CN113189096A - Reagent for detecting nitrate ions in explosives and powders and detection method thereof - Google Patents
Reagent for detecting nitrate ions in explosives and powders and detection method thereof Download PDFInfo
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- CN113189096A CN113189096A CN202110697158.9A CN202110697158A CN113189096A CN 113189096 A CN113189096 A CN 113189096A CN 202110697158 A CN202110697158 A CN 202110697158A CN 113189096 A CN113189096 A CN 113189096A
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
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Abstract
The invention belongs to the field of explosive detection, and particularly relates to a reagent for detecting nitrate ions in explosives and powders and a detection method thereof. A reagent for detecting nitrate ions in explosives and powders comprises the following components in parts by weight: 0.5-3.0 parts of 8-hydroxyquinoline, 0.5-3.0 parts of 4-aminobenzoic acid, 5-10 parts of manganese sulfate, 50-60 parts of barium sulfate, 1-3 parts of zinc powder and 30-50 parts of strong acid. The method mainly aims at detecting the components and the contents of the residual nitrate ions in the scene of the explosive explosion case, and solves the technical problem that the current scene of the explosive explosion case can not directly, quickly, visually and detect the components and the contents of the nitrate ions at low cost. The reagent has low detection limit, strong anti-interference performance and short reaction time, and can completely realize the purpose of detecting nitrate ions by real-time colorimetric detection at low cost. The reagent can be applied to qualitative and semi-quantitative analysis of nitrate in explosive residues on explosive fields. In addition, the reagent has no interference to common ions.
Description
Technical Field
The invention belongs to the field of explosive detection, and particularly relates to a reagent for detecting nitrate ions in explosives and powders and a detection method thereof.
Background
For many years, due to the fact that the safety cognition degree of people on explosives and powders is not high enough, many combustion and explosion accidents occur in the processes of production, storage, transportation and use of the explosives and powders, and serious casualties and property loss are caused. Therefore, researchers have developed many detection methods for nitro explosives. Such as: the M.R.Mahmoudian group of university of Malaysia successfully achieved nitrate detection using electrochemical methods with limits of detection as low as 0.4535. mu.M (Journal of electrochemical Chemistry, 2015, 751: 30-36). The Paul J.Worsfold project group of the university of Primedes, UK achieved detection limits of 0.02 μ gN/L and 0.02 μ g N/L for nitrate and nitrite, respectively, using chemiluminescence (Luminesconce, 2012,27.5: 419-425). Detection of nitrate in river water, pond water, rainwater, commercial mineral water and tap water was achieved by liquid Chromatography (Journal of Chromatography A,2009,1216: 3163-. The Shinichi Wakida project group of the national institute of Industrial and technology successfully realizes detection of nitrate at the detection limit of 2.6 and 1.5. mu.M by capillary electrophoresis (Journal of chromatography A,2004,1051: 185-191). Among The numerous detection methods, spectroscopic techniques are widely used due to their low detection limit and ease of operation, including UV-visible analysis (Analytical chip acta,1994,299:81-90), chemiluminescence analysis (Freenius' Journal of Analytical Chemistry,2000,367.3: 264-. However, these methods of detecting nitrate by chemical reaction, including the most commonly used Grignard reagents, are all performed by reducing nitrate to nitrite with higher chemical activity (analytical chimica acta,1995,308: 413-424). According to extensive literature research, only the Michael Gozin subject group of Delavav university in Israel utilizes the characteristic that nitrate can oxidize thioether into sulfoxide under a molybdenum-copper catalytic system, and the aim of directly detecting nitrate by a fluorescence method is successfully achieved (Organic letters,2011,13: 5532-.
The colorimetric method is the most promising method in the detection field because of simple operation and visual and reliable result. Unfortunately, however, to date, no one has been able to rapidly and accurately quantify suspected nitrate species at the explosive site of a gunpowder explosive. In order to realize the on-site rapid detection and analysis of suspicious nitrate explosives, the development of a reagent capable of directly detecting nitrate through colorimetric detection is an urgent and most challenging problem.
Disclosure of Invention
In view of the problems of the prior art, the invention aims to provide a reagent for detecting nitrate ions in explosives and a detection method thereof. The reagent of the invention changes color immediately after contacting with nitrate, and complex analysis equipment is not needed, thereby realizing low-cost, instant and trace detection of nitrate. The reagent has simple operation, high sensitivity and low cost. Overcomes the defects of complex synthesis, low sensitivity, long reaction time and the like of probe molecules used in the colorimetric detection method of nitrate radical in the prior art, and provides an effective technical means for the field of detection of explosive raw materials. The detection reagent has a lower detection limit (naked eye detection limit of 0.1mg/mL) and extremely high selectivity for nitrate, so that the nitrate in the explosive raw material can be detected.
In order to achieve the purpose, the invention adopts the following technical scheme.
