CN201637703U - Combustion tube for CHN analyzer - Google Patents
Combustion tube for CHN analyzer Download PDFInfo
- Publication number
- CN201637703U CN201637703U CN2009202125453U CN200920212545U CN201637703U CN 201637703 U CN201637703 U CN 201637703U CN 2009202125453 U CN2009202125453 U CN 2009202125453U CN 200920212545 U CN200920212545 U CN 200920212545U CN 201637703 U CN201637703 U CN 201637703U
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- tube
- silica wool
- flame tube
- chn
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Abstract
The utility model relates to a combustion tube for a CHN analyzer. A protective tube and an ash tube are sequentially ranged in the combustion tube from top to bottom, and then, filamentary silver, silica wool, PbCrO4, silica wool, MgO<->Ag2WO4 and silica wool are sequentially filled in the combustion tube from bottom to top following the ash tube. The utility model is applicable to the analysis of fluorine-containing organic compounds, including high-fluorine compounds and perfluor compounds, all measured values are in the permissible error range of the microanalysis precision, and the absolute error is +/-0.30 percent. The utility model is also applicable to the CHN analysis of other organic compounds in various types.
Description
Technical field
The utility model belongs to the parts of a kind of hydrocarbon nitrogen (CHN) elemental analyser, is a kind of flame tube of CHN analyzer specifically.
Background technology
The test philosophy of CHN elemental analyser is that sample perfect combustion is decomposed, and products of combustion is through purifying the place to go chaff interference and only keeping later tested gas componant N by the reduction tube conversion
2, CO
2And H
2O separates these compositions and detection with suitable method.In this process, the perfect combustion of sample is crucial, the character of this and sample, and the character of catalytic oxidant is relevant with the combustion system of sample.
Flame tube is a vitals of CHN automatic elemental analyzer, and its effect is that the catalytic oxidation sample makes it to decompose fully.The size of flame tube is different and different with model because of the manufacturer of instrument, and the filling of each catalytic oxidant highly can separate with silica wool between the different catalytic oxidant because of the size of flame tube is different.The flame tube that common hydrocarbon nitrogen automatic elemental analyzer is joined is a quartz ampoule, and protection tube and ash pipe are the accessory of flame tube, make by quartzy material.
Fluorinated organic compound, the microanalysis of hydrocarbon nitrogen element is a difficult problem that perplexs people for a long time in particularly high fluorine, the perfluoro organic compound, this is not only because C-F key stability is strong, easy fracture not, prior reason is that the products of combustion hydrogen fluoride of fluorochemicals can generate volatile silicon tetrafluoride with silicon dioxde reaction, thereby the introducing analytical error, heavy corrosion gas circuit tube wall simultaneously shortens instrument serviceable life.Hydrogen richness is very low even be zero in high fluorine, the perfluoro organic compound, and the hydrogen atom in the combustion decomposition process in the compound is obviously not enough, thereby causes the direct carburet of fluorine and generate carbon tetrafluoride.The carbon tetrafluoride thermal stability is extremely strong, is difficult for decomposing, and goes out the peak immediately following nitrogen in the detachment process of products of combustion, and thermal conductivity cell detector can't be distinguished this, thereby causes the negative error of carbon value and the positive error of nitrogen value.Architectural characteristic in view of above-mentioned high fluorine, perfluorochemical, most CHN automatic elemental analyzers are unsuitable for analyzing fluorine-containing particularly high fluorine, perfluoro organic compound, its key reason is that the filling material of the flame tube that traditional CHN automatic elemental analyzer is adopted does not have very strong catalytic oxidation ability on the one hand, can not eliminate chaff interference and pollutant that fluorochemicals burning back is produced on the other hand.Flame tube provided by the utility model has overcome the deficiency of traditional filling material for this type of compound analysis effectively.In addition, the utility model also improves the weighing technique of high fluorine and perfluoro organic compound.
The utility model content
The utility model purpose is the deficiency that overcomes traditional flame tube, and a kind of flame tube of improved CHN automatic elemental analyzer is provided.
The flame tube that CHN automatic elemental analyzer of the present utility model is joined and the accessories protecting pipe and the ash pipe of flame tube are quartzy material.Fill filamentary silver, silica wool, PbCrO in the flame tube from bottom to top successively
4, silica wool, MgO-Ag
2WO
4And silica wool, on this layer silica wool, be arranged in order ash pipe and protection tube from bottom to top.
