CN109507327B - Quantitative determination of TNT content by GC-AED independent calibration curve method (CIC method) - Google Patents
Quantitative determination of TNT content by GC-AED independent calibration curve method (CIC method) Download PDFInfo
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- 238000000034 method Methods 0.000 title claims abstract description 38
- 238000011088 calibration curve Methods 0.000 title description 3
- 238000001514 detection method Methods 0.000 claims abstract description 22
- 239000003153 chemical reaction reagent Substances 0.000 claims abstract description 10
- 239000007789 gas Substances 0.000 claims abstract description 9
- -1 TNT compound Chemical class 0.000 claims abstract description 5
- 230000005540 biological transmission Effects 0.000 claims abstract description 4
- 238000012937 correction Methods 0.000 claims abstract description 4
- 239000012495 reaction gas Substances 0.000 claims abstract description 4
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 10
- 239000000834 fixative Substances 0.000 claims description 10
- 239000012086 standard solution Substances 0.000 claims description 4
- 239000002904 solvent Substances 0.000 claims description 3
- 238000011084 recovery Methods 0.000 claims description 2
- 150000001875 compounds Chemical class 0.000 abstract description 14
- 238000004587 chromatography analysis Methods 0.000 abstract description 10
- 238000002347 injection Methods 0.000 abstract description 4
- 239000007924 injection Substances 0.000 abstract description 4
- 238000004458 analytical method Methods 0.000 abstract description 2
- 239000000015 trinitrotoluene Substances 0.000 description 44
- SPSSULHKWOKEEL-UHFFFAOYSA-N 2,4,6-trinitrotoluene Chemical compound CC1=C([N+]([O-])=O)C=C([N+]([O-])=O)C=C1[N+]([O-])=O SPSSULHKWOKEEL-UHFFFAOYSA-N 0.000 description 40
- 239000000126 substance Substances 0.000 description 12
- 239000002360 explosive Substances 0.000 description 10
- 238000004445 quantitative analysis Methods 0.000 description 8
- 239000000463 material Substances 0.000 description 7
- 239000000203 mixture Substances 0.000 description 5
- 238000009472 formulation Methods 0.000 description 4
- 239000000243 solution Substances 0.000 description 4
- 238000000921 elemental analysis Methods 0.000 description 3
- 239000000543 intermediate Substances 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 238000005481 NMR spectroscopy Methods 0.000 description 2
- 238000001636 atomic emission spectroscopy Methods 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 238000013375 chromatographic separation Methods 0.000 description 2
- 238000010812 external standard method Methods 0.000 description 2
- 239000003721 gunpowder Substances 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 238000004451 qualitative analysis Methods 0.000 description 2
- 238000011002 quantification Methods 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- ADCBKYIHQQCFHE-UHFFFAOYSA-N 1,3-dimethyl-1,3-diphenylurea Chemical group C=1C=CC=CC=1N(C)C(=O)N(C)C1=CC=CC=C1 ADCBKYIHQQCFHE-UHFFFAOYSA-N 0.000 description 1
- KIJCKNUNZABDBC-UHFFFAOYSA-N 3,4-dinitro-1,2,5-oxadiazole Chemical compound [O-][N+](=O)C1=NON=C1[N+]([O-])=O KIJCKNUNZABDBC-UHFFFAOYSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 241001411320 Eriogonum inflatum Species 0.000 description 1
- 238000005033 Fourier transform infrared spectroscopy Methods 0.000 description 1
- 238000004566 IR spectroscopy Methods 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000012847 fine chemical Substances 0.000 description 1
- JKFAIQOWCVVSKC-UHFFFAOYSA-N furazan Chemical compound C=1C=NON=1 JKFAIQOWCVVSKC-UHFFFAOYSA-N 0.000 description 1
- 238000010813 internal standard method Methods 0.000 description 1
- 238000004811 liquid chromatography Methods 0.000 description 1
- 238000004949 mass spectrometry Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
- 230000003472 neutralizing effect Effects 0.000 description 1
- 125000001893 nitrooxy group Chemical group [O-][N+](=O)O* 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 238000000638 solvent extraction Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 239000003381 stabilizer Substances 0.000 description 1
- 239000010421 standard material Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 238000009210 therapy by ultrasound Methods 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
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- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/86—Signal analysis
- G01N30/8675—Evaluation, i.e. decoding of the signal into analytical information
- G01N30/8679—Target compound analysis, i.e. whereby a limited number of peaks is analysed
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Abstract
The invention discloses an irrelevant correction curve method (CIC method) for quantitatively determining TNT content of GC-AED. The chromatographic column used in the disclosed gas chromatographic analysis method is an HP-5 weak polarity capillary column, the temperature of a sample inlet is 200 ℃, the temperature of a column incubator is 180 ℃, the split ratio is 20:1, the sample injection amount is 0.5uL, and the column flow rate is 3 mL/min. The AED parameters were: the temperature of the transmission line is 220 ℃ and the temperature of the cavity is 250 ℃; the detection element used is C, the wavelength is C193 nm; the reaction gas used is O2，H2(ii) a The pressure of the supplementary gas He is 200 KPa. The quantitative detection method of TNT disclosed is to use chromatographic analysis method to respectively carry out 2 pairs#Analysis of neutraceuticals and TNT, using AED Detector Pair 2#Detection of the C elements of the mesogen and TNT at a detection wavelength of C193nm and 2#Calculating the content of the C element of the TNT by taking the content of the C element of the medium reagent as a standard so as to obtain the content of the TNT compound. The element chromatographic analysis method has good peak shape, and the compound is quantitatively prepared from a non-self and non-energetic standard sample, so that the accuracy is high and the repeatability is strong.
