Detection tube and detection method for detecting phenol in liquid

Abstract

The invention belongs to the field of phenol detection, and particularly relates to a detection tube and a detection method for detecting phenol in liquid. The detection tube for detecting phenol in liquid comprises a tube body, a hollow glass tube is arranged in the middle of the tube body, the two ends of the tube body are closed-up sealed ends, and three glass columns and a plastic column are sequentially arranged on the portion, close to one sealed end, in the hollow glass tube; a baffle layer sheet is arranged between every two of the three glass columns; a reagent a and a reagent b are respectively filled in the two layers of barrier sheets. The detection tube provided by the invention is simple in structure and easy to operate; the detection tube provided by the invention has the advantages that the color development reaction is fast, the color development can be completed within one minute, the determination condition is loose, the sensitivity is high, the influence of other toxicants in the liquid is avoided, the influence of the temperature is very small, and the phenol concentration in the sensitivity range can be detected as long as the liquid to be detected is not frozen; the detection tube provided by the invention is good in stability.

Description

Technical Field

[0001] The invention belongs to the field of phenol detection, and in particular relates to a detection tube and a detection method for detecting phenol in liquid. Background Art

[0002] Phenol (chemical formula: C6H5OH), also known as carbolic acid, is a colorless needle-shaped crystal with a special smell. It is toxic and is mainly used in the production of phenolic resin, caprolactam, bisphenol A, adipic acid, aniline, alkylphenol, salicylic acid, etc. In addition, it can also be used as a solvent, reagent and disinfectant, etc. It has a wide range of applications in synthetic fibers, synthetic rubber, plastics, medicines, pesticides, spices, dyes and coatings. The freezing point of phenol is 40.6°C, and it is a colorless needle-shaped crystal at room temperature. It is slightly soluble in water and can be liquefied when mixed with about 8% water. It is miscible with water above 65°C, easily soluble in organic solvents, and miscible in ether, chloroform, glycerol, carbon disulfide, vaseline, volatile oils, and strong alkali aqueous solutions.

[0003] Phenol is extremely corrosive. It denatures local proteins after contact and has a strong corrosive effect on the skin and mucous membranes. It is highly toxic and can inhibit the central nervous system or damage liver and kidney function. Inhalation of high concentrations of phenol gas can cause dizziness, headache, fatigue, blurred vision, pulmonary edema, and ingestion into the digestive tract can cause burns and gastrointestinal perforation. In severe cases, it can cause renal failure and respiratory failure. Phenol is an endocrine disruptor that promotes the activation and proliferation of cancer cells. It can show significant interference effects on animal estrogen, thyroid hormone, catecholamines, etc., and can cause reproductive disorders, developmental abnormalities, cancer and complex ecological effects in humans. Phenol in the air enters the human body through breathing and skin, denaturing proteins, precipitating, damaging and inhibiting mucous membranes, cardiovascular and central nervous systems.

[0004] Phenol waste gas entering the water body will affect the physiological functions of aquatic organisms and crops. Phenol is difficult to volatilize and can exist in the soil and water environment for a long time, causing serious pollution to the environment. When the content of phenols in water reaches 0.1002 mg / L, phenol odor will be produced during the chlorination process of the water body, affecting the water quality of drinking water sources; when the concentration is greater than 0.1005 mg / L, it cannot be used as drinking water; when the concentration is greater than 0.11 mg / L, the fish in the water will have a bad smell and cannot be eaten; when the concentration is greater than 1 mg / L, it will have a serious impact on the reproduction of fish and other activities; and when the phenol content in the water is greater than 10 mg / L, aquatic organisms such as fish cannot survive. In addition, the toxicity of phenol can greatly inhibit the growth rate of microorganisms (such as algae, bacteria, mollusks, etc.) in the water, affecting the ecological balance of the water. Direct irrigation of farmland with wastewater containing more than 100 mg / L of phenol will cause crop death and reduced production.

[0005] At present, there are many methods for detecting phenol, such as bromine titration, spectrophotometry, and high-performance liquid chromatography. However, the detection error of bromine titration is large and the sensitivity is insufficient; spectrophotometry is only applicable to the determination of phenol content in water, the detection object is single, the test process is complicated and cumbersome, and the result error is large. High-performance liquid chromatography, such as CN108872440A, discloses a method for measuring the phenol content in water. In this method, high-performance liquid chromatography needs to be used in conjunction with a fluorescence detector, and toxic reagents such as acetonitrile and methanol are required. The detection cost is expensive, the detection process is cumbersome, and professional personnel are required to operate.

