CN106644980A - Method for detecting oil content in sewage - Google Patents

Method for detecting oil content in sewage Download PDF

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Publication number
CN106644980A
CN106644980A CN201611149121.8A CN201611149121A CN106644980A CN 106644980 A CN106644980 A CN 106644980A CN 201611149121 A CN201611149121 A CN 201611149121A CN 106644980 A CN106644980 A CN 106644980A
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CN
China
Prior art keywords
water sample
absorbance
water
ultraviolet
sewage
Prior art date
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Pending
Application number
CN201611149121.8A
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Chinese (zh)
Inventor
周琳
孙福凯
史万军
姜明涛
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North Huajin Chemical Industries Group Co Ltd
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North Huajin Chemical Industries Group Co Ltd
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Publication date
Application filed by North Huajin Chemical Industries Group Co Ltd filed Critical North Huajin Chemical Industries Group Co Ltd
Priority to CN201611149121.8A priority Critical patent/CN106644980A/en
Publication of CN106644980A publication Critical patent/CN106644980A/en
Pending legal-status Critical Current

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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/17Systems in which incident light is modified in accordance with the properties of the material investigated
    • G01N21/25Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
    • G01N21/31Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/17Systems in which incident light is modified in accordance with the properties of the material investigated
    • G01N21/25Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
    • G01N21/31Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
    • G01N21/33Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using ultraviolet light
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/17Systems in which incident light is modified in accordance with the properties of the material investigated
    • G01N21/25Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
    • G01N21/31Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
    • G01N21/35Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
    • G01N21/3577Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light for analysing liquids, e.g. polluted water

Abstract

The invention discloses an oil content detection method which comprises the following steps: (1) measuring the absorbance of a first water sample under the irradiation of light rays different in wavelength by use of an ultraviolet-visible spectrophotometer, and determining wavelength lambda as absorption wave; (2) fetching n second water samples, and measuring the oil content of each second water sample diluted to different concentration; (3) directly measuring the absorbance of n second water samples by use of the light ray absorbing wavelength lambda; (4) setting an equation y=k*A+alpha, and inputting the oil content of each second water sample and corresponding absorbance obtained in the step (3) into a computer for linear regression calculation to obtain the values of k and alpha; and (5) measuring the absorbance of a third water sample by use of an ultraviolet-visible spectrophotometer and substituting the value of absorbance into the equation obtained in the step (4) to obtain the oil content y of the third water sample. The invention aims at providing a method for detecting oil content in sewage, which is environment-friendly and harmless and simpler and more convenient to operate.

