CN103257137A - Method of determining content of methyl ethyl ketone peroxide in workplace air through UV spectrophotometer - Google Patents
Method of determining content of methyl ethyl ketone peroxide in workplace air through UV spectrophotometer Download PDFInfo
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- CN103257137A CN103257137A CN2012100356089A CN201210035608A CN103257137A CN 103257137 A CN103257137 A CN 103257137A CN 2012100356089 A CN2012100356089 A CN 2012100356089A CN 201210035608 A CN201210035608 A CN 201210035608A CN 103257137 A CN103257137 A CN 103257137A
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- ethyl ketone
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Abstract
The invention relates to a method of determining content of methyl ethyl ketone peroxide in workplace air through UV spectrophotometer. The method comprises absorbing the methyl ethyl ketone peroxide in the air by using an absorption tube with fillers, putting the adsorbent into glacial acetic acid for analyzing, performing ultrasonic vibration, adding 4-isobutyl catechol for chromogenic reaction, and performing colorimetric determination at a wavelength of 395 nm through the spectrophotometer, wherein shades of colors is in direct proportion with concentrations of the methyl ethyl ketone peroxide. The method can eliminate interferences of styrene, acetone, dimethyl phthalate, etc. collected in the samples, and has a detection limit being up to 0.05 mg/m<3> and being far lower than a limit of 1.5 mg/m<3> required by American Government Industrial Hygienists (ACGIH). Therefore, the method provided by the invention provides a reliable and conveniently-implemented method for detecting the content of the methyl ethyl ketone peroxide in the workplace air, and can meet requirements of environmental monitoring, occupational health testing, and factory production.
Description
Technical field
The present invention relates to a kind of method of measuring methyl ethyl ketone peroxide content in the workplace air by ultraviolet spectrophotometer, particularly relating to No. 2 solid adsorbent of a kind of utilization activated bauxite adsorbs, the glacial acetic acid desorption, 4-isobutyl catechol (4-TBC) colour developing, ultraviolet spectrophotometer carries out method for measuring to methyl ethyl ketone peroxide in the workplace.
Background technology
Methyl ethyl ketone peroxide (claiming methylethyl ketone peroxide liquid again, catalyzer M) belongs to ketone peroxide.It is unsaturated polyester resin most widely used initiating agent in the world.Methyl ethyl ketone peroxide produce and use in all can produce injury to skin and respiratory tract, bring certain threat to exposed population group healthy.
Abroad the detection method to methyl ethyl ketone peroxide mainly is to adopt fluorophotometric method, vapor-phase chromatography, liquid phase chromatography and paper chromatography etc.But because such peroxidating material has thermal instability and be difficult for volatile characteristics, thereby vapor-phase chromatography can not get better application, and the methyl ethyl ketone peroxide of lower content generally uses visible spectrophotometry or liquid phase chromatography to detect.
At present, China does not have corresponding standard method to methyl ethyl ketone peroxide, the research of the detection of this aspect simultaneously is also less, according to foreign method, large-scale expensive instruments such as use liquid chromatography detect, can bring certain burden to enterprise undoubtedly, also make the detection of this material be subjected to certain restriction, thereby to set up a kind of simple assay method that is suitable for be very necessary.Utilize the method for the mensuration methyl ethyl ketone peroxide of visible spectrophotometer both can fill up the blank that China does not have related detecting method, can satisfy the needs that this material detects again.
Summary of the invention
The present invention is to provide a kind of with methyl ethyl ketone peroxide in No. 2 solid adsorbent absorbed airs of the activated bauxite sample, glacial acetic acid carries out desorb, add developer 4-isobutyl catechol and develop the color, measure the method for methyl ethyl ketone peroxide content in the workplace air by ultraviolet-visible pectrophotometer.
