CN101782568B - Method for comprehensively detecting minute amount of wooden meal in crime scene - Google Patents

Method for comprehensively detecting minute amount of wooden meal in crime scene Download PDF

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CN101782568B
CN101782568B CN 200910010234 CN200910010234A CN101782568B CN 101782568 B CN101782568 B CN 101782568B CN 200910010234 CN200910010234 CN 200910010234 CN 200910010234 A CN200910010234 A CN 200910010234A CN 101782568 B CN101782568 B CN 101782568B
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wood chip
chip sample
wooden meal
wooden
sample
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CN101782568A (en
Inventor
史晓凡
王景翰
张振宇
姚丽娟
许英健
李心倩
马子宁
王岩
李继民
赵鹏程
赵彦军
邹宁
苏红英
许江萍
吴正荣
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CHINA COLLEGE OF CRIMINAL POLICE
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Abstract

The invention relates to a method for detecting a minute amount of wooden meal in a crime scene, belonging to the field of criminal case material evidence detection. The method comprises the following steps of: (1) identifying the wooden meal according to the characteristics of wooden meal detection material cell pits and the composition of inorganic elements, and analyzing and comparing the numbers, the sizes and the shape characteristics of the pits positioned on wooden meal detection material cell walls and the kinds and the difference the relative contents of the contained inorganic elements by a scanning electron microscope-energy spectrometer; (2) identifying the wooden meal according to the difference of principle components of wooden meal detection materials, and analyzing chemical components contained in the wooden meal detection materials by cracking gas chromatography and Fourier infrared spectrometry; (3) identifying the wooden meal according to the difference of leaching components of the wooden meal detection materials, and analyzing the leaching components of the wooden meal detection materials by using a gas chromatography, a high efficiency liquid chromatography and a Fourier transform infrared spectrometry. The invention has scientific and accurate detection conclusion and high applicability.

Description

Method for comprehensively detecting minute amount of wooden meal in crime scene
Technical field
The invention belongs to criminal case material evidence detection field, relate in particular to a kind of minute amount of wooden meal in crime scene detection method.
Background technology
Trace material evidence is the little material of all amount corpusculums that can prove the case truth.So-called amount corpusculum is little except there being quality few, outside the little implication of volume, sometimes also has the extremely low implication of component content to be checked.
Because trace material evidence amount corpusculum is little, the crime molecule is difficult to damage them, so the possibility of leaving at the scene is large, namely the upper probability that occurs is large at the scene, just may find as long as conscientiously seek.The trace material evidence majority is attached on other object or is mingled in other material, and is often contaminated, must first extract or separate when check.Although trace material evidence not necessarily possesses the mode of appearance of the original, it still keeps the composition of the original, and this is can be by the reason of the trace material evidence Analysis deterrmination original.
From the classification of trace material evidence, micro-wood chip namely belongs to natural material class trace material evidence.In all kinds of criminal case crime scenes, often can extract due to criminal offence from wooden residue or the broken end that Wooden Object separates.Check timely and accurately above-mentioned micro-wood chip material evidence, can point the direction for clear up a criminal case, give a clue, provide the foundation of science for confirming crime.At present, also do not have the similarities and differences of a kind of microstructure take micro-wood chip, chemical composition and lixiviate composition to be point of penetration in prior art, the wood chip sample is carried out the method that analysis-by-synthesis is identified.
Summary of the invention
The present invention is intended to overcome the deficiencies in the prior art part and a kind of method for comprehensively detecting minute amount of wooden meal in crime scene is provided, it can realize the comprehensive detection to the micro-structural feature of minute amount of wooden meal in crime scene sample, inorganic constituents, principal ingredient and lixiviate composition, test result is accurate, highly versatile, easy and simple to handle.
