CN109612958A - The method and device thereof of a variety of oils concentration in water can be measured simultaneously - Google Patents
The method and device thereof of a variety of oils concentration in water can be measured simultaneously Download PDFInfo
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- CN109612958A CN109612958A CN201811549305.2A CN201811549305A CN109612958A CN 109612958 A CN109612958 A CN 109612958A CN 201811549305 A CN201811549305 A CN 201811549305A CN 109612958 A CN109612958 A CN 109612958A
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- 239000003921 oil Substances 0.000 title claims abstract description 169
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 33
- 238000000034 method Methods 0.000 title claims abstract description 23
- 241001465754 Metazoa Species 0.000 claims abstract description 62
- 239000003208 petroleum Substances 0.000 claims abstract description 9
- 239000000243 solution Substances 0.000 claims description 82
- 238000002835 absorbance Methods 0.000 claims description 75
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 33
- 239000000126 substance Substances 0.000 claims description 27
- 239000012086 standard solution Substances 0.000 claims description 20
- 239000007788 liquid Substances 0.000 claims description 19
- 238000000870 ultraviolet spectroscopy Methods 0.000 claims description 15
- HCWCAKKEBCNQJP-UHFFFAOYSA-N magnesium orthosilicate Chemical compound [Mg+2].[Mg+2].[O-][Si]([O-])([O-])[O-] HCWCAKKEBCNQJP-UHFFFAOYSA-N 0.000 claims description 14
- 239000000391 magnesium silicate Substances 0.000 claims description 14
- 229910052919 magnesium silicate Inorganic materials 0.000 claims description 14
- 235000019792 magnesium silicate Nutrition 0.000 claims description 14
- 238000010521 absorption reaction Methods 0.000 claims description 13
- 238000005070 sampling Methods 0.000 claims description 12
- 235000013311 vegetables Nutrition 0.000 claims description 11
- 238000001514 detection method Methods 0.000 claims description 10
- 230000003287 optical effect Effects 0.000 claims description 9
- 238000000605 extraction Methods 0.000 claims description 7
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims description 6
- YZCKVEUIGOORGS-OUBTZVSYSA-N Deuterium Chemical group [2H] YZCKVEUIGOORGS-OUBTZVSYSA-N 0.000 claims description 4
- 229910052805 deuterium Inorganic materials 0.000 claims description 4
- 230000031700 light absorption Effects 0.000 claims description 4
- 230000018044 dehydration Effects 0.000 claims description 3
- 238000006297 dehydration reaction Methods 0.000 claims description 3
- 239000012530 fluid Substances 0.000 claims description 3
- 230000000694 effects Effects 0.000 abstract description 3
- 235000019198 oils Nutrition 0.000 description 118
- 241000196324 Embryophyta Species 0.000 description 62
- 238000005259 measurement Methods 0.000 description 27
- 239000000523 sample Substances 0.000 description 18
- 238000001179 sorption measurement Methods 0.000 description 10
- 230000008033 biological extinction Effects 0.000 description 9
- 238000002474 experimental method Methods 0.000 description 7
- 239000000463 material Substances 0.000 description 7
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 5
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 3
- 235000019486 Sunflower oil Nutrition 0.000 description 3
- 238000000862 absorption spectrum Methods 0.000 description 3
- 239000002285 corn oil Substances 0.000 description 3
- 235000005687 corn oil Nutrition 0.000 description 3
- 238000001228 spectrum Methods 0.000 description 3
- 239000002600 sunflower oil Substances 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 235000019483 Peanut oil Nutrition 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 239000010775 animal oil Substances 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 239000000944 linseed oil Substances 0.000 description 2
- 235000021388 linseed oil Nutrition 0.000 description 2
- 239000000312 peanut oil Substances 0.000 description 2
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 2
- 239000004810 polytetrafluoroethylene Substances 0.000 description 2
- 239000010453 quartz Substances 0.000 description 2
- 239000012488 sample solution Substances 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 102100027324 2-hydroxyacyl-CoA lyase 1 Human genes 0.000 description 1
- RZVAJINKPMORJF-UHFFFAOYSA-N Acetaminophen Chemical compound CC(=O)NC1=CC=C(O)C=C1 RZVAJINKPMORJF-UHFFFAOYSA-N 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 101001009252 Homo sapiens 2-hydroxyacyl-CoA lyase 1 Proteins 0.000 description 1
- -1 Polytetrafluoroethylene Polymers 0.000 description 1
- 230000010165 autogamy Effects 0.000 description 1
- 235000013405 beer Nutrition 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000003086 colorant Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 229960000935 dehydrated alcohol Drugs 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 230000002452 interceptive effect Effects 0.000 description 1
- 239000006101 laboratory sample Substances 0.000 description 1
- 239000011490 mineral wool Substances 0.000 description 1
- 230000010355 oscillation Effects 0.000 description 1
- 230000020477 pH reduction Effects 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 238000002203 pretreatment Methods 0.000 description 1
- 239000005297 pyrex Substances 0.000 description 1
