CN108717043B

CN108717043B - Nitrite detection board

Info

Publication number: CN108717043B
Application number: CN201810530686.3A
Authority: CN
Inventors: 史绵红; 朱敏; 胡雅琴; 杨晓冉; 张敏; 朱余
Original assignee: Anhui Ecological Environment Monitoring Center Anhui Heavy Pollution Weather Forecast And Early Warning Center
Current assignee: Anhui Ecological Environment Monitoring Center Anhui Heavy Pollution Weather Forecast And Early Warning Center
Priority date: 2018-05-29
Filing date: 2018-05-29
Publication date: 2020-12-15
Anticipated expiration: 2038-05-29
Also published as: CN108717043A

Abstract

The invention belongs to the field of chemical detection instruments, and particularly relates to a nitrite detection plate which comprises a plate body and a cover body; a detection hole sealed by a cover body is arranged on the plate body, and a nitrite gel detection layer is arranged in the detection hole; the volume ratio of the alumina sol to the nitrite color developing agent solution in the nitrite gel detection layer is 1: 3-3: 1; the detection hole is provided in plurality. The detection plate disclosed by the invention is simple in structure, can be manufactured in batch, is low in reagent consumption, and realizes rapid green and environment-friendly detection of nitrite.

Description

Nitrite detection board

Technical Field

The invention belongs to the field of chemical detection devices, and particularly relates to a nitrite detection plate.

Background

Nitrite is widely present in human living environments, especially in water environments and in the food sector. Due to the potential toxicity of nitrite, the content determination of nitrite has important practical significance in the fields of environmental science, public health and the like. The nitrite determination method mainly comprises spectrophotometry, ion chromatography, electrochemical method and the like. Among them, the national standard analysis methods mostly adopt visible spectrophotometry and ion chromatography, and visible spectrophotometry is used in actual detection activities due to low instrument and equipment cost and relatively simple operation.

The rapid detection of nitrite plays an important role in the activities of on-site emergency monitoring of emergency environmental events, general investigation of underground water environmental quality, rapid screening of food safety and the like. At the present stage, mature nitrite rapid detection is mainly used as solid/state detection tools such as test paper, powder, capsules and the like, but the rapid detection method has the defects of large reagent consumption, difficulty in batch operation, low detection speed and the like.

Disclosure of Invention

According to the problems in the prior art, the invention provides the nitrite detection plate which is simple in structure, can be manufactured in batch, is low in reagent consumption, and realizes rapid green and environment-friendly detection of nitrite.

The invention adopts the following technical scheme:

a nitrite detection plate comprises a plate body and a cover body; the detection hole sealed through the cover body is formed in the plate body, and a nitrite gel detection layer is arranged in the detection hole.

Preferably, the nitrite gel detection layer is formed by gelling a mixture of alumina sol and nitrite developer solution in the detection pores.

Preferably, 0.02-0.05 g/mL of aluminum isopropoxide solution is prepared, after heating and stirring, hydrochloric acid is added to enable the concentration of the hydrochloric acid in the mixed solution to be 0.02-0.04 mol/L, the mixed solution is continuously heated, and finally, the mixed solution is transferred and bottled after cooling.

Preferably, the aluminum isopropoxide solution is heated to 70-80 ℃ and stirred for 30-60 minutes; and heating the mixed solution to 85-95 ℃, opening the opening for 1-2 hours, refluxing for 12-18 hours, cooling to room temperature, transferring and bottling to obtain the alumina sol.

Preferably, a phosphoric acid solution with the volume percentage concentration of 5-20% is prepared, p-aminobenzenesulfonamide and N-ethylenediamine dihydrochloride are sequentially added and dissolved in the phosphoric acid solution, so that the concentration of the p-aminobenzenesulfonamide in the nitrite color developing agent solution is 2-6 g/mL, the concentration of the N-ethylenediamine dihydrochloride in the nitrite color developing agent solution is 0.1-0.3 g/mL, and the finally prepared nitrite color developing agent solution is placed in a brown bottle and is refrigerated for storage.