For achieving the above object, the present invention is achieved in that
Minute amount of wooden meal in crime scene sample detection method, can implement as follows:
(1) according to the difference of wood chip sample cell pit feature and contained inorganic elements, wood chip is differentiated;
Utilize the analyses of scanning electron microscope (SEM) and X-ray energy spectrometer (EDX) to compare number, size, shape facility and the contained inorganic elements kind of pit on wood chip sample cell membrane, the similarities and differences of relative content, described wood chip sample and the similarities and differences of comparing object of reference wood chip sample are identified;
(2) according to the difference of wood chip sample chemical composition, wood chip is differentiated;
Get micro-wood chip, adopt pyrolysis gas chromatography (PYGC) that the cellulose in the wood chip sample, hemicellulose, lignin component are analyzed, according to the difference of chromatographic peak peak number, retention time and ratio of peak in the cracking fingerprint image, wood chip sample and the similarities and differences of comparing object of reference wood chip sample are identified;
(3) according to the difference of wood chip sample lixiviate composition, wood chip is differentiated;
Utilize the lixiviate composition in the micro-wood chip of ultrasonic extraction extraction; Adopt vapor-phase chromatography (GC) that the volatile components in described wood chip sample lixiviate composition is analyzed; According to the gained chromatographic data, wood chip sample and the similarities and differences of comparing object of reference wood chip sample are identified.
As a kind of preferred version, in step of the present invention (3), utilize polyhydric phenol, terpene and geocerellite lixiviate composition in ultrasonic extraction extraction wood chip; Adopt high performance liquid chromatography (HPLC), the gradient elution mode minute is analyzed being leached into of described wood chip sample; According to the gained chromatographic data, wood chip sample and the similarities and differences of comparing object of reference wood chip sample are identified.
As another kind of preferred version, step of the present invention (2) adopts pellet technique to carry out FFIR (FTIR) analysis to the chemical composition of wood chip sample, according to the gained spectroscopic data, wood chip sample and the similarities and differences of comparing object of reference wood chip sample are identified.
In addition, in step of the present invention (3), after the extract of wood chip sample can being volatilized, adopt FFIR (FTIR) pellet technique that being leached into of wood chip sample minute analyzed, according to the gained spectroscopic data, wood chip sample and the similarities and differences of comparing object of reference wood chip sample are identified.
Secondly, in step of the present invention (2), pyrolysis time is 8~12 seconds.
In step of the present invention (2), cracking temperature is 500~800 ℃.
Again, in step of the present invention (2), can adopt DB-FFAP polyglycol capillary chromatographic column.
In step of the present invention (2), adopt the condition of pyrolysis gas chromatography (PYGC) temperature programme to be followed successively by:
40~60 ℃ of a, setting initial values, constant temperature was kept 1~3 minute;
B, the speed that continues with 6~9 ℃ of per minutes are warming up to 200~240 ℃;
C, constant temperature were kept 15~20 minutes.
In step of the present invention (3), adopt the condition of vapor-phase chromatography (GC) temperature programme to be followed successively by:
90~110 ℃ of a, setting initial values;
B, the speed that continues with 10~15 ℃ of per minutes are warming up to 180~200 ℃;
C, rise to 210~240 ℃ with the speed of 5~8 ℃ of per minutes
D, constant temperature were kept 14~18 minutes.
As preferred version, in step of the present invention (3), can consider to adopt DB-FFAP polyglycol capillary chromatographic column; Carrier gas is N2, and flow rate of carrier gas is 1~3ml/min.
As preferred version, in step of the present invention (3), the detection wavelength that wood chip sample lixiviate composition high performance liquid chromatography (HPLC) is analyzed can be selected 260~300nm; Adopt the C18 chromatographic column.
As preferred version, in step of the present invention (3), high performance liquid chromatography (HPLC) is completed wash-out in the gradient elution mode; In described elution program, mobile phase adopts methyl alcohol and water; During 0~8 minute or 35.1~45 minutes, the volume ratio of methyl alcohol and water is 18~20: 60~80 when elution time; During at 8.1~35 minutes, the volume ratio of methyl alcohol and water is 60~80: 20~40 when elution time.