1 principle
Solid alumina has suction-operated preferably to airborne methyl ethyl ketone peroxide, use glacial acetic acid can resolve the methyl ethyl ketone peroxide that is adsorbed in the aluminium oxide fully, add 4-isobutyl catechol (4-TBC) and generate light yellow benzoquinones with methyl ethyl ketone peroxide.Benzoquinones is that 395nm has maximum absorbance at wavelength.
2 reagent and material
Except as otherwise herein provided, it is pure that all reagent are analysis, and experimental water is ultrapure water.
2.1 glacial acetic acid is analyzed pure;
2.2 repefral is analyzed pure;
2.34-isobutyl catechol colour developing liquid: take by weighing 3g isobutyl catechol and put into the 250mL beaker, add an amount of glacial acetic acid dissolving, be settled to 100mL;
2.4 methyl ethyl ketone peroxide (MEKP), top grade is pure;
2.5 methyl ethyl ketone peroxide (MEKP) standard reserving solution (1.00mg/mL): accurately take by weighing the pure methyl ethyl ketone peroxide of top grade (MEKP) 0.0100g, be settled to 10.00mL with phthalic ester
2.6 methyl ethyl ketone peroxide (MEKP) standard serial solution: preparation methyl ethyl ketone peroxide (MEKP) standard series, methyl ethyl ketone peroxide (MEKP) concentration is: 0.0,0.1,0.2,0.5,1.0,1.5 μ g/mL.
3 instrument and equipments
3.1 ultraviolet-visible pectrophotometer: be furnished with 1cm light path cuvette;
3.2 high pressure steam pot: temperature can be set to 95 ± 2 ℃;
3.3 ultrasonic oscillator;
3.4 filling material is the sampling pipe of aluminium oxide.
4 sample collection and preservations
4.1 sampling flow is 0.25L/min, the series connection of two absorption tubes is gathered, and sampling time and detection limit see Table 1.
4.2 after the sample sampling, seal aluminium oxide collection tube two ends immediately, put transportation and preservation in the cleaning container.
Sample at room temperature can be preserved 24h.
Table 1: gather flow, time and detection limit
5 measure
5.1 control test: sampling pipe is brought to the scene, gather the air sample except not connecting sampling thief, all the other operate same sample, as the blank of sample.
5.2 sample preparation: the alumina filled material of front and back section that will adopt sample is poured into respectively in the solvent desorption bottle, each adds the 2.00mL glacial acetic acid, after the sealing, room temperature is placed 30min, ultrasonic jolting 5min then, then use glass wool to filter desorbed solution, get the stripping liquid 1.0mL after the filtration, add 1.0mL4-isobutyl catechol colour developing liquid.Put into pressure cooker 30min, the pressure cooker temperature remains on 95 ± 2 ℃.Cool in the room temperature behind the taking-up sample, shake up, for measuring.If the concentration of determinand surpasses measurement range in the stripping liquid, the blank solution dilution back after the available colour developing is measured, and multiply by extension rate during calculating.
5.3 the drafting of typical curve: to methyl ethyl ketone peroxide (MEKP) standard serial solution (2.6), add the alumina filled material (consumption and sample are gathered consistent) with same batch of sampling respectively.Processing mode is carried out according to 5.2.Measure absorbance under the 395nm wavelength, each concentration replication 3 times is with content (μ g/mL) the drawing standard curve of absorbance average to methyl ethyl ketone peroxide
5.4 sample determination: with operating conditions working sample and the blank desorbed solution of bioassay standard series.The sample absorbance that records deducts the blank absorbance, is calculated the content (μ g/mL) of methyl ethyl ketone peroxide by typical curve.
6 results calculate
In the formula: the concentration of methyl ethyl ketone peroxide in the C-air, mg/m
3
M-records the concentration of methyl ethyl ketone peroxide in the desorbed solution, μ g/mL;
V-standard sample volume, L;
The dilution of f-sample.