A reagent for detecting nitrate ions in explosives and powders comprises the following components in parts by weight:
0.5-3.0 parts of 8-hydroxyquinoline, 0.5-3.0 parts of 4-aminobenzoic acid, 5-10 parts of manganese sulfate, 50-60 parts of barium sulfate, 1-3 parts of zinc powder and 30-50 parts of strong acid.
Further, the strong acid is one of tartaric acid, glycolic acid, oxalic acid and citric acid, and citric acid is preferred.
Further, the manganese sulfate and zinc powder are used as a catalyst.
Further, the barium sulfate solid powder is used for dilution, so that the concentration is prevented from being too high.
The method for detecting nitrate ions in explosives and powders comprises the following steps:
step 1, preparing potassium nitrate solutions at concentrations of 8mg/mL, 4mg/mL, 2mg/mL, 1mg/mL, 0.7mg/mL, 0.5mg/mL, 0.2mg/mL, 0.1mg/mL, 0.05mg/mL and 0mg/mL, respectively, for use.
And 2, mixing 0.5-3.0 parts of 8-hydroxyquinoline, 0.5-3.0 parts of 4-aminobenzoic acid, 5-10 parts of manganese sulfate, 50-60 parts of barium sulfate, 1-3 parts of zinc powder and 30-50 parts of strong acid to obtain a detection reagent, and putting the detection reagent into 10 colorimetric bottles.
And 3, respectively dripping 2-3 drops of potassium nitrate solution with different concentrations in the step 1 into the colorimetric bottle in the step 2, and drawing a colorimetric card according to the displayed color.
And 4, taking the explosive dust, adding deionized water for extraction, filtering, and transferring the filtrate into a test tube to serve as an extracting solution for later inspection. Dripping 2-3 drops of the extracting solution, comparing with a blank extracting agent, and checking to obtain the content of nitrate ions by comparing with a standard colorimetric card.
Further, the weight ratio of the explosion dust to the deionized water in the step 4 is 1: 5-10.
Further, the extraction and filtration in the step 4 are to pour the solution into a funnel with filter paper for filtration.
Further, the hollow extracting agent in the step 4 is deionized water with the same weight as that of the extracting solution.
Compared with the prior art, the invention has the following beneficial effects.
1. The raw materials of the reagent used in the invention can be purchased from commercial markets.
2. The detection reagent can detect nitrate sensitively and selectively.
3. The detection reagent provided by the invention is used for detecting nitrate ions, does not need complex analysis equipment, and can be directly identified and detected by naked eyes.
4. The reagent does not need to carry out any pretreatment on the object to be detected, is simple to operate and convenient to popularize and apply, has low detection limit, strong anti-interference performance and short reaction time, and can completely realize the aim of colorimetric detection of nitrate ions in real time at low cost.
5. The reagent can be applied to qualitative and semi-quantitative analysis of nitrate in explosive residues on explosive fields. In addition, the reagent has no interference to common ions.
6. The reagent for rapidly detecting nitrate ions by colorimetry mainly detects the components and the contents of the residual nitrate ions in the scene of the explosive explosion case, and solves the technical problem that the current scene of the explosive explosion case can not directly, rapidly, visually and inexpensively detect the components and the contents of the nitrate ions.
Drawings
FIG. 1 is a color comparison bottle and a drawn standard color comparison card in which a formula 1 is acted with potassium nitrate solutions with different concentrations.
FIG. 2 illustrates an example of a test result.
FIG. 3 shows the results of example two tests.
Fig. 4 illustrates the results of the three tests.
Detailed Description
The following describes in detail specific embodiments of the present invention. It should be understood that the detailed description and specific examples, while indicating the present invention, are given by way of illustration and explanation only, not limitation.
A reagent for detecting nitrate ions in explosives and powders comprises the following components in parts by weight:
0.5-3.0 parts of 8-hydroxyquinoline, 0.5-3.0 parts of 4-aminobenzoic acid, 5-10 parts of manganese sulfate, 50-60 parts of barium sulfate, 1-3 parts of zinc powder and 30-50 parts of strong acid.
Further, the strong acid is one of tartaric acid, glycolic acid, oxalic acid and citric acid, and citric acid is preferred.
Further, the manganese sulfate and zinc powder are used as a catalyst.
Further, the barium sulfate solid powder is used for dilution, so that the concentration is prevented from being too high.
The method for detecting nitrate ions in explosives and powders comprises the following steps:
step 1, preparing potassium nitrate solutions at concentrations of 8mg/mL, 4mg/mL, 2mg/mL, 1mg/mL, 0.7mg/mL, 0.5mg/mL, 0.2mg/mL, 0.1mg/mL, 0.05mg/mL and 0mg/mL, respectively, for use.