- 239000013558 reference substance Substances 0.000 description 1
- 239000012898 sample dilution Substances 0.000 description 1
- 238000009738 saturating Methods 0.000 description 1
- 239000000344 soap Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 235000011149 sulphuric acid Nutrition 0.000 description 1
- 230000009182 swimming Effects 0.000 description 1
- 238000002834 transmittance Methods 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/33—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using ultraviolet light
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- Physics & Mathematics (AREA)
- Spectroscopy & Molecular Physics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Investigating Or Analysing Materials By Optical Means (AREA)
Abstract
The invention belongs to the technical fields using Ultraviolet Photometric Method, provide a kind of method that can measure a variety of oils concentration in water simultaneously.Water sample is pre-processed, solution is divided into two parts: first extract liquors and the second extract liquor thereafter；The light splitting degree for measuring the first extract liquor and the second extract liquor respectively by measuring device, obtains the concentration of petroleum class and zoology and botany oil class in solution；It is summed to obtain the concentration of total oil according to the concentration of animals and plants oils concentration and petroleum-type, petroleum-type, animals and plants oils, the technical effect of total oil concentration in water is measured while may be implemented quick and easy.
Description
Technical field
It the present invention relates to the use of the technical field of Ultraviolet Photometric Method, and in particular to one kind can measure a variety of oil in water simultaneously
The method of class concentration.
Background technique
UV-VIS spectrophotometry is the absorbance that substance is measured in 190~800nm wave-length coverage, for identifying,
The method of determination of foreign matter and quantitative determination.When light passes through measured matter solution, substance is to the degree of absorption of light with the wavelength of light
It is different and change.Therefore, the absorbance by measurement substance at different wave length, and draw the relational graph of its absorbance and wavelength
Up to the absorption spectrum of measured matter.From absorption spectrum, maximum absorption wavelength λ can be determinedmaxWith minimal absorption wavelength Xmin。
The absorption spectrum of substance has characteristic relevant to its structure.Therefore, the spectrum of sample in particular range of wavelengths can be passed through
Compared with reference substance spectrum, or by determining maximum absorption wavelength, or the absorption ratio by measuring two certain wave strong points
And identify substance.In certain wavelength XmaxThe absorbance of the standard serial solution of lower measurement something makees standard curve, then measures
The absorbance value of sample solution is acquired the concentration of sample solution by standard curve.The traditional measurement of the concentration of oily substance in water
Method is exactly to be measured by UV-VIS spectrophotometry.UV-VIS spectrophotometry is only capable of individually measuring petroleum at present
Class or animals and plants oils concentration, and cannot be measured simultaneously.
Summary of the invention
For the defects in the prior art, the present invention provides the method that can measure a variety of oils concentration in water simultaneously, can
Petroleum-type in water, animals and plants oils, total oil concentration are measured with simple and quick.
In order to achieve the above objectives, the method provided by the invention that a variety of oils concentration in water can be measured simultaneously, by water sample
It is divided into two parts: first solution and the second solution of same volume after sampling pretreatment；
S1 is directed to the first solution；
S1.1 adsorbs the first solution by magnesium silicate；
The first solution after S1.2 absorption measures to obtain wherein petroleum-type absorbance by UV-VIS spectrophotometry
A1；
S1.3 brings the petroleum-type absorbance A 1 into first formula and petroleum-type concentration C in solution is calculatedPetroleum-type, described
First formula is as follows: CPetroleum-type=a1*A1；
S2 is directed to the second solution；
The second solution of S2.1 measures to obtain wherein total absorbance A by UV-VIS spectrophotometry；
S2.2 brings the total absorbance A into second formula and animals and plants oils absorbance A 2 in solution is calculated, described
Second formula is as follows: A2=A-A1；
S2.3 brings the animals and plants oils absorbance A 2 into third formula and animals and plants oils concentration in solution is calculated
CAnimals and plants oils, the third formula is as follows: CAnimals and plants oils=a2*A2；
S3 is by the petroleum-type concentration CPetroleum-typeWith the animals and plants oils concentration CAnimals and plants oilsIt brings the 4th formula into and obtains solution
Interior total oil concentration CAlways, the 4th formula is as follows: CAlways=CPetroleum-type+CAnimals and plants oils；
A1: the absorptivity of petroleum-type standard solution；
A2: the absorptivity of vegetable and animals oils class standard solution.