Embodiment
Embodiment: the detection of methyl ethyl ketone peroxide in the air
A) in a plastics-production processing enterprise, carry out, in the factory building of ordinary production, select identical sampled point to place 3 KB-6E atmosphere sampling instruments.Two gas circuits of every KB-6E, each gas circuit connects the aluminium oxide sampling pipe of 2 series connection, and the sampling flow velocity is 0.25L/min, and the sampling time is 4h.
B) preparation of working curve
Methyl ethyl ketone peroxide (MEKP) standard series, methyl ethyl ketone peroxide (MEKP) concentration is: 0.0,0.1,0.2,0.5,1.0,1.5 μ g/mL.Add respectively with the activated bauxite inserts (consumption and sample are gathered consistent) of same batch of sampling and respectively add the 2.00mL glacial acetic acid, after the sealing, room temperature is placed 30min, ultrasonic jolting 5min then, then use glass wool to filter desorbed solution, get the stripping liquid 1.0mL after the filtration, add 1.0mL 4-isobutyl catechol colour developing liquid.Put into pressure cooker 30min, the pressure cooker temperature remains on 95 ± 2 ℃.Cool in the room temperature behind the taking-up sample, shake up, sentencing glacial acetic acid at wavelength 395nm is that reference is measured, and the light absorption value of its respective concentration correspondence sees Table 1.
Table 1
C) sample determination
Activated bauxite inserts in two sections sampling pipes of sampling back series connection is poured into respectively in the solvent desorption bottle.According to b) sequence of operation carries out.
1. measurement result:
In the parallel sample of six collections methyl ethyl ketone peroxide content by formula (1) calculate.Record:
| 1 | 2 | 3 | 4 | 5 | 6 | |
| Light absorption value A | 0.4684 | 0.4275 | 0.4476 | 0.4578 | 0.4712 | 0.4376 |
| Concentration (μ g/mL) | 0.5836 | 0.5266 | 0.5546 | 0.5688 | 0.5875 | 0.5406 |
| Extension rate f | 10 | 10 | 10 | 10 | 10 | 10 |
| Calibration sampling volume (L) | 61.8 | 62.4 | 61.4 | 65.7 | 62.2 | 60.7 |
| MEKP concentration (mg/m 3) | 0.19 | 0.17 | 0.18 | 0.17 | 0.19 | 0.18 |
The precision of 2 measurement results:
The precision of methyl ethyl ketone peroxide in the parallel sample of six collections:
Obviously, those of ordinary skill in the art can constitute methyl ethyl ketone peroxide Determination on content method with the present invention by the assay method of ultraviolet-visible pectrophotometer to methyl ethyl ketone peroxide in the workplace air.
Above-described embodiment is only for the usefulness that the present invention is described; and be not to be limitation of the present invention; the those of ordinary skill in relevant technologies field; without departing from the present invention; can also make a variety of changes and modification; therefore all technical schemes that are equal to also should belong to category of the present invention, and scope of patent protection of the present invention should be limited by each claim.
Claims (5)
1. the mensuration of methyl ethyl ketone peroxide in the workplace air is characterized in that, described assay method comprises the steps:
1. absorption: carry out on-the-spot sample collecting with the absorption tube that filling agent is housed, by atmosphere sampling instrument, methyl ethyl ketone peroxide is adsorbed in the filling agent alumina adsorption pipe, and low temperature is preserved transportation;
2. resolve: under the laboratory condition, collect the filling agent activated bauxite in the sampling pipe, add the 2.00mL glacial acetic acid and resolve, bottle is resolved in sealing, and room temperature is placed 30min, and ultrasonic jolting 5min uses glass wool to filter desorbed solution then;
3. colour developing: get the desorbed solution 1mL after the filtration, add 1mL developer 4-isobutyl catechol (4-TBC) and develop the color, put into the high compressed steam pot and be heated to 95 ± 2 ℃ and keep 30min, fully reaction solutions;
4. extract reaction solution with colorimetric pool in, be the colorimetric estimation of 395nm punishment light luminosity at wavelength.
