CN101661002B - Preparation method and use method of reagent for determining total phenol in water - Google Patents
Preparation method and use method of reagent for determining total phenol in water Download PDFInfo
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- CN101661002B CN101661002B CN2009103077540A CN200910307754A CN101661002B CN 101661002 B CN101661002 B CN 101661002B CN 2009103077540 A CN2009103077540 A CN 2009103077540A CN 200910307754 A CN200910307754 A CN 200910307754A CN 101661002 B CN101661002 B CN 101661002B
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Abstract
The invention provides a reagent for determining total phenols in water, a preparation and usage thereof and solves disadvantages of an existing method for determining the total phenols in water. The reagent for determining phenols in water is composed of sodium tungstate, sodium molybdate, concentrated phosphoric acid, concentrated hydrochloric acid, lithium sulfate and water. Detection of contentof the total phenols in water by the reagent has advantages of low detection limit, high detection speed, fewer limits on determination condition, wide-range and stable color development, high precision and accuracy, simple and easy operation and the like.
Description
Technical field
The present invention is specifically related to a kind of preparation method and using method of reagent for determining total phenol in water.
Background technology
Phenols is a protoplasm poison, belongs to highly toxic substance.Phenol content is atomic in the natural water, but because it is the important basic organic synthesis material of a class, a large amount of in recent years is applied in the industry manufacturing.Industrial, phenolic compound is used to make phenolics, macromolecular material, ion exchange resin, synthon, fuel, medicine, explosive etc. in a large number, all contain a large amount of aldehydes matters in the industrial waste water of dischargings such as associated all kinds of industries such as coal gas, coking, oil, chemical industry, preparation pharmacy, paint, caused serious pollution to environment.
Aldehydes matter all can produce murder by poisoning to biological living, and the water that people's long-term drinking is polluted by phenol can cause dizziness, anaemia and various the nervous system disease.When aldehydes matter content in the water reached 6.5mg/L～9.3mg/L, fish will mass mortality.Water irrigated farmland with containing phenol 50mg/L～100mg/L can make crop production reduction even withered.Therefore it is significant to ensureing health and crop production fast, accurately to detect phenolic wastewater.The assay method of the relevant aldehydes matter of having reported at present has a variety of, as ferrous tartrate method, permanganimetric method, atomic absorption method, ultraviolet spectrophotometry, liquid phase chromatography etc.But all there is certain shortcoming in actual applications in the whole bag of tricks, can't accurately determine its titration end-point as permanganimetric method; Ferrous tartrate colourimetry complex operation, poor repeatability; Atomic absorption method and high performance liquid chromatography cost of equipment are big, complex operation.Therefore developing a kind of method accurate and easy, that measure water body aldehydes matter total amount apace has great importance.
Summary of the invention
Purpose of the present invention is in order to solve the deficiency of above-mentioned existing total phenol in water content assaying method, and a kind of reagent and method thereof of accurate and easy, fast measuring total phenol in water content is provided.
Reagent for determining total phenol in water of the present invention is an aqua, and raw material comprises: sodium tungstate, sodium molybdate, strong phosphoric acid, concentrated hydrochloric acid, lithium sulfate and distilled water; The concentration of described each raw material is: sodium tungstate 0.300～0.400mol/L, sodium molybdate 0.150～0.250mol/L, strong phosphoric acid 0.500～0.600mol/L, concentrated hydrochloric acid 1.000～2.000mol/L, lithium sulfate 0.300～0.400mol/L.
The preparation method of reagent for determining total phenol in water of the present invention: according to the raw material matched proportion density, calculate the consumption of the volume required various raw materials that will add: in container, add sodium tungstate, sodium molybdate, a part of distilled water, strong phosphoric acid and concentrated hydrochloric acid, abundant mixing, boiling water bath added lithium sulfate after refluxing 11 hours again, a small amount of distilled water, uncovered boiling 20 minutes, the cooling back is settled to volume required with distilled water; Liquid filtering obtains described reagent for determining total phenol in water behind the constant volume, is positioned over to preserve in the brown reagent bottle to use.
