Microwave sample pretreatment method applied to organic carbon detection

A treatment method, organic carbon technology, applied in the field of microwave chemistry, to achieve the effects of easy operation, sufficient reaction, and fast heating speed

Inactive Publication Date: 2013-03-27
TIANJIN NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

And using microwave as the pretreatment method when measuring the total organic carbon in various samples has not been reported yet.

Method used

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  • Microwave sample pretreatment method applied to organic carbon detection
  • Microwave sample pretreatment method applied to organic carbon detection
  • Microwave sample pretreatment method applied to organic carbon detection

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] according to figure 1 As shown, put a 10-gram, 40-mesh carbon-free nickel oxide absorbing material into a 20-ml quartz or ceramic crucible, and then put 0.2 grams of the soil sample to be tested into the crucible. The crucible is put into the bottom of a sealed suitable quartz container permeable to microwave radiation, the upper part of the container is connected with the carrier gas inlet, and the lower part is connected with the carrier gas outlet. The carrier gas is a mixed gas of high-purity nitrogen with a flow rate of 100 ml / min and pure oxygen at 20 ml / min. When a microwave oven radiation device with a power of 800W is used, the temperature of the absorbing material rises to 1100°C in 2 minutes, and the organic carbon in the soil sample is oxidized to carbon dioxide and then carried by the carrier gas into the non-dispersive infrared spectrometer for measurement. The measurement results are consistent with those of commercial products. The results of the resist...

Embodiment 2

[0033] according to figure 1 As shown, a 15-gram, 60-mesh carbon-free cobalt trioxide absorbing material is put into a 30-milliliter quartz colorimetric tube, and then 0.2 g of the soil sample to be tested is also put into the colorimetric tube. The upper part of the colorimetric tube is tightly plugged with a stopper, which is provided with a carrier gas inlet and a carrier gas outlet, and the carrier gas inlet pipe extends into the depth of the colorimetric tube and is close to the position of the wave-absorbing material. The carrier gas is a mixed gas of high-purity nitrogen and 10 ml / min of pure oxygen at a flow rate of 50 ml / min. The colorimetric tube is inserted into the microwave oven at the upper middle part of the microwave oven and the part of the colorimetric tube containing the absorbing material is completely exposed to the interior of the microwave oven. When a microwave radiation device with a power of 800W is used, the temperature of the absorbing material ris...

Embodiment 3

[0035] according to figure 2 As shown, the ferrosilicon absorbing material with a weight of 20 grams and a particle size of 50 mesh is made into a molding device with a groove in the center. The groove is just enough to insert the quartz tube (1 cm in diameter) containing the sample, and the depth of the groove is 2 cm so that all the samples at the bottom of the tube can be fully heated by the wave-absorbing material. The quartz or ceramic tube containing the sample has a carrier gas inlet and a carrier gas outlet. The carrier gas is a mixed gas of high-purity nitrogen and 10 ml / min of pure oxygen at a flow rate of 30 ml / min. When using a microwave radiation device with a power of 800W, the temperature of the absorbing material rises to 120°C in 2 minutes, and the organic carbon in the water sample in the quartz tube is oxidized to carbon dioxide and then loaded into the non-dispersive infrared spectrometer by the carrier gas for measurement. The results are consistent wit...

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Abstract

The invention discloses a microwave sample pretreatment method applied to organic carbon detection, which is characterized in that when the sample is heated by a wave-absorbing material in a manner of direct contacting, silicon iron, nickel sesquioxide, cobalt sesquioxide, molybdenum sulfide, ferric sulfide, ferroferric oxide, manganese dioxide, nickel oxide, tungsten trioxide, molybdenum sulfide, copper pyrite, cuprous sulfide, ferrite compound, or other wave-absorbing materials free from carbon are adopted as wave-absorbing media; and when the sample is indirectly heated by the wave-absorbing material, carbon, silicon carbide, silicon iron, nickel sesquioxide, cobalt sesquioxide, molybdenum sulfide, ferric sulfide, ferroferric oxide, manganese dioxide, nickel oxide, tungsten trioxide, molybdenum disulfide, copper pyrite, cuprous sulfide, ferrite compound, or other wave-absorbing materials are taken as the wave-absorbing media. The sample pretreatment method disclosed by the invention has the advantages of being rapid in temperature raising speed, complete in reaction and the like, and is suitable for pretreatment of detection of various organic carbon samples.

Description

technical field [0001] The invention belongs to the field of microwave chemistry, in particular to a method and a device for sample pretreatment when microwaves are used for organic carbon determination. Background technique [0002] Microwave is an electromagnetic wave with a frequency of 0.3-300 GHz and a wavelength of 0.1-100 cm. Utilize microwave energy as a kind of energy, and selectively heat the material through energy dissipation inside the material, which has the incomparable advantages of traditional heating methods such as uniform heating, high thermal efficiency, rapid heating and stopping of heating, and improved material properties. It has obvious advantages in improving production efficiency and improving production conditions, so it has been widely used in many fields such as chemistry, metallurgy and materials. As a rapid heating method, microwave heating has been widely used in the field of analytical chemistry. However, the current applications are mainl...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N1/44
Inventor 段旭川
Owner TIANJIN NORMAL UNIVERSITY
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