Description
Technical Field
The invention belongs to the technical field of explosives and powders, and particularly relates to a quantitative determination method of 2.4.6-trinitrotoluene (TNT) by using a gas chromatography-atomic emission spectrometry method (CIC method) through an irrelevant correction curve method.
Background
The qualitative and quantitative analysis of organic components in explosives and powders is one of the core work contents of physicochemical detection researchers, and comprises the qualitative and quantitative analysis of unknown substances in the synthesis process of energetic materials and the quantitative analysis of organic components in the formula of explosives and powders products. At present, the qualitative and quantitative determination of organic impurities in compounds mainly adopts Mass Spectrometry (MS), infrared spectroscopy (FTIR), Nuclear Magnetic Resonance (NMR), chromatography (GC/LC) and the like; the quantitative analysis of the components of the organic matters in the gunpowder generally adopts a solvent extraction method and then adopts a chromatographic external standard method or an internal standard method for quantitative analysis. However, the above techniques require a compound standard spectrum or a standard substance of the object to be detected as a support to achieve quantification, and accurate quantitative detection of the object cannot be achieved under the conditions that the chemical structure of impurities is unclear and a standard sample is difficult to prepare.
Therefore, a new quantitative detection method for energetic materials without a standard sample needs to be developed for solving the problem that the traditional detection method needs a standard substance per se. At present, no relevant technical report exists about quantitative detection of explosive components without self standard samples.
Gas chromatography-atomic emission spectrometry (GC-AED) uses an element-selective detector whose peak area of the element signal is proportional to the mass of the element in the composition, regardless of the molecular structure of the element, and a known standard compound containing the element being measured can be used in quantitative analysis to correct compounds containing the same element, a method that is unique to GC-AED, the CIC of compounds.
In addition, energetic compounds have the characteristics of flammability, explosiveness and high sensitivity, and if the energetic compounds are used as standard substances, certain potential safety hazards exist in the transportation process of the compounds, so that quantitative analysis of explosive components by using non-self and non-energetic compounds is a technical problem to be overcome in the field.
2#The chemical name of the stabilizer is dimethyl diphenyl urea, which is an organic chemical and is commonly used as a gunpowder stabilizerOr as intermediates for fine chemicals, which do not contain C-NO in their structure2、N-NO2、O-NO2、N3N ═ N, and other energy-containing groups. The invention uses non-energetic material 2#And the middle determination agent is a standard substance, GC-AED is adopted to carry out research on a TNT quantitative detection method without self standard sample, the research on the wavelength selection of C element, chromatographic separation condition and AED condition optimization is carried out, accurate quantitative experimental data of the element in the TNT is obtained, the content of the TNT compound is further measured, and a novel method for quantitatively detecting the TNT by adopting non self standard sample and non-energetic material is established.
Disclosure of Invention
One of the objects of the present invention is to provide a 2#A GC-AED (gas chromatography-AED) C element chromatography method of a neutralizing agent and TNT (trinitrotoluene).
Therefore, the chromatographic column used in the chromatographic analysis method provided by the invention is HP-5, the temperature of a sample inlet is 200 ℃, the temperature of a column incubator is 180 ℃, the split ratio is 20:1, the sample injection amount is 0.5uL, and the flow rate of the column is 3 mL/min.
The AED parameters were: the transmission line temperature is 220 ℃ and the cavity temperature is 250 ℃. The detection element used is C, the wavelength is C193 nm; the reaction gas used is O2，H2(ii) a The pressure of the supplementary gas He is 200 KPa.
Another objective of the present invention is to provide a method for quantitatively detecting TNT.
The quantitative TNT detecting method includes the first analysis of two compounds with the chromatographic analysis method and the subsequent detection of C element content in two compounds with the chromatographic signal of C element channel of AED detector.