And 2, mixing 0.5-3.0 parts of 8-hydroxyquinoline, 0.5-3.0 parts of 4-aminobenzoic acid, 5-10 parts of manganese sulfate, 50-60 parts of barium sulfate, 1-3 parts of zinc powder and 30-50 parts of strong acid to obtain a detection reagent, and putting the detection reagent into 10 colorimetric bottles.
And 3, respectively dripping 2-3 drops of potassium nitrate solution with different concentrations in the step 1 into the colorimetric bottle in the step 2, and drawing a colorimetric card according to the displayed color.
And 4, taking the explosive dust, adding deionized water for extraction, filtering, and transferring the filtrate into a test tube to serve as an extracting solution for later inspection. Dripping 2-3 drops of the extracting solution, comparing with a blank extracting agent, and checking to obtain the content of nitrate ions by comparing with a standard colorimetric card.
Further, the weight ratio of the explosion dust to the deionized water in the step 4 is 1: 5-10.
Further, the extraction and filtration in the step 4 are to pour the solution into a funnel with filter paper for filtration.
Further, the hollow extracting agent in the step 4 is deionized water with the same weight as that of the extracting solution.
Response time of reagents with different proportions.
Formula 1: 0.5 part of 8-hydroxyquinoline, 1.5 parts of 4-aminobenzoic acid, 30 parts of citric acid, 7 parts of manganese sulfate, 2 parts of zinc powder and 59 parts of barium sulfate.
And (2) formula: 0.5 part of 8-hydroxyquinoline, 1.0 part of 4-aminobenzoic acid, 30 parts of citric acid, 7 parts of manganese sulfate, 2 parts of zinc powder and 59.5 parts of barium sulfate.
And (3) formula: 0.5 part of 8-hydroxyquinoline, 0.5 part of 4-aminobenzoic acid, 30 parts of citric acid, 7 parts of manganese sulfate, 2 parts of zinc powder and 60 parts of barium sulfate.
And (4) formula: 1.0 part of 8-hydroxyquinoline, 0.5 part of 4-aminobenzoic acid, 30 parts of citric acid, 7 parts of manganese sulfate, 2 parts of zinc powder and 59.5 parts of barium sulfate.
And (5) formula: 1.5 parts of 8-hydroxyquinoline, 0.5 part of 4-aminobenzoic acid, 30 parts of citric acid, 7 parts of manganese sulfate, 2 parts of zinc powder and 59 parts of barium sulfate.
Taking a colorimetric bottle with the formula of 1-5 and 2 drops of 0.1mg/mL nitrate ions to act respectively, and discussing the response time relationship. The response speed of the formula 1 is the fastest, about 20 seconds; the response time for formulation 2 was about 40 seconds; the response time for formulation 3 was about 90 seconds; the response time for formulation 4 was about 70 seconds; the response time for formulation 5 was about 90 seconds.
Potassium nitrate solutions at concentrations of 8mg/mL, 4mg/mL, 2mg/mL, 1mg/mL, 0.7mg/mL, 0.5mg/mL, 0.2mg/mL, 0.1mg/mL, 0.05mg/mL and 0mg/mL were prepared for use.
And (3) taking the colorimetric bottle of the formula 1 to react with standard solutions of potassium nitrate solutions with different concentrations to draw a colorimetric card. The lowest visually detectable concentration for formulation 1 was 0.1 mg/mL.
Examples are given.
Example one: taking suspected black powder explosive residue (i) as a test material 1, weighing 1.0 g of explosive dust, adding 8.0 mL of deionized water for extraction, filtering, dropwise adding 2 drops of extracting solution into a colorimetric bottle with the formula 1, comparing with a blank extracting agent for inspection, and comparing by a standard colorimetric card to obtain that the test material contains about 2mg/mL of nitrate ions. Therefore, the mass concentration of nitrate ions in the sample was 16.0 mg/g.
Example two: and taking suspected black powder explosive residues (II) as a detection material (2), weighing 1.0 g of explosive dust, adding 8.0 mL of deionized water for extraction, filtering, dropwise adding 2 drops of an extracting solution into a colorimetric bottle, comparing with a blank extracting agent for inspection, and comparing by using a standard colorimetric card to obtain that the content of nitrate ions in the detection material is about 8 mg/mL. Therefore, the mass concentration of nitrate ions in the sample was 64.0 mg/g.
Example three: taking suspected ammonium nitrate explosive residue (c) as a test material 3, weighing 1.0 g of explosive dust, adding 8.0 mL of deionized water for extraction, filtering, dropwise adding 2 drops of extracting solution into a colorimetric bottle, comparing with a blank extracting agent for inspection, and comparing by a standard colorimetric card to obtain that the test material contains about 0.1mg/mL of nitrate ions. Therefore, the mass concentration of nitrate ions in the sample was 0.8 mg/g.
