CN102305770A - Method for quantificationally detecting olefinic-bond-containing substance - Google Patents
Method for quantificationally detecting olefinic-bond-containing substance Download PDFInfo
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- CN102305770A CN102305770A CN201110128415A CN201110128415A CN102305770A CN 102305770 A CN102305770 A CN 102305770A CN 201110128415 A CN201110128415 A CN 201110128415A CN 201110128415 A CN201110128415 A CN 201110128415A CN 102305770 A CN102305770 A CN 102305770A
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Abstract
The invention discloses a method for quantificationally detecting an olefinic-bond-containing substance. The method comprises the following steps of: oxidizing an olefinic bond into vicinal diol by using potassium permanganate which is taken as an oxidant, wherein the potassium permanganate is reduced and an absorption value of the potassium permanganate at the wavelength of 546nm is reduced at the same time; and calculating the content of the olefinic-bond-containing substance by the reduced absorbance by measuring an absorption value of reacted potassium permanganate solution at the wavelength of 546nm. By the method, the total amount of the olefinic-bond-containing substance can be truly showed, and only the approximate total amount of concentration integral of the olefinic-bond-containing substance is obtained by integral-based chromatography; and the sampling can be performed every several hours according to the actual demand and is more convenient and quicker than the sampling which is performed every several minutes by the traditional chromatography.
Description
Technical field
The present invention relates to a kind of quantitative detecting method that contains the ethylene linkage material.
Technical background
Olefinic double bonds is present in multiple native compound and the active component, and these compounds are important platform chemicals and are widely used in multiple field.Utilizing reproducible biomass material to come alkene such as biosynthesizing isoprene, ethene, styrene oxide is a present research focus.Because the complicacy of bioprocesses needs to create a kind of suitable analytical approach and comes these bio-based chemicals are carried out quantitatively, thereby parameters such as the output of sweat, productive rate, production intensity there is an evaluation preferably.At present to containing the ethylene linkage material, mainly contain high performance liquid chromatography (HPLC), vapor-phase chromatography (GC) such as the analytical approach of isoprene, these methods isoprene concentration of liquid towards or gaseous state are delicately measured.But the isoprene concentration in that the different phase of aerobic fermentation produces is very inequality, and the total amount that chromatography is measured isoprene in the sweat is to measure isoprene concentration through every at a distance from a few minutes, and last integration draws total amount.The frequent sampling of needs when this just must cause chromatography to survey the isoprene total production, complex operation, and chromatography itself also has the sample preparation trouble, measurement shortcoming such as cost an arm and a leg.In view of chromatographic these inferior positions, the isoprene output of utilizing traditional AAS to measure in the fermentation tail gas is a kind of more convenient, accurate, inexpensive method.
Summary of the invention
The object of the present invention is to provide a kind of to containing the quantitative detecting method of ethylene linkage material.
For realizing above-mentioned purpose, the quantitative detecting method that contains the ethylene linkage material provided by the invention is oxidized to adjacent glycol to ethylene linkage with potassium permanganate as oxygenant, and potassium permanganate is reduced simultaneously, reduces in the 546nm absorption value; Through measuring the absorption value of reacted liquor potassic permanganate, calculate the content that contains the ethylene linkage material with the absorbance that reduces at 546nm.
The said quantitative detecting method that contains the ethylene linkage material, wherein, the calculating that contains the ethylene linkage content of material is:
1) standard solution that contains the ethylene linkage material with variable concentrations adds in the liquor potassic permanganate, is mixed with the potassium permanganate standard solution that contains the ethylene linkage material of series concentration gradient, measures the absorption value of this potassium permanganate standard solution at 546nm; The ethylene linkage material concentration that contains with each adding is the X axle, and corresponding absorption value is done typical curve for the Y axle and drawn regression equation;
2) will contain the ethylene linkage material and add the potassium permanganate standard solution, measure the 546nm absorption value, bring this absorption value into content that said regression equation obtains containing in the sample ethylene linkage material.
The said quantitative detecting method that contains the ethylene linkage material, wherein, step 1 and step 2 are to measure getting supernatant behind the solution dilution.
The said quantitative detecting method that contains the ethylene linkage material, wherein, rare multiple is 15-20 times.
The said quantitative detecting method that contains the ethylene linkage material, wherein, this contains the ethylene linkage material and comprises: liquid isoprene, gaseous state isoprene, cyclohexene, styrene, cinnamic acid, cinnamic acid, styron etc.