The effect of ash pipe is that the combustion residue of sample with the Xi Zhou of parcel sample temporarily collected, and regularly removes with convenient.The external diameter of protection tube is slightly littler than the internal diameter of flame tube, and its effect is the protection flame tube.Falling into flame tube but before not entering the ash pipe as yet, can not contact with the sample of Xi Zhou parcel, can cause flame tube to break otherwise Xi Zhou meets a large amount of heats that the oxygen burning emits, so need add a protection tube with the flame tube inwall.In the filling material of flame tube, magnesium oxide also can at high temperature generate the very strong magnesium fluoride (MgO+2HF=MgF of stability with hydrogen fluoride reaction except that having stronger catalytic oxidation performance
2+ H
2O), thus reach the purpose that efficient removal fluorine disturbs.Common described MgO-Ag
2WO
4Be both potpourris, mass ratio is about 1: 12.Be in the graininess MgO-Ag of flame tube high-temperature region
2WO
4Thereby not only having overcome magnesium oxide volume behind high temperature sintering effectively easily shrinks and is broken into the unimpeded defective of powder retardance air-flow, and having utilized the silver salt oxidizing agent can the efficient absorption halogen and the character of interference element such as sulphur, two kinds of oxygenants can act synergistically to improve oxidation usefulness simultaneously.Facts have proved MgO-Ag
2WO
4Be a kind of catalytic oxidant of effective function admirable, can successfully analyze high fluorine organic compound.Be in the low temperature catalyst PbCrO of flame tube low-temperature space
4, be to absorb the higher oxygenant of fluorine efficient.Filamentary silver can be got rid of the interference of halogen, sulphur.Silica wool gets rid of interference products of combustion such as halogen, phosphorus pentoxide, metal oxide in the mode of physisorption.
Recommend one high be 370mm, diameter is that the protection tube height of flame tube of the CHN automatic elemental analyzer of 27mm is 65mm, the height of ash pipe is 32mm.
Filling mode is: fill 5mm filamentary silver/5mm silica wool/10mmPbCrO from bottom to top successively
4/ 5mm silica wool/120mmMgO-Ag
2WO
4/ 3mm silica wool is loaded onto ash pipe and protection tube successively on the silica wool of the superiors.Separate with silica wool between each filling material in the flame tube.As shown in Figure 1.
The utility model is used for the analysis of a series of high fluorine organic compounds, measured value all in microanalysis precision permissible error scope, absolute error ± 0.30%.
Description of drawings
Fig. 1 is the synoptic diagram of flame tube of the present invention;
Among Fig. 1,1-protection tube, 2-ash pipe, 3-silica wool, 4-wolframic acid silver+magnesium oxide, 5-silica wool, 6-plumbous chromate, 7-silica wool, 8-filamentary silver.
Fig. 2 is the CHN ultimate analysis spectrogram of standard substance antifebrin;
Peak in the spectrogram is followed successively by the N peak, C peak and H peak.
Fig. 3 is the CHN ultimate analysis spectrogram with the teflon of traditional flame tube gained;
Peak in the spectrogram is followed successively by the N peak, C peak and H peak.
Fig. 4 is the CHN ultimate analysis spectrogram with the teflon of flame tube gained of the present invention.
Embodiment
To help to understand the utility model by following embodiment, but not limit content of the present utility model.
With the height that adopts method shown in Figure 1 to load is 370mm, and diameter is that the flame tube of 27mm is installed on a kind of CHN automatic elemental analyzer, and the height of arranging and load material is as shown in the table:
| Numbering | Title |
| 1 | Protection tube 65mm |
| 2 | Ash pipe 32mm |
| 3 | Silica wool 3mm |
| 4 | Wolframic acid silver+ |
| 5 | Silica wool 5mm |
| 6 | Plumbous chromate 10mm |
| 7 | Silica wool 5mm |
| 8 | Filamentary silver 5mm |
Other operating conditions of analyser is all continued to use the condition of common sample, comprises the filling (using Cu) of reduction tube etc.
(perfluorochemical is sneaked into V with the fluorinated organic compound of the accurate weighing of tin container made (Xi Zhou) parcel
2O
5, WO
3) sample gone in the combustion reaction pipe by the auto injection dribbling of elemental analyser, owing to meet the moment burning of oxygen and tin container made, the decomposition temperature of sample can reach about 1800 ℃, under the effect of the catalytic oxidant of filling out, the special filler in the tested fluorochemicals in the burned pipe in F burning back absorbs in the combustion reaction pipe.The graininess MgO-Ag of high-temperature region
2WO
4In MgO and HF reaction and F absorbed Ag
2WO
4Strong catalysed oxidn fluorine-containing even high fluorine or perfluorochemical are decomposed fully, be in the PbCrO of low-temperature space
4The effect of strong absorption F F that burning is produced further absorb.Sneak into the oxygenant V in the perfluorochemical
2O
5, WO
3Reduced CF
4The generation probability, improved burning efficiency.Filamentary silver can be got rid of the interference of halogen, sulphur.Silica wool gets rid of interference products of combustion such as halogen, phosphorus pentoxide, metal oxide in the mode of physisorption.In combustion process, the CHN element in the tested fluorochemicals is converted into CO respectively
2, H
2The oxide NOx of O and N.This mixed gas as carrier gas, enters reduction tube and the reduction Cu effect of being loaded with He, removes excessive O
2, and NOx is converted into N fully
2N
2, CO
2And H
2O is taken out of afterwards separated from reduction tube by He and is brought into conductance cell successively by He and measure, and the electric signal that chemical composition changes into is transfused to computing machine and carries out data processing.