[0006] In view of this, the present invention is proposed. Summary of the invention

[0007] The purpose of the present invention is to provide a detection tube and a detection method for detecting phenol in liquid. The detection tube provided by the present invention has a simple structure and is easy to operate; the detection tube provided by the present invention has a fast color development reaction, and the color development can be completed in less than one minute. The measurement conditions are loose, the sensitivity is high, and it is not affected by other poisons in the liquid. The influence of temperature is very small. As long as the liquid to be detected is not frozen, the phenol concentration within the sensitivity range can be detected; the detection tube provided by the present invention has good stability.

[0008] To achieve the above object, the present invention adopts the following technical solution:

[0009] A detection tube for detecting phenol in liquid comprises a tube body 11, the middle part of the tube body 11 is a hollow glass tube, and both ends are sealed ends 12, wherein:

[0010] The inner part of the hollow glass tube near the sealed end 12 is provided with three glass columns 13 and one plastic column 14 in sequence;

[0011] A barrier sheet 15 is provided between each of the three glass columns 13;

[0012] The two barrier sheets 15 are filled with reagent a and reagent b respectively.

[0013] Further,

[0014] Reagent a is a mixture of potassium ferrocyanide and sodium carbonate in a mass ratio of 1:10;

[0015] Reagent b is 4-aminoantipyrine.

[0016] The reaction principle of the detection tube of the present invention is as follows:

[0017] Based on the condensation of 4-aminoantipyrine and phenol in the presence of alkaline oxides, red color is displayed. The reaction process is as follows:

[0018]

[0019] In the present invention, reagent a and reagent b are filled in two layers of barrier sheets in layers, thereby preventing the reagents from reacting with each other and preventing the problem of reagent failure and decreased sensitivity of color development reaction due to long storage time of the detection tube.

[0020] Furthermore, the outer diameter of the glass column 13 and the outer diameter of the plastic column 14 are the same as the inner diameter of the hollow glass tube.

[0021] Furthermore, a detection object mark is marked on the portion of the hollow glass tube corresponding to the other sealed end 12 .

[0022] Furthermore, the barrier sheet 15 is glass wool.

[0023] Furthermore, the detection tube is made by packaging reagent a and reagent b in layers and sealing them by fusion.

[0024] The present invention also provides a method for preparing the detection tube, which comprises the following steps:

[0025] S1. Prepare reagents

[0026] S11, mixing potassium ferrocyanide and sodium carbonate in a mass ratio of 1:10 and grinding them to obtain reagent a;

[0027] S12, grinding 4-aminoantipyrine as reagent b;

[0028] S2. Preparation of test tubes

[0029] S21, sealing one end of the tube body 11 by melting to form a sealed end 12;

[0030] S22, loading into glass column 13;

[0031] S23, inserting the barrier sheet 15, which is filled with reagent a;

[0032] S24, loading the glass column 13;

[0033] S25, inserting the barrier sheet 15, which is filled with reagent b;

[0034] S26, inserting plastic column 14;

[0035] S27, sealing the other end of the tube body to form a sealed end 12, and marking a detection object mark on the portion of the hollow glass tube corresponding to the sealed end.

[0036] In the above preparation method, the filling amount of reagent a is 30 mg, and the filling amount of reagent b is 10 mg.

[0037] The present invention also provides a method for detecting phenol in liquid, wherein the method comprises using the detection tube of the present invention for detection.

[0038] Specifically, the method comprises the following steps:

[0039] Step 1, breaking off the sealed ends 12 at both ends of the detection tube;

[0040] Step 2: Install the rubber suction tip on the marked end;

[0041] Step 3: Use a rubber suction tip to suck the liquid to be tested from the other end of the test tube;

[0042] Step 4: After the liquid to be tested is sucked to 1 cm from the upper edge of the plastic column 14, let it stand, observe the color change, and judge the test result.

[0043] Compared with the prior art, the present invention has the following advantages:

[0044] (1) The detection tube provided by the present invention has a simple structure and is easy to operate;

[0045] (2) The detection tube provided by the present invention has a fast color development reaction, which can be completed in less than one minute. The detection conditions are flexible, the sensitivity is high, and it is not affected by other poisons in the liquid. It is slightly affected by temperature. As long as the liquid to be tested is not frozen, phenol concentrations within the sensitivity range can be detected;

[0046] (3) The detection tube provided by the present invention has good stability. BRIEF DESCRIPTION OF THE DRAWINGS

[0047] Figure 1 It is a schematic diagram of the structure of the detection tube of the present invention. DETAILED DESCRIPTION

[0048] The following are specific embodiments of the present invention, and the embodiments are intended to further describe the present invention rather than to limit the present invention.