The using method of reagent for determining total phenol in water of the present invention: adding 3.25mL liquid to be measured, the described reagent for determining total phenol in water of 0.5mL, 1.25mL concentration are the aqueous sodium carbonate of 2.0mol/L in the 10mL centrifuge tube, after mixing, after the room temperature lucifuge is placed 40min, measure absorbance down in the 770nm wavelength, try to achieve the content of total phenol in water again according to typical curve.
Reagent for determining total phenol in water of the present invention has the following advantages:
(1) the present invention adopts five yuan of secondary rotational regression composite design schemes, determine the best proportioning of each material in the reagent for determining total phenol in water, simultaneously on this basis this research continuation to return time, reflux temperature, the boiling time of this reagent, and this reagent colorimetric condition (colour temp, developing time and Na
2CO
3Content) be optimized, finally obtain the reagent compound method and the using method of a complete and accurate.
(2) this reagent for determining total phenol in water can be measured total phenol in water content and stability, reappearance and precision are all higher accurately, and this reagent at room temperature just can use simultaneously, and is convenient and swift.
(3) existing determining total phenol in water method relative merits
| Assay method | Relative merits |
| Atomic absorption method | Cost of equipment is big, complex operation |
| The ferrous tartrate method | Complex operation, poor repeatability |
| Permanganimetric method | Titration end-point is difficult observes, and it is lower to measure sensitivity |
| The amino peace of 4-is for the woods method | Only be suitable for measuring volatile phenol |
| The Folin-denis method | Folin-denis developer poor stability |
| The Folin-Ciocalteu method | Price is low, and is easy to operate and simple and easy to do, but the developer collocation method is indeterminate and the chromogenic reaction system has to be optimized. |
| Vanillic aldehyde method and potassium ferricyanide spectrophotometric method | Strict to condition determination, less stable, disturbing factor is more, is prone to precipitation |
| Ply of paper is analysed and thin-layer chromatography | There are defective in separating effect, speed and accurately quantitative aspect |
| High performance liquid chromatography | Can accurately measure single aldehydes matter, but pre-treatment is loaded down with trivial details, must adds the standard sample, relatively more expensive, be unsuitable for a large amount of quantitative test, can not be used to measure total phenol |
| Gas chromatography | Be used for the separation of plant class material, finding speed is fast, highly sensitive, but this method needs derivatization treatment, and pre-treatment is cumbersome |
From above-mentioned comparative descriptions, there are numerous defectives in the determining total phenol method of existing pertinent literature report, determining total phenol in water method of the present invention is the improvement to the Folin-Ciocalteu method, it is low to have detectability, detection speed is fast, condition determination restriction is few, and color range is wide and stable, and has good precision and accuracy, advantage such as simple and easy to do.
Description of drawings
Fig. 1 is the abosrption spectrogram after the P-hydroxybenzoic acid chromogenic reaction in the inventive method checking one.
Fig. 2 is the canonical plotting of P-hydroxybenzoic acid in the inventive method checking one.
Fig. 3 is the abosrption spectrogram after the phenol chromogenic reaction in the inventive method checking two.
Fig. 4 is the canonical plotting of phenol in the inventive method checking two.
Fig. 5 is the abosrption spectrogram after the P-hydroxybenzoic acid chromogenic reaction in the inventive method checking three.
Fig. 6 is the canonical plotting that mixes phenolic acid in the inventive method checking three.
Fig. 7 is the abosrption spectrogram after mixed phenol and the phenolic acid chromogenic reaction in the inventive method checking four.
Fig. 8 is the canonical plotting of mixed phenol and phenolic acid in the inventive method checking four.
Fig. 9 is the abosrption spectrogram after the actual sample chromogenic reaction in the application example of the present invention.
Embodiment
It is pure that medicine used in the present invention is analysis.
The concentration of each raw material is:
Raw material final concentration mol/L
Sodium tungstate 0.300～0.400
Sodium molybdate 0.150～0.250
Strong phosphoric acid 0.500～0.600
Concentrated hydrochloric acid 1.000～2.000
Lithium sulfate 0.300～0.400
Solvent is a distilled water.