Advantage of the present invention is:
1, can really embody the total amount that contains the ethylene linkage material, and based on the chromatography of integration just to containing the approximate total amount that ethylene linkage material concentration integration obtains.
2, the present invention only needs according to the actual requirements in measuring sweat, and sampling in every separated several hours gets final product, and is every more convenient at a distance from a few minutes sampling than traditional chromatography.
3, instrument that chromatography is relevant and consumptive material are relatively more expensive, and the reagent such as potassium permanganate that the present invention uses are dirt cheap.
In a word, the present invention is more suitable for measuring and contains ethylene linkage material output, productive rate and correlation parameter during the fermentation, to optimizing sweat and technology a useful instrument is provided.
Embodiment
Technical scheme of the present invention is:
Be oxidized to adjacent glycol to ethylene linkage with potassium permanganate as oxygenant, potassium permanganate is reduced simultaneously, reduces in 546nm characteristic optical absorption value.Through measuring the characteristic absorption value of reacted liquor potassic permanganate, calculate the content that contains the ethylene linkage material with the characteristic absorption value that reduces at 546nm.
Quantitative detecting method step of the present invention is following:
1) standard solution that contains the ethylene linkage material of configuration series concentration gradient, as: 5,10,20,30,40,60,80,120,160,240,320mg/l.
2) configuration potassium permanganate standard solution, potassium permanganate concentration of standard solution be such as can being 1g/l, and regulate pH=12 with NaOH.
3) standard solution that contains the ethylene linkage material with the series concentration gradient adds liquor potassic permanganate, after the concussion mixing makes and reacts completely in the room temperature, centrifugally supernatant is diluted 15-20 doubly measures the 546nm light absorption value; The standard items concentration that contains the ethylene linkage material with each adding is the X axle, and corresponding absorption value is done typical curve for the Y axle, and linear fit draws regression equation, and the drawing standard curve.
4) measurement of sample: the ethylene linkage material that contains of getting certain volume or quality adds the potassium permanganate standard solution, 3 operates set by step, and the absorption value that obtains is brought the content that above-mentioned regression equation obtains containing in the sample ethylene linkage material into.
The present invention can be used for detecting the isoprene that produces in the sweat; The isoprene that produces in the sweat is present in the fermentation tail gas; The fermentation tail gas pipe is immersed liquor potassic permanganate, and different time point detects the liquor potassic permanganate absorbance and comes the isoprene in the sweat is carried out quantitatively.
Wherein fermentation tail gas can be used for part tail gas to measure through gas meter, and other are used for collecting.
Below through some embodiment the present invention is made and to further specify, enumerated the different ethylene linkage materials that contain among each embodiment.But need to prove; As long as can satisfy potassium permanganate ethylene linkage is oxidized to adjacent glycol; What simultaneously potassium permanganate was reduced condition contains the ethylene linkage material, all can adopt method of the present invention to carry out detection by quantitative, and the embodiment that is therefore lifted does not limit the scope of the present invention's protection.
Embodiment 1: utilize the potassium permanganate colourimetry to detect liquid isoprene sample
With the liquid isoprene sample of three concentration known (40,80,120mg/l) add respectively the potassium permanganate standard solution (1g/l, pH=12).The concussion mixing is 10 minutes in the room temperature, and above-mentioned solution after centrifugal 2 minutes of 13000rpm, is measured the 546nm light absorption value for 20 times with the supernatant dilution, according to the concentration of regression equation calculation isoprene.Each sample is done the degree of accuracy (relative standard deviation %RSD) that repeats to measure this method for 6 times.Draw the accuracy (relative error %RE) of this method through the contrast of measured value and actual value.Regression equation is: C=-359.71A+280.43 (C: detectable isoprene concentration, mg/l, 20mg/l＜C＜160mg/l; A: liquor potassic permanganate is in the absorbance at 546nm place), regression coefficient (r)=0.99931.Table 1 is accuracy and the degree of accuracy that embodiment 1 measures liquid isoprene sample.But have degree of accuracy (%RSD＜3.92) and accuracy (%RE＜2.43) preferably by table 1 knowledge capital method.