Preferably, the volume ratio of the alumina sol to the nitrite color developing agent solution in the nitrite gel detection layer is 1: 3-3: 1, 5-100 microliters of the mixed solution of the alumina sol and the nitrite color developing agent solution is dropped into the detection hole, and the detection hole is gelled under the condition of refrigeration and light shielding to realize the fixation of the nitrite gel detection layer.

More preferably, the detection hole is provided in plurality; and the preparation of the nitrite gel detection layer is completed until the nitrite gel detection layer is sealed and sealed until the whole storage period is kept in a light-shielding state.

The invention has the beneficial effects that:

1) the nitrite gel detection layer provided by the invention embeds and fixes the nitrite color developing agent in the alumina gel with a three-dimensional space network structure by utilizing a sol-gel technology, and the alumina gel also provides a micro-water environment, and the micro-water network structure in the micro-water environment avoids the dissolving step of conventional reagent pack detection in the nitrite detection process, thereby being beneficial to the rapid reaction of nitrite ions and the color developing agent and realizing the rapid realization of nitrite detection.

2) The invention effectively protects the nitrite gel detection layer under the sealed and lightproof storage conditions, avoids the slow decomposition and invalidation of the N- (1-naphthyl) -ethylenediamine dihydrochloride in the color developing agent under the action of light, and prolongs the validity period of the reagent.

3) The reagent of the mixed liquid of the alumina sol and the nitrite color developing agent solution has very small dosage, and the dosage of the reagent in a single detection plate is only microgram level, thereby realizing the purpose of green and environment-friendly detection process.

4) The whole preparation process of the nitrite gel detection layer is controllable, and the standardized implementation of the preparation of the nitrite gel detection layer is facilitated.

Drawings

Fig. 1 is a schematic view of a detection plate of the present invention.

Fig. 2 is a schematic diagram of the separation of the plate body and the cover body of the detection plate of the present invention.

Reference numerals: 1-plate body, 2-cover body, 11-detection hole and 12-nitrite gel detection layer.

Detailed Description

The technical solution in the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present invention. It is to be understood that the described embodiments are merely exemplary of the invention, and not restrictive of the full scope of the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.

As shown in fig. 1 and 2, the nitrite detection plate comprises a plate body 1 and a cover body 2; the detection hole 11 sealed by the cover body 2 is arranged on the plate body 1, and a nitrite gel detection layer 12 is arranged in the detection hole 11.

The nitrite gel detection layer 12 is formed by gelling a mixed solution of alumina sol and nitrite developer solution in the detection hole 11.

The preparation process of the alumina sol is as follows: preparing an aluminum isopropoxide solution with the concentration of 0.02-0.05 g/mL, heating and stirring, adding hydrochloric acid to enable the concentration of the hydrochloric acid in the mixed solution to be 0.02-0.04 mol/L, continuously heating the mixed solution, cooling, transferring and bottling to finally obtain the alumina sol.

Heating the aluminum isopropoxide solution to 70-80 ℃, and stirring for 30-60 minutes; and heating the alumina mixed solution to 85-95 ℃, opening the opening for 1-2 hours, refluxing for 12-18 hours, cooling to room temperature, transferring and bottling.

The preparation process of the nitrite color developing agent solution is as follows: preparing a phosphoric acid solution with the volume percentage concentration of 5-20%, sequentially adding p-aminobenzenesulfonamide and N-1-naphthyl-ethylenediamine dihydrochloride, dissolving the p-aminobenzenesulfonamide and the N-1-naphthyl-ethylenediamine dihydrochloride in the phosphoric acid solution to ensure that the concentration of the p-aminobenzenesulfonamide in the nitrite color developing agent solution is 2-6 g/mL and the concentration of the N-1-naphthyl-ethylenediamine dihydrochloride in the nitrite color developing agent solution is 0.1-0.3 g/mL, placing the finally prepared nitrite color developing agent solution in a brown bottle, and refrigerating for storage.