The present invention passes through the similarities and differences of microstructure, principal ingredient and the lixiviate composition of the micro-wood chip of analysis, and wood chip sample and the character pair of comparing object of reference wood chip sample are comprehensively identified, gained expert's conclusion science is accurate, and highly versatile is easy to operate.
The present invention has following features:
(1) can differentiate the micro-wood chip residue of leaving on tool used in crime and the similarities and differences of comparing sample, thereby for inferring that the suspect provides foundation.
(2) can differentiate criminal case, traffic accident case the scene micro-wood chip residue of leaving over and the similarities and differences of comparing sample, thereby for inferring that case character provides foundation.
(3) wood chip sample consumption is few.
Description of drawings
The invention will be further described below in conjunction with the drawings and specific embodiments.Protection scope of the present invention not only is confined to the statement of following content.
Fig. 1 is trace routine FB(flow block) of the present invention;
Fig. 2 is pyrolysis gas chromatography of the present invention (PYGC) temperature programme curve map;
Fig. 3 is gas chromatographic analysis temperature programme curve map of the present invention.
Embodiment
As shown in Figure 1, at first the minute amount of wooden meal in crime scene detection method observes the appearance color of wood chip sample, smell etc., determines the comprehensive detection scheme according to the sample amount.
Can implement as follows when concrete the detection:
(1) according to wood chip sample cell pit feature, wood chip is differentiated;
Pit is architectural feature important on wood cell wall, to the identification of wood chip sample kind highly significant.The present invention utilizes scanning electron microscope (SEM) analysis to compare the similarities and differences of number, size and the shape facility of pit on wood chip sample cell membrane, and the kind of the contained inorganic elements of wood chip sample and the relative content of each element are tested, thereby described wood chip sample and the similarities and differences of comparing object of reference wood chip sample are identified;
(2) according to the difference of wood chip sample principal ingredient, wood chip is differentiated;
The principal ingredient of wood chip is the macromolecular compounds such as cellulose, hemicellulose, lignin, and the kind of these constituents and the content often difference because of the wood chip seeds are different, make it to have formed personal feature.Utilize pyrolysis gas chromatography, macromolecular compound with these difficult volatilizations is cracked into little molecule at a certain temperature, analyze under the chromatographic condition of determining, according to gained pyrolysis chromatography fingerprint image, wood chip sample and the similarities and differences of comparing object of reference wood chip sample are identified.
Sample treatment:
1, pyrolysis time
The length of sample dissociation time can produce significant impact to analysis result.Because the cracking primary reaction of sample was completed in moment, extend pyrolysis time under certain condition, can increase secondary reaction, the time is too short, and primary reaction is incomplete.Therefore, in pyrolysis chromatography was analyzed, it was vital selecting a better pyrolysis time.Through great many of experiments and be in optimized selection, the present invention determines that the pyrolysis time of wood chip is 10s.
2, cracking temperature
The composition of pyrolysis product and distribution depend on cracking temperature consumingly, and it is very important therefore selecting better cracking temperature.Usually, cracking temperature is too high, the primary reaction aggravation, and the non-feature sliver of low carbon number increases, and secondary reaction increases, the experiment poor reproducibility; Temperature is too low, and rate of cleavage is slow, and subsidiary reaction is many, and feature sliver productive rate is low.Through great many of experiments and be in optimized selection, the present invention determines that it is 700 ℃ that pyrolysis gas chromatography is analyzed the cracking temperature of wood chip.When cracking temperature was 700 ℃, in wood chip sample dissociation chromatogram, the peak number of chromatographic peak was many, and the difference between different types of wood chip sample is obvious.
