].[O-2].[O-2].[Ti+4] VDGJOQCBCPGFFD-UHFFFAOYSA-N 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 230000007096 poisonous effect Effects 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000007781 pre-processing Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000004445 quantitative analysis Methods 0.000 description 1
- 229910001948 sodium oxide Inorganic materials 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000007619 statistical method Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000011282 treatment Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 238000004846 x-ray emission Methods 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/22—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material
- G01N23/223—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material by irradiating the sample with X-rays or gamma-rays and by measuring X-ray fluorescence
Landscapes
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Analysing Materials By The Use Of Radiation (AREA)
Abstract
The present invention provides a kind of method measuring various heavy content in flying dust using XRF instrument quantitatives, includes the following steps：1）Flying dust is collected, as sample to be tested；2）It takes flying dust standard sample, substrate is added, be made into a series of flying dust standard sample of lead containing various concentration, chromium, copper, zinc, arsenic, caesium, cadmium, barium element；3）Sample to be tested, flying dust standard sample are subjected to Xray fluorescence spectrometer detection respectively, quantified using calibration curve method, the content of lead, chromium, copper, zinc, arsenic, caesium, cadmium, barium element in sample to be tested is obtained.A kind of method that various heavy content in flying dust is measured using XRF instrument quantitatives provided by the invention, shortcoming existing for existing flying dust detection technique " resolution pretreatment+ICP OES detections ", realization can be overcome accurately and rapidly to quantitative determine the content of detection device for multi metallic elements in flying dust.
Description
Technical field
The invention belongs to field of environment engineering technology, it is related to a kind of measuring an a variety of huge sum of moneys in flying dust using XRF instrument quantitatives
Belong to the method for content.
Background technology
Flying dust (hereinafter referred to as " flying dust ") in the flue gas purification system of municipal solid waste incinerator is《National Hazard waste name
It records (2016 editions)》Defined hazardous waste contains the poisonous and hazardous heavy metal such as Pb, Cr, Zn, Cu, As, Cd, it is necessary to by steady
Determining processing, makes flying dust Leaching reach landfill yard admissions criteria, could carry out landfill stabilization.Each heavy metal member in flying dust
Cellulose content is higher, and the corresponding leaching concentration of the element is higher.Therefore, quickly, accurately measure heavy metal element in flying dust
Total content can instruct optimization stabilizing fly ash technological parameter, for example add suitable amount of chelant so that flying dust can reach
Mark landfill.
Traditional assay method of fly-ash heavy metal total amount is using " resolution pretreatment+ICP-OES " method, and this method can be with
Accomplish accurate quantitative analysis, but time-consuming for preprocessing process, third party testing laboratory, which generally requires 5~7 days, could provide detection
Report, cannot be satisfied the quick testing requirements of the total metals to each batch flying dust, especially cannot be satisfied stabilizing fly ash
The real-time monitoring for changing production scene instructs the requirement of chelating agent dosage.
X-ray fluorescence spectra (X Ray Fluorescence Spectrometry) is analyzed, abbreviation XRF analysis, is a kind of
Quickly, lossless detection method, is suitable for the detection of powder, bulk and other items, and each sample only needs 1~3min that can measure weight
The total amount of metal.But XRF analysis method is a kind of qualitative, sxemiquantitative method, cannot accurately measure the heavy metal member in flying dust
The content of element.
Invention content
In view of the foregoing deficiencies of prior art, it is surveyed using XRF instrument quantitatives the purpose of the present invention is to provide a kind of
The method of various heavy content in flying dust is determined, for solving to lack in the prior art quickly, in accurate, quantitative determination flying dust
The problem of method of eight Heavy Metallic Elements of Pb, Cr, Cu, Zn, As, Se, Cd and Ba.
In order to achieve the above objects and other related objects, the present invention provides a kind of use in XRF instrument quantitatives measurement flying dust
The method of various heavy content, includes the following steps：
1) flying dust is collected, as sample to be tested；
2) flying dust standard sample is taken, substrate is added, is made into a series of lead (Pb), chromium (Cr), copper containing various concentration
(Cu), the flying dust standard sample of zinc (Zn), arsenic (As), caesium (Se), cadmium (Cd), barium (Ba) element；
3) the flying dust standard sample that sample to be tested, step 2) are prepared in step 1) is subjected to Xray fluorescence spectrometer respectively
(XRF) it detects, is quantified using calibration curve method, obtain lead (Pb), chromium (Cr), copper (Cu), zinc (Zn), arsenic in sample to be tested
(As), the content of caesium (Se), cadmium (Cd), barium (Ba) element.
