CN104865213A - Method for rapidly analyzing NTO (3-nitro-1,2,4-triazol-5-one) explosive content by ultraviolet spectrophotometer method - Google Patents
Method for rapidly analyzing NTO (3-nitro-1,2,4-triazol-5-one) explosive content by ultraviolet spectrophotometer method Download PDFInfo
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- CN104865213A CN104865213A CN201510224811.4A CN201510224811A CN104865213A CN 104865213 A CN104865213 A CN 104865213A CN 201510224811 A CN201510224811 A CN 201510224811A CN 104865213 A CN104865213 A CN 104865213A
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Abstract
The invention relates to a method for rapidly analyzing NTO (3-nitro-1,2,4-triazol-5-one) explosive content by an ultraviolet spectrophotometer method and belongs to the field of explosive detection. NTO explosive is dissolved in water, then ultraviolet spectrum scanning is performed respectively by an ultraviolet spectrophotometer, ultraviolet absorbancy degree at 336nm positions in measured ultraviolet spectrogram is put in a standard equation y=a+bx for quantitative detection of NTO concentration to obtain an x value, and the x value is detected NTO content. According to the method for rapidly analyzing NTO explosive content by the ultraviolet spectrophotometer method, operation is simple, the detecting range is wide, detection sensitivity is high, the method is suitable for rapid detection of NTO explosive with the concentration which is 4*10-6mol/L to 6*10-4mol/L, and the method for rapidly analyzing NTO explosive content by the ultraviolet spectrophotometer method can be widely applied to the field of industry and explosive detection.
Description
Technical field
The present invention relates to a kind of method of ultraviolet spectrophotometer method express-analysis NTO explosive content, belong to explosive detection field.
Background technology
Along with the development of modern science and technology, ammunition is the pith directly injuring target in weaponry, more and more higher to the requirement of ammunition in recent years, so strengthen just seeming particularly important to the detection of ammunition.
3-nitro-1,2,4-triazole-5-ketone (NTO) is one of study hotspot of recent domestic explosive research worker as a kind of high-energy insensitive energetic material.NTO is a kind of novel high-density, high-energy, low sensitivity, be easy to formed single chmical compound explosive.Its theoretical detonation rate is up to 8500m/s, and explosion velocity is close to RDX, and sensitivity is close to TATB, and toxicity is little, starting material are cheap and easy to get, easily prepare, better with the compatibility of other materials, therefore obtaining and pay attention to widely, is the important component of rifle propellant powder, casting blasting charge and composition explosive.But so far, the report about NTO explosive detection is little, the representational report (CN104155257A) having the synthesis squaric amide derivants such as Beijing Institute of Technology Shu Qinghai to be detected NTO explosive by the principle of complexing.But but have no report with ultraviolet spectrophotometer method direct and quick determination NTO content, its advantage is need not synthesising probing needle molecule, greatly can simplify testing process, reduces testing cost.Ultraviolet spectrophotometer is due to its fast response and device is simple and easy, with low cost etc. that advantage is widely used in constituent analysis field.Therefore, invent a kind of method, the synthesis of chemical probe need not be carried out, directly use that ultraviolet spectrophotometer is simple and convenient, fast and effeciently to detect NTO explosive be an important innovations in detection method, for the detection application of NTO improves feasibility and convenience.
Summary of the invention
The invention provides a kind of method of ultraviolet spectrophotometer method express-analysis NTO explosive content.The method fast and effeciently can detect the content of NTO.
The object of the invention is to be achieved through the following technical solutions.
A method for ultraviolet spectrophotometer method express-analysis NTO explosive content, concrete steps are as follows:
Step one, by soluble in water for NTO standard items, be mixed with the aqueous solution of variable concentrations NTO standard items.
The ultra-violet absorption spectrum of the NTO standard items aqueous solution of the variable concentrations obtained in step 2, determination step one, the absorbance of the NTO aqueous solution of variable concentrations at 336nm place and its concentration are done x-y curve respectively, establish corresponding relation, quantitatively detected the standard equation y=a+bx of NTO concentration.Wherein y is the ultraviolet absorptivity of surveyed NTO aqueous solution maximum absorption wavelength 336nm place correspondence, and x is the content (unit: 10 of NTO in sample
-5m), a=0.01421, b=0.02581; By detectability formula: detection limit=3 σ
bi/ m (σ: the standard deviation of response, m: the slope of calibration curve) tries to achieve detection and is limited to 1.78mg/L
Step 3, by soluble in water for NTO testing sample, be made into NTO aqueous solution, survey its ultra-violet absorption spectrum; By in the ultra-violet absorption spectrum of measured sample, the absorbance at 336nm place substitutes in the NTO quantitative criterion equation of step 2 gained, can determine the content of NTO in sample.
