Cadmium lead electrochemical detection method based on sulfur-doped graphene
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A technology of sulfur-doped graphene and detection method, applied in the direction of material electrochemical variables, etc., can solve problems such as no relevant reports, and achieve the effect of low detection limit
Active Publication Date: 2017-11-17
XINJIANG TECHN INST OF PHYSICS & CHEM CHINESE ACAD OF SCI
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Although there are a few reports on the modification of polysulfide compounds on the surface of graphene, there are no related reports on the modification principle of...
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preparation example Construction
[0043] b, preparation of graphene oxide suspension:
[0044] Accurately weigh 80 mg of the graphite oxide powder obtained in step a, dissolve it in 40 mL of deionized water, make a 2 mg / mL suspension, ultrasonically disperse for 50 minutes, and adjust the pH to 7-8 with 1 mol / L potassium hydroxide solution;
[0045] c. Preparation of polysulfide / graphene composites:
[0046] Dissolve 0.385g of sodium sulfide into 7mL of deionized water to form an aqueous solution of sodium sulfide, add 0.1536g of sulfur powder, and stir ultrasonically until it becomes clear and transparent. The reaction equation is:
[0047] Na 2 S+(x-1)S=Na 2 Sx (x=2, 3, 4, 5)
[0048] Then, under the protection of nitrogen, the transparent solution was added dropwise to the graphene oxide suspension solution dispersed by ultrasound in step b, and refluxed at a temperature of 80°C for 24 hours, and the obtained solution was filtered and washed with deionized water for 3-5 Then ultrasonically disperse in 8...
Embodiment 2
[0056] By the method of the present invention to the detection of water sample:
[0057] Use laboratory tap water samples to make HAc-NaAc solution with pH=5.0, take 10mL, add heavy metals in the following amounts (μg / L): 0, 50, 100, record the peak current intensity at different concentrations, measure 3 times respectively, and then according to See Table 2 for linear equation calculation recovery rate and relative standard deviation;
[0058] Table 2
[0059]
[0060] As can be seen from the table: the heavy metal recovery rate is between 95.8%-103.8%, illustrating that the cadmium lead electrochemical detection method based on sulfur-doped graphene of the present invention can be used for the cadmium lead concentration detection in the water sample, has better results.
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Abstract
The invention discloses a cadmium lead electrochemical detection method based on sulfur-doped graphene. An electrochemical sensor involved in the method is composed of a polysulfide/graphene-Nafion modified working electrode, an Ag/AgCl reference electrode, a Pt wire counter electrode, an electrolytic tank and an electrochemical workstation. The adopted electrochemical technology is differential pulse anodic stripping voltammetry. The sensor has a cadmium ion detection range of 2.0-300microgL<-1>, a lead ion detection range of 1.0-300microgL<-1>, and the detection limits are 0.67microgL<-1> and 0.17microgL<-1> respectively, and are both 4.5 times and 59 times lower than standard drinking water values given by WHO. At the same time, the sensor shows good reproducibility, stability and anti-interference performance. In detection of the content of lead and cadmium ions in tap water, the sensor shows good sensitivity and reproducibility. The sensor can accurately, quickly and simultaneously detect the content of cadmium and lead ions on site, and therefore has good practical application prospect.
Description
technical field [0001] The invention relates to an electrochemical detection method of cadmium and lead based on sulfur-doped graphene, and the electrochemical technology: differential pulse anode stripping voltammetry. Background technique [0002] Graphene has attracted extensive attention in the field of electrochemical analysis of highly toxic heavy metal ions due to its good electrical conductivity, large specific surface area, and many active sites. However, most of the functionalized active sites of graphene are located on the edge of graphite, and the basal carbon, which accounts for most of the atoms in graphene, does not participate in the effective enrichment of heavy metals. Aiming at the problem of making full use of the graphene carbon-based surface, research on high-sensitivity heavy metal electrochemical sensing based on graphene composite nanomaterials is carried out. Using low-cost polysulfides as graphene functional modifiers, the strong chemical adsorpti...
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IPC IPC(8): G01N27/48
CPCG01N27/48
Inventor 胡广志姜如愿夏木西卡玛尔·买买提
Owner XINJIANG TECHN INST OF PHYSICS & CHEM CHINESE ACAD OF SCI
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