阅读说明：本技术 一种***物中硝酸盐的比色检测方法 (Colorimetric detection method for nitrate in explosive ) 是由 窦新存 张天实 于 2019-10-26 设计创作，主要内容包括：本发明提供了一种爆炸物中硝酸盐的比色检测方法,该检测方法所述检测试剂为N-1-萘乙二胺盐酸盐、对氨基苯磺酰胺、硫酸联氨、水和磷酸配制而成,测试纸为锌粉均匀涂抹在滤纸上,之后滴加压敏胶,用棉棒采集样品,将样品置于测试纸上,将检测试剂滴加到含有样品的测试纸上,通过观察是否产生玫瑰红色复合物,以此确定硝酸盐的存在。本发明所述的检测方法可用于现场搜爆及爆炸案中对爆炸物自制炸药及爆炸残留物中硝酸盐的定性检测,检测限可达到100μg。该方法无须将可疑物样品溶解,具有操作简单迅速,特异性强,反应灵敏,使用方便,成本低的特点,可为公安系统刑侦部门爆炸案的侦破提供有效技术手段。(The invention provides a colorimetric detection method for nitrate in explosives, which is characterized in that a detection reagent is prepared from N-1-naphthyl ethylenediamine hydrochloride, sulfanilamide, hydrazine sulfate, water and phosphoric acid, test paper is prepared by uniformly coating zinc powder on filter paper, then dropwise adding a pressure-sensitive adhesive, collecting a sample by using a cotton stick, placing the sample on the test paper, dropwise adding the detection reagent on the test paper containing the sample, and determining the existence of the nitrate by observing whether a rose-red compound is generated or not. The detection method can be used for qualitatively detecting nitrate in self-made explosives of explosives and explosive residues in field explosion searching and explosion cases, and the detection limit can reach 100 mu g. The method does not need to dissolve suspicious samples, has the characteristics of simple and rapid operation, strong specificity, sensitive reaction, convenient use and low cost, and can provide an effective technical means for the detection of the explosion case of the public security system criminal detection department.)

1. A colorimetric detection method for nitrate in explosives is characterized by comprising the following operation steps:

preparing a detection reagent:

a. weighing 0.015-0.02g of sulfanilamide, 0.005-0.015g of N-1-naphthyl ethylenediamine hydrochloride and 0.01-0.05g of hydrazine sulfate at room temperature, putting into a container, adding 20mL of water, fully stirring until the mixture is completely dissolved, adding 20 mu L of phosphoric acid, continuously stirring for 10min, sealing, introducing nitrogen for 20min to obtain a detection reagent, and packaging the detection reagent in a reagent bottle;

preparing test paper;

b. uniformly coating 0.1g of zinc powder (2) on filter paper (1), then dropwise adding a pressure-sensitive adhesive (3), airing, cutting to obtain test paper (4), and then filling the test paper (4) into a test bag;

c. b, extracting a detection sample from the explosive to be detected by using a cotton swab, wiping the detection sample onto the test paper (4), dropwise adding the detection reagent obtained in the step a onto the test paper (4) containing the detection sample, and observing the color change of the test paper (4).

2. The colorimetric detection method of nitrate in explosives according to claim 1, characterized in that the explosives in step c are nitrate in homemade explosives or explosive residues.

Technical Field

The invention relates to a colorimetric detection method for nitrate in explosives, in particular to a colorimetric detection method for nitrate in self-made explosives and explosive residues.

Background

In recent years, the number of terrorist explosions in the world is increasing, and a rapid and convenient detection and analysis technology for explosives is urgently needed. At present, the commercialized portable explosive detection means include ion mobility spectrometry, metal detectors, portable raman technology, fluorescence method, etc., wherein only the ion mobility spectrometry and the portable raman technology can identify explosive components, but the ion mobility spectrometry has the disadvantages of time consumption in calibration and high cost; portable raman techniques generally require large sample volumes and expensive instruments.

At present, nitrate detection methods mainly comprise two methods, one method is a method of diphenyl benzidine and analogues thereof, nitrate ions can react with diphenyl benzidine to generate blue compounds in the presence of concentrated sulfuric acid, the method utilizes the oxidability of nitrate in the environment of concentrated sulfuric acid, but nitrite can also form similar reaction under the condition, and differentiation cannot be carried out. The other method is to utilize a Griess reagent, firstly dissolve a sample through a cadmium column, reduce nitrate into nitrite by utilizing cadmium, and react the sample after the cadmium column reaction with the Griess reagent to verify the existence of nitrate. The method needs a cadmium column, and has high cost and poor portability.