Description

A kind of method of detection Oil in Sewage Water content
Technical field
The present invention relates to sewage treatment area, specially a kind of method of detection Oil in Sewage Water content.
Background technology
For in production process produce sewage enterprise for, the process of sewage is an important job, for example for For the enterprise of petroleum refining, the oil content in water is the main target for showing water quality, is needed in many production stage intermediate frequencies The oil content in sewage is detected numerously.At present the method for the oil content in detection sewage mainly has two kinds.One kind is to perform earliest Standard GB/T/T7490-1987 specified in, using petroleum ether extraction oil, then contained with determined by ultraviolet spectrophotometry oil Amount.Another kind is specified in standard HJ637-2012, using carbon tetrachloride extraction oil, Wastewater Sample to be transferred completely into In 2000mL separatory funnels, 25.0mL carbon tetrachloride washing sample bottles are measured, in being transferred completely into separatory funnel.Concussion 3min, And the normally open cock exhausts of Jing, after static layering, other process are done, then use Infrared Spectralcolorimetry Detect Oil content.
Both the above method is directed to be extracted using solution, is then detected, its operating procedure is more numerous and diverse.Together When, the carbon tetrachloride used in later approach is poisonous and the volatile nerve to people has paralysis to act on.Especially in summer temperature Higher, carbon tetrachloride is more volatile, for the experimenter for frequently being detected, the injury to body can be caused really, separately Outward, the discharge of raffinate will also result in pollution to environment after test.
The content of the invention
Present invention solves the technical problem that being to provide a kind of environmentally friendly and operate easier detection Oil in Sewage Water to contain The method of amount.
The method of the detection Oil in Sewage Water content that the present invention is provided, comprises the steps:
(1) with distilled water as blank, shone using light of the water sample of ultraviolet-visible photometer measurement first in different wave length Absorbance under penetrating, and wherein absorbance highest wavelength X is found out, and using the wavelength X as absorption ripple;
(2) take the water sample of n parts second, different degrees of dilution carried out to the water sample of n parts second, using ultraviolet spectrophotometry or Person's infrared spectrophotometer measures per part of oil content y1......yn for being diluted as the second water sample of variable concentrations;
(3) using ultraviolet-uisible spectrophotometer with the absorbance of light direct measurement n second water sample of part of absorbing wavelength λ A1......An;
(4) arrange equation y it is straight=k × A+ α, wherein y is directly the sewage oil obtained by direct ultraviolet AAS Content, A is the absorbance of the second water sample measured by ultraviolet-visible spectrophotometry measurement, and k is the slope of straight line, and α is intercept, Absorbance A 1......An by the oil content y1......yn of per part of second water sample obtained in step (3) and corresponding thereto Input computer carries out linear regression calculating, the value of k and α is obtained, so as to obtain the equation of direct ultraviolet spectrophotometry de termination Formula;
(5) with the absorbance of the water sample of measurement of ultraviolet-visible spectrophotometer the 3rd, and the value of absorbance is substituted into into step (4) The equation of middle acquisition can obtain the oil content y of the 3rd water sampleDirectly
The method of the detection Oil in Sewage Water content of the present invention has the advantages that:After equation is determined, as long as Directly measure the absorbance of water sample and the oil content of water sample is obtained by calculating, this method can be referred to as direct ultraviolet light splitting light Degree method first extracts in prior art and then measures the ultraviolet spectrophotometry of oil content and compares with infrared spectrophotometer, no The step of only eliminating extraction causes operation easier, and will not produce danger to human body using chemical reagent due to extraction Evil, also will not be to environment.
Description of the drawings
The step of Fig. 1 is the method for the detection Oil in Sewage Water content of one embodiment of the invention rough schematic view.
The step of Fig. 2 is the method according to the detection Oil in Sewage Water content of one embodiment of the invention
(1) data for obtaining are drawn absorbance A and the graph of relation of wavelength X.
Specific embodiment
As shown in figure 1, the method for the detection Oil in Sewage Water content of invention, it is not necessary to the oil in sewage is extracted, is wrapped Include following steps:
(1) with distilled water as blank, using ultraviolet-uisible spectrophotometer light of first water sample in different wave length is obtained Absorbance under irradiation, and wherein absorbance highest wavelength X is found out, and using the wavelength X as absorption ripple.
In the present embodiment, using TU-1810 measurement of ultraviolet-visible spectrophotometer absorbances, and by absorbance A and ripple Long λ mappings, obtain Fig. 2.As can be drawn from Figure 2, water sample to wavelength for 200nm light trap highest, therefore, select 200nm is absorbing wavelength.
(2) water sample of n parts second is taken, and different degrees of dilution is carried out to the water sample of n parts second, and the n parts are diluted as Second water sample of variable concentrations carries out ultraviolet spectrophotometry or infrared spectrophotometer measures its oil content y1......yn。 In the present embodiment, 5 part of second water sample is have chosen, the 1st part of the second water sample is raw water sample, that is, be not diluted.2nd part of the second water Sample carries out 75% dilution, and the 3rd part of the second water sample carries out 50% dilution, and the 4th part of the second water sample carries out 25% dilution, the 5th part second Water sample carries out 12.5% dilution.