3, chromatographic column
Chromatographic column is the heart of gas chromatograph, is the key of chromatographic column mutually and fix, and selecting chromatographic column is mainly to select fixedly phase.The selection of the chromatographic column principle that can similarly according to polarity mix is selected, and by the fixing power of phase polarity on chromatographic column, chromatographic column commonly used can be divided into polarity chromatographic column, low pole chromatographic column and nonpolar chromatographic column.When separated component when fixedly phase polarity is similar, separated component molecule the and fixedly acting force between phase molecule is strong, component is large in fixing solubleness in mutually, partition factor is large, retention time is long; Otherwise, opposite.Separated component is different because of polarity, and the retention behavior in chromatographic column is different and separated.
Mostly contain hydroxyl, carboxyl isopolarity group in the molecular structure of the difficult volatile components such as the cellulose in wood chip, hemicellulose, lignin, have certain polarity.Therefore, the present invention determines to select DB-FFAP polyglycol capillary chromatographic column.
4, chromatographic column temperature programme condition
Column temperature major effect partition factor, distribution ratio, the coefficient of diffusion of component in mobile phase with at fixing coefficient of diffusion in mutually, thereby by affect the post selectivity, post imitates to affect degree of separation and analysis time.Therefore, column temperature is an important analytical conditions for gas chromatography, and the variation of column temperature is inequivalence to the influence degree of different component.
The potpourri that the chemical composition of wood chip is comprised of macromolecular compounds such as cellulose, hemicellulose, lignin, the composition of its pyrolysis product is more complicated, and for such potpourri, its boiling spread is wider, should adopt temperature programme.Referring to Fig. 2, when lower initial temperature, the component that boiling point is lower can obtain good separation.The component that increases higher along with column temperature also can flow out chromatographic column quickly, and equally with low boiling component is effectively separated.Therefore, the present invention has adopted temperature programme, and its actual conditions is:
50 ℃ of a, setting initial values, constant temperature was kept 1 minute;
B, the speed that continues with 8 ℃ of per minutes are warming up to 220 ℃;
C, constant temperature were kept 17.75 minutes.
No matter be the difficult volatile ingredient of macromolecular compound in the chemical composition of wood chip, or low molecular lixiviate composition, the functional group that can produce infrared absorption all contained.The present invention adopts pressing potassium bromide troche, Fourier transform infrared spectrometry that the contained chemical composition of wood chip sample is analyzed, and according to the gained spectroscopic data, wood chip sample and the similarities and differences of comparing object of reference wood chip sample is identified.
(3) according to the difference of wood chip sample lixiviate composition, wood chip is differentiated;
The lixiviate composition is the submember of timber, although quantity seldom, kind is more.In the different tree species wood chip, the kind of lixiviate composition and content have obvious difference, and is different because of its growing environment with the timber in the different places of production of seeds, causes its lixiviate composition that certain difference is also arranged.
The present invention adopts vapor-phase chromatography, high performance liquid chromatography that being leached into of wood chip sample minute analyzed, and according to the gained chromatographic data, wood chip sample and the similarities and differences of comparing object of reference wood chip sample is identified.
Chromatography is a kind of important method for separating and analyzing, and it is to utilize different material to have different partition factors in two-phase, and when two-phase was done relative motion, these materials repeatedly repeatedly distributed in two-phase and realize separating.In chromatographic technique, mobile phase is the vapor-phase chromatography of crying of gas, and mobile phase is the liquid phase chromatography of crying of liquid.Based on above-mentioned theory, the present invention adopts vapor-phase chromatography, high performance liquid chromatography that being leached into of wood chip sample minute analyzed in reality detects, and according to the gained chromatographic data, wood chip sample and the similarities and differences of comparing object of reference wood chip sample is identified.
Sample source and preprocess method thereof:
The sample of vapor-phase chromatography (GC) Direct Analysis must be gas or liquid, and the sample of high-efficient liquid phase chromatogram technique analysis must be liquid, so the lixiviate composition of wood chip sample should be dissolved in suitable solvent before analysis.
