CN105067537A - Method for detecting trace lead in particulate matters - Google Patents
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- CN105067537A CN105067537A CN201510417255.2A CN201510417255A CN105067537A CN 105067537 A CN105067537 A CN 105067537A CN 201510417255 A CN201510417255 A CN 201510417255A CN 105067537 A CN105067537 A CN 105067537A
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Abstract
The invention discloses a method for detecting trace lead in particulate matters. The method comprises following steps: the particulate matters are collected on a filter membrane by an impact type dry sampler; the filter membrane is cut into pieces and placed in a beaker, a concentrated nitric acid and perchloric acid mixed solution is added, the mixture is heated by a heating plate until the particulate matters are totally dissolved, and a transparent digestion solution is obtained; the digestion solution is added to a colorimetric tube, ammonium citrate and hydroxylamine hydrochloride are added respectively, the PH value of the digestion solution is regulated with ammonium hydroxide, potassium tartrate, a dithizone-ethanol solution and a CTAB (cetyltrimethyl ammonium bromide)-ethanol solution are added to the digestion solution after PH value regulation, and nitric acid is adopted for constant volume finally; the solution absorbance is measured by an ultraviolet-visible spectrophotometer at 470 nm and is compared with a standard curve, and the content of lead in the particulate matters is obtained. Non-poisonous drugs are adopted in a detection process, higher safety is realized, lead ions are enriched and calcium ions, sodium ions and the like influencing lead ion detection are covered during detection, and the detection is efficient and accurate.
Description
Technical field
The present invention relates to environmental monitoring technology field, particularly the detection method of micro lead in a kind of particle.
Background technology
Along with the quickening of world industry process, plumbous and compound usable range and scale expanding day, make plumbous pollution develop into global environmental problem from localised region property environmental problem.Lead a kind ofly has metallic poison that is accumulative, polyaffinity, respectively organizes all toxic effect to human body, is an important indicator during health detects.May be degraded to harmless finalization compound after many chemicals are detained a period of time in the environment, but lead cannot be degraded again, once enter environment still keep its availability for a long time.Due to lead long-term persistence in the environment, there is stronger potentiality toxicity to many vital tissues again, so lead is listed in strong pollutant scope always.
The method of current mensuration lead has atomic absorption method, atomic fluorescence spectrometry, catalytic polarographic method, By Catalytic Kinetics, photometry etc.Compared with other several detection methods, photometry have easy, quick, highly sensitive, instrument is simple, cheap, easy universal, low cost and other advantages, be used widely.
The People's Republic of China's Occupational hygienic standard assay method (GBZ/T160.10-2004) of plumbous and compound " in the workplace air ", Lead in Air dirt, lead fume miillpore filter gather, after salpeter solution dissolves, lead ion reacts the plumbous red complex of the dithizone generated in the solution of pH8.5 ~ 11.0 with dithizone, can by chloroform recovery, under 520nm wavelength, measure the absorbance of extract, carry out quantitatively.But, the method complex operation, and employ severe toxicity KCN makes screening agent, poisonous phenixin makes extractant, deleterious effect is caused to human body and environment.
Summary of the invention
The object of the present invention is to provide the detection method of micro lead in a kind of functional, particle that toxicity is low.
The technical solution realizing the object of the invention is: the detection method of micro lead in a kind of particle, comprises the following steps:
Step 1, utilizes impacting type dry method sampling thief to be collected on filter membrane by particle;
Step 2, shreds filter membrane and is placed in beaker, adds the mixed solution of red fuming nitric acid (RFNA) and perchloric acid, with heater plate until particle all dissolves, obtains the digestion solution of transparent shape;
Step 3, in color comparison tube, add digestion solution, add ammonium citrate, oxammonium hydrochloride respectively, utilize ammoniacal liquor to modulate the pH value of digestion solution, in the digestion solution after modulation pH value, add potassium tartrate, dithizone-ethanolic solution and CTAB-ethanolic solution again, finally use nitric acid constant volume;
Step 4, utilizes ultraviolet-visible spectrophotometer to measure solution absorbance in 470nm place, with typical curve comparison, draws lead content in particle.
Preferably, filter membrane described in step 1 is glass fiber filter, and described nitric acid mass concentration is 0.6-1.2%.
