CN105067537B - The detection method of micro lead in a kind of particulate matter - Google Patents
The detection method of micro lead in a kind of particulate matter Download PDFInfo
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- CN105067537B CN105067537B CN201510417255.2A CN201510417255A CN105067537B CN 105067537 B CN105067537 B CN 105067537B CN 201510417255 A CN201510417255 A CN 201510417255A CN 105067537 B CN105067537 B CN 105067537B
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Abstract
The invention discloses a kind of detection methods of micro lead in Atmospheric particulates, include the following steps：Particulate matter is collected on filter membrane using impacting type dry method sampler；Filter membrane is shredded and is placed in beaker, adds in the mixed solution of concentrated nitric acid and perchloric acid, with heater plate until particle all dissolves, the digestion solution that must be transparent；Digestion solution is added in colorimetric cylinder, it is separately added into ammonium citrate, hydroxylamine hydrochloride, using the pH value of ammonium hydroxide modulation digestion solution, potassium tartrate, dithizone ethanol solution and CTAB ethanol solutions are added into the digestion solution after modulation pH value, finally with nitric acid constant volume；Solution absorbance is measured at 470nm using ultraviolet-uisible spectrophotometer, is compared with standard curve, obtains lead content in particulate matter.What detection process of the present invention used is no poisonous drugs, and safety is preferable, and when detection is not only enriched with lead ion, has also covered the calcium for influencing lead ion detection, sodium plasma, detection efficiently, it is accurate.
Description
Technical field
The present invention relates to environmental monitoring technology field, the detection method of micro lead in particularly a kind of particulate matter.
Background technology
With the quickening of world industry process, lead and its compound use scope and scale are growing, and make the dirt of lead
Dye develops into global environmental problem from localised region environmental problem.Lead is a kind of with accumulative, polyaffinity
Metallic poison, all toxic effect is respectively organized to human body, be health detection in an important indicator.Many chemicals are in ring
Harmless final compound may be degraded to after being detained a period of time in border, but lead can not degrade again, once it is discharged into environment very
Still maintain its availability for a long time.Due to the long-term persistence of lead in the environment, and have to many vital tissues stronger latent
In property toxicity, so lead is listed in strong pollutant range always.
The method for measuring lead at present has atomic absorption method, atomic fluorescence spectrometry, catalytic polarographic method, catalytic kinetics
Method, photometry etc..Compared with other several detection methods, photometry is with simplicity, quick, high sensitivity, instrument are simple, price
It the advantages that cheap, easily universal, at low cost, is used widely.
People's Republic of China's Occupational sanitary standard《Lead and its assay method of compound in workplace air
(GBZ/T160.10-2004)》, Lead in Air dirt, lead fume acquire with miillpore filter, and after salpeter solution dissolving, lead ion is in pH
The dithizone lead red complex of generation is reacted with dithizone in 8.5~11.0 solution, it can be by chloroform recovery, in 520nm wavelength
The lower absorbance for measuring extracting solution, is quantified.But this method is cumbersome, and the KCN of severe toxicity has been used to shelter
Agent, toxic carbon tetrachloride make extractant, and adverse effect is caused to human body and environment.
Invention content
The purpose of the present invention is to provide a kind of detection methods of micro lead in particulate matter functional, toxicity is low.
Realize the object of the invention technical solution be：The detection method of micro lead in a kind of particulate matter, including following
Step：
Step 1, particulate matter is collected on filter membrane using impacting type dry method sampler；
Step 2, filter membrane is shredded and be placed in beaker, added in the mixed solution of concentrated nitric acid and perchloric acid, use heater plate
Until particle all dissolves, the digestion solution that must be transparent；
Step 3, digestion solution is added in colorimetric cylinder, is separately added into ammonium citrate, hydroxylamine hydrochloride, is disappeared using ammonium hydroxide modulation
The pH value of solution is solved, potassium tartrate, dithizone-ethanol solution and CTAB- second are added into the digestion solution after modulation pH value
Alcoholic solution, finally with nitric acid constant volume；
Step 4, solution absorbance is measured at 470nm using ultraviolet-visible spectrophotometer, is compared with standard curve,
Obtain lead content in particulate matter.
Preferably, filter membrane described in step 1 is glass fiber filter, and the nitric acid mass concentration is 0.6-1.2%.
Preferably, the usage amount of the mixed solution of concentrated nitric acid described in step 2 and perchloric acid be 10-20ml, concentrated nitric acid with
The volume ratio of perchloric acid is (6-9):1.