1, the extraction conditions of wood chip sample lixiviate composition
1.1 the extraction agent of wood chip sample lixiviate composition
Need follow extraction agent when selecting wood chip lixiviate composition extraction agent large to the solubleness of various lixiviate compositions in wood chip, extraction effect is good, with in wood chip variously is not leached into the biochemical reaction of distribution; Extraction agent is nontoxic, colourless, and the principles such as noiseless are measured in follow-up analysis.Select through optimizing, the present invention determines that methyl alcohol is the extraction agent of wood chip lixiviate composition.
1.2 the extracting mode of wood chip sample lixiviate composition
Ultrasonic extraction is mechanical effect, cavitation effect and the thermal effect that the using ultrasound ripple has, and by increasing the movement velocity of medium molecule, the penetration power of amplified medium is come the effective constituent in extraction of substance, is a kind of physics leaching process.Ultrasound wave mainly produces unique mechanical vibration effect and cavitation to wood chip.Can produce and transmit powerful energy when ultrasonic vibration, make wood chip enter vibrational state with larger speed and acceleration, the structure of wood chip changes, and impels effective constituent to enter in solvent; Ultrasonic vibration can cause system temperature to raise simultaneously, has accelerated the dissolution velocity of lixiviate composition.Therefore ultrasonic extraction is a kind of effective ways that extract lixiviate composition in wood chip.
1.3 the extraction time of wood chip sample lixiviate composition
Extraction time is short, and extraction agent does not fully infiltrate wood chip, and it is complete not that the lixiviate composition extracts.Be 15min through testing the extraction time of determining wood chip lixiviate composition.
2, the analytical conditions for gas chromatography of wood chip sample lixiviate composition
2.1 the flow rate of carrier gas condition of wood chip sample lixiviate composition gas chromatographic analysis
To certain chromatographic column and sample, select the flow rate of carrier gas an of the best, can improve the post effect.Through the impact of experiment exam flow rate of carrier gas on the compartment analysis effect of wood chip lixiviate composition, result shows, when flow rate of carrier gas was 2.5ml/min, the gas chromatogram of wood chip lixiviate composition had the advantages that the chromatogram peak number is many, analysis time is short.When therefore, determining the gas chromatographic analysis of lixiviate composition, the flow velocity of carrier gas is 2.5ml/min.
2.2 the temperature programme condition of wood chip sample lixiviate composition gas chromatographic analysis
Referring to Fig. 3, through experimental selection, when temperature programme condition initial temperature was low, heating rate was little, and wood chip lixiviate ingredient components is fully separated; When heating rate was too fast, each component in the lixiviate composition of constituent complexity was separated fully.When the temperature programme condition is:
100 ℃ of a, setting initial values;
B, the speed that continues with 12 ℃ of per minutes are warming up to 190 ℃;
C, rise to 230 ℃ with the speed of 6 ℃ of per minutes
D, constant temperature were kept 16 minutes.
With this understanding, each component of wood chip lixiviate composition is separated fully, and the difference between different tree species wood chip sample is apparent in view.
2.3 other condition
Flame ionization ditector (FID), detector temperature are 250 ℃, and chromatographic column is polyglycol (DB-FFAP) capillary chromatographic column, and temperature of vaporization chamber is 230 ℃, Splitless injecting samples, and carrier gas is N 2, carrier gas flux is 2.5mL/min.
3, the efficient liquid phase chromatographic analysis condition of wood chip lixiviate composition
3.1 detection wavelength
Polyhydric phenol in the wood chip extract, terpene, lipid, geocerellite and carbohydrates etc., all can absorb certain wavelength ultraviolet light and at ultraviolet region generation absorption peak.Therefore the detection wavelength of determining wood chip extract efficient liquid phase chromatographic analysis (HPLC) is 280nm.