Preferably, in step 1), the flying dust be municipal solid waste incinerator flue gas purification system in the dust that generates.
Preferably, in step 2), the flying dust standard sample is to contain a certain concentration by what domestic and international authoritative institution produced
Lead (Pb), chromium (Cr), copper (Cu), zinc (Zn), arsenic (As), caesium (Se), cadmium (Cd), barium (Ba) element flying dust sample, can be from
Purchase obtains in the market.Specific such as European Commission, Joint Research Centre, Institute for
The Certified Reference Material BCR- that Reference Material and Measurements are provided
The flying dust standard sample of 176R.
Preferably, in step 2), a concentration of 800~6000mg/kg of lead in the flying dust standard sample, chromium it is a concentration of
60~4000mg/kg, a concentration of 300~6500mg/kg of copper, zinc concentration be 2500~75000mg/kg, a concentration of the 5 of arsenic
~150mg/kg, a concentration of 1~50mg/kg of caesium, a concentration of 160~350mg/kg of cadmium, barium a concentration of 200~
12000mg/kg。
It is further preferred that in the flying dust standard sample lead a concentration of 5000mg/kg, a concentration of 810mg/ of chromium
Kg, a concentration of 1050mg/kg of copper, zinc concentration 16800mg/kg, a concentration of 54mg/kg of arsenic, caesium it is a concentration of
18.3mg/kg, a concentration of 226mg/kg of cadmium, a concentration of 4650mg/kg of barium.
Preferably, in step 2), the substrate is selected from calcium hydroxide (Ca (OH)2), calcium oxide (CaO), titanium dioxide
Silicon (SiO2), aluminium oxide (Al2O3), potassium oxide (K2O), sodium oxide molybdena (Na2O), iron oxide (Fe2O3), one in magnesia (MgO)
Kind or multiple combinations.
It is highly preferred that the substrate is calcium oxide (CaO) and silica (SiO2)。
It is further preferred that the calcium oxide is 3 with the weight ratio that silica is added:7~7:3.
It is further preferred that the calcium oxide is 6 with the weight ratio that silica is added:4.
Preferably, in step 2), in the flying dust standard sample, the weight of the substrate and the addition of flying dust standard sample
The ratio between amount is 5:0~0:5.It is highly preferred that in the flying dust standard sample, the substrate is added with flying dust standard sample
Weight ratio is 4:1~1:4.
Preferably, in step 3), the sample to be tested or flying dust standard sample are put into sample test box, are made by vibration
The bottom surface of sample to be tested or flying dust standard sample is smooth, not loose, free from flaw.The vibration is vibration manually.
Preferably, in step 3), the instrument testing conditions of the Xray fluorescence spectrometer (XRF) are：Measurement atmosphere：It is empty
Gas atmosphere or vacuum；Sample formulations：Blocky or film；Collimator：1mm, 3mm, 5mm or 10mm.
It is highly preferred that the instrument testing conditions of the Xray fluorescence spectrometer (XRF) are：Measurement atmosphere：Air atmosphere；
Sample formulations：It is blocky；Collimator：10mm.
Preferably, in step 3), the calibration curve method includes the following steps：
A, the substrate and flying dust standard sample that will be obtained in step 2), is made into a series of flying dust standard of various concentrations
Sample carries out XRF detections, obtains the mass concentration of the x-ray fluorescence intensity and corresponding element to be measured of each element to be measured respectively
Linear relationship, to fitting draw out corresponding unitary linear work curve, calculate separately to obtain the standard of 8 kinds of elements to be measured
The regression equation of curve.
More preferably, in the standard curve, using the x-ray fluorescence intensity of each element to be measured as ordinate (Y-axis), phase
It is abscissa (X-axis) to answer the mass concentration of element to be measured.
B, sample to be tested in step 1) is subjected to XRF detections, by the X-ray of the element to be measured of each in the sample to be tested of acquisition
Fluorescence intensity substitutes into the regression equation of the standard curve of corresponding element to be measured in step A, is calculated in sample to be tested and accordingly waits for
Survey the mass concentration of element.
