CN102410949A - Sample preparation device for fire scene oxidant infrared spectrum testing - Google Patents
Sample preparation device for fire scene oxidant infrared spectrum testing Download PDFInfo
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- CN102410949A CN102410949A CN2011102099982A CN201110209998A CN102410949A CN 102410949 A CN102410949 A CN 102410949A CN 2011102099982 A CN2011102099982 A CN 2011102099982A CN 201110209998 A CN201110209998 A CN 201110209998A CN 102410949 A CN102410949 A CN 102410949A
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Abstract
The invention relates to a sample preparation device for fire scene oxidant infrared spectrum testing. The sample preparation device comprises a loading container, a connecting piece, a sample pool, an empting valve, a three-opening device and a gas leading hose. The loading container is connected with the emptying valve, and is hermetically connected with a lower end opening of a buffering pipe at a lower part of the sample pool through the connecting piece; an upper part of the sample pool is connected with the buffering pipe through an atmosphere balancing pipe; a gas duct is arranged in the buffering pipe, the gas duct is connected with a liquid pool, and a piston is arranged at the connecting part; an upper part opening of the buffering pipe is connected with the three-opening device through the gas leading hose; a lower end of the three-opening device is connected with a gas receiver, and the gas receiver is connected with a vacuum pump through the gas leading hose. The sample preparation device has the advantages of simple structure, low cost, good stability, high enriching efficiency, small solvent background influence and rapidness and convenience in operation.
Description
Technical field
The present invention relates to target detection thing adsorption and enrichment device, particularly the adsorption and enrichment device of flammable flammable liquid composition in the scene of fire burning remains.
Background technology
The generation of the case of setting fire causes serious harm to social stability and people life property safety.The offender usually utilizes some combustion adjuvants, sets fire like flammable flammable liquids such as gasoline, diesel oil.When getting into the scene of fire, the fire investigation personnel reconnoitre; Find that low-burning, a plurality of point of origins etc. are doubtful and set fire during vestige; Suspected Area and burning remains on every side thereof will be extracted; In order to the chamber check and analysis that experimentize, further whether evaluation has the existence of combustion adjuvant and has used which kind of combustion adjuvant, thus the carrying out and help cracking of case of the work that carries investigation forward.
The context of detection in the laboratory, the Fourier infrared spectrum technology is quick, convenient with it, chemical functional group's characteristic features has obtained good application by force on the combustion adjuvant residue detection is identified.Yet, when examination of infrared spectrum, aspect the specimen preparation of committed step, also exist some shortcomings at present.In actual conditions; Combustion adjuvant is ignited and most of can the burning totally under the condition of the scene of a fire; Only there is combustion adjuvant composition a small amount of or trace to residue in the burning remains matrix; Need extract it this moment with organic solvents such as a certain amount of carbon disulphide, chloroforms, and the organic solvent extraction liquid that will contain the combustion adjuvant composition is after being concentrated on a small quantity, and is very undesirable through the IR spectroscopy effect of classic method ATR (attenuated total reflection) annex or liquid cell.This is because the combustion adjuvant composition is with respect to extracting with organic solvent content very little, and this will cause infrared analysis result's the solvent background of gained very high, cover the infrared absorption peak information of the combustion adjuvant composition that will detect.In addition,, the extraction drop after concentrating is carried out infrared analysis on kbr tablet,, in the infrared scan process, can volatilize poor stability because the boiling point of organic solvents such as carbon disulphide is lower if adopt pellet technique; And treat that the combustion adjuvant oil film that forms after solvent evaporates is fully is thin, be unfavorable for detecting of characteristic absorption peak; Drip repeatedly and can form thick relatively rete; But this method is complex operation on the one hand; Cause big analyte loss on the other hand, this is for being that a spot of measured object is extremely disadvantageous, and produced simultaneously poisonous organic solvent volatile gas body also is a kind of harm to the experimenter.Because potassium bromide has suction-operated to combustion adjuvants such as gasoline; The potassium bromide powder is mixed the back concentrate the removal organic solvent with the organic solvent of extraction; Has good stability; And can realize concentration effect preferably, yet blank kbr tablet causes error with the heavy different meetings of potassium bromide sample strip, and this method required time is longer.
Therefore, to the problem of above-mentioned existence, a kind of method for making sample of IR spectroscopy and device thereof of can effectively cooperating of development and Design has positive meaning.
Summary of the invention
The objective of the invention is to overcome the deficiency that exists in the combustion adjuvant infrared analysis method of the existing scene of a fire, provide a cover cost low, have good stability, bioaccumulation efficiency is high, the solvent background influence is little, operation is a fast and convenient sample preparation device that is used for scene of a fire combustion adjuvant examination of infrared spectrum.