[0049] Example 1

[0050] This embodiment provides a detection tube for detecting phenol in a liquid, such as Figure 1 As shown, the detection tube comprises a tube body 11, the middle part of the tube body 11 is a hollow glass tube, and both ends are sealed ends 12, wherein:

[0051] The inner part of the hollow glass tube near the sealed end 12 is provided with three glass columns 13 and one plastic column 14 in sequence;

[0052] A barrier sheet 15 is provided between each of the three glass columns 13;

[0053] The two barrier sheets 15 are filled with reagent a and reagent b respectively;

[0054] Reagent a is a mixture of potassium ferrocyanide and sodium carbonate in a mass ratio of 1:10;

[0055] Reagent b is 4-aminoantipyrine.

[0056] The outer diameter of the glass column 13 and the outer diameter of the plastic column 14 are the same as the inner diameter of the hollow glass tube.

[0057] The portion of the hollow glass tube corresponding to the other sealed end 12 is marked with a detection object mark, such as Figure 1 As shown, it can be labeled as phenol-1.

[0058] The blocking layer 15 is glass wool.

[0059] The detection tube is made by layering reagent a and reagent b in tubes and fusing and sealing.

[0060] Example 2

[0061] This embodiment provides a method for preparing the detection tube, which comprises the following steps:

[0062] S1. Prepare reagents

[0063] S11, mixing potassium ferrocyanide and sodium carbonate in a mass ratio of 1:10 and grinding them to obtain reagent a;

[0064] S12, grinding 4-aminoantipyrine as reagent b;

[0065] S2. Preparation of test tubes

[0066] S21, sealing one end of the tube body 11 by melting to form a sealed end 12;

[0067] S22, loading into glass column 13;

[0068] S23, inserting the barrier sheet 15, the barrier sheet 15 is filled with reagent a, and the filling amount of reagent a is 30 mg;

[0069] S24, loading the glass column 13;

[0070] S25, inserting the blocking layer sheet 15, the blocking layer sheet 15 is filled with reagent b, and the filling amount of reagent b is 10 mg;

[0071] S26, inserting plastic column 14;

[0072] S27, sealing the other end of the tube body to form a sealed end 12, and marking the detection object mark on the portion of the hollow glass tube corresponding to the sealed end, for example, the present invention marks it as phenol-1.

[0073] Example 3

[0074] This embodiment describes a method for detecting phenol in a liquid using the detection tube of the present invention.

[0075] Specifically, the method comprises the following steps:

[0076] Step 1, breaking off the sealed ends 12 at both ends of the detection tube;

[0077] Step 2: Install the rubber suction tip on the marked end;

[0078] Step 3: Use a rubber suction tip to suck the liquid to be tested from the other end of the test tube;

[0079] Step 4: After the liquid to be tested is sucked to 1 cm from the upper edge of the plastic column 14, let it stand, observe the color change, and judge the test result.

[0080] Test Example 1: Preparation of solid reagents

[0081] 1. Research on basic formula

[0082] The detection agent is composed of 4-aminoantipyrine, potassium ferrocyanide and anhydrous sodium carbonate. 4-aminoantipyrine is a condensation agent, potassium ferrocyanide is an oxidant, and anhydrous sodium carbonate provides alkalinity.

[0083] 2. Optimization of solid mixed reagent formula

[0084] Weigh 1g of potassium ferrocyanide and 10g of sodium carbonate and grind them into reagent a, and grind 10g of 4-aminoantipyrine into reagent b. A two-level orthogonal experiment was performed to obtain the optimal dosage. The results are shown in Tables 1 and 2.

[0085] Table 1. Factors and levels of orthogonal experiment

[0086] factor Reagent a(mg) Reagent b(mg) Level 1 10 10 Second level 30 30

[0087] Table 2. Results of orthogonal experiment L4(2 3 )

[0088] Serial number Reagent a / mg Reagent b / mg Reaction Color Blank Color evaluate 1 10 10 Light red Light yellow 2 10 30 Light yellow Light yellow 3 30 10 red Light yellow most 4 30 30 Orange Light yellow

[0089] (Note): The concentration of phenol test solution is 1 μg / mL

[0090] The experimental results show that the effect of test number 3 is the best. Therefore, the best reagent ratio is 30 mg of reagent a and 10 mg of reagent b. Test Example 2: Performance test of the test tube

[0091] 1. Sensitivity test of detection tube

[0092] Experimental method: Break off both ends of the phenol-1 detection tube of Example 1, install a rubber pipette tip on the marked end, suck the phenol test solution to 1 cm above the plastic column, and observe the color change. The positive reaction is red, and the blank is light yellow. The experimental results are shown in Table 3, and the sensitivity is determined to be 1 μg / mL.