The technical principle and technical effect of this programme are as follows:
CPetroleum-type: the actual concentrations of solution petroleum-type to be measured, this is the parameter for needing to acquire；
CAnimals and plants oils: the actual concentrations of solution animals and plants oils to be measured, this is the parameter for needing to acquire；
CAlways: the actual concentrations of the total oil of solution to be measured, this is the parameter for needing to acquire；
A1: the absorptivity of petroleum-type standard solution, extinction of the extinction material in unit concentration and unit liquid layer thickness
Degree, is the absorptivity of this substance, which can be drawn petroleum-type concentration of standard solution-extinction and be write music by many experiments
Line obtains；
A2: the absorptivity of vegetable and animals oils class standard solution, extinction material is in unit concentration and unit liquid layer thickness
Absorbance is the absorptivity of this substance, which can draw vegetable and animals oils class standard solution concentration-by many experiments
Absorbance curve obtains；
A: actually measured total absorbance value measures to obtain by colorimetric pool is put into without the extract liquor of adsorption of magnesium silicate, this suction
Luminosity includes the absorbance A 1 of petroleum-type and the absorbance A 2 of animals and plants oils；
A1: the absorbance value of actually measured petroleum-type will obtain in treated liquid is put into colorimetric pool in measurement；
A2: the absorbance value of actually measured animals and plants oils can be acquired by aforementioned formula.
This programme is easy to operate, and the concentration of petroleum-type, animals and plants oils and total oil can quickly be calculated, entirely measured
The simple and quick convenience of journey is omitted various oils compared to traditional measurement and detects respectively, in the tedious steps calculated, can save
Save a large amount of time.
Further, pretreatment includes that step is successively as follows after solution sampling: being 1. acidified；2. extracting；3. being dehydrated, reduce to rear
The interfering substance of continuous measurement.
Further, step is acidified to pH value≤2 after 1. sampling, and provides acid environment in advance.
Further, 2. step uses the oily substance in n-hexane extraction sample, can be easier to extract oily substance
Come.
Further, 3. step uses anhydrous sodium sulfate to be dehydrated, and the dehydrating effect of anhydrous sodium sulfate is more preferable.
Further, if strength of fluid is more than measurement device range, the liquid that the step (3) dehydration obtains is carried out dilute
It releases, it need to be multiplied by diluted multiple, convenient for measuring the solution concentration more than range under the device of limited range when reading.
A kind of device that can measure a variety of oils concentration in water simultaneously, including detection unit, control unit and output are single
Member；
The detection unit, for measuring wherein stone by UV-VIS spectrophotometry to the first solution after absorption
Oils absorbance A 1 measures to obtain wherein total absorbance A by UV-VIS spectrophotometry to the second solution, and by petroleum
Class absorbance A 1 and total absorbance A are transmitted to control unit；
Described control unit,
Petroleum-type concentration C in solution is calculated for bringing the petroleum-type absorbance A 1 into first formulaPetroleum-type, and will
Petroleum-type concentration CPetroleum-typeIt is transmitted to output unit, first formula is as follows: CPetroleum-type=a1*A1；The total absorbance A is brought into
Animals and plants oils absorbance A 2 in solution is calculated in second formula, and second formula is as follows: A2=A-A1；
Being also used to bring into the animals and plants oils absorbance A 2 third formula, that animals and plants oils in solution is calculated is dense
Spend CAnimals and plants oils, the third formula is as follows: CAnimals and plants oils=a2*A2, and by animals and plants oils concentration CAnimals and plants oilsIt is single to be transmitted to output
Member；
It is also used to the petroleum-type concentration CPetroleum-typeWith the animals and plants oils concentration CAnimals and plants oilsThe 4th formula is brought into obtain
Total oil concentration C in solutionAlways, the 4th formula is as follows: CAlways=CPetroleum-type+CAnimals and plants oils, and by total oil concentration CAlwaysIt is single to be transmitted to output
Member；
Output unit, for showing petroleum-type concentration CPetroleum-type, animals and plants oils concentration CAnimals and plants oilsWith total oil concentration CAlways；
A1: the absorptivity of petroleum-type standard solution；
A2: the absorptivity of vegetable and animals oils class standard solution；
CPetroleum-type: the actual concentrations of solution petroleum-type to be measured, this is the parameter for needing to acquire；
CAnimals and plants oils: the actual concentrations of solution animals and plants oils to be measured, this is the parameter for needing to acquire；
CAlways: the actual concentrations of the total oil of solution to be measured, this is the parameter for needing to acquire；
A1: the absorptivity of petroleum-type standard solution, extinction of the extinction material in unit concentration and unit liquid layer thickness
Degree, is the absorptivity of this substance, which can be drawn petroleum-type concentration of standard solution-extinction and be write music by many experiments
Line obtains；
A2: the absorptivity of vegetable and animals oils class standard solution, extinction material is in unit concentration and unit liquid layer thickness
Absorbance is the absorptivity of this substance, which can draw vegetable and animals oils class standard solution concentration-by many experiments
Absorbance curve obtains；
A: actually measured total absorbance value measures to obtain by colorimetric pool is put into without the extract liquor of adsorption of magnesium silicate, this suction
Luminosity includes the absorbance A 1 of petroleum-type and the absorbance A 2 of animals and plants oils；
A1: the absorbance value of actually measured petroleum-type will obtain in treated liquid is put into colorimetric pool in measurement；
A2: the absorbance value of actually measured animals and plants oils can be acquired by aforementioned formula.
