CN102565049A - Method for qualitatively verifying explosive type with chemical developing process through explosion residues - Google Patents

Method for qualitatively verifying explosive type with chemical developing process through explosion residues Download PDF

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CN102565049A
CN102565049A CN2012100043262A CN201210004326A CN102565049A CN 102565049 A CN102565049 A CN 102565049A CN 2012100043262 A CN2012100043262 A CN 2012100043262A CN 201210004326 A CN201210004326 A CN 201210004326A CN 102565049 A CN102565049 A CN 102565049A
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explosive
solution
sample
acid
residues
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刘吉平
王银杰
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Beijing Institute of Technology BIT
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Abstract

The invention relates to a method for qualitatively verifying an explosive type with a chemical developing process through explosion residues, belonging to the technical fields of rapid explosion case detection and public security. The method disclosed by the invention comprises the following steps of: dissolving a sample in a sodium hydroxide water solution or a sodium hydroxide-methyl alcohol solution; and adding a sodium nitrite solution; slowly dropwise adding sulfuric acid after cooling in ice water. If the sample includes primary nitro-alkenes, a reaction liquid is red or orange-red and becomes transparent by continuously adding the acid. If the sample includes secondary nitro-alkenes, a methylbenzene layer becomes blue by shaking the acidulated reaction liquid with methylbenzene. A spot test of nitro-compound in aliphatic series, sodium nitrite and acid is simple, selective and sensitive.