Optimum feed stock concentration is:
Raw material final concentration mol/L
Sodium tungstate 0.364
Sodium molybdate 0.207
Strong phosphoric acid 0.588
Concentrated hydrochloric acid 1.440
Lithium sulfate 0.313
Solvent is a distilled water.
Can also add bromine water in the reagent for determining total phenol in water, measure effect to strengthen; The consumption of described bromine water is to add 4mL bromine water in every 1L reagent for determining total phenol in water.The concentration of bromine water is: bromine content 3% (weight concentration) in the bromine aqueous solution.
The weight concentration of described strong phosphoric acid is 85%; The weight concentration of described concentrated hydrochloric acid is 36%～38%.
The preparation method is as follows, according to the raw material matched proportion density, calculate the consumption of the volume required various raw materials that will add: in container, add sodium tungstate, sodium molybdate, part distilled water, strong phosphoric acid and concentrated hydrochloric acid, abundant mixing is after boiling water bath refluxed 11 hours, add lithium sulfate again, a small amount of distilled water, uncovered boiling 20 minutes, the cooling back is settled to volume required with distilled water; Liquid filtering obtains described reagent for determining total phenol in water behind the constant volume, is positioned over to preserve in the brown reagent bottle to use.
More than in the preparation, after boiling water bath refluxed 11 hours, can add bromine water when adding lithium sulfate and a small amount of distilled water.
The using method of the reagent for determining total phenol in water for preparing: adding 3.25mL liquid to be measured, the described reagent for determining total phenol in water of 0.5mL, 1.25mL concentration are the aqueous sodium carbonate of 2.0mol/L in the 10mL centrifuge tube, after mixing, after the room temperature lucifuge is placed 40min, measure absorbance down in the 770nm wavelength, try to achieve the content of total phenol in water again according to typical curve.
Most preferred embodiment
Add 120g sodium tungstate, 50g sodium molybdate, 700mL distilled water in the cucurbit of 1L, the 40mL strong phosphoric acid, 120mL concentrated hydrochloric acid, fully mixing, boiling water bath added the 60g lithium sulfate, 50mL distilled water after refluxing 11 hours again, 4mL bromine water, electric jacket split shed boiling 20 minutes is settled to 1L, liquid filtering behind the constant volume after the cooling, and place brown reagent bottle, can use.
For fully disclosing a kind of reagent for determining total phenol in water of the present invention and preparation method thereof, be illustrated below in conjunction with method validation and embodiment.
P-hydroxybenzoic acid Determination on content result and accuracy in method validation one, the water body
Preparation reagent for determining total phenol in water by " summary of the invention ".
Get the P-hydroxybenzoic acid standard solution 0.5mL of 50mg/L, add the aqueous sodium carbonate of 2.75mL distilled water, 0.5mL reagent for determining total phenol in water, 1.25mL concentration 2.0mol/L, after mixing, the room temperature lucifuge is placed 40min.Testing sample adopts ultraviolet-visible spectrophotometer to carry out length scanning (Fig. 1) in 500-1000nm, and obtaining the maximum absorption wavelength of P-hydroxybenzoic acid standard items after chromogenic reaction is 770nm.
In one group of 9 10mL centrifuge tube, add 0.00 respectively, 0.04,0.05,0.06,0.07,0.08,0.10,0.20,0.30,0.40mL P-hydroxybenzoic acid standard mother liquor (50mg/L), add distilled water 3.25 respectively, 3.21,3.20,3.19,3.18,3.17,3.15,3.05,2.95,2.85mL distilled water, 0.5mL reagent for determining total phenol in water, 1.25mL the aqueous sodium carbonate of concentration 2.0mol/L, after mixing, after the room temperature lucifuge is placed 40min, measure absorbance down in the 770nm wavelength, deducting the absorbance of zero pipe by the light absorption value that records except that other calibration series of zero pipe, is that ordinate and concentration (mg/L) are carried out linear regression analysis for horizontal ordinate with the absorbance.Adopt this colorimetric method for determining P-hydroxybenzoic acid to become good linear relationship between the absorbance under the 770nm as shown in Figure 2 in the concentration range of 0.4 ~ 4mg/L, linear equation is y=0.1288x+0.0092, R
2=0.9997, illustrate in the concentration range internal linear relation of being measured good.