By 2#The medium reagent is used as a standard substance, acetone is used as a solvent to prepare 2 solutions with the concentration of 26.5625ug/mL, 53.125ug/mL, 212.5ug/mL, 425ug/mL and 850ug/mL respectively#Standard solutions of the medium, 2 for each concentration#Repeat 6 injections of the standard solution of the mediator, determine the peak area of the chromatogram for each concentration using the C (193nm) channel of the GC-AED, and average the peak area of the C element to 2#Linear fitting of the concentration of element C in the fixative, i.e. 2#-independent calibration curves (CIC curves), curves and curves for the C element in the fixativeThe equations are shown in figure 1. In order to verify the accuracy and precision of the method, TNT standard solutions of 162ug/mL, 810ug/mL and 1620ug/mL were prepared, and each concentration was injected for 6 times, and 2 times was used#Calculating the detection concentration of the C element by using a CIC curve equation of the C element in the neutralization reagent, and calculating the standard recovery rates of the method to be 94.6%, 99.7% and 101.3% respectively according to the detection concentration and the theoretical concentration of the C element, thereby showing that the method has good accuracy; the precision of the method is shown by Relative Standard Deviation (RSD) of the C element peak area, and RSD of the C element peak area under three concentration conditions is respectively 0.3%, 0.5% and 0.7%, which shows that the precision of the method is good.
GC-AED measurement of known concentrations of TNT formulated gave the peak area for element C, 2#And calculating the peak area by using a CIC curve of the medium reagent to obtain the concentration of the C element of the TNT, further obtaining the concentration of the TNT compound, and comparing the calculated concentration of the TNT with the theoretical concentration to obtain a relative error. The TNT compound was quantitated and its relative error was calculated.
The TNT quantitative detection method provided by the invention has the advantages of good carbon element chromatographic peak shape, good separation degree, high accuracy and strong repeatability; in addition, the method adopts non-energetic materials and non-self-standard substances 2#The quantitative determination of the C element is carried out by the medium-concentration reagent, so that the quantitative determination of the TNT component is completed, the problem of lack of standard substances in a laboratory is solved, a referable thought is provided for the subsequent quantitative determination of a plurality of organic matters containing the same element by using non-self and non-energy-containing standard substances, and the major safety risk existing in the transportation of energy-containing materials can be avoided.
Drawings
FIG. 12#CIC plot of the C element in the fixative
FIG. 2C 193nm elemental analysis chart for TNT
FIG. 32#Elemental analysis (C193 nm) plot of the intermediate reagent
FIG. 4 is a C193nm elemental analysis chart of TNT in an explosive formulation
Detailed Description
The separation and quantitative detection method of the invention is mainly carried out on a GC-AED instrument, and a sample passes through HP-5 weakly polar chromatography column, 2#The median and TNT appeared separately and then according to 2#-CIC curve equation for the median fixative and intensity of TNT flow through the detector signal to quantify TNT. The method can realize accurate quantification of TNT.
The following are examples provided by the inventors to further illustrate the technical solution of the present invention.
Example 1:
the experimental apparatus of this example:
an Agilent 7890A gas chromatograph, an autosampler with a 16-bit sample rotating stand, a JAS AED II Plus type multi-element detector and JAS multi-element detector software.
Test conditions for this example:
a chromatographic column: HP-5 chromatography column;
sample inlet temperature: 200 ℃;
column temperature: 180 ℃;
the split ratio is as follows: 20: 1;
sample introduction amount: 0.5 uL;
flow rate: 3 mL/min;
AED detector transmission line temperature: 220 ℃;
AED detector cavity temperature: 250 ℃;
detection wavelength of element C: c193 nm;
the reaction gas being O2，H2；
The pressure of the supplementary gas He is 200 KPa.
Preparing a TNT solution of 810ug/mL by using acetone as a solvent; sample introduction volume: 0.5 uL; after the instrument is stabilized, sample introduction is carried out for 6 times, and the average value of the peak area is obtained according to the reference 2#And obtaining the concentration of the C element of the TNT by a CIC curve equation of the medium reagent, and further obtaining the concentration of the compound of the TNT.
TNT and 2 in this example#The results of GC-AED elemental chromatography detection of the-fixative are shown in FIGS. 2 and 3.
The results of the quantitative determination of the sample to be tested in this example are as follows: the average value of the peak area of the C element in the TNT is 27239.03, the detection concentration of the C element in the TNT is 298.86ug/mL through calculation of a CIC curve equation, the detection concentration of the TNT can be 807.63ug/mL according to the detection concentration of the C element in the TNT, the known theoretical concentration of the TNT is 810ug/mL, and therefore the relative error is 0.29%.
Example 2:
the experimental equipment and test conditions used in this example were the same as in example 1.
