CN105823741A - Air for detecting content of butyraldehyde in air - Google Patents
Air for detecting content of butyraldehyde in air Download PDFInfo
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- CN105823741A CN105823741A CN201610137888.2A CN201610137888A CN105823741A CN 105823741 A CN105823741 A CN 105823741A CN 201610137888 A CN201610137888 A CN 201610137888A CN 105823741 A CN105823741 A CN 105823741A
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Abstract
The invention belongs to the technical field of air detection, and concretely relates to a method for detecting the content of butyraldehyde in air. The detection method is realized through the following concrete steps: sampling, solvent stripping, refrigerating, centrifuging and spectrophotometer detection. A determination device spectrophotometer used in the invention has high popularity rate and low price, and effectively reduces the detection cost; the detection process is simple, and is easy to operate; and the method using combination of composite solvent stripping and low temperature refrigeration maximally improves the detection accuracy, and reduces the detection cost.
Description
Technical field
The invention belongs to air detection technical field, be specifically related to the detection method of butyraldehyde content in a kind of air.
Background technology
Butyraldehyde is moderate noxious substance, and in air, butyraldehyde has asphyxiating aldehyde smelly, and eye, respiratory mucosa are had stimulation and made
With.In workplace air, the short-time contact safe level of butyraldehyde is 10mg/m3.In accurate detection air, butyraldehyde content is to guarantor
Protect operating personnel healthy significant.The industries such as petrochemical industry, rubber, fire coal all can produce butyraldehyde, motor-vehicle tail-gas,
Cooking fume, smoke from cigarette also contain butyraldehyde.
At present, the method for butyraldehyde in air that measures mainly has gas chromatography and liquid chromatography.Wherein gas chromatography
Using thermal desorption type silica gel tube to gather, sample introduction after thermal desorption, after chromatographic column separates, flame ionization ditector detects；Liquid
Phase chromatography uses 2,4 dinitrophenyl hydrazine silica gel tube to gather, with the ultrasonic eluting of acetonitrile, after high performance liquid chromatography separates, two poles
Pipe array detector detects, and the shortcoming of prior art is as follows: (1) gas chromatography need to configure pyrolysis haustorium simultaneously, and this instrument exists
The use frequency of laboratory is the highest, causes testing cost to raise；Calibrating gas need to carry out secondary dilution before use, exists accurately
The risk that degree reduces；If the butyraldehyde concentration in stripping gas exceedes measurement range, need to measure again after being diluted with clean air, meeting
Cause measurement result on the low side.(2) the 2,4 dinitrophenyl hydrazine silica gel tube preparation process used in liquid chromatography is loaded down with trivial details, gathers effect
Rate is the highest；Diode array detector detection is the highest in the use frequency of laboratory, causes testing cost to raise.Owing to butyraldehyde should
During spectrophotometer method, preparation detection liquid, the formaldehyde in sample etc. understands interference detection results and fourth to a certain extent
Aldehyde can not resolve completely, causes testing result accuracy rate to reduce.
Summary of the invention
The present invention is the deficiency overcoming existing analysis method, it is provided that a kind of solvent-borne type silica gel tube collection, mixed solvent desorbing,
The detection method of butyraldehyde content in Air by Spectrophotometry, its detection process is simple, the instrument and equipment popularity rate used
Height, measurement result is accurately and reliably.
The technical scheme is that
The invention provides the detection method of butyraldehyde content in a kind of air, comprise the following steps:
(1) at sampled point, open solvent-borne type silica gel tube two ends and gather air sample；
(2) being respectively put in solvent desorption bottle by the silica gel in sample and blank silica gel tube, each 5.00mL ethanol-propanol that adds mixes
Bonding solvent, after closing, shakes 1min, desorbing 30min, obtains stripping liquid；
(3) stripping liquid is placed in-15 DEG C of freezing 30min, is centrifuged immediately after taking-up processing, takes supernatant；
(4) take 1.00mL supernatant in color comparison tube, add 1.0mL2,4-dinitrophenylhydrazine alcohol saturated solution and 0.05mL salt
Acid, capping plug, place 30min, cooling in 50 DEG C of water-baths, add the potassium hydroxide-ethanol solution of 5.0mL100g/L, mixing, place
After 5min, on spectrophotometer, measure absorbance.
Further, described solvent-borne type silica gel tube is the flow collection air sample with 500mL/min, and acquisition time is
30min。
Ethanol and the volume of propanol in the mixed solvent-ethanol-propanol solvent mixture used when the present invention resolves
Ratio is 92:8.
Further, in step (4), on spectrophotometer, at 480nm wavelength, measure absorbance.