This programme is easy to operate, after the absorbance rapid survey of absorbance and total oil to petroleum, can pass through control
The concentration of petroleum-type, animals and plants oils and total oil is quickly calculated in unit processed, and the entire simple and quick convenience of measurement process is compared
Traditional measurement is omitted various oils and detects respectively, in the tedious steps calculated, can save a large amount of time.
Further, the detection unit includes ultraviolet source, colorimetric pool, the cuvette and photoelectric sensor for storing solution；
The colorimetric pool is set between the ultraviolet source and the photoelectric sensor, and the cuvette is placed in the colorimetric pool
Interior, cuvette uses quartz material, ultraviolet light can be made to more easily pass；It is also set between the ultraviolet source and the colorimetric pool
There is the optical filter of 225nm wavelength；The light of the ultraviolet source passes through the optical filter and the colorimetric pool exposes to the light
Electric transducer.Using the available wavelength more needed of ultraviolet source, then by the optical filter of 225nm wavelength directly into
Row filtering, only allows the light of 225nm wavelength to penetrate optical filter, and the light of 225nm wavelength passes through the solution in colorimetric pool, solution
Part light intensity is absorbed, generates decaying through light intensity, according to bright brother's Beer law, the decaying that different solution generates is different, into
And the absorbance of particular solution is obtained, according to the absorptivity of standard solution, the concentration of solution can be obtained by calculating.
Further, the transparent surface of the colorimetric pool, bottom and upper cover are equipped with black light-absorption layer, the colorimetric pool it is saturating
Smooth surface is equipped with the window passed in and out for the light of the ultraviolet source, by providing dark environment around colorimetric pool contrastive colours ware,
It avoids other light sources from entering in colorimetric pool to interfere, improves the precision of measurement.
Further, the ultraviolet source is deuterium lamp, and deuterium lamp is ultraviolet light source, and the wave-length coverage for the light that it is issued is generally
The continuous spectrum band of 190-400nm can satisfy and require to provide the light wave of 225nm.
Detailed description of the invention
It, below will be to specific in order to illustrate more clearly of the specific embodiment of the invention or technical solution in the prior art
Embodiment or attached drawing needed to be used in the description of the prior art are briefly described.In all the appended drawings, similar element
Or part is generally identified by similar appended drawing reference.In attached drawing, each element or part might not be drawn according to actual ratio.
Fig. 1 is the step block diagram that can measure the method for a variety of oils concentration in water simultaneously；
Fig. 2 is the schematic diagram that can measure the device of a variety of oils concentration in water simultaneously.
In attached drawing, 1- ultraviolet source, 2- optical filter；3- cuvette；4- photoelectric sensor；5- colorimetric pool.
Specific embodiment
It is described in detail below in conjunction with embodiment of the attached drawing to technical solution of the present invention.Following embodiment is only used for
Clearly illustrate technical solution of the present invention, therefore be only used as example, and cannot be used as a limitation and limit protection model of the invention
It encloses.It should be noted that unless otherwise indicated, technical term or scientific term used in this application are should be belonging to the present invention
The ordinary meaning that field technical staff is understood.
Embodiment:
It defines first:
Petroleum-type: referring under conditions of pH value≤2, can be by n-hexane extraction not by adsorption of magnesium silicate, and has at 225nm
The substance of characteristic absorption；
Animals and plants oils: referring under conditions of pH value≤2, can be by n-hexane extraction, and can be by adsorption of magnesium silicate
Polar substances；
Total oil: the summation of petroleum class and zoology and botany oil class.
Show that test substance will meet following characteristics from definition:
First, petroleum class and zoology and botany oil class is different two substances.
Second, two substances can be separated by adsorption of magnesium silicate column.
Third, these two types of substances have different Absorption Characteristics when passing through 225nm ultraviolet light.
4th, each component of each substance has common Absorption Characteristics.