A kind of sample preparation device that is used for scene of a fire combustion adjuvant examination of infrared spectrum that the present invention proposes; Form by slide glass container, web member, sample cell, atmospheric valve, three mouthfuls of devices and soft air-guide pipe; Wherein: the slide glass container is connected to atmospheric valve, and the slide glass container is through web member and airtight connection of separator tube lower ending opening place that is positioned at the sample cell bottom; Sample cell top links to each other through barometric pipe with separator tube; Separator tube inside is provided with mozzle, and mozzle links to each other with sample cell, and the junction is provided with piston; Separator tube upper opening place connects three mouthfuls of devices through wireway, and three mouthfuls of device lower ends connect the gas receptacle; Three mouthfuls of devices link to each other with vacuum pump through soft air-guide pipe again.
Among the present invention, said slide glass container ratio of height to diameter is 0.1:1～10:1.
Among the present invention, said separator tube height is 40:1～1:1 with the diameter ratio.
Among the present invention, said sample cell is provided with barometric pipe.
The invention has the advantages that:
(1) this apparatus structure is simple, and cost is low, and is easy to assembly;
(2) this device adopts the sample preparation ability big, can be used in the continuous processing of many amount of liquid;
(3) device has the gas receiver, prevents the environmental hazard that poisonous organic solvent volatilization causes;
(4) this device can be under negative pressure constantly with flammable flammable liquid residual component adsorption and enrichment on kbr tablet, raise the efficiency thereby shorten extraction time greatly;
(5) this device sample preparation adopts all risk insurance to stay method, directly implements the enrichment of maximum target detection thing as the liquid-solid extraction subsequent step.
Description of drawings
Fig. 1 is a kind of sample preparation device synoptic diagram that is used for scene of a fire combustion adjuvant examination of infrared spectrum.
Label among the figure, 1 is the slide glass container, and 2 is web member, and 3 is separator tube, and 4 for having the mozzle of piston, and 5 is barometric pipe, and 6 is sample cell, and 7 is three mouthfuls of devices, and 8 is the gas receptacle, and 9 is atmospheric valve, and 10 is soft air-guide pipe.
Embodiment
Combine accompanying drawing to further specify the present invention through embodiment below.
Embodiment 1: as shown in Figure 1; This device is made up of slide glass container 1, web member 2, separator tube 3, mozzle 4, barometric pipe 5, sample cell 6, three mouthfuls of devices 7, gas receptacle 8, atmospheric valve 9 and soft air-guide pipes 10; It is characterized in that; Slide glass container 1 is connected to atmospheric valve 9, and the lower ending opening place is airtight is connected through web member 2 and the separator tube that is positioned at sample cell 6 bottoms 3 for slide glass container 1; Sample cell 6 tops link to each other through barometric pipe 5 with separator tube 3; Separator tube 3 inside are provided with mozzle 4, and mozzle 4 links to each other with sample cell 6, and the junction is provided with piston; Separator tube 3 upper opening places connect 7, three mouthfuls of device 7 lower ends of three mouthfuls of devices through wireway and connect gas receptacle 8; Three mouthfuls of devices 7 link to each other with vacuum pump through soft air-guide pipe 10.
The course of work of the present invention is following:
1, slide glass container 1 bottom that kbr tablet a is placed horizontally at, slide glass container 1 usefulness web member 2 is connected with separator tube 3, closes atmospheric valve 9;
2, absorbent solution c liquid level is opened vacuum pump a little more than conduit K1 lower end in the gas receptacle;
3, pour organic extract into sample cell 6, there is piston mozzle 4 slowly to drip on kbr tablet through forward (FWD), and the control rate of addition, keep organic extract a little more than the KBr sheet;
4, organic extract drips on the KBr sheet time, under condition of negative pressure; The volatilization of rising rapidly of light constituent organic solvent; Get into k1 through soft air-guide pipe and be absorbed the liquid absorption, treat that the whole volatilizations of organic solvent finish, the combustion adjuvant composition is adsorbed and is enriched on the kbr tablet of bottom in the solvent;
5, slowly open atmospheric valve 9 and purge, go out residual solvent;
6, take off slide glass container 1, close vacuum pump, take out kbr tablet, carry out the Fourier infrared spectrum analysis.
During use, step 1: take by weighing about 200mgKBr pressed powder, on Fourier transform infrared spectroscopy, carry out the background test; Keep background, take out the KBr sheet, and be put in the slide glass container bottom, will install assembling in a manner described and accomplish.