As described above, a kind of side measuring various heavy content in flying dust using XRF instrument quantitatives provided by the invention
Method, for shortcoming existing for existing flying dust detection technique " resolution pretreatment+ICP-OES detections ", by the substrate of autogamy
Matter and flying dust standard sample are mixed with certain proportion, prepare the flying dust standard sample of different heavy metal element concentration, are used
XRF detects flying dust standard sample and sample to be tested, using calibration curve method, to realize to detection device for multi metallic elements in flying dust
Content is accurately and rapidly measured, to instruct and optimize the additive amount of stabilizing fly ash treatment agent.It is provided by the invention
Assay method, easy to operate, accuracy stability is high, timeliness is strong, the advantages of on-line checking can be achieved, highly in reality
It is promoted and applied in detection work.
Description of the drawings
Fig. 1 be shown as canonical plotting 1a, 1b of Cu, Zn, Ba, Pb, Cr, As, Se and Cd in flying dust, 1c, 1d, 1e, 1f,
1g、1h。
The content that Fig. 2 is shown as Pb, Cd, Cu, Cr in flying dust in embodiment 6 continuously detects Fig. 2 a, 2b, 2c, 2d.
Specific implementation mode
With reference to specific embodiment, the present invention is further explained, it should be appreciated that these embodiments are merely to illustrate the present invention
Rather than it limits the scope of the invention.
Illustrate that embodiments of the present invention, those skilled in the art can be by this specification below by way of specific specific example
Disclosed content understands other advantages and effect of the present invention easily.The present invention can also pass through in addition different specific realities
The mode of applying is embodied or practiced, the various details in this specification can also be based on different viewpoints with application, without departing from
Various modifications or alterations are carried out under the spirit of the present invention.
The reagent used in the present invention and instrument are as follows：
1, reagent
Flying dust (flue gas purification system of municipal solid waste incinerator generates)；Calcium oxide：(AR, Tianjin big chemical reagent forever
Co., Ltd)；Silica (AR, the prosperous prosperous Chemical Co., Ltd. in Tianjin)；Flying dust standard sample (European
Commission,Joint Research Centre,Institute for Reference Material and
Measurements, Certified Reference Material BCR-176R).
2, instrument
EDX7000 type energy dispersion types Xray fluorescence spectrometer (Japanese Shimadzu Corporation).
Embodiment 1
1, sample pre-treatments
The flying dust generated in the flue gas purification system of municipal solid waste incinerator is taken, as sample to be tested.
2, flying dust standard sample is prepared
It is 6 the ratio between by weight:4, it is made into substrate after taking calcium oxide and silica to be mixed.Known concentration is taken again
Flying dust standard sample, substrate mixing is added, the weight ratio that substrate and flying dust standard sample are added is 5:0~0:
5, to be made into flying dust standard sample.Wherein, in the flying dust standard sample lead a concentration of 5000mg/kg, chromium it is a concentration of
810mg/kg, a concentration of 1050mg/kg of copper, zinc concentration 16800mg/kg, a concentration of 54mg/kg of arsenic, the concentration of caesium
For 18.3mg/kg, a concentration of 226mg/kg of cadmium, a concentration of 4650mg/kg of barium.
3, it measures
The flying dust standard sample for respectively preparing sample to be tested, step 2 in step 1 carries out XRF detections, using standard curve
Method is quantified, and the content of lead, chromium, copper, zinc, arsenic, caesium, cadmium, barium element in sample to be tested is obtained.
Specifically, it is dense to be first made into a series of differences for the substrate obtained in above-mentioned steps 2 and flying dust standard sample
The flying dust standard sample of degree carries out XRF detections, obtains the x-ray fluorescence intensity of each element to be measured and corresponding member to be measured respectively
The linear relationship of the mass concentration of element, it is corresponding to be measured using the x-ray fluorescence intensity of each element to be measured as ordinate (Y-axis)
The mass concentration of element is abscissa (X-axis), calculates separately to obtain the regression equation of the standard curve of 8 kinds of elements to be measured.
Then, XRF detections then by sample to be tested in step 1 are carried out, by the X of the element to be measured of each in the sample to be tested of acquisition
Ray fluorescence intensity substitutes into the regression equation of the standard curve of corresponding element to be measured in step A, phase in sample to be tested is calculated
Answer the mass concentration of element to be measured.
Wherein, sample to be tested takes 5g, is put into sample test box, gently up-down vibration, makes the bottom surface of sample to be tested (i.e.