The compound method of the NTO aqueous solution described in step one, concrete steps are as follows:
Because required NTO concentration of aqueous solution is lower, during preparation, weighing error is comparatively large, so first prepare 10
-2the variable concentrations NTO aqueous solution of the mol/L order of magnitude, then corresponding dilution obtains 10 respectively
-4, 10
-6, 10
-8the variable concentrations NTO aqueous solution of the mol/L order of magnitude.Because NTO dissolves comparatively slow in water, and its thermal stability is good, so heating water bath that can be suitable, and accelerate dissolution.
Beneficial effect
The method of a kind of ultraviolet spectrophotometer method express-analysis NTO explosive content of the present invention, use ultraviolet spectrophotometer direct-detection NTO explosive first, eliminate loaded down with trivial details probe synthesis, enormously simplify testing process, reduce testing cost, and improve the sensitivity of sensing range and detection, the widespread use for NTO explosive provides important technical support.
Accompanying drawing explanation
Fig. 1 is the UV-Vis spectra figure of NTO aqueous solution under variable concentrations in the present invention;
Fig. 2 is the graph of a relation of 336nm place ultraviolet absorptivity and NTO concentration in NTO aqueous solution ultraviolet spectrogram in the present invention.
Embodiment
Below in conjunction with embodiment and accompanying drawing, the present invention will be further described.
Embodiment 1
For verifying accuracy and the reliability of the detection method of NTO explosive of the present invention, artificial preparation is containing the sample of NTO explosive.First prepare 10
-2the variable concentrations NTO aqueous solution of the mol/L order of magnitude, then dilution obtains NTO content and is respectively 2.0 × 10
-6, 4.0 × 10
-6, 5.0 × 10
-6, 6.0 × 10
-6, 7.0 × 10
-6the sample of mol/L.Uv scan is carried out respectively with ultraviolet spectrophotometer after NTO aqueous solution is even, the ultraviolet absorptivity at 336nm place in the ultraviolet spectrogram recorded is brought in the standard equation y=a+bx quantitatively detecting NTO concentration, the x value obtained and the detection level of NTO.Wherein y is the ultraviolet absorptivity of surveyed NTO aqueous solution maximum absorption wavelength 336nm place correspondence, and x is the content (unit: 10 of NTO in sample
-5m), a=0.01421, b=0.02581; Testing result is as shown in table 1.
Table 1: to the detection of NTO explosive content
| Sample | 1 | 2 | 3 | 4 | 5 |
| Theoretical content | 2.0×10 -6 | 4.0×10 -6 | 5.0×10 -6 | 6.0×10 -6 | 7.0×10 -6 |
| Detection level | 1.98×10 -6 | 4.02×10 -6 | 5.03×10 -6 | 5.94×10 -6 | 7.07×10 -6 |
Embodiment 2
By method described in embodiment 1, manually preparation is containing five groups of samples of NTO explosive again, and the content of its NTO is respectively 1.0 × 10
-5, 2.0 × 10
-5, 3.0 × 10
-5, 5.0 × 10
-5, 8.0 × 10
-5mol/L.Uv scan is carried out respectively with ultraviolet spectrophotometer after NTO aqueous solution is even, the ultraviolet absorptivity at 336nm place in the ultraviolet spectrogram recorded is brought in the standard equation y=a+bx quantitatively detecting NTO concentration, the x value obtained and the detection level of NTO.Wherein y is the ultraviolet absorptivity of surveyed NTO aqueous solution maximum absorption wavelength 336nm place correspondence, and x is the content (unit: 10 of NTO in sample
-5m), a=0.01421, b=0.02581; Its testing result is as shown in table 2.
Table 2: to the detection of NTO explosive content
| Sample | 1 | 2 | 3 | 4 | 5 |
| Theoretical content | 1.0×10 -5 | 2.0×10 -5 | 3.0×10 -5 | 5.0×10 -5 | 8.0×10 -5 |
| Detection level | 1.04×10 -5 | 2.03×10 -5 | 3.04×10 -5 | 4.97×10 -5 | 8.02×10 -5 |
Embodiment 3
Again manually prepare five groups of samples containing NTO explosive by method described in embodiment 1, the content of its NTO is respectively 2.5 × 10
-4, 4.0 × 10
-4, 5.0 × 10
-4, 7.0 × 10
-4, 9.0 × 10
-4mol/L.Uv scan is carried out respectively with ultraviolet spectrophotometer after NTO aqueous solution is even, the ultraviolet absorptivity at 336nm place in the ultraviolet spectrogram recorded is brought in the standard equation y=a+bx quantitatively detecting NTO concentration, the x value obtained and the detection level of NTO.Wherein y is the ultraviolet absorptivity of surveyed NTO aqueous solution maximum absorption wavelength 336nm place correspondence, and x is the content (unit: 10 of NTO in sample
-5m), a=0.01421, b=0.02581; Its testing result is as shown in table 3.