Claims (8)
1. The reagent for detecting nitrate ions in explosives and powders is characterized by comprising the following components in parts by weight:
0.5-3.0 parts of 8-hydroxyquinoline, 0.5-3.0 parts of 4-aminobenzoic acid, 5-10 parts of manganese sulfate, 50-60 parts of barium sulfate, 1-3 parts of zinc powder and 30-50 parts of strong acid.
2. The reagent for detecting nitrate ions in explosives and powders of claim 1, wherein the strong acid is one of tartaric acid, glycolic acid, oxalic acid and citric acid.
3. The reagent for detecting nitrate ions in explosives and powders as claimed in claim 1, wherein manganese sulfate and zinc powder are used as catalysts.
4. The reagent for detecting nitrate ions in explosives and powders of claim 1, wherein the reagent is diluted with barium sulfate solid powder to prevent excessive concentration.
5. The method for detecting nitrate ions in explosives and powders is characterized by comprising the following steps:
step 1, preparing potassium nitrate solutions with the concentrations of 8mg/mL, 4mg/mL, 2mg/mL, 1mg/mL, 0.7mg/mL, 0.5mg/mL, 0.2mg/mL, 0.1mg/mL, 0.05mg/mL and 0mg/mL respectively for later use;
step 2, mixing 0.5-3.0 parts of 8-hydroxyquinoline, 0.5-3.0 parts of 4-aminobenzoic acid, 5-10 parts of manganese sulfate, 50-60 parts of barium sulfate, 1-3 parts of zinc powder and 30-50 parts of strong acid to obtain a detection reagent, and putting the detection reagent into 10 colorimetric bottles;
step 3, respectively dripping 2-3 drops of potassium nitrate solution with different concentrations in the step 1 into the colorimetric bottle in the step 2, and drawing a colorimetric card according to the displayed color;
step 4, adding deionized water into the explosive dust for extraction and filtration, and transferring the filtrate into a test tube to serve as an extracting solution for standby inspection;
dripping 2-3 drops of the extracting solution, comparing with a blank extracting agent, and checking to obtain the content of nitrate ions by comparing with a standard colorimetric card.
6. The method for detecting nitrate ions in explosives and powders according to claim 1, wherein the weight ratio of the dust and the deionized water in the step 4 is 1: 5-10.
7. The method for detecting nitrate ions in explosives and powders according to claim 1, wherein the extraction and filtration in step 4 are carried out by pouring the solution into a funnel with filter paper for filtration.
8. The method for detecting nitrate ions in explosives and powders of claim 1, wherein the white extractant in step 4 is deionized water with the same weight as that in the extracting solution.
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| CN202110697158.9A CN113189096A (en) | 2021-06-23 | 2021-06-23 | Reagent for detecting nitrate ions in explosives and powders and detection method thereof |
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| CN202110697158.9A CN113189096A (en) | 2021-06-23 | 2021-06-23 | Reagent for detecting nitrate ions in explosives and powders and detection method thereof |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1084276A (en) * | 1992-09-03 | 1994-03-23 | 以色列生物学研究院 | The detection method of explosive and detection bag |
| CN1614397A (en) * | 2004-11-23 | 2005-05-11 | 浙江省农业科学院 | Reagent box and detecting method for nitrate and nitrite content of vegetables and fruits |
| US20060121621A1 (en) * | 2004-12-06 | 2006-06-08 | Basant Bhandari | Nitrate/nitrite assay reagents, kit, and method of use |
| CN104316517A (en) * | 2014-10-09 | 2015-01-28 | 西安华陆环保设备有限公司 | Detection method of nitrite content |
| CN108872226A (en) * | 2018-08-30 | 2018-11-23 | 中国科学院新疆理化技术研究所 | A kind of reagent of quick colorimetric detection nitrate anion and nitrite anions |
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- 2021-06-23 CN CN202110697158.9A patent/CN113189096A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1084276A (en) * | 1992-09-03 | 1994-03-23 | 以色列生物学研究院 | The detection method of explosive and detection bag |
| CN1614397A (en) * | 2004-11-23 | 2005-05-11 | 浙江省农业科学院 | Reagent box and detecting method for nitrate and nitrite content of vegetables and fruits |
| US20060121621A1 (en) * | 2004-12-06 | 2006-06-08 | Basant Bhandari | Nitrate/nitrite assay reagents, kit, and method of use |
| CN104316517A (en) * | 2014-10-09 | 2015-01-28 | 西安华陆环保设备有限公司 | Detection method of nitrite content |
| CN108872226A (en) * | 2018-08-30 | 2018-11-23 | 中国科学院新疆理化技术研究所 | A kind of reagent of quick colorimetric detection nitrate anion and nitrite anions |
Non-Patent Citations (1)
| Title |
|---|
| 安登魁 等主编: "《药物分析》", 30 June 1992, 人民卫生出版社 * |
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