Step 2: burning remains in the scene of fire are used CS
2Solvent extraction is after drying agent is removed moisture, with CS
2Extract is poured in the sample cell, covers sealing-plug, regulates the mozzle upper piston, CS
2Extract slowly drips on the KBr sheet, and keeps liquid level a little more than the KBr sheet.Along with light constituent extract solvent evaporates, combustion adjuvant composition wherein is fully by the adsorbed enrichment of KBr sheet under negative pressure.Firing equipments such as employing hair dryer that can be suitable in this process heat the slide glass container, and the running time is shortened in the accelerated solvent volatilization.
Step 3: treat that adsorption and enrichment finishes, open atmospheric valve and purge, take out residual organic solvent on the KBr sheet.Take out the KBr sheet and carry out examination of infrared spectrum, gather experimental data.
Claims (3)
1. sample preparation device that is used for scene of a fire combustion adjuvant examination of infrared spectrum; Form by slide glass container (1), web member (2), separator tube (3), mozzle (4), barometric pipe (5), sample cell (6), three mouthfuls of devices (7), gas receptacle (8), atmospheric valve (9) and soft air-guide pipe (10); It is characterized in that; Slide glass container (1) is connected to atmospheric valve (9), and slide glass container (1) is through web member (2) and airtight connection of separator tube (3) lower ending opening place that is positioned at sample cell (6) bottom; Sample cell (6) top links to each other through barometric pipe (5) with separator tube (3); Separator tube (3) inside is provided with mozzle (4), and mozzle (4) links to each other with sample cell (6), and the junction is provided with piston; Separator tube (3) upper opening place connects three mouthfuls of devices (7) through wireway, and three mouthfuls of devices (7) lower end connects gas receptacle (8); Three mouthfuls of devices (7) link to each other with vacuum pump through soft air-guide pipe (10).
2. the sample preparation device that is used for scene of a fire combustion adjuvant examination of infrared spectrum according to claim 1 is characterized in that the ratio of height to diameter of said slide glass container (1) is 0.1:1～10:1.
3. the sample preparation device that is used for scene of a fire combustion adjuvant examination of infrared spectrum according to claim 1 is characterized in that, the height of said separator tube (2) is 40:1～1:1 with the diameter ratio.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201110209998 CN102410949B (en) | 2011-07-26 | 2011-07-26 | Sample preparation device for fire scene oxidant infrared spectrum testing |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201110209998 CN102410949B (en) | 2011-07-26 | 2011-07-26 | Sample preparation device for fire scene oxidant infrared spectrum testing |
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| CN102410949A true CN102410949A (en) | 2012-04-11 |
| CN102410949B CN102410949B (en) | 2013-07-17 |
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| CN 201110209998 Active CN102410949B (en) | 2011-07-26 | 2011-07-26 | Sample preparation device for fire scene oxidant infrared spectrum testing |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108457038A (en) * | 2018-05-29 | 2018-08-28 | 武汉理工大学 | Clothing based on ultrasonic washing and vacuum microwave drying principle washes baking and shares cavity all-in-one machine |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20080022786A1 (en) * | 2004-01-14 | 2008-01-31 | Heiner Sann | Device And Method For Taking Samples |
| CN201072389Y (en) * | 2007-07-30 | 2008-06-11 | 和舰科技(苏州)有限公司 | Negative pressure closed sampling device |
| CN101393087A (en) * | 2008-10-23 | 2009-03-25 | 公安部上海消防研究所 | On site volatile residue evidence extracting device for public security fire protection |
| CN101913977A (en) * | 2010-08-26 | 2010-12-15 | 上海立科药物化学有限公司 | Method for preparing high-purity cyclopentadiene with high yield |
-
2011
- 2011-07-26 CN CN 201110209998 patent/CN102410949B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20080022786A1 (en) * | 2004-01-14 | 2008-01-31 | Heiner Sann | Device And Method For Taking Samples |
| CN201072389Y (en) * | 2007-07-30 | 2008-06-11 | 和舰科技(苏州)有限公司 | Negative pressure closed sampling device |
| CN101393087A (en) * | 2008-10-23 | 2009-03-25 | 公安部上海消防研究所 | On site volatile residue evidence extracting device for public security fire protection |
| CN101913977A (en) * | 2010-08-26 | 2010-12-15 | 上海立科药物化学有限公司 | Method for preparing high-purity cyclopentadiene with high yield |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108457038A (en) * | 2018-05-29 | 2018-08-28 | 武汉理工大学 | Clothing based on ultrasonic washing and vacuum microwave drying principle washes baking and shares cavity all-in-one machine |
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| CN102410949B (en) | 2013-07-17 |
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