Preferably, the digestion solution volume added in described in step 3 in colorimetric cylinder is 8~15ml；The matter of the ammonium citrate
Measure a concentration of 15-25%, the 10-15% that volume is the digestion solution；The mass concentration of the hydroxylamine hydrochloride for 15-25%,
Volume is the 5-10% of the digestion solution.
Preferably, using the pH value of ammonium hydroxide modulation digestion solution described in step 3, pH value modulation range is 8-9.
Preferably, potassium tartrate mass concentration described in step 3 is 8-12%, and volume is the digestion solution modulated after pH value
25-35%；The mass concentration of the dithizone-ethanol solution is 0.03-0.07%, and volume is the digestion solution modulated after pH value
25-35%；The mass concentration of the CTAB- ethanol solutions is 8-15%, and volume is that the digestion solution after modulation pH value is
10-15%.
Compared with prior art, the present invention its remarkable advantage is：(1) what detection process used is no poisonous drugs,
Safety is preferable；(2) lead ion is not only enriched with when detecting, has also covered the calcium for influencing lead ion detection, sodium plasma, detection is high
It imitates, is accurate.
Description of the drawings
Fig. 1 is the full wavelength scanner figure of lead standard solution of the present invention.
Fig. 2 is the canonical plotting of lead in the embodiment of the present invention 1.
Fig. 3 is the canonical plotting of lead in the embodiment of the present invention 2.
Fig. 4 is the canonical plotting of lead in the embodiment of the present invention 3.
Specific embodiment
Below in conjunction with the accompanying drawings and specific embodiment is described in further detail the present invention.
The detection method of micro lead, includes the following steps in particulate matter of the present invention：
Step 1, particulate matter is collected on filter membrane using impacting type dry method sampler；The filter membrane is filtered for glass fibre
Film, the nitric acid mass concentration are 0.6-1.2%.
Step 2, filter membrane is shredded and be placed in beaker, added in the mixed solution of concentrated nitric acid and perchloric acid, use heater plate
Until particle all dissolves, the digestion solution that must be transparent；The usage amount of the mixed solution of the concentrated nitric acid and perchloric acid is
The volume ratio of 10-20ml, concentrated nitric acid and perchloric acid is (6-9):1.
Step 3, digestion solution is added in colorimetric cylinder, is separately added into ammonium citrate, hydroxylamine hydrochloride, the addition colorimetric cylinder
In digestion solution volume be 8~15ml；The mass concentration of the ammonium citrate is 15-25%, volume is the digestion solution
10-15%；The 5-10% that the mass concentration of the hydroxylamine hydrochloride is 15-25%, volume is the digestion solution；Utilize ammonium hydroxide
Modulate digestion solution pH value, pH value modulation range be 8-9, to modulation pH value after digestion solution in add potassium tartrate,
Dithizone-ethanol solution and CTAB- ethanol solutions, finally with nitric acid constant volume；The potassium tartrate mass concentration be 8-12%, body
25-35% of the product for the digestion solution after modulation pH value；The mass concentration of the dithizone-ethanol solution is 0.03-0.07%,
Volume be modulate pH value after digestion solution 25-35%；The mass concentration of the CTAB- ethanol solutions be 8-15%, volume
It is 10-15% for the digestion solution after modulation pH value.
Step 4, solution absorbance is measured at 470nm using ultraviolet-visible spectrophotometer, is compared with standard curve,
Obtain lead content in particulate matter.
Embodiment 1
The Pb standard solutions of 10 μ g/ml are made into 1% nitric acid.0ml, 0.05ml are added in the colorimetric cylinder of 25ml,
The lead standard solution of 0.1ml, 0.2ml, 0.4ml, 0.6ml, 0.8ml add 15% ammonium citrate 0.8ml, 15% hydroxylamine hydrochloride
0.4ml modulates PH=8 or so, then add the potassium tartrate of 2ml 8% with ammonium hydroxide (1+1), and 0.03% dithizone-ethyl alcohol of 2ml is molten
Liquid and 8%CTAB- ethanol solution 0.8ml, are finally settled to 25ml with 1% nitric acid.It is complete with ultraviolet-visible spectrophotometer
Length scanning standard specimen is as shown in Figure 1, it is known that has an Absorption Characteristics peak, therefore other standards solution is measured at 470nm in 470nm
It is as shown in Figure 2 to obtain standard curve for absorbance：Y=0.3469x+0.0103, R2=0.9958.