The present invention utilizes mixed solvent resolve, in prior art, all use single alcohol to do when resolving molten
Agent, interacts owing to single alcohol cannot produce as the surface of surfactant molecule with silica gel, it is impossible to reach to resolve completely,
Thus affect testing result.When the present invention utilizes ethanol-propanol solvent mixture to use, propanol is except playing the work of solvent
With, what is more important can be covered in adsorbing material surface as surfactant molecule, at utmost resolves.This
Bright creativeness desorbed solution is carried out the most at low temperatures freezing, formaldehyde easily forms precipitation when low temperature, after processing by centrifugation,
Content of formaldehyde in desorbed solution can be reduced, combine mixed solvent synergism, thus improve the accuracy of detection.Additionally, this Shen
Inventor please finds through great many of experiments, changes the volume content of ethanol-propanol, and the accuracy of its testing result has dropped
Low.
Advantages of the present invention is:
(1) the determining instrument spectrophotometer popularity rate that this method uses is high, cheap, effectively reduces testing cost；
Detection process is relatively easy, simple to operate；
(2) present invention utilizes double solvents to carry out resolving associating deepfreeze, farthest improves Detection accuracy.
Detailed description of the invention
Embodiment 1
The detection method of butyraldehyde content in a kind of air, step is as follows:
(1) at sampled point, the silica gel tube two ends flow collection 30min air sample with 500mL/min is opened, by another silica gel tube
Band, to sampled point, opens silica gel tube two ends, is not connected to sampler and places 30min；
(2) being respectively put in solvent desorption bottle by the silica gel in sample and blank silica gel tube, each 5.00mL ethanol-propanol that adds mixes
Bonding solvent, after closing, shakes 1min, desorbing 30min, obtains stripping liquid；Stripping liquid is placed in-15 DEG C of freezing 30min, vertical after taking-up
I.e. it is centrifuged processing, takes supernatant；
Described ethanol is 92:8 with the volume ratio of propanol；
(3) standard solution preparation: weigh 0.0500g butyraldehyde in 100mL volumetric flask, be settled to scale with ethanol, shake up, pipette
This solution 2.00mL, in 100mL volumetric flask, is settled to scale with ethanol, shakes up, and in this solution, butyraldehyde concentration is 10 μ g/mL；
(4) drafting of standard curve: pipette 0.00mL, 0.20mL, 0.40mL, 0.60mL, 0.80mL, 1.00mL butyraldehyde mark respectively
Quasi-solution, in 6 color-comparison tubes, adds absorbing liquid to 2.0mL, is made into 0.0 μ g/mL, 2.0 μ g/mL, 4.0 μ g/mL, 6.0 μ g/
ML, 8.0 μ g/mL, 10.0 μ g/mL butyraldehyde series.In each standard series pipe, add 1.0mL2,4-dinitrophenylhydrazine-ethanol satisfy
With solution and 1 hydrochloric acid, capping plug, placing 30min in 50 DEG C of water-baths, cooling, the potassium hydroxide-ethanol adding 5.0mL100g/L is molten
Liquid, mixing, after placing 5min, on spectrophotometer, at 480nm, measure absorbance.With the absorbance that records to butyraldehyde concentration
(μ g/mL) draws standard curve, and equation of linear regression is A=0.0101c+0.0118, coefficient R2=0.9997；
(5) sample determination: take 1.00mL supernatant in color comparison tube, adds 1.0mL2,4-dinitrophenylhydrazine alcohol saturated solution
With 0.05mL hydrochloric acid, capping plug, place 30min, cooling in 50 DEG C of water-baths, add the potassium hydroxide-ethanol solution of 5.0mL100g/L, mixed
Even, after placing 5min, on spectrophotometer, measure absorbance；The absorbance recording sample solution is 0.103, and blank sample is molten
The absorbance of liquid is 0.000.
(6) look into standard curve obtaining butyraldehyde concentration in sample solution is 10.0 μ g/mL, butyraldehyde concentration in blank sample solution
It is 0.0 μ g/mL；
(7) calculating the butyraldehyde concentration in sampled point air by formula is 1.7mg/m3；
Specific formula for calculation is:
In formula: the concentration values of butyraldehyde in C air, unit is milligram every cubic metre (mg/m3)；
C measures the concentration values of butyraldehyde in sample absorbing liquid, and unit is micrograms per millilitre (μ g/mL)；
c0Measuring the concentration values of butyraldehyde in blank sample absorbing liquid, unit is micrograms per millilitre (μ g/mL)；
2.5 diluted sample multiples；
The standard sample volume of V sample.
Comparative example 1
The detection method of butyraldehyde content in a kind of air, concrete steps are essentially identical with embodiment 1, and difference is: sample
During parsing, only using ethanol single solvent, other steps are with embodiment 1.
Comparative example 2
The detection method of butyraldehyde content in a kind of air, concrete steps are essentially identical with embodiment 1, and difference is: resolve
The etoh solvent that Shi Caiyong is single, omits simultaneously and " stripping liquid is placed in-15 DEG C of freezing 30min, is centrifuged place after taking-up immediately
Reason, takes supernatant " process of this step, other steps are with embodiment 1.