The accuracy of this method is tested with average recovery.The sample liquid (paddy rice nutrient solution) that in one group of 4 10mL centrifuge tube, adds 2mL, and add 0.00 respectively, 0.10,0.30,0.50mL P-hydroxybenzoic acid mother liquor (50mg/L), add 1.25,1.15,0.95 respectively, the distilled water developer of 0.75mL, 0.5mL reagent for determining total phenol in water, 1.25mL the aqueous sodium carbonate of concentration 2.0mol/L, after mixing, after the room temperature lucifuge is placed 40min, measure absorbance down in the 770nm wavelength, each sample repeats for 3 times, and the result shows (table 1): adopt this method can accurately measure P-hydroxybenzoic acid in the water body.
Table 1 reagent for determining total phenol in water is to P-hydroxybenzoic acid measurement result in the water body
Remarks: minimum detection limit and determination limit have approached the index of correlation data of liquid chromatography.Average recovery meets the requirement of US EPA (U.S. environmental protection general administration) standard between 70% ~ 120%.
The measurement result of phenol content and accuracy in method validation two, the water body
Get the phenol standard solution 0.5mL of 50mg/L, add the aqueous sodium carbonate of 2.75mL distilled water, 0.5mL reagent for determining total phenol in water, 1.25mL concentration 2.0mol/L, after mixing, the room temperature lucifuge is placed 40min.Testing sample adopts ultraviolet-visible spectrophotometer to carry out length scanning (Fig. 3) in 500-1000nm, and obtaining the maximum absorption wavelength of phenol standard items after chromogenic reaction is 770nm.
In one group of 9 10mL centrifuge tube, add 0.00 respectively, 0.04,0.05,0.06,0.07,0.08,0.10,0.20,0.30,0.40mL phenol standard mother liquor (50mg/L), add distilled water 3.25 respectively, 3.21,3.20,3.19,3.18,3.17,3.15,3.05,2.95,2.85mL distilled water, 0.5mL reagent for determining total phenol in water, 1.25mL the aqueous sodium carbonate of concentration 2.0mol/L, after mixing, after the room temperature lucifuge is placed 40min, measure absorbance down in the 770nm wavelength, deducting the absorbance of zero pipe by the light absorption value that records except that other calibration series of zero pipe, is that ordinate and concentration (mg/L) are carried out linear regression analysis for horizontal ordinate with the absorbance.Adopt this colorimetric method for determining phenol to become good linear relationship between the absorbance under the 770nm as shown in Figure 4 in the concentration range of 0.4-4mg/L, linear equation is y=0.1618x+0.0127, R
2=0.9998, illustrate in the concentration range internal linear relation of being measured good.
The accuracy of this method is tested with average recovery.The sample liquid (paddy rice nutrient solution) that in one group of 4 10mL centrifuge tube, adds 2mL, and add 0.00 respectively, 0.10,0.30,0.50mL phenol mother liquor (50mg/L), add 1.25,1.15,0.95 respectively, the distilled water developer of 0.75mL, 0.5mL reagent for determining total phenol in water, 1.25mL the aqueous sodium carbonate of concentration 2.0mol/L, after mixing, after the room temperature lucifuge is placed 40min, measure absorbance down in the 770nm wavelength, each sample repeats for 3 times, and the result shows (table 2): adopt this method can accurately measure phenol in the water body.
Table 2 reagent for determining total phenol in water is to phenol measurement result in the water body
Remarks: minimum detection limit and determination limit have approached the index of correlation data of liquid chromatography.Average recovery meets the requirement of US EPA (U.S. environmental protection general administration) standard between 70% ~ 120%.
