Method for detecting trace lead in particulate matters

A detection method and particle technology, applied in the preparation of test samples, color/spectral characteristic measurement, etc., can solve the problems of harmful effects on the human body and the environment, cumbersome operation, etc., and achieve the effect of good safety and high detection efficiency

Inactive Publication Date: 2015-11-18
NANJING UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the method is cumbersome to operate, and highly toxic KCN is used as a masking agent and toxic ca

Method used

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  • Method for detecting trace lead in particulate matters
  • Method for detecting trace lead in particulate matters
  • Method for detecting trace lead in particulate matters

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Use 1% nitric acid to prepare 10μg / ml Pb standard solution. Add 0ml, 0.05ml, 0.1ml, 0.2ml, 0.4ml, 0.6ml, 0.8ml of lead standard solution in a 25ml colorimetric tube, add 0.8ml of 15% ammonium citrate, 0.4ml of 15% hydroxylamine hydrochloride, and use Ammonia water (1+1) is used to adjust the pH to about 8, then add 2ml of 8% potassium tartrate, 2ml of 0.03% dithizone-ethanol solution, and 0.8ml of 8% CTAB-ethanol solution, and finally dilute with 1% nitric acid to 25ml. Scan the standard sample at full wavelength with a UV-Vis spectrophotometer such as figure 1 As shown, it can be seen that there is an absorption characteristic peak at 470nm, so other standard solution absorbances are measured at 470nm, and the standard curve is obtained as figure 2 Shown: y=0.3469x+0.0103, R 2 = 0.9958.

[0029] Take a blank glass fiber filter membrane and weigh it to obtain m 0 =357.2mg, use the TSP impact dry sampler to collect atmospheric particulate matter, the gas flow rate ...

Embodiment 2

[0032] Use 0.6% nitric acid to prepare 10μg / ml Pb standard solution. Add 0ml, 0.1ml, 0.2ml, 0.4ml, 0.8ml, 1.2ml, 1.6ml lead standard use solution in the colorimetric tube of 50ml, add 25% ammonium citrate 3ml, 25% hydroxylamine hydrochloride 3ml, use ammoniacal liquor ( 1+1) Adjust the pH to about 9, add 7ml of 12% potassium tartrate, 7ml of 0.07% dithizone-ethanol solution and 3ml of 15% CTAB-ethanol solution, and finally dilute to 50ml with 0.6% nitric acid. Measure the absorbance of other standard solutions at 470nm to obtain a standard curve such as image 3 Shown: y=0.3469x+0.0103, R 2 = 0.9958.

[0033] Take a blank glass fiber filter membrane and weigh it to obtain m 0 =369.7mg, use the TSP impact dry sampler to collect atmospheric particulate matter, the gas flow rate is 100L / min, the on-site sampling is carried out according to GBZ159, and the sampling time is 24h. After the sampling is completed, weigh the weight of the glass fiber filter membrane as m 1 = 398.2...

Embodiment 3

[0036]Use 1% nitric acid to prepare 10μg / ml Pb standard solution. Add 0ml, 0.1ml, 0.2ml, 0.4ml, 0.8ml, 1.2ml, 1.6ml of lead standard solution in a 25ml colorimetric tube, add 1.5ml of 20% ammonium citrate, 0.8ml of 20% hydroxylamine hydrochloride, and use Ammonia water (1+1) was used to adjust the pH to about 9, and then 4ml of 10% potassium tartrate, 5ml of 0.05% dithizone-ethanol solution and 2ml of 10% CTAB-ethanol solution were added, and finally the volume was adjusted to 25ml with 1% nitric acid. Measure the absorbance of other standard solutions at 470nm to obtain a standard curve such as Figure 4 Shown: y=0.3474x+0.0137, R 2 = 0.992.

[0037] Take a blank glass fiber filter membrane and weigh it to obtain m 0 =375.6mg, use the TSP impact dry sampler to collect atmospheric particulate matter, the gas flow rate is 100L / min, the on-site sampling is carried out in accordance with GBZ159, and the sampling time is 24h. After the sampling is completed, weigh the weight o...

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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 [0001] The invention relates to the technical field of environmental monitoring, in particular to a method for detecting trace amounts of lead in particulate matter. Background technique [0002] With the acceleration of the world's industrialization process, the scope and scale of the use of lead and its compounds are expanding day by day, making lead pollution develop from a local and regional environmental problem to a global environmental problem. Lead is an accumulative and multi-affinity metal poison that has toxic effects on various tissues of the human body and is an important indicator in health testing. Many chemicals may degrade to harmless final compounds after a period of time in the environment, but lead cannot be degraded and remains available for a long time once released into the environment. Due to the long-term persistence of lead in the environment and its strong potential toxicity to many living tissues, lead has always been listed as a ...

Claims

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Application Information

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IPC IPC(8): G01N21/31G01N1/28
Inventor 杨毅茆平李展蒋婷梅冯曙艳刘颖李燕
Owner NANJING UNIV OF SCI & TECH
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