Effect test
1, in blank silica gel tube, accurately add the butyraldehyde standard solution (concentration is 500 μ g/mL) of 15 μ L, be utilized respectively embodiment
1 and the method that provides of comparative example 1-2 carry out the detection of butyraldehyde content, concrete outcome is shown in Table 1.
Table 1
2, in blank silica gel tube, accurately add the butyraldehyde standard solution (concentration is 500 μ g/mL) of 15 μ L, be subsequently adding a little first
Aldehyde standard solution, the method being utilized respectively embodiment 1 and comparative example 2 offer carries out the detection of butyraldehyde content, and concrete outcome is shown in Table
2。
Table 2
3, recovery test (method accuracy test): the most accurately add different volumes butyraldehyde standard in blank silica gel tube molten
Liquid (concentration is 500 μ g/mL), the method utilizing embodiment 1 to provide measures its response rate.Determination of recovery rates the results are shown in Table/3.
Table 3
4, standard deviation (method precision) test: take 11 blank silica gel tubes, the most all add 20 μ L butyraldehyde standard solution
(concentration is 500 μ g/mL), the method provided by embodiment 1 is measured, according to the absorbance recorded and equation of linear regression,
Calculating butyraldehyde concentration, result of calculation is shown in Table 4.
Table 4 precision measurement result (n=11)
Above-mentioned specific embodiment is only to illustrate spirit of the present invention.Those skilled in the art can
Substitute in the way of described specific embodiment being made various amendment, supplements or be similar to employing.But can't be inclined
From the spirit of the present invention or surmount scope defined in appended claims.
Claims (4)
1. the detection method of butyraldehyde content in an air, it is characterised in that comprise the following steps:
(1) at sampled point, open solvent-borne type silica gel tube two ends and gather air sample；
(2) being respectively put in solvent desorption bottle by the silica gel in sample and blank silica gel tube, each 5.00mL ethanol-propanol that adds mixes
Bonding solvent, after closing, shakes 1min, desorbing 30min, obtains stripping liquid；
(3) stripping liquid is placed in-15 DEG C of freezing 30min, is centrifuged immediately after taking-up processing, takes supernatant；
(4) take 1.00mL supernatant in color comparison tube, add 1.0mL2,4-dinitrophenylhydrazine alcohol saturated solution and 0.05mL salt
Acid, capping plug, place 30min, cooling in 50 DEG C of water-baths, add the potassium hydroxide-ethanol solution of 5.0mL100g/L, mixing, place
After 5min, on spectrophotometer, measure absorbance.
Detection method the most according to claim 1, it is characterised in that described solvent-borne type silica gel tube is with 500mL/min
Flow collection air sample, acquisition time is 30min.
Detection method the most according to claim 1, it is characterised in that ethanol and third in described ethanol-propanol solvent mixture
The volume ratio of alcohol is 92:8.
Detection method the most according to claim 1, it is characterised in that in step (4), 480nm ripple on spectrophotometer
Strong point measures absorbance.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110794061A (en) * | 2019-11-14 | 2020-02-14 | 苏州新世纪检测技术服务有限公司 | Butyraldehyde automatic thermal analysis gas chromatography detection method |
| CN111257264A (en) * | 2020-03-18 | 2020-06-09 | 上海纽脉医疗科技有限公司 | Method for detecting aldehyde group content in biological tissue |
| CN112129748A (en) * | 2019-06-25 | 2020-12-25 | 内蒙古伊泰煤基新材料研究院有限公司 | Method suitable for determining carbonyl compounds in FT synthetic oil |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112129748A (en) * | 2019-06-25 | 2020-12-25 | 内蒙古伊泰煤基新材料研究院有限公司 | Method suitable for determining carbonyl compounds in FT synthetic oil |
| CN110794061A (en) * | 2019-11-14 | 2020-02-14 | 苏州新世纪检测技术服务有限公司 | Butyraldehyde automatic thermal analysis gas chromatography detection method |
| CN111257264A (en) * | 2020-03-18 | 2020-06-09 | 上海纽脉医疗科技有限公司 | Method for detecting aldehyde group content in biological tissue |
| CN111257264B (en) * | 2020-03-18 | 2023-02-28 | 上海纽脉医疗科技有限公司 | Method for detecting aldehyde group content in biological tissue |
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Inventor after: Yu Quande Inventor after: Zhao Yumei Inventor after: Qu Pengfei Inventor after: Chen Ju Inventor after: Yu Pengling Inventor after: Li Shihui Inventor after: Zhang Guiying Inventor before: Yu Pengling Inventor before: Li Shihui Inventor before: Zhao Yumei Inventor before: Qu Pengfei Inventor before: Chen Ju Inventor before: Zhang Guiying |
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Effective date of registration: 20180419 Address after: No. 53, Zhengzhou Road, North District, Qingdao, Shandong Applicant after: Qingdao University of Science & Technology Address before: 250014 Ji'nan Province, Lixia District, Shandong Province Cultural Road, No. 80 Applicant before: Chemical Inst., Shandong Prov. |
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