Embodiment 2: utilize the potassium permanganate colourimetry to detect the isoprene in the fermentation tail gas
The sweat temperature is 37 ℃, because the low boiling (34 ℃) of isoprene makes the isoprene that produces in the sweat evaporate into fermentation tail gas.Through gas meter 1/30 tail gas is used for measuring; The branch row tracheae is immersed the potassium permanganate standard solution; Get the 1ml liquor potassic permanganate in fermentation different time (4h, 6h, 8h, 10h, 12h, 14h, 16h, 20h, 24h, 28h, 32h, 36h, 40h, 44h, 48h); Above-mentioned solution after centrifugal 2 minutes of 13000rpm, is measured the 546nm light absorption value for 20 times with the supernatant dilution, according to the concentration of regression equation calculation isoprene.Regression equation is: C=-359.71A+280.43 (C: detectable isoprene concentration, mg/l, 20mg/l＜C＜160mg/l; A: liquor potassic permanganate is in the absorbance at 546nm place), regression coefficient (r)=0.99931.
With vapor-phase chromatography total isoprene output is analyzed (whenever surveyed concentration at a distance from 10 minutes, integration gets yield) simultaneously, and gas chromatograph (Varian 450-GC, USA): capillary column (FFAP; 25m*0.25mm*0.20 μ m; USA), flame ionization detector (FID), Sample Room and sensing chamber's temperature are 100 ℃, and column temperature is constant to be 50 ℃.
Every at a distance from four hours, calculate isoprene output (the isoprene output * 30 in the branch row tracheae) with this method, measure with vapor-phase chromatography simultaneously, and these two kinds of methods are carried out T check contrast.Table 2 is the output that embodiment 2 measures isoprene in the sweat.Can be known by table 2: actual T value is the T value of overshoot (4.303, degree of confidence 95%) not, and this is explanation just: in the sensing range of regulation, these two kinds of methods difference aspect degree of accuracy and accuracy is little.Vapor-phase chromatography needs continuous every at a distance from 10 minutes sampling and measurings, and this law only needed take a sample in per 4 hours or 2 hours.
Embodiment 3: utilize potassium permanganate colourimetry detection ring hexene
With the cyclohexene sample add the potassium permanganate standard solution (1g/l, pH=12).The concussion mixing is 10 minutes in the room temperature, and above-mentioned solution after centrifugal 2 minutes of 13000rpm, is measured the 546nm light absorption value for 20 times with the supernatant dilution, according to the concentration of regression equation calculation cyclohexene.Regression equation is: C=-671.14A+503.40 (C: detectable cyclohexene concentration, mg/l, 10mg/l＜C＜240mg/l; A: liquor potassic permanganate is in the absorbance at 546nm place), regression coefficient (r)=0.99915.
Embodiment 4: utilize the potassium permanganate colourimetry to detect styrene
With the styrene sample add the potassium permanganate standard solution (1g/l, pH=12).The concussion mixing is 10 minutes in the room temperature, and above-mentioned solution after centrifugal 2 minutes of 13000rpm, is measured the 546nm light absorption value for 20 times with the supernatant dilution, according to the cinnamic concentration of regression equation calculation.Regression equation is: C=-584.80A+442.19 (C: detectable concentration of styrene, mg/l, 10mg/l＜C＜320mg/l; A: liquor potassic permanganate is in the absorbance at 546nm place), regression coefficient (r)=0.99838.
Embodiment 5: utilize the potassium permanganate colourimetry to detect cinnamic acid
With the cinnamic acid sample add the potassium permanganate standard solution (1g/l, pH=12).The concussion mixing is 10 minutes in the room temperature, and above-mentioned solution after centrifugal 2 minutes of 13000rpm, is measured the 546nm light absorption value for 20 times with the supernatant dilution, according to the concentration of regression equation calculation cinnamic acid.Regression equation is: C=-662.25A+487.22 (C: detectable cinnamic acid concentration, mg/l, 20mg/l＜C＜400mg/l; A: liquor potassic permanganate is in the absorbance at 546nm place), regression coefficient (r)=0.99607.
Embodiment 6: utilize the potassium permanganate colourimetry to detect cinnamic acid
With the cinnamic acid sample add the potassium permanganate standard solution (1g/l, pH=12).The concussion mixing is 10 minutes in the room temperature, and above-mentioned solution after centrifugal 2 minutes of 13000rpm, is measured the 546nm light absorption value for 20 times with the supernatant dilution, according to the concentration of regression equation calculation cinnamic acid.Regression equation is: C=-393.70A+301.34 (C: detectable cinnamic acid concentration, mg/l, 10mg/l＜C＜160mg/l; A: liquor potassic permanganate is in the absorbance at 546nm place), regression coefficient (r)=0.99711.