(3) using ultraviolet-uisible spectrophotometer with the absorbance of light direct measurement n second water sample of part of absorbing wavelength λ A1......An.In the present embodiment, the light with wavelength as 200nm irradiates 5 part of second water sample, the absorbance such as form 1 of acquisition It is shown:
Form 1:
(4) equation y is setDirectly=k × A+ α, wherein yDirectlyFor the sewage oil content that direct ultraviolet AAS is obtained, A The absorbance of the second water sample obtained for ultraviolet-uisible spectrophotometer, k is the slope of straight line, and α is intercept.By in step (3) The oil content y of per part of second water sample for obtaining1......ynAnd absorbance A corresponding thereto1......AnInput computer enters Row linear regression is calculated, and the value of k and α is obtained, so as to obtain the equation of direct ultraviolet spectrophotometry de termination.
In the present embodiment, the data input computer in form 1 is carried out into linear regression calculating, obtains k=5.51, α =-0.2, therefore, can show that the equation for calculating sewage oil content according to absorbance is yDirectly=5.51 × A-0.2.Meanwhile, may be used also Correlation coefficient r=0.9999 of party's formula is calculated, its value is closer to 1, and the linear correlation property of party's formula is better. In practical operation, it is desirable to r >=0.997, if the value of r is not in this range, need to re-start step (1) to (4), until r The satisfactory scope of value.
(5) with the absorbance of the water sample of measurement of ultraviolet-visible spectrophotometer the 3rd, and the value of absorbance is substituted into into step (4) The equation of middle acquisition can obtain the oil content y of the 3rd water sampleDirectly
So after equation is determined, as long as the oil directly measured the absorbance of water sample and water sample is obtained by calculating contains Amount, this method can be referred to as direct ultraviolet AAS, with prior art in first extract and then measure the ultraviolet of oil content AAS is compared with infrared spectrophotometer, causes the step of the method for the present invention not only eliminates extraction operation simpler Just, and will not due to extraction using chemical reagent and to human body produce harm, also will not be to environment.
As preferred scheme, five part of second water sample is chosen in step (2), wherein, water sample 1 is raw water sample, and water sample 2 is 75% dilution raw water sample, water sample 3 is 50% dilution raw water sample, and water sample 4 is 25% dilution raw water sample, and water sample 5 is that 15% dilution is former Water sample.
As preferred scheme, the method for the present invention can be verified by following steps whether reliably, specially:Root Measure the oil content of m water sample respectively successively according to step (5), obtain yStraight 1、yStraight 2......yStraight m, m that calculation procedure (5) is measured The mean value of the oil content of water sample is yIt is straight flat, standard deviation is yIt is straight poor, as > 2.54%, step (1) to (4) is re-started to obtain New equation is taken, until the y of the new measured value obtained according to new equationIt is straight poor/yIt is straight flat≤ 2.54%.By preferred side Case, standard deviation can be controlled in the range of setting, so as to ensure the accuracy of direct ultraviolet AAS.
In the present embodiment, 5 water samples are measured on the different dates by direct ultraviolet AAS respectively, obtains it A in oil content such as form 23Shown in one hurdle, its mean value is 7.328, and standard deviation is 0.1509, yIt is straight poor/yIt is straight flat=2.59%.
Measure the oil content of m water sample respectively successively by infrared spectrophotometer, obtain yRed 1、yRed 2......yRed m, meter The mean value for calculating the oil content of the m water sample that infrared spectrophotometer is measured is yIt is red flat, standard deviation is yRed difference.By ultraviolet spectrometry Photometry measures respectively successively the oil content of m water sample, obtains yPurple 1、yPurple 2......yPurple m, calculate ultraviolet spectrophotometry and measure M water sample oil content mean value be yPurple is flat.Detection order and above-mentioned direct ultraviolet light splitting of two kinds of detection methods to water sample Photometry is identical to the detection order of water sample.In the present embodiment, the A in form 21The data on one hurdle are according to ultraviolet spectrometry light The data that degree method is obtained, A2The data on one hurdle are the data obtained according to infrared spectrophotometer.
Form 2:
Note:A1Be with GB/T7490-1987 determined by ultraviolet spectrophotometry obtain data, A2It is red with HJ637-2012 The data that outer spectrophotometry is obtained, A3It is the data obtained with direct ultraviolet spectrophotometry.
Standard deviation is less, illustrates that measurement result is more accurate.By the data in form 2, it is known that using the side of the present invention Oil content in method measurement sewage is reliable.
In practical operation, at set intervals, can with repeat step (1) to step (4) to obtain new k values, so as to More adapt to the situation of change of sewage.Preferably, a period of time is 30-60 days.
Above example is only the exemplary embodiment of the present invention, is not used in the restriction present invention, protection scope of the present invention It is defined by the claims.Those skilled in the art are in the essence and protection domain of the present invention, and what the present invention was made is various Modification or equivalent are also within the scope of the present invention.