A kind of device that can measure a variety of oils concentration in water simultaneously, which is characterized in that single including detection unit, control
Member and output unit；
Detection unit, for measuring wherein petroleum-type by UV-VIS spectrophotometry to the first solution after absorption
Absorbance A 1 measures to obtain wherein total absorbance A by UV-VIS spectrophotometry to the second solution, and petroleum-type is inhaled
Luminosity A1 and total absorbance A are transmitted to control unit；
As shown in Fig. 2, the detection unit include ultraviolet source 1, colorimetric pool 5, store solution cuvette 3 and with control
The photoelectric sensor 4 that unit is electrically connected.Photoelectric sensor 4 is as detection ultraviolet source 1 by the sensor of solution photon absorbing intensity, when
The instrument that light intensity can also can be so detected using other.
The ultraviolet source 1 is deuterium lamp, and colorimetric pool 5 is set between the ultraviolet source 1 and the photoelectric sensor 4,
The cuvette 3 is placed in the colorimetric pool 5；225nm wavelength is additionally provided between the ultraviolet source 1 and the colorimetric pool 5
Optical filter 2；The light of the ultraviolet source 1 passes through the optical filter 2 and the colorimetric pool 5 exposes to the photoelectric sensor
4.Transparent surface, bottom and the upper cover of the colorimetric pool 5 are equipped with black light-absorption layer, and the transparent surface of the colorimetric pool 5, which is equipped with, to be supplied
The window of the light disengaging of the ultraviolet source.
Control unit
It brings the petroleum-type absorbance A 1 into first formula and petroleum-type concentration C in solution is calculatedPetroleum-type, and by petroleum
Class concentration CPetroleum-typeIt is transmitted to output unit, first formula is as follows: CPetroleum-type=a1*A1；Bring the total absorbance A into second
Animals and plants oils absorbance A 2 in solution is calculated in formula, and second formula is as follows: A2=A-A1；
It brings the animals and plants oils absorbance A 2 into third formula and animals and plants oils concentration in solution is calculated
CAnimals and plants oils, the third formula is as follows: CAnimals and plants oils=a2*A2, and by animals and plants oils concentration CAnimals and plants oilsIt is transmitted to output unit；
By the petroleum-type concentration CPetroleum-typeWith the animals and plants oils concentration CAnimals and plants oilsThe 4th formula is brought into obtain in solution
Total oil concentration CAlways, the 4th formula is as follows: CAlways=CPetroleum-type+CAnimals and plants oils, and by total oil concentration CAlwaysIt is transmitted to output unit.
Control unit is AT89S51 single-chip microcontroller.
Output unit, for showing petroleum-type concentration CPetroleum-type, animals and plants oils concentration CAnimals and plants oilsWith total oil concentration CAlways.Output
Unit is LCD display.
A1: the absorptivity of petroleum-type standard solution；
A2: the absorptivity of vegetable and animals oils class standard solution；
CPetroleum-type: the actual concentrations of solution petroleum-type to be measured, this is the parameter for needing to acquire；
CAnimals and plants oils: the actual concentrations of solution animals and plants oils to be measured, this is the parameter for needing to acquire；
CAlways: the actual concentrations of the total oil of solution to be measured, this is the parameter for needing to acquire；
A1: the absorptivity of petroleum-type standard solution, extinction of the extinction material in unit concentration and unit liquid layer thickness
Degree, is the absorptivity of this substance, which can be drawn petroleum-type concentration of standard solution-extinction and be write music by many experiments
Line obtains, and the parameter preset in advance is in control unit；
A2: the absorptivity of vegetable and animals oils class standard solution, extinction material is in unit concentration and unit liquid layer thickness
Absorbance is the absorptivity of this substance, which can draw vegetable and animals oils class standard solution concentration-by many experiments
Absorbance curve obtains, and the parameter preset in advance is in control unit；
A: actually measured total absorbance value measures to obtain by colorimetric pool is put into without the extract liquor of adsorption of magnesium silicate, this suction
Luminosity includes the absorbance A 1 of petroleum-type and the absorbance A 2 of animals and plants oils；
A1: the absorbance value of actually measured petroleum-type will obtain in treated liquid is put into colorimetric pool in measurement；
A2: the absorbance value of actually measured animals and plants oils can be acquired by aforementioned formula.
1, Method And Principle
Under the acid condition of pH value≤2, with the oily substance in n-hexane extraction sample, it is dehydrated through anhydrous sodium sulfate
Afterwards, then with adsorption of magnesium silicate remove animals and plants oils class isopolarity substance, at 225nm wavelength measure absorbance, solution it is dense
It spends directly proportional to absorbance value；Extract liquor absorbance without adsorption of magnesium silicate subtracts the extract liquor absorbance through adsorption of magnesium silicate
The as absorbance of animals and plants oils.