The sample tested in this example was an explosive formulation of TNT, dinitrofurazan-based furazan (DNTF) and Benzotrifurannitroxide (BTF), where the conventional test method for TNT is a liquid chromatography external standard method requiring TNT standard materials. The method established by this study can be used with 2's of non-self, non-energetic materials#-the intermediate reagent is used as a standard sample for the determination of the TNT content of the explosive formulation.
The pretreatment steps of the sample are as follows: weighing 0.2g of sample into a clean and dry 50mL volumetric flask, adding 30mL of acetone, plugging a bottle stopper, performing ultrasonic treatment until the solution is completely dissolved, performing constant volume to a scale mark by using the acetone, and uniformly mixing. Filtering with organic solvent filter, and analyzing by sample injection. The chromatographic separation pattern of the C element of the sample is shown in FIG. 4. Wherein peak No. 2 is the peak given by TNT. The peak areas of the two samples were measured in parallel and averaged to be 14400.44, 14202.34, respectively.
According to 2#And (4) calculating the concentration of the C element of the TNT according to the CIC curve equation y of the median fixative 92.227x-323.570, and further obtaining the concentration of the compound of the TNT. And further calculating to obtain the mass percentage content of TNT in the explosive formula. The experimental data are shown in table 1. As can be seen from Table 1, the TNT content calculated by the method is substantially consistent with the theoretical dosage.
TABLE 1 determination of TNT content in certain explosive formulations
Claims (3)
1. A method for quantitatively determining TNT content by a CIC method of a GC-AED irrelevant correction curve method is characterized in that a chromatographic column used in the method is an HP-5 weak polarity capillary column, the temperature of a sample inlet is 200 ℃, the temperature of a column incubator is 180 ℃, the split ratio is 20:1, the sample volume is 0.5 mu L, and the flow rate of the column is 3 mL/min;
the AED parameters were: the temperature of the transmission line is 220 ℃ and the temperature of the cavity is 250 ℃; the detection element used is C, the wavelength is C193 nm; the reaction gas used is O2，H2(ii) a The pressure of the supplementary gas He is 200KPa and 2#-the fixative is a standard.
2. The method for measuring the TNT content of claim 1,
at different concentrations 2#-the C content of the fixative is plotted against the corresponding C element chromatographic peak area, 2#The linear equation for C in the fixative isy=92.227x-323.570，R2= 0.9998; the standard recovery rates of the C element concentration when the TNT concentration is 162 mu g/mL, 810 mu g/mL and 1620 mu g/mL are respectively 94.6%, 99.7% and 101.3%; the precision was expressed as relative standard deviation RSD, and RSD of the C element peak area was 0.3%, 0.5%, 0.7% for each of the three concentrations.
3. The method for determining the content of TNT according to claim 1, characterized in that the two components are analyzed separately:
is expressed by 2#-a series of 2 with different concentrations prepared with a medium reagent as a standard and acetone as a solvent#-a standard solution of a fixative, the elemental chromatographic peak area at the corresponding concentration being measured using the C193 channel of the GC-AED;
② by peak area pair 2#C content of the median, plotted 2#-an irrelevant correction curve CIC curve for the fixative;
③ GC-AED for measuring the area of peak obtained by formulating TNT with known concentration, 2#And calculating the peak area by using a CIC curve of the medium reagent to obtain the C content of the TNT, further obtaining the content of the TNT compound, and comparing the TNT content obtained by calculation with the known concentration to obtain a relative error.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102866224A (en) * | 2012-09-17 | 2013-01-09 | 四川大学 | Gas chromatographic detection method for determining carbon-containing compound based on carbon atomic emission spectroscopy |
| CN103616458A (en) * | 2013-12-14 | 2014-03-05 | 环境保护部南京环境科学研究所 | Method for quantitatively detecting six kinds of nitrobenzene compounds in fine atmospheric particles PM2.5 |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102866224A (en) * | 2012-09-17 | 2013-01-09 | 四川大学 | Gas chromatographic detection method for determining carbon-containing compound based on carbon atomic emission spectroscopy |
| CN103616458A (en) * | 2013-12-14 | 2014-03-05 | 环境保护部南京环境科学研究所 | Method for quantitatively detecting six kinds of nitrobenzene compounds in fine atmospheric particles PM2.5 |
Non-Patent Citations (2)
| Title |
|---|
| Compound-Independent Calibration by Gas Chromatography-Atomic Emission Detection (GC-AED): Analysis of Molecules with 12 Carbon Atoms;W. Elbast et al.;《ANALYTICAL LETTERS》;19991231;第1627-1641页 * |
| 气相色谱法检测CS混合炸药中CS、RDX和增塑剂;周明明 等;《含能材料》;20041223;第231-233页 * |
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