According to the described yard air of claim 1 in the assay method of methyl ethyl ketone peroxide, it is characterized in that: described step 1. in, carry out on-the-spot sample collecting with the absorption tube that filling agent is housed, filling agent is No. 2, activated bauxite;
According to the described yard air of claim 1 in the assay method of methyl ethyl ketone peroxide, it is characterized in that: described step 2. in, adopt the 2.00mL glacial acetic acid to resolve.
According to the described yard air of claim 1 in the assay method of methyl ethyl ketone peroxide, it is characterized in that: described step 3. in, developer adopts 4-isobutyl catechol (4-TBC) to develop the color, and puts into the high compressed steam pot and is heated to 95 ± 2 ℃ of maintenance 30min.
5. according to the assay method of methyl ethyl ketone peroxide in the described workplace air of claim 1, it is characterized in that: measuring wavelength in described step in 4. is 395nm.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105823741A (en) * | 2016-03-11 | 2016-08-03 | 山东省化工研究院 | Air for detecting content of butyraldehyde in air |
| CN106908548A (en) * | 2017-03-30 | 2017-06-30 | 浙江中检测研究院股份有限公司 | The detection method of carboxylic acid content in a kind of air |
| CN114002346A (en) * | 2021-10-21 | 2022-02-01 | 国网吉林省电力有限公司电力科学研究院 | Method for detecting methyl ethyl ketone peroxide in air of workplace |
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| RU2217745C2 (en) * | 2002-01-25 | 2003-11-27 | Военный университет радиационной, химической и биологической защиты | Method of quantitative determination of cyanides |
| CN1603822A (en) * | 2004-11-03 | 2005-04-06 | 山西大学 | Method for detecting phosphate radical in blood |
| CN1865925A (en) * | 2006-05-26 | 2006-11-22 | 山西大学 | Method for detecting inorganic phosphorus in milk |
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2012
- 2012-02-17 CN CN2012100356089A patent/CN103257137A/en active Pending
Patent Citations (3)
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| RU2217745C2 (en) * | 2002-01-25 | 2003-11-27 | Военный университет радиационной, химической и биологической защиты | Method of quantitative determination of cyanides |
| CN1603822A (en) * | 2004-11-03 | 2005-04-06 | 山西大学 | Method for detecting phosphate radical in blood |
| CN1865925A (en) * | 2006-05-26 | 2006-11-22 | 山西大学 | Method for detecting inorganic phosphorus in milk |
Non-Patent Citations (1)
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| PIRKKO PFÄFFLI: "Determination of airborne methyl ethyl ketone peroxide", 《FRESENIUS J ANAL CHEM.》 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105823741A (en) * | 2016-03-11 | 2016-08-03 | 山东省化工研究院 | Air for detecting content of butyraldehyde in air |
| CN105823741B (en) * | 2016-03-11 | 2018-05-15 | 青岛科技大学 | The detection method of butyraldehyde content in a kind of air |
| CN106908548A (en) * | 2017-03-30 | 2017-06-30 | 浙江中检测研究院股份有限公司 | The detection method of carboxylic acid content in a kind of air |
| CN106908548B (en) * | 2017-03-30 | 2019-07-12 | 浙江中一检测研究院股份有限公司 | The detection method of carboxylic acid content in a kind of air |
| CN114002346A (en) * | 2021-10-21 | 2022-02-01 | 国网吉林省电力有限公司电力科学研究院 | Method for detecting methyl ethyl ketone peroxide in air of workplace |
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Address after: 100080, room 205, Ying Zhi building, 49-3 Suzhou Street, Beijing, Haidian District Applicant after: Spectrum Buddhist nun tests Group Plc Address before: 100080, Beijing, Suzhou Street, Haidian District No. 49-3 Ying Chi Building, 11 floor Applicant before: PONY Test Co. |
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