Table 3: to the detection of NTO explosive content
| Sample | 1 | 2 | 3 | 4 | 5 |
| Theoretical content | 2.5×10 -4 | 4.0×10 -4 | 5.0×10 -4 | 7.0×10 -4 | 9.0×10 -4 |
| Detection level | 2.46×10 -4 | 4.03×10 -4 | 4.98×10 -4 | 6.94×10 -4 | 8.96×10 -4 |
From the result shown in above-mentioned three forms, adopt the inventive method to the actual detected value of NTO content and the content value added when making sample, namely theoretical content value is substantially identical, and error is less, can ignore.
The beneficial effect of the present invention to the method that NTO explosive content detects is simple to operate, and cost is low, and sensing range is wide, substantially increases the efficiency-cost ratio of detection.
Claims (2)
1. a method for ultraviolet spectrophotometer method express-analysis NTO explosive content, is characterized in that: concrete steps are as follows:
Step one, by soluble in water for NTO standard items, be mixed with variable concentrations NTO standard items aqueous solution;
The ultra-violet absorption spectrum of the NTO standard items aqueous solution of the variable concentrations obtained in step 2, determination step one, the absorbance of the NTO aqueous solution of variable concentrations at 336nm place and its concentration are done x-y curve respectively, establish corresponding relation, quantitatively detected the standard equation y=a+bx of NTO concentration; Wherein y is the ultraviolet absorptivity of surveyed NTO aqueous solution maximum absorption wavelength 336nm place correspondence, and x is the content (unit: 10 of NTO in sample
-5m), a=0.01421, b=0.02581; By detectability formula: detection limit=3 σ
bi/ m (σ: the standard deviation of response, m: the slope of calibration curve) tries to achieve detection and is limited to 1.78mg/L
Step 3, by soluble in water for NTO testing sample, be made into NTO aqueous solution, survey its ultra-violet absorption spectrum; By in the ultra-violet absorption spectrum of measured sample, the absorbance at 336nm place substitutes in the NTO quantitative criterion equation of step 2 gained, can determine the content of NTO in sample.
2. the method for a kind of ultraviolet spectrophotometer method express-analysis NTO explosive content as claimed in claim 1, is characterized in that: the compound method of the NTO standard items aqueous solution described in step one is: first prepare 10
-2the NTO aqueous solution of the variable concentrations of the mol/L order of magnitude, then corresponding dilution obtains 10 respectively
-4, 10
-6, 10
-8the variable concentrations of the mol/L order of magnitude.
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|---|---|---|---|
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107727556A (en) * | 2017-09-15 | 2018-02-23 | 天津大学 | Microcystic aeruginosa Rapid Quantification in a kind of water |
| CN107991257A (en) * | 2018-01-30 | 2018-05-04 | 石家庄市和合化工化肥有限公司 | The quantitative detecting method of Sulphur Monochloride and sulphur dichloride impurity content in thionyl chloride |
| CN111948369A (en) * | 2020-07-23 | 2020-11-17 | 西安近代化学研究所 | Passivation NTO coating quality evaluation method prepared by supercritical method |
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|---|---|---|---|---|
| CN1733739A (en) * | 2005-07-28 | 2006-02-15 | 中北大学 | 3-nitro-1,2,4-triazole-5-ketone superfining process |
| US20070212791A1 (en) * | 2006-03-10 | 2007-09-13 | Hummel Rolf E | Differential reflection spectroscopy system and method for detecting explosives and other target materials |
| US8174691B1 (en) * | 2007-03-15 | 2012-05-08 | Arkansas State University—Jonesboro | Detection of a component of interest with an ultraviolet laser and method of using the same |
| CN104155257A (en) * | 2014-07-23 | 2014-11-19 | 北京理工大学 | Method for detecting NTO explosive by utilizing squaramide derivative |
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2015
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| CN1733739A (en) * | 2005-07-28 | 2006-02-15 | 中北大学 | 3-nitro-1,2,4-triazole-5-ketone superfining process |
| US20070212791A1 (en) * | 2006-03-10 | 2007-09-13 | Hummel Rolf E | Differential reflection spectroscopy system and method for detecting explosives and other target materials |
| US8174691B1 (en) * | 2007-03-15 | 2012-05-08 | Arkansas State University—Jonesboro | Detection of a component of interest with an ultraviolet laser and method of using the same |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107727556A (en) * | 2017-09-15 | 2018-02-23 | 天津大学 | Microcystic aeruginosa Rapid Quantification in a kind of water |
| CN107991257A (en) * | 2018-01-30 | 2018-05-04 | 石家庄市和合化工化肥有限公司 | The quantitative detecting method of Sulphur Monochloride and sulphur dichloride impurity content in thionyl chloride |
| CN107991257B (en) * | 2018-01-30 | 2020-06-09 | 石家庄市和合化工化肥有限公司 | Quantitative detection method for content of sulfur monochloride and sulfur dichloride impurities in thionyl chloride |
| CN111948369A (en) * | 2020-07-23 | 2020-11-17 | 西安近代化学研究所 | Passivation NTO coating quality evaluation method prepared by supercritical method |
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Application publication date: 20150826 |