[0093] Table 3. Sensitivity of phenol-1 detection tube

[0094]

[0095] 2. Interference experiment of detection tube

[0096] The results of experiments on the phenol-1 detection tube with various poisons at a concentration of 20 μg / mL are shown in Table 4. The experiments show that various poisons have no interference with the phenol-1 tube.

[0097] Table 4. Color development of phenol-1 detection tube for various poisons

[0098] Type of substance <![CDATA[NO2 - ]]> <![CDATA[F - ]]> <![CDATA[Hg 2+ ]]> <![CDATA[Pb 2+ ]]> <![CDATA[Cr 6+ ]]> <![CDATA[Ba 2+ ]]> <![CDATA[Cd 2+ ]]> phenol aniline phenol Display Color Light yellow Light yellow Light yellow Light yellow Light yellow Light yellow Light yellow Light yellow Light yellow red

[0099] 3. Effect of test medium on reaction

[0100] The test solution was prepared with water, alcohol and alcohol water as solvents. The effect of the experimental medium on the detection reaction of phenol-1 was 5 μg / mL. The results are shown in Table 5. The experimental results show that water is the best test solution medium.

[0101] Table 5. Effect of medium on phenol-1 detection tube

[0102]

[0103] 4. Effect of temperature on detection reaction

[0104] The effect of temperature on the reaction of the phenol-1 detection tube is shown in Table 6.

[0105] Table 6. Effect of temperature on reaction

[0106]

[0107] Experiments show that as long as the test solution is not frozen, the phenol-1 detection tube can detect phenol within the sensitivity range.

[0108] 5. Test tube stability test

[0109] The experimental method adopts the accelerated storage test method. According to the method described in AD-A057233, the phenol-1 detection tube is placed in a constant temperature water bath at 90°C for two weeks, and then taken out to test its sensitivity to phenol at 1μg / mL. The results show that the sensitivity has not changed, which is equivalent to a storage period of five years.

Claims

1. A detection tube for detecting phenol in a liquid, comprising a tube body (11), the middle part of the tube body (11) is a hollow glass tube, and both ends are sealed ends (12) with closed ends, characterized in that: Three glass columns (13) and one plastic column (14) are sequentially arranged in a portion of the hollow glass tube near a sealed end (12); A blocking sheet (15) is provided between each of the three glass columns (13); The two barrier sheets (15) are filled with reagent a and reagent b respectively.

2. The detection tube according to claim 1, characterized in that: Reagent a is a mixture of potassium ferrocyanide and sodium carbonate in a mass ratio of 1:10; Reagent b is 4-aminoantipyrine.

3. The detection tube according to claim 2, characterized in that: The outer diameter of the glass column (13) and the outer diameter of the plastic column (14) are both the same as the inner diameter of the hollow glass tube.

4. The detection tube according to any one of claims 1 to 3, characterized in that: A detection object mark is marked on the portion of the hollow glass tube corresponding to the other sealed end (12).

5. The detection tube according to any one of claims 1 to 3, characterized in that: The blocking layer (15) is glass wool.

6. The method for preparing a detection tube according to claim 4, characterized in that: The detection tube is made by layering reagent a and reagent b into tubes and fusing and sealing.

7. A method for preparing a detection tube according to any one of claims 1 to 6, characterized in that: The preparation method comprises the following steps: S1. Prepare reagents S11, mixing potassium ferrocyanide and sodium carbonate in a mass ratio of 1:10 and grinding them to obtain reagent a; S12, grinding 4-aminoantipyrine as reagent b; S2. Preparation of test tubes S21, sealing one end of the tube body (11) by melting to form a sealed end (12); S22, loading into glass column (13); S23, inserting the barrier sheet (15), the barrier sheet (15) being filled with reagent a; S24, loading into glass column (13); S25, inserting the barrier sheet (15), the barrier sheet (15) being filled with reagent b; S26, inserting into plastic column (14); S27, sealing the other end of the tube body by melting to form a sealed end (12), and marking a detection object mark on the portion of the hollow glass tube corresponding to the sealed end.

8. The preparation method according to claim 7, characterized in that: The filling amount of reagent a was 30 mg, and the filling amount of reagent b was 10 mg.

9. A method for detecting phenol in a liquid, characterized in that: The method described is to use the detection tube described in any one of claims 1-6 for detection.

10. The method according to claim 9, characterized in that The method comprises the following steps: Step 1, breaking off the sealed ends (12) at both ends of the detection tube; Step 2: Install the rubber suction tip on the marked end; Step 3: Use a rubber suction tip to suck the liquid to be tested from the other end of the test tube; Step 4: After the liquid to be tested is sucked to 1 cm above the upper edge of the plastic column (14), it is allowed to stand, and the color change is observed to determine the test result.

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