3.2 chromatographic column
Chromatographic column is the pith in high performance liquid chromatography, the degree of separation when it directly affects the potpourri compartment analysis, and the C18 chromatographic column of the different trades mark shows different chromatographic separation performances.Determine in experimental study that Diamonsil (diamond) C18 chromatographic column is the separating column of wood chip lixiviate composition.
3.3 mobile phase
In efficient liquid phase chromatographic analysis (HPLC), after chromatographic column was determined, the kind of mobile phase, proportioning all had a strong impact on separating effect.Therefore the mobile phase composition in high performance liquid chromatography, proportioning are selected particularly important.Experimental studies results shows, during 0~8 minute or 35.1~45 minutes, the volume ratio that the mobile phase condition satisfies methyl alcohol and water is 20: 80 (v/v) when elution time, and in high-efficient liquid phase chromatogram, the peak number of chromatographic peak is more, and peak shape is better.Therefore determine the mobile phase of the efficient liquid phase chromatographic analysis of wood chip extract, during 0~8 minute or 35.1~45 minutes, the volume ratio of methyl alcohol and water is 20: 80 (v/v) when elution time.
3.4 elution mode
In wood chip lixiviate composition, the structure of each component is different, and polarity difference is larger mutually, and the stronger geocerellite of polarity, phenolic compound are arranged, and also has lipid, the terpenoid of low pole.For containing so multi-component complex sample, be difficult to realize effective separation by isocratic elution.Gradient elution is in detachment process, allows the composition of mobile phase change continuously by certain procedures, makes each component in potpourri go out chromatographic column the partition factor (k value) of the best is dirty.Under the condition of gradient elution, the component that wood chip lixiviate composition Semi-polarity is larger is first to flow out chromatographic column under the condition of 20: 80 (v/v) in the volume ratio that mobile phase is methyl alcohol and water, the component that polarity is less is separated when methyl alcohol is 70: 30 (v/v) with the volume ratio of water, thereby effectively improved the peak shape of chromatographic peak, reduce hangover, improved degree of separation.Therefore determine to adopt in the present invention the gradient elution mode to analyze the lixiviate composition of wood chip.
3.5 the selection of gradient elution program
Four kinds of gradient elution programs have been examined or check respectively in experiment to the separating effect of wood chip lixiviate composition.In four kinds of elution programs, when initial, the concentration of methyl alcohol and water is 20: 80, but in elution process, methyl alcohol is different from the concentration change scope of water.Experimental result shows, under the determined elution program condition of the present invention, each component of wood chip lixiviate composition has obtained good separation.
Figure G2009100102343D00101
Figure G2009100102343D00111
Qualitative identify
Must be noted that during qualitative identify, wood chip sample and object of reference are compared the check of must comparing of wood chip sample under identical analysis condition.
Microstructure, inorganic elements composition, principal ingredient, the lixiviate composition that must adopt scanning electron microscope-spectroscopy, pyrolysis gas chromatography, vapor-phase chromatography, high performance liquid chromatography, Fourier transform infrared spectrometry to compare the wood chip sample to wood chip sample and object of reference are measured respectively, after gained spectroscopic data, chromatographic data are carried out analysis-by-synthesis, just can draw the expert's conclusion that wood chip sample and object of reference wood chip are compared the sample similarities and differences.