The shadow surface of X-ray) in flat smooth, free from flaw, not loose state.Similarly, flying dust standard sample takes 5g respectively, puts respectively
Enter in sample test box, gently up-down vibration, it is bottom surface flat smooth, free from flaw and not loose school to make flying dust standard sample
Quasi- print.Then, respectively by equipped with sample to be tested sample test box, equipped with the sample test box of flying dust standard sample, examining
It surveys end and wraps Mylar films (i.e. mylar film), be put into XRF and be detected.
The instrument testing conditions of the Xray fluorescence spectrometer (XRF) are：Measurement atmosphere：Air atmosphere；Sample formulations：
It is blocky；Collimator：10mm.
Embodiment 2
1, sample pre-treatments
The flying dust generated in the flue gas purification system of municipal solid waste incinerator is taken, as sample to be tested.
2, control sample is prepared
It is 3 the ratio between by weight:7~7:3, it is made into substrate after taking calcium oxide and silica to be mixed.It takes again
Know the flying dust standard sample of concentration, substrate mixing is added, the weight ratio that substrate is added with flying dust standard sample is
4:1~1:4, to be made into flying dust standard sample.Wherein, in the flying dust standard sample lead a concentration of 800~6000mg/
Kg, a concentration of 60~4000mg/kg of chromium, a concentration of 300~6500mg/kg of copper, zinc concentration are 2500~75000mg/
Kg, a concentration of 5~150mg/kg of arsenic, a concentration of 1~50mg/kg of caesium, a concentration of 160~350mg/kg of cadmium, barium it is dense
Degree is 200~12000mg/kg.
3, it measures
The flying dust standard sample for respectively preparing sample to be tested, step 2 in step 1 carries out XRF detections, using standard curve
Method is quantified, and the content of lead, chromium, copper, zinc, arsenic, caesium, cadmium, barium element in sample to be tested is obtained.
Specifically, it is dense to be first made into a series of differences for the substrate obtained in above-mentioned steps 2 and flying dust standard sample
The flying dust standard sample of degree carries out XRF detections, obtains the x-ray fluorescence intensity of each element to be measured and corresponding member to be measured respectively
The linear relationship of the mass concentration of element, it is corresponding to be measured using the x-ray fluorescence intensity of each element to be measured as ordinate (Y-axis)
The mass concentration of element is abscissa (X-axis), calculates separately to obtain the regression equation of the standard curve of 8 kinds of elements to be measured.
Then, XRF detections then by sample to be tested in step 1 are carried out, by the X of the element to be measured of each in the sample to be tested of acquisition
Ray fluorescence intensity substitutes into the regression equation of the standard curve of corresponding element to be measured in step A, phase in sample to be tested is calculated
Answer the mass concentration of element to be measured.
Wherein, sample to be tested takes 5g, is put into sample test box, gently up-down vibration, makes the bottom surface of sample to be tested (i.e.
The shadow surface of X-ray) in flat smooth, free from flaw, not loose state.Similarly, flying dust standard sample takes 5g respectively, puts respectively
Enter in sample test box, gently up-down vibration, it is bottom surface flat smooth, free from flaw and not loose school to make flying dust standard sample
Quasi- print.Then, respectively by equipped with sample to be tested sample test box, equipped with the sample test box of flying dust standard sample, examining
It surveys end and wraps Mylar films (i.e. mylar film), be put into XRF and be detected.
The instrument testing conditions of the Xray fluorescence spectrometer (XRF) are：Measurement atmosphere：Air atmosphere or vacuum；Sample
Pattern：Blocky or film；Collimator：1mm, 3mm, 5mm or 10mm.
Embodiment 3
It is 6 the ratio between by weight by the preparation method of flying dust standard sample in step 2 in embodiment 1:4, take calcium oxide and two
Silica is made into substrate after being mixed.The flying dust standard sample of known concentration is taken again, and substrate mixing, substrate is added
The weight ratio that substance is added with flying dust standard sample is followed successively by 5:0、4:1、3:2、2:3、1:4、0:5,6 flying dust marks are prepared altogether
Quasi- sample, according in flying dust standard sample each Heavy Metallic Elements contain numerical quantity, calculate each in 6 flying dust standard patterns
Heavy metal element contains numerical quantity.The concrete content of eight Heavy Metallic Elements of Pb, Cr, Cu, Zn, As, Se, Cd and Ba therein is shown in
Table 1.
Content/(mg/kg) of eight Heavy Metallic Elements in 1 flying dust standard sample of table
5g is taken to be packed into the mating sample test box of XRF instruments respectively 6 flying dust standard samples, flying dust standard sample is in sample
It is in powdered in product testing cassete, X ray test face flat smooth, the free from flaw of sample test box is made by gently up-down vibration.