Embodiment 7: utilize the potassium permanganate colourimetry to detect styron
With the styron sample add the potassium permanganate standard solution (1g/l, pH=12).The concussion mixing is 10 minutes in the room temperature, and above-mentioned solution after centrifugal 2 minutes of 13000rpm, is measured the 546nm light absorption value for 20 times with the supernatant dilution, according to the concentration of regression equation calculation styron.Regression equation is: C=-431.03A+336.78 (C: detectable styron concentration, mg/l, 5mg/l＜C＜240mg/l; A: liquor potassic permanganate is in the absorbance at 546nm place), regression coefficient (r)=0.99949.
Table 1
Table 2
Claims (5)
1. a quantitative detecting method that contains the ethylene linkage material is oxidized to adjacent glycol to ethylene linkage with potassium permanganate as oxygenant, and potassium permanganate is reduced simultaneously, reduces in the 546nm absorption value; Through measuring the absorption value of reacted liquor potassic permanganate, calculate the content that contains the ethylene linkage material with the absorbance that reduces at 546nm.
2. according to the said quantitative detecting method that contains the ethylene linkage material of claim 1, wherein, the calculating that contains the ethylene linkage content of material is:
1) standard solution that contains the ethylene linkage material with variable concentrations adds in the liquor potassic permanganate, is mixed with the potassium permanganate standard solution that contains the ethylene linkage material of series concentration gradient, measures the absorption value of this potassium permanganate standard solution at 546nm; The ethylene linkage material concentration that contains with each adding is the X axle, and corresponding absorption value is done typical curve for the Y axle and drawn regression equation;
2) will contain the ethylene linkage material and add the potassium permanganate standard solution, measure the 546nm absorption value, bring this absorption value into content that said regression equation obtains containing in the sample ethylene linkage material.
3. according to the said quantitative detecting method that contains the ethylene linkage material of claim 1, wherein, step 1 and step 2 are to measure getting supernatant behind the solution dilution.
4. according to the said quantitative detecting method that contains the ethylene linkage material of claim 3, wherein, rare multiple is 15-20 times.
5. according to the said quantitative detecting method that contains the ethylene linkage material of claim 1, wherein, this contains the ethylene linkage material and comprises: liquid isoprene, gaseous state isoprene, cyclohexene, styrene, cinnamic acid, cinnamic acid, styron.
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| JP2012215440A (en) * | 2011-03-31 | 2012-11-08 | Tokyo Gas Co Ltd | Method and device to detect cyclohexene in fuel gas |
| CN103808715A (en) * | 2013-10-12 | 2014-05-21 | 苏州金宏气体股份有限公司 | Method for rapidly detecting content of unsaturated hydrocarbon in industrial ammonia gas |
| CN104502521A (en) * | 2014-12-16 | 2015-04-08 | 苏州金宏气体股份有限公司 | Method for detecting contents of total olefin hydrocarbon and total alkyne in natural gas |
| CN110736711A (en) * | 2019-09-16 | 2020-01-31 | 南京趣酶生物科技有限公司 | Detection method for preparation process of R- (+) -3- (dimethylamino) -1- (2-thienyl) -1-propanol |
| CN112557312A (en) * | 2020-11-04 | 2021-03-26 | 浙江工业大学 | Spectrophotometry for detecting olefine acid |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2012215440A (en) * | 2011-03-31 | 2012-11-08 | Tokyo Gas Co Ltd | Method and device to detect cyclohexene in fuel gas |
| CN103808715A (en) * | 2013-10-12 | 2014-05-21 | 苏州金宏气体股份有限公司 | Method for rapidly detecting content of unsaturated hydrocarbon in industrial ammonia gas |
| CN103808715B (en) * | 2013-10-12 | 2016-05-11 | 苏州金宏气体股份有限公司 | A kind of method of unsaturated hydrocarbons content in fast detecting industry ammonia |
| CN104502521A (en) * | 2014-12-16 | 2015-04-08 | 苏州金宏气体股份有限公司 | Method for detecting contents of total olefin hydrocarbon and total alkyne in natural gas |
| CN104502521B (en) * | 2014-12-16 | 2017-05-10 | 苏州金宏气体股份有限公司 | Method for detecting contents of total olefin hydrocarbon and total alkyne in natural gas |
| CN110736711A (en) * | 2019-09-16 | 2020-01-31 | 南京趣酶生物科技有限公司 | Detection method for preparation process of R- (+) -3- (dimethylamino) -1- (2-thienyl) -1-propanol |
| CN112557312A (en) * | 2020-11-04 | 2021-03-26 | 浙江工业大学 | Spectrophotometry for detecting olefine acid |
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Application publication date: 20120104 |