A blank glass fiber filter membrane is taken, weigh to obtain m0=357.2mg utilizes TSP impacting type dry method samplers samples
Atmospheric particulates, gas flow 100L/min, spot sampling are performed according to GBZ 159, and the sampling time is for 24 hours.Sampling is completed
Afterwards, it is m to weigh glass fiber filter weight1=379.7mg.Filter membrane is shredded, is placed in 50ml beakers, adds in 9:1 dense nitre
Acid and perchloric acid 15ml, are cleared up with heater plate, until particle all dissolves, the digestion solution that must be transparent.
Digestion solution 8ml is taken to be placed in 25ml colorimetric cylinders, adds 15% ammonium citrate 0.8ml, 15% hydroxylamine hydrochloride 0.4ml,
With ammonium hydroxide (1+1) modulation PH=8 or so, then add the potassium tartrate of 2ml 8%, 0.03% dithizone-ethanol solution of 2ml and
8%CTAB- ethanol solution 0.8ml, are finally settled to 25ml with 1% nitric acid.Solution absorbance is measured at 470nm, with mark
Directrix curve compares, and show that lead content is 0.2056 μ g/ml in particulate matter, then the lead content of Atmospheric Grains is 228.4 μ g/
G, lead tolerance is 0.036 μ g/m in air3。
Embodiment 2
The Pb standard solutions of 10 μ g/ml are made into 0.6% nitric acid.0ml, 0.1ml are added in the colorimetric cylinder of 50ml,
The lead standard solution of 0.2ml, 0.4ml, 0.8ml, 1.2ml, 1.6ml add 25% ammonium citrate 3ml, 25% hydroxylamine hydrochloride
3ml modulates PH=9 or so, then add the potassium tartrate of 7ml 12% with ammonium hydroxide (1+1), and 0.07% dithizone-ethyl alcohol of 7ml is molten
Liquid and 15%CTAB- ethanol solution 3ml, are finally settled to 50ml with 0.6% nitric acid.It is molten that other standards are measured at 470nm
Liquid absorbance, it is as shown in Figure 3 to obtain standard curve：Y=0.3469x+0.0103, R2=0.9958.
A blank glass fiber filter membrane is taken, weigh to obtain m0=369.7mg utilizes TSP impacting type dry method samplers samples
Atmospheric particulates, gas flow 100L/min, spot sampling are performed according to GBZ 159, and the sampling time is for 24 hours.Sampling is completed
Afterwards, it is m to weigh glass fiber filter weight1=398.2mg.Filter membrane is shredded, is placed in 50ml beakers, adds in 6:1 dense nitre
Acid and perchloric acid 20ml, are cleared up with heater plate, until particle all dissolves, the digestion solution that must be transparent.
Digestion solution 15ml is taken to be placed in 50ml colorimetric cylinders, adds 25% ammonium citrate 2.25ml, 25% hydroxylamine hydrochloride
2.25ml modulates PH=9 or so, then add the potassium tartrate of 5.25ml 12%, the 0.07% pair of sulphur of 5.25ml with ammonium hydroxide (1+1)
Hydrazone-ethanol solution and 15%CTAB- ethanol solution 2.25ml, are finally settled to 50ml with 0.6% nitric acid.It is surveyed at 470nm
Determine solution absorbance, compared with standard curve, show that lead content is 0.2461 μ g/ml in particulate matter, then Atmospheric Grains
Lead content for 431.8 μ g/g, lead tolerance is 0.085 μ g/m in air3。
Embodiment 3
The Pb standard solutions of 10 μ g/ml are made into 1% nitric acid.0ml, 0.1ml are added in the colorimetric cylinder of 25ml,
The lead standard solution of 0.2ml, 0.4ml, 0.8ml, 1.2ml, 1.6ml add 20% ammonium citrate 1.5ml, 20% hydroxylamine hydrochloride
0.8ml modulates PH=9 or so, then add the potassium tartrate of 4ml 10%, 0.05% dithizone-ethyl alcohol of 5ml with ammonium hydroxide (1+1)
Solution and 10%CTAB- ethanol solution 2ml, are finally settled to 25ml with 1% nitric acid.It is molten that other standards are measured at 470nm
Liquid absorbance, it is as shown in Figure 4 to obtain standard curve：Y=0.3474x+0.0137, R2=0.992.