2, the acquisition and preservation of sample
Acquire sample: sample must be representative, and oily substance will be sampled individually, not allow to divide again in laboratory
Sample is all tested whole bottle sample when measurement, cannot outwell or residual fraction sample.Sampling bottle should be (500ml) of constant volume
Vial is cleaned, sampling bottle is cleaned up with solvent, cannot be cleaned with soap, every time when sampling, should fill water sample to graticule.When only
It measures in water emulsified state and when dissolubility oil, the oil film for swimming in water surface is avoided, 20-generally below water surface
It fetches water at 50cm.To be acquired together with oil film, it should be noted that depth, oil film thickness and the area coverage of water.After sample acquisition,
Hydrochloric acid is added and is acidified to PH≤2.
It saves sample: if sample cannot measure in 24 hours, the sample of acidification should be placed at 2--5 DEG C after sampling
It is stored refrigerated.
3, reagent
A) hydrochloric acid ρ (HCl)=1.19g/L；B) sulfuric acid ρ (H2SO4)=1.84mg/L；C) n-hexane
D) dehydrated alcohol；E) anhydrous sodium sulfate；F) magnesium silicate；G) mineral wool；H) adsorption of magnesium silicate column
4, instrument and equipment
A) ultraviolet oil content analyzer；B) automatic extraction apparatus；C) colorimetric pool: 2cm quartz cuvette pond；D) separatory funnel: 1000ml,
Polytetrafluoroethylene (PTFE) cock；E) sampling bottle: 500ml brown Pyrex bulb；F) conical flask: 50ml ground is with cover；G) horizontal oscillations
Device；H) centrifuge: it is equipped with glass centrifuge tube；I) common laboratory often uses vessel and equipment；
5, operating process
As shown in Figure 1, measuring process is as follows:
Firstly, solution sampling is pre-processed, pre-treatment step includes the following:
(1) it is acidified to pH value≤2 at once after sampling；
(2) oily substance in n-hexane extraction sample；
(3) extract liquor is dehydrated using anhydrous sodium sulfate, if strength of fluid is more than device range, is obtained after dehydration
Liquid be diluted, need to be more than amount convenient for being measured under the device of limited range multiplied by diluted multiple when reading
The solution concentration of journey.
It is divided into two parts: first extract liquors and the second extract liquor of same volume by pretreated solution.
S1 is directed to the first solution；
S1.1 adsorbs the first solution by magnesium silicate；
The first solution after S1.2 absorption measures to obtain wherein petroleum-type absorbance by UV-VIS spectrophotometry
A1；
S1.3 brings the petroleum-type absorbance A 1 into first formula and petroleum-type concentration C in solution is calculatedPetroleum-type, described
First formula is as follows: CPetroleum-type=a1*A1；
S2 is directed to the second solution；
The second solution of S2.1 measures to obtain wherein total absorbance A by UV-VIS spectrophotometry；
S2.2 brings the total absorbance A into second formula and animals and plants oils absorbance A 2 in solution is calculated, described
Second formula is as follows: A2=A-A1；
S2.3 brings the animals and plants oils absorbance A 2 into third formula and animals and plants oils concentration in solution is calculated
CAnimals and plants oils, the third formula is as follows: CAnimals and plants oils=a2*A2；
S3 is by the petroleum-type concentration CPetroleum-typeWith the animals and plants oils concentration CAnimals and plants oilsIt brings the 4th formula into and obtains solution
Interior total oil concentration CAlways, the 4th formula is as follows: CAlways=CPetroleum-type+CAnimals and plants oils。
Experimental record
One, petroleum standard specimen
Oil ga(u)ge sample concentration: 1000mg/L
Use liquid oil: 20 times of standard sample dilution are 50mg/L
The standard liquid that liquid will be used to be diluted to 2.5mg/L, 5mg/L, 10mg/L, 15mg/L, 20mg/L concentration respectively again.
Oil sample calibration result:
| 0 | 1 | 2 | 3 | 4 | 5 | |
| L luminous intensity | 321 | 274 | 232 | 174 | 130 | 98 |
| A absorbance | 0 | 0.069 | 0.141 | 0.266 | 0.393 | 0.515 |
| D standard liquid concentration | 0 | 2.5 | 5 | 10 | 15 | 20 |
Curve: Y=Ax+b
A=38.924194 b=-0.228512 r=0.999705
Linear preferably to measure standard liquid, resultant error can be applied less than 2%.