The measurement result of mixed phenol acid content and accuracy in method validation three, the water body
Get the standard mother liquor (forulic acid that consists of that wherein mixes phenolic acid: P-hydroxybenzoic acid: salicylic acid: vanillic acid=1: 1: 1: 1) 0.5mL of the mixing phenolic acid of 50mg/L, the aqueous sodium carbonate that adds 2.75mL distilled water, 0.5mL reagent for determining total phenol in water, 1.25mL concentration 2.0mol/L, after mixing, the room temperature lucifuge is placed 40min.Testing sample adopts ultraviolet-visible spectrophotometer to carry out length scanning (Fig. 5) in 500-1000nm, and the maximum absorption wavelength of standard items after chromogenic reaction that obtains mixing phenolic acid is 770nm.
In one group of 9 10mL centrifuge tube, add 0.00 respectively, 0.04,0.05,0.06,0.07,0.08,0.10,0.20,0.30,0.40mL the standard mother liquor (50mg/L) of above-mentioned mixing phenolic acid, add distilled water 3.25 respectively, 3.21,3.20,3.19,3.18,3.17,3.15,3.05,2.95,2.85mL distilled water, 0.5mL reagent for determining total phenol in water, 1.25mL the aqueous sodium carbonate of concentration 2.0mol/L, after mixing, after the room temperature lucifuge is placed 40min, measure absorbance down in the 770nm wavelength, deducting the absorbance of zero pipe by the light absorption value that records except that other calibration series of zero pipe, is that ordinate and concentration (mg/L) are carried out linear regression analysis for horizontal ordinate with the absorbance.Adopt each phenolic acid of this colorimetric method for determining to become good linear relationship between the absorbance under the 770nm as shown in Figure 6 in the concentration range of 0.4-4mg/L, linear equation is y=0.1162x+0.0062, R
2=0.9991, illustrate in the concentration range internal linear relation of being measured good.
The accuracy of this method is tested with average recovery.The sample liquid (paddy rice nutrient solution) that in one group of 4 10mL centrifuge tube, adds 2mL, and add 0.00 respectively, 0.10,0.30,0.50mL above-mentioned mixed phenol acid mother liquor (50mg/L), add 1.25,1.15,0.95 respectively, the distilled water developer of 0.75mL, 0.5mL reagent for determining total phenol in water, 1.25mL the aqueous sodium carbonate of concentration 2.0mol/L, after mixing, after the room temperature lucifuge is placed 40min, measure absorbance down in the 770nm wavelength, each sample 3 times repeats, and the result shows (table 3): adopt this method can accurately measure phenolic acid in the water body.
Table 3 reagent for determining total phenol in water is to mixing the phenolic acid recovery of standard addition in the water body
Remarks: average recovery meets the requirement of US EPA (U.S. environmental protection general administration) standard between 70%-120%.
The measurement result of mixed phenol and phenolic content and accuracy in method validation four, the water body
Get the mixed phenol of 50mg/L and phenolic acid standard solution (wherein mix phenolic acid and phenolic acid consist of consist of phenol: catechol: resorcinol: forulic acid: P-hydroxybenzoic acid: salicylic acid: vanillic acid=1: 1: 1: 1: 1: 1: 1) 0.5mL, the aqueous sodium carbonate that adds 2.75mL distilled water, 0.5mL reagent for determining total phenol in water, 1.25mL concentration 2.0mol/L, after mixing, the room temperature lucifuge is placed 40min.Testing sample adopts ultraviolet-visible spectrophotometer to carry out length scanning (Fig. 7) in 500-1000nm, obtains mixed phenol and the maximum absorption wavelength of phenolic acid standard solution standard items after chromogenic reaction is 770nm.
In one group of 9 10mL centrifuge tube, add 0.00 respectively, 0.04,0.05,0.06,0.07,0.08,0.10,0.20,0.30,0.40mL above-mentioned mixed phenol and phenolic acid standard solution standard mother liquor (50mg/L), add distilled water 3.25 respectively, 3.21,3.20,3.19,3.18,3.17,3.15,3.05,2.95,2.85mL distilled water, 0.5mL reagent for determining total phenol in water, 1.25mL the aqueous sodium carbonate of concentration 2.0mol/L, after mixing, after the room temperature lucifuge is placed 40min, measure absorbance down in the 770nm wavelength, deducting the absorbance of zero pipe by the light absorption value that records except that other calibration series of zero pipe, is that ordinate and concentration (mg/L) are carried out linear regression analysis for horizontal ordinate with the absorbance.Adopt each aldehydes matter of this colorimetric method for determining to become good linear relationship between the absorbance under the 770nm as shown in Figure 8 in the concentration range of 0.4-4mg/L, linear equation is y=0.1365x+0.0049, R
2=0.9990, illustrate in the concentration range internal linear relation of being measured good.