Claims (7)

1. it is a kind of detection Oil in Sewage Water content method, it is characterised in that comprise the steps:
(1) with distilled water as blank, using the water sample of ultraviolet-visible photometer measurement first under the light irradiation of different wave length Absorbance, and find out wherein absorbance highest wavelength X, and using the wavelength X as absorbing ripple;
(2) water sample of n parts second is taken, different degrees of dilution is carried out to the water sample of n parts second, using ultraviolet spectrophotometry or red Outer AAS measures per part of oil content y for being diluted as the second water sample of variable concentrations1......yn
(3) using ultraviolet-uisible spectrophotometer with the absorbance of light direct measurement n second water sample of part of absorbing wavelength λ A1......An
(4) equation y is setDirectly=k × A+ α, wherein yDirectlyIt is the sewage oil content obtained by direct ultraviolet AAS, A It is the absorbance of the second water sample measured by ultraviolet-visible spectrophotometry measurement, k is the slope of straight line, and α is intercept, by step (3) the oil content y of per part of second water sample obtained in1......ynAnd absorbance A corresponding thereto1......AnInput meter Calculation machine carries out linear regression calculating, the value of k and α is obtained, so as to obtain the equation of direct ultraviolet spectrophotometry de termination;
(5) with the absorbance of the water sample of measurement of ultraviolet-visible spectrophotometer the 3rd, and will obtain in value substitution step (4) of absorbance The equation for obtaining can obtain the oil content y of the 3rd water sampleDirectly
2. the method for detection Oil in Sewage Water content according to claim 1, it is characterised in that five are chosen in the step (2) The second water sample of part, wherein, water sample 1 is raw water sample, and water sample 2 is 75% dilution raw water sample, and water sample 3 dilutes raw water sample, water for 50% Sample 4 is 25% dilution raw water sample, and water sample 5 is 15% dilution raw water sample.
3. the method for detection Oil in Sewage Water content according to claim 1, it is characterised in that obtain in calculation procedure (4) Equation coefficient correlation γ, as γ < 0.997, step (1) to (4) is re-started, until γ >=0.997.
4. according to the method for the detection Oil in Sewage Water content in claim 2, it is characterised in that distinguished successively according to step (5) The oil content of m water sample of measurement, obtains yStraight 1、yStraight 2......yStraight m, the mean value for calculating the oil content of m water sample is yIt is straight flat, standard Deviation is yIt is straight poor, work as yIt is straight poor/yIt is straight flatDuring > 2.54%, step (1) to (4) is re-started to obtain new equation, until according to new The y of new measured value that obtains of equationIt is straight poor/yIt is straight flat≤ 2.54%.
5. the method for detection Oil in Sewage Water content according to claim 4, it is characterised in that m water sample is not same date The water sample of acquirement.
6. it is according to claim 2 detection Oil in Sewage Water content method, it is characterised in that at set intervals, repeat Step (1) is to step (4) obtaining new k values.
7. it is according to claim 6 detection Oil in Sewage Water content method, it is characterised in that be for a period of time 30-60 days.
CN201611149121.8A 2016-12-14 2016-12-14 Method for detecting oil content in sewage Pending CN106644980A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109612958A (en) * 2018-12-18 2019-04-12 海阳市启恒环保科技有限公司 The method and device thereof of a variety of oils concentration in water can be measured simultaneously
CN112161980A (en) * 2020-08-04 2021-01-01 刘邦楠 Water quality detection method and system for network and mobile terminal
US11460461B2 (en) 2019-04-17 2022-10-04 Ypf Sociedad Anónima Method for determining oil concentration in water

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1888869A (en) * 2005-06-29 2007-01-03 赵菊英 Method for making oil content in water have comparability measured by fluorescent method and other methods

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1888869A (en) * 2005-06-29 2007-01-03 赵菊英 Method for making oil content in water have comparability measured by fluorescent method and other methods

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
高武民等: "《紫外可见分光光度计在污水含油分析中的应用》", 《石油和化工设备》 *

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109612958A (en) * 2018-12-18 2019-04-12 海阳市启恒环保科技有限公司 The method and device thereof of a variety of oils concentration in water can be measured simultaneously
US11460461B2 (en) 2019-04-17 2022-10-04 Ypf Sociedad Anónima Method for determining oil concentration in water
CN112161980A (en) * 2020-08-04 2021-01-01 刘邦楠 Water quality detection method and system for network and mobile terminal

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