The measurement of two, peanut oil
N-hexane: 30ml
Oily weight: 131mg
Oil concentration: 4367mg/L
Oil is diluted:
No. 1 25 times of 175mg/L
No. 2 12.5 times of 349mg/L
No. 3 10 times of 437mg/L
Measurement result:
The measurement of three, corn oils
N-hexane: 30ml
Oily weight: 35.9mg
Oil concentration: 1197mg/L
Oil is diluted:
No. 14 times of 299mg/L
No. 23 times of 399mg/L
No. 32 times of 599mg/L
Measurement result:
(the new bottle T=82% of HPCL) is done with new n-hexane
N-hexane: 30ml
Oily weight: 39.4mg
Oil concentration: 1313mg/L
Oil is diluted:
No. 14 times of 328mg/L
No. 23 times of 438mg/L
No. 32 times of 656mg/L
Measurement result:
(the new bottle T=34% of ACS) is done with new n-hexane
N-hexane: 30ml
Oily weight: 46mg
Oil concentration: 1533mg/L
Oil is diluted:
No. 14 times of 383mg/L
No. 23 times of 511mg/L
No. 32 times of 766mg/L
Measurement result:
Brief summary:, linearly can be with the n-hexane of light transmittance difference, but fluctuation range is very big it is not recommended that using, such as T=82%
N-hexane fluctuation range ± 0.2mg/L, and T=34% n-hexane fluctuation range ± 0.5mg/L.The experiment of corn oil is more steady
Fixed, good linearity, the difference reason tested several times is that the oily water content (pure concentration) taken every time changes, and difference is small negligible.
The measurement of four, linseed oil
N-hexane: 30ml
Oily weight: 39.7mg
Oil concentration: 1197mg/L
Oil is diluted:
No. 14 times of 331mg/L
No. 23 times of 441mg/L
No. 32 times of 662mg/L
Measurement result:
The measurement of five, sunflower oils
N-hexane: 30ml
Oily weight: 42.2mg
Oil concentration: 1407mg/L
Oil is diluted:
No. 14 times of 352mg/L
No. 23 times of 469mg/L
No. 32 times of 703.5mg/L
Measurement result:
Renew n-hexane and cooks sunflower oil
N-hexane: 30ml
Oily weight: 21.5mg
Oil concentration: 717mg/L
Oil is diluted:
No. 14 times of 179mg/L
No. 23 times of 239mg/L
No. 32 times of 358mg/L
Measurement result:
The measurement of six, animal oil
N-hexane: 30ml
Oily weight: 40.9mg
Oil concentration: 1363mg/L
Oil is diluted:
No. 14 times of 341mg/L
No. 23 times of 454mg/L
No. 32 times of 682mg/L
Measurement result:
The measurement of petroleum-type is noiseless than more visible, and with regular standard liquid, good linearity, stable testing, error is small, is not changing
The curve is used in the case where becoming instrument.
Petroleum-type curve: y=ax+ba=38.924194b=-0.228512r=0.999705
Animals and plants oils chooses peanut oil, corn oil, linseed oil, sunflower oil, animal oil etc. and does standard sample, uses autogamy
Standard liquid, linear preferably stable testing, error is small, and several oil curves are close, and maximum differential is less than 10%, due to animals and plants oils
Standard specimen acquisition difficulty is big, considers that the purity of oil is different, and error can be ignored, and be comprehensively compared, and animals and plants oils chooses a=1056 and is
Curve.
In specification of the invention, numerous specific details are set forth.It is to be appreciated, however, that the embodiment of the present invention can be with
It practices without these specific details.In some instances, well known method, structure and skill is not been shown in detail
Art, so as not to obscure the understanding of this specification.
Finally, it should be noted that the above embodiments are only used to illustrate the technical solution of the present invention., rather than its limitations；To the greatest extent
Pipe present invention has been described in detail with reference to the aforementioned embodiments, those skilled in the art should understand that: its according to
So be possible to modify the technical solutions described in the foregoing embodiments, or to some or all of the technical features into
Row equivalent replacement；And these are modified or replaceed, various embodiments of the present invention technology that it does not separate the essence of the corresponding technical solution
The range of scheme should all cover within the scope of the claims and the description of the invention.