The accuracy of this method is tested with average recovery.The sample liquid (paddy rice nutrient solution) that in one group of 4 10mL centrifuge tube, adds 2mL, and add 0.00 respectively, 0.10,0.30,0.50mL above-mentioned mixed phenol and phenolic acid standard solution standard mother liquor (50mg/L), add 1.25 respectively, 1.15,0.95,0.75mL the distilled water developer, 0.5mL reagent for determining total phenol in water, 1.25mL the aqueous sodium carbonate of concentration 2.0mol/L, after mixing, after the room temperature lucifuge is placed 40min, measure absorbance down in the 770nm wavelength, each sample 3 times repeats, and the result shows (table 4): adopt this method can accurately measure total phenol in the water body.The reappearance experiment is to carry out replication 9 times by above-mentioned mixed phenol and phenolic acid standard solution standard mother liquor to 50mg/L, and obtaining the coefficient of variation is 1.59%, illustrates that the reappearance of this method is better.The check of precision is by to 4 kinds of variable concentrations (1mg/L, 2mg/L, 3mg/L, 4mg/L) above-mentioned mixed phenol and phenolic acid standard solution standard mother liquor carry out 5 replicate determinations respectively, obtain the coefficient of variation and be respectively 0.06%, 0.08%, 0.14%, show that this method has higher precision, meets the sample analysis requirement.
Table 4 reagent for determining total phenol in water is to mixed phenol in the water body and phenolic acid recovery of standard addition
Remarks: average recovery meets the requirement of US EPA (U.S. environmental protection general administration) standard between 70% ~ 120%.
Application example: total phenol content is measured in the rice root secretion
Liquid to be measured is one month nutrient solution of paddy rice PI312777 water planting plantation.Get 3.25mL liquid to be measured, add the 0.5mL reagent for determining total phenol in water, the aqueous sodium carbonate of 1.25mL concentration 2.0mol/L, after mixing, the room temperature lucifuge is placed 40min.Testing sample adopts ultraviolet-visible spectrophotometer to carry out length scanning (Fig. 9) in 500-1000nm, and obtaining the maximum absorption wavelength of actual sample after chromogenic reaction is 770nm.
The above-mentioned liquid to be measured of adding 3.25mL, 0.5mL reagent for determining total phenol in water, 1.25mL concentration are the aqueous sodium carbonate of 2.0mol/L in the 10mL centrifuge tube, after mixing, after the room temperature lucifuge is placed 40min, down measuring absorbance in the 770nm wavelength is 0.4344, and the content of trying to achieve total phenol in water according to Fig. 8 mixed phenol and phenolic acid typical curve is 3.15mg/L again.
Sodium tungstate of the present invention, sodium molybdate, strong phosphoric acid, concentrated hydrochloric acid, lithium sulfate can be buied by market, analyze pure.Reagent for determining total phenol in water of the present invention is through one matter (P-hydroxybenzoic acid, phenol), (consist of forulic acid: P-hydroxybenzoic acid: salicylic acid: the mass ratio of vanillic acid is 1: 1: 1: 1) to mix phenolic acid, and mixed phenol and phenolic acid (consist of phenol: catechol: resorcinol: forulic acid: P-hydroxybenzoic acid: salicylic acid: the mass ratio of vanillic acid is 1: 1: 1: 1: 1: 1: 1) measure checking, it is low that the result shows that this determining total phenol in water method has a detectability, detection speed is fast, the condition determination restriction is few, color range is wide and stable, has good precision and accuracy and simple and easy to do.Reagent for determining total phenol in water of the present invention is through the exemplary application of paddy rice plantation liquid actual sample, and its maximum absorption wavelength can be applied to actual sample mensuration with single and to mix phenolic acid in full accord, and have quick and precisely, advantage such as simple and easy to do.