Preferably, the use amount of the mixed solution of red fuming nitric acid (RFNA) described in step 2 and perchloric acid is 10-20ml, and the volume ratio of red fuming nitric acid (RFNA) and perchloric acid is (6-9): 1.
Preferably, the digestion solution volume added described in step 3 in color comparison tube is 8 ~ 15ml; The 10-15% that the mass concentration of described ammonium citrate is 15-25%, volume is described digestion solution; The 5-10% that the mass concentration of described oxammonium hydrochloride is 15-25%, volume is described digestion solution.
Preferably, utilize ammoniacal liquor to modulate the pH value of 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 25-35% of the digestion solution after modulation pH value; The mass concentration of described dithizone-ethanolic solution is 0.03-0.07%, and volume is the 25-35% of the digestion solution after modulation pH value; The mass concentration of described CTAB-ethanolic solution is 8-15%, volume be digestion solution after modulation pH value for 10-15%.
Compared with prior art, its remarkable advantage is in the present invention: what (1) testing process adopted is without poisonous drugs, and security is better; (2) not only enriched lead ion when detecting, has also covered the calcium, the sodium plasma that affects lead ion and detect, detects efficient, accurate.
Accompanying drawing explanation
Fig. 1 is the full wavelength scanner figure of the plumbous standard solution of the present invention.
Fig. 2 is canonical plotting plumbous in the embodiment of the present invention 1.
Fig. 3 is canonical plotting plumbous in the embodiment of the present invention 2.
Fig. 4 is canonical plotting plumbous in the embodiment of the present invention 3.
Embodiment
Below in conjunction with drawings and the specific embodiments, the present invention is described in further detail.
The detection method of micro lead in particle of the present invention, comprises the following steps:
Step 1, utilizes impacting type dry method sampling thief to be collected on filter membrane by particle; Described filter membrane is glass fiber filter, and described nitric acid mass concentration is 0.6-1.2%.
Step 2, shreds filter membrane and is placed in beaker, adds the mixed solution of red fuming nitric acid (RFNA) and perchloric acid, with heater plate until particle all dissolves, obtains the digestion solution of transparent shape; The use amount of the mixed solution of described red fuming nitric acid (RFNA) and perchloric acid is 10-20ml, and the volume ratio of red fuming nitric acid (RFNA) and perchloric acid is (6-9): 1.
Step 3, adds digestion solution in color comparison tube, adds ammonium citrate, oxammonium hydrochloride respectively, described in the digestion solution volume added in color comparison tube be 8 ~ 15ml; The 10-15% that the mass concentration of described ammonium citrate is 15-25%, volume is described digestion solution; The 5-10% that the mass concentration of described oxammonium hydrochloride is 15-25%, volume is described digestion solution; Utilize ammoniacal liquor to modulate the pH value of digestion solution, pH value modulation range is 8-9, adds potassium tartrate, dithizone-ethanolic solution and CTAB-ethanolic solution again, finally use nitric acid constant volume in the digestion solution after modulation pH value; Described potassium tartrate mass concentration is 8-12%, and volume is the 25-35% of the digestion solution after modulation pH value; The mass concentration of described dithizone-ethanolic solution is 0.03-0.07%, and volume is the 25-35% of the digestion solution after modulation pH value; The mass concentration of described CTAB-ethanolic solution is 8-15%, volume be digestion solution after modulation pH value for 10-15%.
Step 4, utilizes ultraviolet-visible spectrophotometer to measure solution absorbance in 470nm place, with typical curve comparison, draws lead content in particle.
Embodiment 1
Nitric acid with 1% is made into the Pb standard solution of 10 μ g/ml.0ml is added, 0.05ml, 0.1ml in the color comparison tube of 25ml, 0.2ml, 0.4ml, 0.6ml, the plumbous standard solution of 0.8ml, add 15% ammonium citrate 0.8ml, 15% oxammonium hydrochloride 0.4ml, modulate about PH=8 with ammoniacal liquor (1+1), add the potassium tartrate of 2ml8% again, 0.03% dithizone-the ethanolic solution of 2ml, and 8%CTAB-ethanolic solution 0.8ml, be finally settled to 25ml with the nitric acid of 1%.With ultraviolet-visible spectrophotometer full wavelength scanner standard specimen as shown in Figure 1, known have an Absorption Characteristics peak at 470nm, therefore measures other standards solution absorbance at 470nm place, obtain typical curve as shown in Figure 2: y=0.3469x+0.0103, R
2=0.9958.