Description

Adopt the method for chemical staining method qualitative test explosive kind through Explosive Residues
Technical field
The present invention relates to adopt the method for chemical staining method qualitative test explosive kind, belong to case of explosion detection and public safety technical field fast through Explosive Residues.
Technical background
In the case of explosion detection, the kind of obtaining explosive is to follow the trail of the important material evidence that explosive source is solved a case fast.How to differentiate fried kind fast by Explosive Residues, be the forward position that countries in the world are tracked down case of explosion fast always.Generally; Only arrest the suspect; Just can know the explosive that case of explosion is used, some developed countries all adopt like states such as the U.S., Britain, Germany, Canada the laboratory are gone back in the dust collection of explosion scene; After extracting, concentrating, carry out Analysis and Identification with methods such as gas chromatography, liquid chromatography, gel chromatography, look/matter logotype appearance and Capillary Electrophoresis; China Material Evidence Identification Center, Ministry of Public Security adopts said method, in authentication because the explosive that relates in the case of explosion is more and wide, so the method for identifying scans electric ytterbium, also the widespread use capillary electrophoresis in addition except above-mentioned.
Above-mentioned these are identified the method for explosion scene explosive charge residue, identify that accuracy rate is high, can only be applicable to the laboratory, and qualification cycle are long, and to quick clear up a criminal case, the suspect that fights crime has effectively delayed the time, and cost of investment is big.
Summary of the invention
The objective of the invention is in order to propose to adopt the method for chemical staining method qualitative test explosive kind through Explosive Residues.
The objective of the invention is to realize through following technical scheme.
Method through Explosive Residues employing chemical staining method qualitative test explosive kind of the present invention specifically is classified as follows:
1) the qualitative evaluation of aliphatic nitro compound
Acid primary nitroparaffin hydrocarbon and sodium nitrite reaction obtain nitrolic acid again after the acidifying:
Figure BDA0000129465750000021
2) with 1) reaction conditions the end of a thread, generate blue false nitric acid by the aliphatic secondary nitro compound:
Figure BDA0000129465750000022
3) the aliphatics tertiary nitro compounds does not take place 1) described reaction.
The droplet test of aliphatic nitro compound and sodium nitrite and acid has simple, selectivity and sensitive advantage.
To aliphatics primary nitrocompounds and aliphatic secondary nitro compound, test method is following.
Sample is dissolved in the sodium hydrate aqueous solution or 40% sodium hydrate methanol solution of about 2mL10%; The sodium nitrite solution that adds 1mL10%; After in frozen water, cooling off; The sulfuric acid that slowly drips
Figure BDA0000129465750000031
again contains the primary nitroparaffin hydrocarbon like sample, and then redness or orange-redness appear in reactant liquor; But continue to add acid, then color disappears.As containing the secondary nitroparaffin hydrocarbon in the sample, then the reactant liquor of acidifying sways with toluene, occurs blue in the toluene layer.
2) with the reaction of sulfuric acid
Can emit nitrous acid when secondary nitro-compounds heats in sulfuric acid with some tertiary nitro compounds, nitrous acid and resorcin reaction then generate strong aubergine, and test method is following.
An amount of sample is heated 5min in the 10mL concentrated sulphuric acid, be cooled to room temperature, again it is added in the resorcinol WS of 5mL%, and this reactant liquor is reheated to 100 ℃ and keeps 15min, then cooling.To most of secondary nitroparaffin hydrocarbon and some tertiary nitroparaffines hydrocarbon, produce aubergine.This test method is a particularly suitable to the halo nitroparaffin that nitro and halogen are positioned on the same carbon atom.Although this test all is sensitive for the nitro compound of number microgram,, still need carry out blank test to the nitro compound solution of low concentration.
3) reduction reaction
Aliphatic nitro compound can be reduced to azanol or amine, and available then appropriate method is identified reduzate, to know original nitro compound by inference.Other groups (for example nitroso-, azo group and hydrazo) that can be reduced to amine have interference to this reaction.
(1) is reduced to amine
The sample that 1. will contain the 4mmol nitro with tin reduction mixes in the 10mL flask with 3mL concentrated hydrochloric acid and 0.25g tin (little granular), behind the 10min, adds 0.25g tin again, then with this mixture heated to seething with excitement and backflow 30min.After the cooling, this reactant liquor of caustic lye of soda dilution with 6mL25% steams 4mL solution again.The flask of accepting this condensed fluid should add several methyl reds, will add the hydrochloric acid of c (HCL)=2mol/L simultaneously, so that this condensed fluid has lower pH value.Subsequently, the 0.4mL chlorobenzoyl chloride is added in the condensed fluid, mix with the caustic lye of soda of 8mL25% again after the cooling, and flask is clogged and fiercely sway 10min, filter isolated benzamide and recrystallization again, identify then.
When reducing high boiling aliphatic nitro compound, generate high boiling amine, recommend with extracted with diethyl ether so that amine is separated this moment.If be unsuitable for amine is processed heterocyclic carbamate derivatives, also can be made into para toluene sulfonamide or picrate.
2. reduce in the 200mL beaker with zinc, the compound that will contain the 4mmol nitro is dissolved in (or being suspended in) 30mL water, and uses hcl acidifying; Again this beaker is placed ice bath, when temperature one is reduced to 5 ℃, promptly under constantly stirring, add the 3g zinc powder; Behind the 30min, add the 2g zinc powder, continue to stir 30min again; Then with this reacting liquid filtering, filtrating is carried out a kind of of following test: a and is heavily fluoridized earlier then and the alpha-Naphthol coupling; B. with diazotising after the para-totuidine coupling; C. carry out acetylation after separating with steam distillation.Identify that product after the above-mentioned test is to know original nitro compound by inference.