Claims (2)
1. the preparation method of a reagent for determining total phenol in water: its raw material comprises: sodium tungstate, sodium molybdate, strong phosphoric acid, concentrated hydrochloric acid, lithium sulfate and distilled water;
The concentration of described each raw material is:
Raw material final concentration mol/L
Sodium tungstate 0.300～0.400
Sodium molybdate 0.150～0.250
Strong phosphoric acid 0.500～0.600
Concentrated hydrochloric acid 1.000～2.000
Lithium sulfate 0.300～0.400
Solvent is a distilled water;
Also add bromine water in the described reagent for determining total phenol in water; The consumption of described bromine water is to add 4mL bromine water in every 1L reagent for determining total phenol in water;
The concentration of described bromine water is: the weight concentration 3% of bromine aqueous solution;
The weight concentration of described strong phosphoric acid is 85%; The weight concentration of described concentrated hydrochloric acid is 36～38%;
It is characterized in that: the preparation method is as follows, according to the raw material matched proportion density, calculates the consumption of the volume required various raw materials that will add: add sodium tungstate in container, sodium molybdate, part distilled water, strong phosphoric acid and concentrated hydrochloric acid, fully mixing, after boiling water bath refluxed 11 hours, add lithium sulfate again, a small amount of distilled water adds bromine water simultaneously, uncovered boiling 20 minutes, the cooling back is settled to volume required with distilled water; Liquid filtering obtains described reagent for determining total phenol in water behind the constant volume, is positioned over to preserve in the brown reagent bottle to use.
2. using method of the reagent for determining total phenol in water of method preparation according to claim 1, it is characterized in that: adding 3.25mL liquid to be measured, the described reagent for determining total phenol in water of 0.5mL, 1.25mL concentration are the aqueous sodium carbonate of 2.0mol/L in the 10mL centrifuge tube, after mixing, after the room temperature lucifuge is placed 40min, measure absorbance down in the 770nm wavelength, try to achieve the content of total phenol in water again according to typical curve.
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| RU2775466C1 (en) * | 2021-03-11 | 2022-07-01 | федеральное государственное бюджетное образовательное учреждение высшего образования "Алтайский государственный университет" | Extraction-fluorimetric method for determining phenols in the solid component of snow cover |
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| CN106468715A (en) * | 2016-06-21 | 2017-03-01 | 安徽康乐美生物科技有限公司 | A kind of cervical cancer urine detection reagent and its preparation method and application |
| CN109444065A (en) * | 2018-12-21 | 2019-03-08 | 天津利海石化有限公司 | The measuring method of phenol content in by-product concentrated hydrochloric acid |
| CN109470696A (en) * | 2018-12-27 | 2019-03-15 | 冀晓玲 | A kind of detection reagent and preparation method thereof of quick detection urine para hydroxybenzene alanine |
| CN112285041B (en) * | 2020-09-30 | 2023-04-11 | 江苏大学 | Rapid detection method for ionic liquid content |
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| US5776415A (en) * | 1994-09-06 | 1998-07-07 | Board Of Trustees Operating Michigan State University | Method and test kit for determining hydroxy aromatic compounds |
| CN101187637A (en) * | 2007-12-18 | 2008-05-28 | 四川大学 | Automatic analysis method for seawater phenols compounds |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5776415A (en) * | 1994-09-06 | 1998-07-07 | Board Of Trustees Operating Michigan State University | Method and test kit for determining hydroxy aromatic compounds |
| CN101187637A (en) * | 2007-12-18 | 2008-05-28 | 四川大学 | Automatic analysis method for seawater phenols compounds |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RU2775466C1 (en) * | 2021-03-11 | 2022-07-01 | федеральное государственное бюджетное образовательное учреждение высшего образования "Алтайский государственный университет" | Extraction-fluorimetric method for determining phenols in the solid component of snow cover |
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