A blank glass fiber filter membrane is taken, weigh to obtain m0=375.6mg utilizes TSP impacting type dry method samplers samples
Atmospheric particulates, gas flow 100L/min, spot sampling are performed according to GBZ 159, and the sampling time is for 24 hours.Sampling is completed
Afterwards, it is m to weigh glass fiber filter weight1=397.3mg.Filter membrane is shredded, is placed in 50ml beakers, adds in 9:1 dense nitre
Acid and perchloric acid 15ml, are cleared up with heater plate, until particle all dissolves, the digestion solution that must be transparent.
Digestion solution 10ml is taken to be placed in 25ml colorimetric cylinders, adds 20% ammonium citrate 1.5ml, 20% hydroxylamine hydrochloride 0.8ml,
With ammonium hydroxide (1+1) modulation PH=9 or so, then add the potassium tartrate of 4ml 10%, 0.05% dithizone-ethanol solution of 5ml and
10%CTAB- ethanol solution 2ml, are finally settled to 25ml with 1% nitric acid.Solution absorbance is measured at 470nm, with standard song
Line compares, and show that lead content is 0.1034 μ g/ml in particulate matter, then the lead content of Atmospheric Grains is 119.1 μ g/g, greatly
Lead tolerance is 0.018 μ g/m in gas3。
To sum up, what detection process of the present invention used is no poisonous drugs, and safety is preferable, can effectively solve existing national standard
Middle the problem of using Severely poisonous reagents.
Claims (3)
1. the detection method of micro lead in a kind of Atmospheric particulates, which is characterized in that include the following steps：
Step 1, particulate matter is collected on filter membrane using impacting type dry method sampler；
Step 2, filter membrane is shredded and is placed in beaker, add in the mixed solution of concentrated nitric acid and perchloric acid, with heater plate until
Particle all dissolves, the digestion solution that must be transparent；
Step 3, digestion solution is added in colorimetric cylinder, is separately added into ammonium citrate, hydroxylamine hydrochloride, it is molten using ammonium hydroxide modulation resolution
The pH value of liquid, into the digestion solution after modulation pH value, to add potassium tartrate, dithizone-ethanol solution and CTAB- ethyl alcohol molten
Liquid, finally with nitric acid constant volume；
Step 4, solution absorbance is measured at 470nm using ultraviolet-visible spectrophotometer, is compared with standard curve, obtained
Lead content in particulate matter；
The digestion solution volume added in described in step 3 in colorimetric cylinder is 8~15ml；The mass concentration of the ammonium citrate is 15-
25%th, volume is the 10-15% of the digestion solution；The mass concentration of the hydroxylamine hydrochloride is 15-25%, volume is described disappears
Solve the 5-10% of solution；
Using the pH value of ammonium hydroxide modulation digestion solution described in step 3, pH value modulation range is 8-9；
Potassium tartrate mass concentration described in step 3 be 8-12%, volume be modulation pH value after digestion solution 25-35%；Institute
The mass concentration of dithizone-ethanol solution is stated as 0.03-0.07%, volume be the 25-35% of the digestion solution after modulation pH value；
The mass concentration of the CTAB- ethanol solutions is 8-15%, and volume is that the digestion solution after modulation pH value is 10-15%.
2. the detection method of micro lead in particulate matter according to claim 1, which is characterized in that filter membrane described in step 1
For glass fiber filter, the nitric acid mass concentration is 0.6-1.2%.
3. the detection method of micro lead in particulate matter according to claim 1, which is characterized in that dense nitre described in step 2
The usage amount of acid and the mixed solution of perchloric acid is 10-20ml, and the volume ratio of concentrated nitric acid and perchloric acid is (6-9):1.
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| CN106770261A (en) * | 2017-02-08 | 2017-05-31 | 北京爱富迪医药科技发展有限公司 | A kind of kit for water sample lead field quick detection |
| CN106546587A (en) * | 2017-02-08 | 2017-03-29 | 北京爱富迪医药科技发展有限公司 | A kind of water sample trace lead quick detection kit |
| CN111060467A (en) * | 2020-01-03 | 2020-04-24 | 四川中衡检测技术有限公司 | Method for rapidly determining trace metals in atmospheric suspended particles |
| CN111707627B (en) * | 2020-06-30 | 2023-03-31 | 武汉钢铁有限公司 | Rapid analysis method for nitrate radical in reusable metallurgical waste ammonia water |
| CN115436309B (en) * | 2022-08-29 | 2023-05-30 | 天津大学 | Ultraviolet detection method for rapidly and accurately measuring lead concentration |
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| CN103487427A (en) * | 2013-09-27 | 2014-01-01 | 苏州国环环境检测有限公司 | Method for detecting metallic elements in atmospheric exhaust gas particulates |
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