The also available gas chromatography of the amine that reduction generates is separated or is used with the color reaction of chloranil and identify.
2) be reduced to azanol
Nitro compound ethanolic solution and 50mg ammonium chloride and 50mg zinc powder azeotropic with 1mL50%; Then with the reactant liquor decant; And in the clear liquid of gained, add a chlorobenzoyl chloride, and use hcl acidifying then, add one 10% liquor ferri trichloridi at last; Reaction mixture takes on a red color, and the azanol and the chlorobenzoyl chloride effect of this explanation nitro compound reduction gained have generated hydroxamic acid.
(3) other reactions
1. hydrolysis
With several milliliters of aliphatic nitro compounds and 1mL solution of potassium carbonate (10g sal tartari is dissolved in 5mL water gained) boiling 2min; The cooling back adds 1mL water; With several these reactant liquors with the acidifying of 1mL watery hydrochloric acid; Add 0.05mLGriss reagent then, produce light red extremely redness, this is because the nitro compound hydrolysis has generated the cause of nitrous acid.Contain the aromatic series neighbour of unstable nitro and also this reaction can take place dinitro compound.
2. coupling
Uncle's aliphatic nitro compound can with diazo salt (for example through diazotizing metanilic acid) coupling, form orange to red.This reaction does not take place in secondary aliphatic nitro compound.The test method of this reaction is following: add 2mL phosphate buffer (pH=4.3) and 5mL reagent (this reagent system with 0.9% sodium nitrite solution of equivalent and 0.72% the horizontal acid solution of m-aminophenyl---solvent is 18% hydrochloric acid---mixed) in 10% methanol solution of 1mL uncle aliphatic nitro compound, reactant liquor shows orange to redness.
3. with the reaction of alkaline peroxide
With uncle or secondary aliphatic nitro compound and alkaline peroxide solution heat altogether, generate sodium nitrite usually, and the latter can use Griss reagent to identify, promptly with sulfanilic acid and naphthalidine in pH=2~2.5 o'clock reaction generation aubergine.
4. with the reaction of diphenylamine sulfuric acid solution
This is a droplet test that is used for secondary nitroparaffin hydrocarbon and tertiary nitroparaffines hydrocarbon, i.e. 50%~90% of diphenylamine and secondary nitroparaffin hydrocarbon and uncle's aliphatics nitro people compound sulfuric acid solution reaction shows blue.But much other oxygenant (like nitrate or ester) also responds to this test, is careful when therefore adopting.
5. with the reaction of fast blue B
This is a droplet test that is used to examine and determine uncle's aliphatic nitro compound; Its method such as following: on filter paper, add a saturated fast blue B ethanolic solution; The sodium hydroxide solution that adds a sample solution and a c (NaOH)=0.5mol/L again; Orange point or ring then on filter paper, occur, and can be transformed into redness (amount that depends on contained nitro compound in the test liquid).This test is 0.5 μ g to the minimum detectable activity of nitro compound.Phenolic compound and aromatic amine have interference to test.
The qualitative evaluation of 2 aromatic nitro compounds
The qualitative reaction of 3 nitrates
Thymol reagent: the 0.05g sample places thymol and 3 sulfuric acid that add on the white porcelain spot plate with sample equivalent, observes virescence behind the stirring 5min.Expression has nitrate to exist.
The fast qualitative of 4 mineral-type explosives detects
1) the qualitative quick test of ammonium nitrate explosive
Ammonium nitrate explosive comprises nitrolite, emulsion [explosive
(1) the qualitative of ammonium nitrate explosive detects fast
The Explosive Residues soil sample that contains nitrolite is used a spot of washing earlier, and washing lotion is divided into 2 parts.Portion is used to identify NH 4+ adding hydrochloric acid carries out acidifying, makes ammonium nitrate generate ammonium chloride and nitric acid; The WS is placed test tube, on spirit lamp, heat, top is with adularescent smog, and the crystal of cooling back adularescent above test tube solution occurs.Above-mentioned reaction appears again after the heating repeatedly.
Another part is used to identify nitrate ion.
(2) the qualitative of emulsion [explosive detects fast
The base stock of emulsion [explosive is ammonium nitrate, four phenol-80 and sensitizer (glass microballoon, perlite etc.) seldom.Detect such explosive first and will confirm to contain in the residue ammonium nitrate; Second also will confirm middle four phenol-80 that contain.
2) the qualitative of black powder detects fast
(1) evaluation of black powder
The composition of black powder is by potassium nitrate, and raw materials such as carbon black and sulphur constitute.The soil sample that contains the black powder Explosive Residues, water dissolves, and resulting solution is divided into four parts.One of which drips 3~5 solution on spot plate, drip 1~2 solution then, and the blood red sulphur iron hydride deposition of very fast change exists and detected sulphur; Another part is used to identify K +In addition, also to identify the existence of nitrate radical, could judge it is black powder.
(2) evaluation of potash chlorate
Mainly generate unique reaction of AgCl black precipitate and differentiate with it.The existence of the potassium ion of identifying simultaneously.In addition also to distinguish potash chlorate, potassium chloride and from the evaluation of potash chlorate.
(3) evaluation of potassium perchlorate
Except the assay method of pressing potash chlorate, also to distinguish potassium chloride, drip on spot plate at the sample that obtains 2~3, add 2~3 KI solution again, become this unique specific reaction of purple.
The scene and the qualitative Rapid identification of fried back residue that relate to case of explosion.The present invention and said method are distinct to be, can adopt chemical staining method quick (several seconds so that several minutes) to draw qualification result in the explosion scene, and it is highly sensitive, and accuracy rate can reach more than 99%.This method is not seen the precedent and the pertinent literature report of application before this.