The invention discloses a colorimetric detection method for nitrate in explosives, which mainly utilizes test paper coated with zinc powder to replace a cadmium column to play a role in reducing nitrate, and then applies a Griess reagent to react with the test paper to achieve the effect of detecting the nitrate. The reagent has the advantages of easily obtained raw materials, simple and convenient preparation, light weight, portability, strong selectivity and wide application potential.

Disclosure of Invention

The invention aims to provide a colorimetric detection method for nitrate in explosives, which is characterized in that a detection reagent is prepared from N-1-naphthyl ethylenediamine hydrochloride, sulfanilamide, hydrazine sulfate, water and phosphoric acid, test paper is prepared by uniformly coating zinc powder on filter paper, then dropwise adding a pressure-sensitive adhesive, collecting a sample by using a cotton stick, placing the sample on the test paper, dropwise adding the detection reagent on the test paper containing the sample, and determining the existence of the nitrate by observing whether a rose-red compound is generated or not. The detection method can be used for qualitatively detecting nitrate in self-made explosives of explosives and explosive residues in field explosion searching and explosion cases, and the detection limit can reach 100 mu g. The method does not need to dissolve suspicious samples, has the characteristics of simple and rapid operation, strong specificity, sensitive reaction, convenient use and low cost, and can provide an effective technical means for the detection of the explosion case of the public security system criminal detection department.

The colorimetric detection method for nitrate in explosives is carried out according to the following operation steps:

preparing a detection reagent:

a. weighing 0.015-0.02g of sulfanilamide, 0.005-0.015g of N-1-naphthyl ethylenediamine hydrochloride and 0.01-0.05g of hydrazine sulfate at room temperature, putting into a container, adding 20mL of water, fully stirring until the mixture is completely dissolved, adding 20 mu L of phosphoric acid, continuously stirring for 10min, sealing, introducing nitrogen for 20min to obtain a detection reagent, and packaging the detection reagent in a reagent bottle;

preparing test paper;

b. uniformly coating 0.1g of zinc powder (2) on filter paper (1), then dropwise adding a pressure-sensitive adhesive (3), airing, cutting to obtain test paper (4), and then filling the test paper (4) into a test bag;

c. b, extracting a detection sample from the explosive to be detected by using a cotton swab, wiping the detection sample onto the test paper (4), dropwise adding the detection reagent obtained in the step a onto the test paper (4) containing the detection sample, and observing the color change of the test paper (4).

The explosive in the step c is self-made explosive, and nitrate in explosive residues.

The invention relates to a colorimetric detection method for nitrate in explosives, which is characterized in that the detection object is self-made explosives and nitrate in explosive residues, the detection reagent is prepared from N-1-naphthyl ethylenediamine hydrochloride, sulfanilamide, hydrazine sulfate, water and phosphoric acid at room temperature, and the test paper is filter paper which is uniformly coated with zinc powder and is dropwise added with pressure-sensitive adhesive. Collecting a sample by using a cotton stick, placing the sample on test paper, dropwise adding a detection reagent on the test paper containing the sample, reducing nitrate into nitrite in the presence of zinc powder, carrying out diazotization reaction on the nitrite and sulfanilamide, and then coupling with N-1-naphthalene ethylene diamine hydrochloride to form a rose-red compound so as to determine the presence of the nitrate.

The invention relates to a colorimetric detection method for nitrate in explosives, which is based on a chemical colorimetric method, does not need to dissolve a suspicious sample, reduces the nitrate by using test paper containing zinc powder, and then reacts with the test paper by using a Griess reagent to generate a rose-red compound, thereby achieving the effect of detecting the nitrate. The detection method can be used for qualitatively detecting the nitrate in the explosive and the explosive residue in the field explosion search and explosion cases, has the characteristics of simple operation, strong specificity, sensitive response, convenient use and low cost, and can provide an effective technical means for detecting the explosion cases of the public security system criminal investigation department.

The invention provides a colorimetric detection method of nitrate in explosives, which can detect at least 100 mu g of nitrate in sulfur in the explosives.

Drawings

FIG. 1 is a schematic structural view of a test sheet according to the present invention;

FIG. 2 is a schematic view of the test paper of the present invention.

Detailed Description