Get a blank glass fiber filter membrane, weigh to obtain m
0=357.2mg, utilize TSP impacting type dry method samplers sample Atmospheric particulates, gas flow is 100L/min, and spot sampling performs according to GBZ159, and the sampling time is 24h.After having sampled, weighing glass fiber filter weight is m
1=379.7mg.Filter membrane is shredded, is placed in 50ml beaker, add red fuming nitric acid (RFNA) and the perchloric acid 15ml of 9:1, clear up with heater plate, until particle all dissolves, obtain the digestion solution of transparent shape.
Get digestion solution 8ml and be placed in 25ml color comparison tube, add 15% ammonium citrate 0.8ml, 15% oxammonium hydrochloride 0.4ml, about PH=8 is modulated with ammoniacal liquor (1+1), add the potassium tartrate of 2ml8% again, 0.03% dithizone-the ethanolic solution of 2ml, and 8%CTAB-ethanolic solution 0.8ml, be finally settled to 25ml with the nitric acid of 1%.Measure solution absorbance in 470nm place, with typical curve comparison, show that in particle, lead content is 0.2056 μ g/ml, so the lead content of Atmospheric Grains is 228.4 μ g/g, and in air, lead tolerance is 0.036 μ g/m
3.
Embodiment 2
Nitric acid with 0.6% is made into the Pb standard solution of 10 μ g/ml.0ml is added, 0.1ml, 0.2ml in the color comparison tube of 50ml, 0.4ml, the plumbous standard solution of 0.8ml, 1.2ml, 1.6ml, add 25% ammonium citrate 3ml, 25% oxammonium hydrochloride 3ml, modulates about PH=9 with ammoniacal liquor (1+1), then adds the potassium tartrate of 7ml12%, 0.07% dithizone-the ethanolic solution of 7ml and 15%CTAB-ethanolic solution 3ml, be finally settled to 50ml with the nitric acid of 0.6%.Measure other standards solution absorbance at 470nm place, obtain typical curve as shown in Figure 3: y=0.3469x+0.0103, R
2=0.9958.
Get a blank glass fiber filter membrane, weigh to obtain m
0=369.7mg, utilize TSP impacting type dry method samplers sample Atmospheric particulates, gas flow is 100L/min, and spot sampling performs according to GBZ159, and the sampling time is 24h.After having sampled, weighing glass fiber filter weight is m
1=398.2mg.Filter membrane is shredded, is placed in 50ml beaker, add red fuming nitric acid (RFNA) and the perchloric acid 20ml of 6:1, clear up with heater plate, until particle all dissolves, obtain the digestion solution of transparent shape.
Get digestion solution 15ml and be placed in 50ml color comparison tube, add 25% ammonium citrate 2.25ml, 25% oxammonium hydrochloride 2.25ml, about PH=9 is modulated with ammoniacal liquor (1+1), add the potassium tartrate of 5.25ml12% again, 0.07% dithizone-the ethanolic solution of 5.25ml and 15%CTAB-ethanolic solution 2.25ml, be finally settled to 50ml with the nitric acid of 0.6%.Measure solution absorbance in 470nm place, with typical curve comparison, show that in particle, lead content is 0.2461 μ g/ml, so the lead content of Atmospheric Grains is 431.8 μ g/g, and in air, lead tolerance is 0.085 μ g/m
3.
Embodiment 3
Nitric acid with 1% is made into the Pb standard solution of 10 μ g/ml.0ml is added, 0.1ml, 0.2ml in the color comparison tube of 25ml, 0.4ml, the plumbous standard solution of 0.8ml, 1.2ml, 1.6ml, add 20% ammonium citrate 1.5ml, 20% oxammonium hydrochloride 0.8ml, modulates about PH=9 with ammoniacal liquor (1+1), then adds the potassium tartrate of 4ml10%, 0.05% dithizone-the ethanolic solution of 5ml and 10%CTAB-ethanolic solution 2ml, be finally settled to 25ml with the nitric acid of 1%.Measure other standards solution absorbance at 470nm place, obtain typical curve as shown in Figure 4: y=0.3474x+0.0137, R
2=0.992.