It is measured respectively using XRF pairs of 6 flying dust standard samples, measures the two of each heavy metal element of each flying dust standard sample
Secondary x-ray fluorescence intensity, according to the secondary x rays fluorescence intensity of same Heavy Metallic Elements in 6 flying dust standard samples with it is right
The content for the heavy metal element answered establishes standard curve, is fitted, is obtained to the curve using simple linear regression analysis method
To unary linear regression equation：Y=ax+b, wherein x are the content of a certain Heavy Metallic Elements in flying dust standard sample, and y is
The corresponding flying dust standard sample that measures of XRF instruments in corresponding heavy metal element secondary x rays fluorescence intensity, a is curve
Slope, b are the intercept of curve.The unary linear regression equation fit standard curve obtained is measured, as shown in Figure 1.It measures and obtains
Unary linear regression equation and its related coefficient be shown in Table 2.
The fit equation and R of 2 eight Heavy Metallic Elements XRF standard working curves of table2Value
| Element | Fit equation | R2Value |
| Pb | Y=0.013x+0.148 | 0.999 |
| Cu | Y=0.018x+1.72 | 0.998 |
| Zn | Y=0.024x-8.847 | 0.998 |
| Ba | Y=0.007x+0.737 | 0.998 |
| As | Y=0.08x-0.153 | 0.990 |
| Se | Y=0.072-0.139 | 0.945 |
| Cd | Y=0.009x+1.662 | 0.989 |
| Cr | Y=0.05x+0.172 | 0.994 |
As shown in Table 2, the XRF standard curves of this eight Heavy Metallic Elements of Pb, Cr, Cu, Zn, As, Se, Cd and Ba is related
Coefficient reaches 0.9, most of to reach 0.99 or more, illustrates that the standard curve accuracy in the present invention is high, it is fixed to can be applied to
Amount analysis.
Embodiment 4
By the flying dust standard sample that number is 6 in the table 1 of embodiment 3, the XRF standard curves established in embodiment 3 are used
20 duplicate measurements have been carried out, it is for statistical analysis to measurement result, as a result shown in table 3.From the data in table 3 Ba, Pb,
The relative deviation of this 8 kinds of metallic element measurement results of Zn, Cr, Cu, As, Se and Cd is respectively 0.50%, 0.35%, 0.17%,
1.24%, 0.89%, 3.18%, 8.92% and 3.07%, relative standard deviation values are smaller, and in credible range, precision can expire
Foot detection needs.
3 method precision of table
Embodiment 5
The incineration of refuse flyash sample to be tested that 6 collection in worksite are had chosen in experiment uses the XRF established in embodiment 3
Standard curve directly detects, meanwhile, it is detected using ICP-OES using after complete resolution, comparing result is shown in Table 4.By
Table 4 is it is found that four Heavy Metallic Elements Pb, Cr, Cu and the Cd most paid close attention in flying dust, XRF measured values most connect with ICP detected values
Closely, also relatively, XRF values and the ICP detected values of Ba elements omit for the XRF values of tri- heavy metal species of Zn, As and Se and ICP detected values
Variant, all in all, the XRF standard curves of this 8 kinds of elements of Pb, Cr, Cu, Cd, Zn, As, Se, Ba have preferably accurately
Degree, can be applied to put into practice, and meet detection needs.
4 flying dust analysis result of table compares (mg/kg)
Embodiment 6
The flying dust of certain garbage burning factory sample within continuous 40 days, has quantitatively been examined using the XRF established in embodiment 3
Mark directrix curve is detected, and obtains the changes of contents situation of tetra- heavy metal species of Pb, Cr, Cu and Cd for containing in daily flying dust
As shown in Figure 2.Tetra- heavy metal species content fluctuation of Pb, Cd, Cu and Cr compares in the incineration plant flying dust it can be seen from attached drawing 2
Greatly, the fluctuation range of Pb is more than 1000mg/kg, and the fluctuation range of Cd is more than 200mg/kg, and the fluctuation range of Cu is more than 200mg/
The fluctuation range of kg, Cr also reach 80mg/kg or so.This also illustrates that garbage burning factory flying dust is during stabilization processes, such as
Fruit adds ratio according to fixed chelating agent, it is impossible to ensure that content of beary metal all stably reaches landfill mark in the flying dust of every day
It is accurate.And since the detection method of the fly-ash heavy metal content used now is complicated for operation, time-consuming, so as to cause stabilization agent
Ratio adjustment seriously lags behind fly-ash heavy metal changes of contents, and the middle XRF detection methods used, reach real-time prison through the invention
It surveys and regulates and controls, this can not only ensure that manufacture stabilizing fly ash is up to standard, moreover it is possible to which that reduces chelating adds cost, is more in line with modern intelligence
The development of energyization level.