Fig. 2 is the CHN ultimate analysis spectrogram of the standard substance antifebrin of ultimate analysis special use, and the peak in the spectrogram is followed successively by the N peak, C peak and H peak.
Fig. 3 is the CHN ultimate analysis spectrogram with the perfluoro organic compound teflon of traditional flame tube gained, owing to do not contain the N element at teflon, the peak that occurs at place, N peak among the figure is the chaff interference CF of incomplete decomposing by analysis
4, the percentage composition with the peak area at the C peak among the figure or the C that peak height calculates is lower than calculated value simultaneously.This explanation, traditional flame tube is not suitable for the analysis of CHN element in the fluorinated organic compound.
The percentage composition of no N peak and the C that calculates is in microanalysis precision permissible error scope (absolute error ± 0.30%) among Fig. 4.Practice is proof also, adopts the automatic elemental analyzer of flame tube of the present utility model not to be corroded because analyze fluorinated organic compound.This explanation, the flame tube of improved of the present utility model has solved inhibition CF
4Generation and get rid of the Air thing and the problem of chaff interference, be applicable to the analysis of CHN element in the fluorinated organic compound.
Claims (2)
1. the flame tube of a CHN analyzer is characterized in that filling filamentary silver, silica wool, PbCrO from bottom to top successively in the flame tube of described CHN analyzer
4, silica wool, MgO-Ag
2WO
4And silica wool, on this layer silica wool, be arranged in order ash pipe and protection tube from bottom to top.
2. the flame tube of CHN analyzer as claimed in claim 1 is characterized in that separating with silica wool between each filling material in the flame tube of described CHN analyzer.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009202125453U CN201637703U (en) | 2009-12-04 | 2009-12-04 | Combustion tube for CHN analyzer |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009202125453U CN201637703U (en) | 2009-12-04 | 2009-12-04 | Combustion tube for CHN analyzer |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN201637703U true CN201637703U (en) | 2010-11-17 |
Family
ID=43082207
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2009202125453U Expired - Fee Related CN201637703U (en) | 2009-12-04 | 2009-12-04 | Combustion tube for CHN analyzer |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN201637703U (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105823041A (en) * | 2016-05-18 | 2016-08-03 | 南京理工大学 | Telescopic nanofluid fuel combustion characteristic testing device |
| CN105864761A (en) * | 2016-05-18 | 2016-08-17 | 南京理工大学 | Nano-fluid fuel combustion characteristic testing device with adjustable top cover |
| CN107174929A (en) * | 2017-06-26 | 2017-09-19 | 北京海光仪器有限公司 | A kind of catalysing tube, preparation method and application method for eliminating Matrix effects |
| CN108196005A (en) * | 2017-12-07 | 2018-06-22 | 中国科学院东北地理与农业生态研究所 | Carbon in a kind of organic liquid sample, nitrogen, hydrogen, sulfur content assay method |
| CN110208319A (en) * | 2019-06-05 | 2019-09-06 | 北京诺德泰科仪器仪表有限公司 | A kind of Dumars azotometer reaction tube |
-
2009
- 2009-12-04 CN CN2009202125453U patent/CN201637703U/en not_active Expired - Fee Related
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105823041A (en) * | 2016-05-18 | 2016-08-03 | 南京理工大学 | Telescopic nanofluid fuel combustion characteristic testing device |
| CN105864761A (en) * | 2016-05-18 | 2016-08-17 | 南京理工大学 | Nano-fluid fuel combustion characteristic testing device with adjustable top cover |
| CN107174929A (en) * | 2017-06-26 | 2017-09-19 | 北京海光仪器有限公司 | A kind of catalysing tube, preparation method and application method for eliminating Matrix effects |
| CN108196005A (en) * | 2017-12-07 | 2018-06-22 | 中国科学院东北地理与农业生态研究所 | Carbon in a kind of organic liquid sample, nitrogen, hydrogen, sulfur content assay method |
| CN110208319A (en) * | 2019-06-05 | 2019-09-06 | 北京诺德泰科仪器仪表有限公司 | A kind of Dumars azotometer reaction tube |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20101117 Termination date: 20141204 |
|
| EXPY | Termination of patent right or utility model |