Get a blank glass fiber filter membrane, weigh to obtain m
0=375.6mg, utilize TSP impacting type dry method samplers sample Atmospheric particulates, gas flow is 100L/min, and spot sampling performs according to GBZ159, and the sampling time is 24h.After having sampled, weighing glass fiber filter weight is m
1=397.3mg.Filter membrane is shredded, is placed in 50ml beaker, add red fuming nitric acid (RFNA) and the perchloric acid 15ml of 9:1, clear up with heater plate, until particle all dissolves, obtain the digestion solution of transparent shape.
Get digestion solution 10ml and be placed in 25ml color comparison tube, add 20% ammonium citrate 1.5ml, 20% oxammonium hydrochloride 0.8ml, about PH=9 is modulated with ammoniacal liquor (1+1), add the potassium tartrate of 4ml10% again, 0.05% dithizone-the ethanolic solution of 5ml and 10%CTAB-ethanolic solution 2ml, be finally settled to 25ml with 1% nitric acid.Measure solution absorbance in 470nm place, with typical curve comparison, show that in particle, lead content is 0.1034 μ g/ml, so the lead content of Atmospheric Grains is 119.1 μ g/g, and in air, lead tolerance is 0.018 μ g/m
3.
To sum up, what testing process of the present invention adopted is without poisonous drugs, and security is better, can effectively solve the problem using Severely poisonous reagents in existing GB.
Claims (6)
1. the detection method of micro lead in Atmospheric particulates, is characterized in that, comprise the following steps:
Step 1, utilizes impacting type dry method sampling thief to be collected on filter membrane by particle;
Step 2, shreds filter membrane and is placed in beaker, adds the mixed solution of red fuming nitric acid (RFNA) and perchloric acid, with heater plate until particle all dissolves, obtains the digestion solution of transparent shape;
Step 3, in color comparison tube, add digestion solution, add ammonium citrate, oxammonium hydrochloride respectively, utilize ammoniacal liquor to modulate the pH value of digestion solution, in the digestion solution after modulation pH value, add potassium tartrate, dithizone-ethanolic solution and CTAB-ethanolic solution again, finally use nitric acid constant volume;
Step 4, utilizes ultraviolet-visible spectrophotometer to measure solution absorbance in 470nm place, with typical curve comparison, draws lead content in particle.
2. the detection method of micro lead in particle according to claim 1, it is characterized in that, filter membrane described in step 1 is glass fiber filter, and described nitric acid mass concentration is 0.6-1.2%.
3. the detection method of micro lead in particle according to claim 1, it is characterized in that, the use amount of the mixed solution of red fuming nitric acid (RFNA) described in step 2 and perchloric acid is 10-20ml, and the volume ratio of red fuming nitric acid (RFNA) and perchloric acid is (6-9): 1.
4. the detection method of micro lead in particle according to claim 1, it is characterized in that, the digestion solution volume added described in step 3 in color comparison tube is 8 ~ 15ml; The 10-15% that the mass concentration of described ammonium citrate is 15-25%, volume is described digestion solution; The 5-10% that the mass concentration of described oxammonium hydrochloride is 15-25%, volume is described digestion solution.
5. the detection method of micro lead in particle according to claim 1, is characterized in that, utilize ammoniacal liquor to modulate the pH value of digestion solution described in step 3, pH value modulation range is 8-9.
6. the detection method of micro lead in particle according to claim 1, it is characterized in that, potassium tartrate mass concentration described in step 3 is 8-12%, and volume is the 25-35% of the digestion solution after modulation pH value; The mass concentration of described dithizone-ethanolic solution is 0.03-0.07%, and volume is the 25-35% of the digestion solution after modulation pH value; The mass concentration of described CTAB-ethanolic solution is 8-15%, volume be digestion solution after modulation pH value for 10-15%.
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| 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 |
| CN111707627A (en) * | 2020-06-30 | 2020-09-25 | 武汉钢铁有限公司 | Rapid analysis method for nitrate radical in reusable metallurgical waste ammonia water |
| CN115436309A (en) * | 2022-08-29 | 2022-12-06 | 天津大学 | Ultraviolet detection method for quickly and accurately measuring lead concentration |
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| 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 |
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| CN115436309A (en) * | 2022-08-29 | 2022-12-06 | 天津大学 | Ultraviolet detection method for quickly and accurately measuring lead concentration |
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