Claims (10)
1. the method that one kind can measure a variety of oils concentration in water simultaneously, which is characterized in that by after water sample sampling pretreatment points
For two parts: first solution of same volume and the second solution；
S1 is directed to the first solution；
S1.1 adsorbs the first solution by magnesium silicate；
The first solution after S1.2 absorption measures to obtain wherein petroleum-type absorbance A 1 by UV-VIS spectrophotometry；
S1.3 brings the petroleum-type absorbance A 1 into first formula and petroleum-type concentration C in solution is calculatedPetroleum-type, described first
Formula is as follows: CPetroleum-type=a1*A1；
S2 is directed to the second solution；
The second solution of S2.1 measures to obtain wherein total absorbance A by UV-VIS spectrophotometry；
S2.2 brings the total absorbance A into second formula and is calculated animals and plants oils absorbance A 2 in solution, and described second
Formula is as follows: A2=A-A1；
S2.3 brings the animals and plants oils absorbance A 2 into third formula and animals and plants oils concentration in solution is calculated
CAnimals and plants oils, the third formula is as follows: CAnimals and plants oils=a2*A2；
S3 is by the petroleum-type concentration CPetroleum-typeWith the animals and plants oils concentration CAnimals and plants oilsThe 4th formula is brought into obtain in solution always
Oil concentration CAlways, the 4th formula is as follows: CAlways=CPetroleum-type+CAnimals and plants oils；
A1: the absorptivity of petroleum-type standard solution；
A2: the absorptivity of vegetable and animals oils class standard solution.
2. the method according to claim 1 that a variety of oils concentration in water can be measured simultaneously, which is characterized in that solution takes
Pretreatment includes that step is successively as follows after sample: being 1. acidified；2. extracting；3. being dehydrated.
3. the method according to claim 2 that a variety of oils concentration in water can be measured simultaneously, which is characterized in that step is 1.
PH value≤2 are acidified to after sampling.
4. the method according to claim 2 that a variety of oils concentration in water can be measured simultaneously, which is characterized in that step is 2.
With the oily substance in n-hexane extraction sample.
5. the method according to claim 2 that a variety of oils concentration in water can be measured simultaneously, which is characterized in that step is 3.
It is dehydrated using anhydrous sodium sulfate.
6. the method according to claim 1-5 that can measure a variety of oils concentration in water simultaneously, feature exist
In if strength of fluid is more than measuring device range, the liquid obtained to step (3) dehydration is diluted, when reading
It need to be multiplied by diluted multiple.
7. the device that one kind can measure a variety of oils concentration in water simultaneously, which is characterized in that including detection unit, control unit
And output unit；
The detection unit, for measuring wherein petroleum-type by UV-VIS spectrophotometry to the first solution after absorption
Absorbance A 1 measures to obtain wherein total absorbance A by UV-VIS spectrophotometry to the second solution, and petroleum-type is inhaled
Luminosity A1 and total absorbance A are transmitted to control unit；
Described control unit,
Petroleum-type concentration C in solution is calculated for bringing the petroleum-type absorbance A 1 into first formulaPetroleum-type, and by petroleum
Class concentration CPetroleum-typeIt is transmitted to output unit, first formula is as follows: CPetroleum-type=a1*A1；Bring the total absorbance A into second
Animals and plants oils absorbance A 2 in solution is calculated in formula, and second formula is as follows: A2=A-A1；
It is also used to bring the animals and plants oils absorbance A 2 into third formula and animals and plants oils concentration in solution is calculated
CAnimals and plants oils, the third formula is as follows: CAnimals and plants oils=a2*A2, and by animals and plants oils concentration CAnimals and plants oilsIt is transmitted to output unit；
It is also used to the petroleum-type concentration CPetroleum-typeWith the animals and plants oils concentration CAnimals and plants oilsIt brings the 4th formula into and obtains solution
Interior total oil concentration CAlways, the 4th formula is as follows: CAlways=CPetroleum-type+CAnimals and plants oils, and by total oil concentration CAlwaysIt is transmitted to output unit；
Output unit, for showing petroleum-type concentration CPetroleum-type, animals and plants oils concentration CAnimals and plants oilsWith total oil concentration CAlways；
A1: the absorptivity of petroleum-type standard solution；
A2: the absorptivity of vegetable and animals oils class standard solution.
8. can measure the device of a variety of oils concentration in water simultaneously according to claim 7, the detection unit includes purple
Outer light source (1), colorimetric pool (5), the cuvette (3) and photoelectric sensor (4) for storing solution；
The colorimetric pool (5) is set between the ultraviolet source (1) and the photoelectric sensor (4), and the cuvette (3) is put
It is placed in the colorimetric pool；
The optical filter (2) of 225nm wavelength is additionally provided between the ultraviolet source (1) and the colorimetric pool (5)；
The light of the ultraviolet source (1) passes through the optical filter and the colorimetric pool (5) exposes to the photoelectric sensor
(4)。
9. the device according to claim 8 that a variety of oils concentration in water can be measured simultaneously, which is characterized in that the ratio
Transparent surface, bottom and the upper cover in color pond are equipped with black light-absorption layer, and the transparent surface of the colorimetric pool, which is equipped with, supplies the ultraviolet light
The window of the light disengaging in source.
10. the device according to claim 8 that a variety of oils concentration in water can be measured simultaneously, which is characterized in that described
Ultraviolet source is deuterium lamp.
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