The above-described embodiments merely illustrate the principles and effects of the present invention, and is not intended to limit the present invention.It is any ripe
The personage for knowing this technology can all carry out modifications and changes to above-described embodiment without violating the spirit and scope of the present invention.Cause
This, institute is complete without departing from the spirit and technical ideas disclosed in the present invention by those of ordinary skill in the art such as
At all equivalent modifications or change, should by the present invention claim be covered.
Claims (8)
1. a kind of method measuring various heavy content in flying dust using XRF instrument quantitatives, includes the following steps：
1) flying dust is collected, as sample to be tested；
2) take flying dust standard sample, substrate be added, be made into a series of lead containing various concentration, chromium, copper, zinc, arsenic, caesium, cadmium,
The flying dust standard sample of barium element；
3) the flying dust standard sample that sample to be tested, step 2) are prepared in step 1) is subjected to Xray fluorescence spectrometer detection respectively,
It is quantified using calibration curve method, obtains the content of lead, chromium, copper, zinc, arsenic, caesium, cadmium, barium element in sample to be tested.
2. a kind of method that various heavy content in flying dust is measured using XRF instrument quantitatives according to claim 1,
Be characterized in that, in step 2), a concentration of 800~6000mg/kg of lead in the flying dust standard sample, chromium a concentration of 60~
4000mg/kg, a concentration of 300~6500mg/kg of copper, zinc concentration be 2500~75000mg/kg, arsenic a concentration of 5~
150mg/kg, a concentration of 1~50mg/kg of caesium, a concentration of 160~350mg/kg of cadmium, a concentration of 200~12000mg/ of barium
kg。
3. a kind of method that various heavy content in flying dust is measured using XRF instrument quantitatives according to claim 1,
It is characterized in that, in step 2), the substrate is selected from calcium hydroxide, calcium oxide, silica, aluminium oxide, potassium oxide, oxidation
One or more combinations in sodium, iron oxide, magnesia.
4. a kind of method that various heavy content in flying dust is measured using XRF instrument quantitatives according to claim 3,
It is characterized in that, the substrate is calcium oxide and silica, and the weight ratio that the calcium oxide is added with silica is
3:7~7:3.
5. a kind of method that various heavy content in flying dust is measured using XRF instrument quantitatives according to claim 1,
It is characterized in that, in step 2), in the flying dust standard sample, the weight ratio of the substrate and the addition of flying dust standard sample
It is 5:0~0:5.
6. a kind of method that various heavy content in flying dust is measured using XRF instrument quantitatives according to claim 1,
It is characterized in that, in step 3), the instrument testing conditions of the Xray fluorescence spectrometer are：Measurement atmosphere：Air atmosphere is true
It is empty；Sample formulations：Blocky or film；Collimator：1mm, 3mm, 5mm or 10mm.
7. a kind of method that various heavy content in flying dust is measured using XRF instrument quantitatives according to claim 6,
It is characterized in that, the instrument testing conditions of the Xray fluorescence spectrometer are：Measurement atmosphere：Air atmosphere；Sample formulations：It is blocky；
Collimator：10mm.
8. a kind of method that various heavy content in flying dust is measured using XRF instrument quantitatives according to claim 1,
It is characterized in that, in step 3), the calibration curve method includes the following steps：
A) by the substrate of acquisition and flying dust standard sample, a series of flying dust standard sample for being made into various concentrations carries out XRF
Detection, obtains the linear relationship of the x-ray fluorescence intensity and the mass concentration of corresponding element to be measured of each element to be measured respectively,
To which corresponding unitary linear work curve is drawn out in fitting, calculate separately to obtain the recurrence of the standard curve of 8 kinds of elements to be measured
Equation；
B sample to be tested) is subjected to XRF detections, by the x-ray fluorescence intensity of the element to be measured of each in the sample to be tested of acquisition, generation
The matter of corresponding element to be measured in sample to be tested is calculated in the regression equation for entering the standard curve of corresponding element to be measured in step A
Measure concentration.
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