Claims (4)

1. adopt the method for chemical staining method qualitative test explosive kind through Explosive Residues, it is characterized in that: the residue sample after will explode is dissolved in the sodium hydrate aqueous solution or 40% sodium hydrate methanol solution of about 2mL10%, the sodium nitrite solution of adding 1mL10%; After in frozen water, cooling off; Slowly drip the sulfuric acid of 6mol/L again, contain the primary nitroparaffin hydrocarbon like sample, then redness or orange-redness appear in reactant liquor; But continue to add acid, then color disappears; As containing the secondary nitroparaffin hydrocarbon in the sample, then the reactant liquor of acidifying sways with toluene, occurs blue in the toluene layer.
2. adopt the method for chemical staining method qualitative test explosive kind through Explosive Residues; It is characterized in that: the residue 0.05g sample after will exploding places thymol and 3 sulfuric acid that add on the white porcelain spot plate with sample equivalent; Observe after stirring 5min, virescence, expression has nitrate to exist.
3. adopt the method for chemical staining method qualitative test explosive kind through Explosive Residues, it is characterized in that: the Explosive Residues soil sample that will contain nitrolite is used a spot of washing earlier, is used to identify NH 4+ adding hydrochloric acid carries out acidifying, makes ammonium nitrate generate ammonium chloride and nitric acid; The WS is placed test tube, on spirit lamp, heat, top is with adularescent smog, and the crystal of cooling back adularescent above test tube solution occurs; Above-mentioned reaction appears again after the heating repeatedly.
4. adopt the method for chemical staining method qualitative test explosive kind through Explosive Residues, it is characterized in that: will contain the soil sample of black powder Explosive Residues, water dissolves, and resulting solution is divided into three parts; One of which drips 3~5 solution on spot plate, drip 1~2 solution then, and the blood red sulphur iron hydride deposition of very fast change exists and detected sulphur; Another part is used to identify K +Also has a existence that is used to identify nitrate radical.
CN2012100043262A 2012-01-09 2012-01-09 Method for qualitatively verifying explosive type with chemical developing process through explosion residues Pending CN102565049A (en)

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Cited By (4)

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Publication number Priority date Publication date Assignee Title
CN103399075A (en) * 2013-07-25 2013-11-20 中国科学院生态环境研究中心 Double-mode detecting method and kit for detecting for organic explosive residues
CN104111280A (en) * 2014-07-30 2014-10-22 杨丽 Rapid and accurate detection method for ammonium nitrate explosive
CN104655623A (en) * 2015-03-24 2015-05-27 中国科学院新疆理化技术研究所 Kit for quickly detecting water-soluble explosive and detecting method of kit
CN112763471A (en) * 2020-12-29 2021-05-07 北京华泰诺安探测技术有限公司 Trace explosive detection method

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103399075A (en) * 2013-07-25 2013-11-20 中国科学院生态环境研究中心 Double-mode detecting method and kit for detecting for organic explosive residues
CN104111280A (en) * 2014-07-30 2014-10-22 杨丽 Rapid and accurate detection method for ammonium nitrate explosive
CN104655623A (en) * 2015-03-24 2015-05-27 中国科学院新疆理化技术研究所 Kit for quickly detecting water-soluble explosive and detecting method of kit
CN112763471A (en) * 2020-12-29 2021-05-07 北京华泰诺安探测技术有限公司 Trace explosive detection method

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Application publication date: 20120711