The volume ratio of the alumina sol to the nitrite color developing agent solution in the nitrite gel detection layer 12 is 1: 3-3: 1, 5-100 microliters of the mixed solution of the alumina sol and the nitrite color developing agent solution is dripped into the detection hole 11, and the mixed solution is gelatinized under the condition of refrigeration and light shielding to realize the fixation of the nitrite gel detection layer 12.

A plurality of detection holes 11 are provided; the nitrite gel detection layer 12 is sealed after being prepared, and the whole storage period is kept in a light-shielding state.

When the detection plate is used, prepared nitrite series standard solutions with different concentrations are respectively dripped into each detection hole 11, and the color development is stable after one minute.

In the same way, the water sample to be detected with the same volume is dripped into other detection holes 11 of the detection plate, and the nitrite concentration of the water sample to be detected can be obtained by comparing the result after the color development with the standard solution.

At the moment, semi-quantitative determination can be carried out through visual inspection, relatively accurate quantitative analysis can be carried out through photographing and gray software analysis, and accurate quantitative analysis can also be carried out through a multi-channel micropore detector.

In conclusion, the invention provides the nitrite detection plate which is simple in structure, can be manufactured in batch, is low in reagent consumption, and realizes rapid green and environment-friendly detection of nitrite.

Claims

1. A nitrite detection plate, comprising: comprises a plate body (1) and a cover body (2); a detection hole (11) sealed through the cover body (2) is formed in the plate body (1), and a nitrite gel detection layer (12) is arranged in the detection hole (11);

the nitrite gel detection layer (12) is formed by gelling a mixed solution of alumina sol and nitrite color developing agent solution in the detection hole (11);

the preparation process of the alumina sol is as follows: preparing an aluminum isopropoxide solution with the concentration of 0.02-0.05 g/mL, heating and stirring, adding hydrochloric acid to enable the concentration of the hydrochloric acid in the mixed solution to be 0.02-0.04 mol/L, continuously heating the mixed solution, cooling, transferring and bottling to finally obtain an aluminum oxide sol;

the volume ratio of the alumina sol to the nitrite color developing agent solution in the nitrite gel detection layer (12) is 1: 3-3: 1, 5-100 microliters of mixed liquid of the alumina sol and the nitrite color developing agent solution is dripped into the detection hole (11), and the mixed liquid is gelatinized under the condition of refrigeration and light shielding to realize the fixation of the nitrite gel detection layer (12).

2. The nitrite detection panel of claim 1, wherein: heating the aluminum isopropoxide solution to 70-80 ℃, and stirring for 30-60 minutes; and heating the mixed solution to 85-95 ℃, opening the opening for 1-2 hours, refluxing for 12-18 hours, cooling to room temperature, transferring and bottling.

3. The nitrite detection plate according to claim 1, wherein the nitrite developer solution is prepared by the following steps: preparing a phosphoric acid solution with the volume percentage concentration of 5-20%, sequentially adding p-aminobenzenesulfonamide and N- (1-naphthyl) -ethylenediamine dihydrochloride into the phosphoric acid solution, dissolving the p-aminobenzenesulfonamide and the N- (1-naphthyl) -ethylenediamine dihydrochloride into the phosphoric acid solution to ensure that the concentration of the p-aminobenzenesulfonamide in the nitrite color developing agent solution is 2-6 g/mL and the concentration of the N- (1-naphthyl) -ethylenediamine dihydrochloride in the nitrite color developing agent solution is 0.1-0.3 g/mL, placing the finally prepared nitrite color developing agent solution into a brown bottle, and refrigerating and storing the bottle.

4. The nitrite detection panel of claim 1, wherein: the number of the detection holes (11) is multiple; the nitrite gel detection layer (12) is sealed after being prepared, and the whole storage period is kept in a light-proof state.