Claims (9)

1. method for comprehensively detecting minute amount of wooden meal in crime scene, is characterized in that, implements as follows:
(1) according to the difference of wood chip sample cell pit feature and contained inorganic elements, wood chip is differentiated;
Utilize the analyses of scanning electron microscope (SEM) and X-ray energy spectrometer (EDX) to compare number, size, shape facility and contained inorganic elements kind, the relative content of pit on wood chip sample cell membrane, described wood chip sample and the similarities and differences of comparing object of reference wood chip sample are identified;
(2) according to the difference of wood chip sample chemical composition, wood chip is differentiated;
Get micro-wood chip, adopt pyrolysis gas chromatography (PYGC) that the cellulose in the wood chip sample, hemicellulose, lignin component are analyzed, according to chromatographic peak peak number, retention time and ratio of peak in the cracking fingerprint image, wood chip sample and the similarities and differences of comparing object of reference wood chip sample are identified; Or adopt pellet technique to carry out FFIR (FTIR) analysis to the chemical composition of wood chip sample, according to the gained spectroscopic data, wood chip sample and the similarities and differences of comparing object of reference wood chip sample are identified;
(3) according to the difference of wood chip sample lixiviate composition, wood chip is differentiated;
Utilize polyhydric phenol, terpene and geocerellite lixiviate composition in ultrasonic extraction extraction wood chip; Adopt vapor-phase chromatography (GC) method that the volatile components in described wood chip sample lixiviate composition is analyzed; According to the gained chromatographic data, wood chip sample and the similarities and differences of comparing object of reference wood chip sample are identified; Perhaps adopt high performance liquid chromatography (HPLC), the gradient elution mode minute is analyzed being leached in described wood chip sample leaching liquor; According to the gained chromatographic data, wood chip sample and the similarities and differences of comparing object of reference wood chip sample are identified; After perhaps the extract of wood chip sample being volatilized, adopt FFIR (FTIR) pellet technique that being leached into of wood chip sample minute analyzed, according to the gained spectroscopic data, wood chip sample and the similarities and differences of comparing object of reference wood chip sample are identified.
2. minute amount of wooden meal in crime scene detection method as claimed in claim 1, it is characterized in that: in described step (2), pyrolysis time is 8~12 seconds.
3. minute amount of wooden meal in crime scene detection method as claimed in claim 2, it is characterized in that: in described step (2), cracking temperature is 500~800 ℃.
4. minute amount of wooden meal in crime scene detection method as claimed in claim 3, is characterized in that: in described step (2), adopt DB-FFAP polyglycol capillary chromatographic column.
5. minute amount of wooden meal in crime scene detection method as claimed in claim 4 is characterized in that: in described step (2), adopt the condition of pyrolysis gas chromatography (PYGC) temperature programme to be followed successively by:
40~60 ℃ of a, setting initial values, constant temperature was kept 1~3 minute;
B, the speed that continues with 6~9 ℃ of per minutes are warming up to 200~240 ℃;
C, constant temperature were kept 15~20 minutes.
6. minute amount of wooden meal in crime scene detection method as claimed in claim 5 is characterized in that: in described step (3), adopt the condition of vapor-phase chromatography (GC) temperature programme to be followed successively by:
90~110 ℃ of a, setting initial values;
B, the speed that continues with 10~15 ℃ of per minutes are warming up to 180~200 ℃;
C, rise to 210~240 ℃ with the speed of 5~8 ℃ of per minutes;
D, constant temperature were kept 14~18 minutes.
7. minute amount of wooden meal in crime scene detection method as claimed in claim 6 is characterized in that: in described step (3), vapor-phase chromatography (GC) adopts DB-FFAP polyglycol capillary chromatographic column; Carrier gas is N2, and flow rate of carrier gas is 1~3ml/min.
8. minute amount of wooden meal in crime scene detection method as claimed in claim 1, it is characterized in that: in described step (3), the detection wavelength of wood chip sample lixiviate composition high performance liquid chromatography (HPLC) is 260~300nm; Chromatographic column adopting C18 chromatographic column.
9. minute amount of wooden meal in crime scene detection method as claimed in claim 8, it is characterized in that: in described step (3), high performance liquid chromatography (HPLC) is completed wash-out in the gradient elution mode; In described elution program, mobile phase adopts methyl alcohol and water; During 0~8 minute or 35.1~45 minutes, the volume ratio of methyl alcohol and water is 18~20: 60~80 when elution time; During at 8.1~35 minutes, the volume ratio of methyl alcohol and water is 60~80: 20~40 when elution time.
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