CN103575692B - A kind of infrared spectrum analysis containing organic fluid sample - Google Patents
A kind of infrared spectrum analysis containing organic fluid sample Download PDFInfo
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- CN103575692B CN103575692B CN201210273810.5A CN201210273810A CN103575692B CN 103575692 B CN103575692 B CN 103575692B CN 201210273810 A CN201210273810 A CN 201210273810A CN 103575692 B CN103575692 B CN 103575692B
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Abstract
The invention provides a kind of infrared spectrum analysis containing organic fluid sample, the method comprises: by containing the organism load in organic fluid sample on microporous barrier, described microporous barrier comprises matrix and grafting at least one grafted moiety on the matrix, described matrix is tygon, polypropylene or ethylene-propylene copolymer, and described grafted moiety is selected from the group shown in the group shown in formula I and formula II; Load there is described organic microporous barrier to be placed in infrared spectrometer and carry out Infrared spectroscopy.Method of the present invention is provide a kind of new infrared spectrum sample preparation and analytical approach containing organic fluid sample, and when analyzing moisture and organic fluid sample, effectively can deduct the interfere information that the water in sample produces, improve validity and the accuracy of Infrared spectroscopy, be applicable to analyze various moisture and organic fluid sample, particularly rapid screening carried out to the organism in sewage.
Description
Technical field
The present invention relates to a kind of infrared spectrum analysis containing organic fluid sample.
Background technology
Near-infrared spectrum technique (FT-NIR) is the high-new analytical technology of one in recent years developed rapidly, have easy, quick, low cost, pollution-free, to sample without destruction and can the advantages such as simultaneous determination of multiponents be realized.Near infrared light is the electromagnetic wave of a kind of wavelength within the scope of 780-2526nm, near infrared spectrum is owing to producing when the anharmonicity of molecular vibration makes molecular vibration from ground state to high level transition, mainly reflecting the information of the chemical bonds such as C-H, O-H, N-H and S-H.Can the compound and composition thereof of the most kind of Fast Measurement by near infrared spectroscopic method, and the mensuration of the organic sample to nearly all states of matter can be realized.
But in the near infrared spectrum qualitative and quantitative analysis of Aquo System, the near infrared absorption of water is far longer than the absorption of other test substance, aquagenic interfere information significantly can reduce the precision of near-infrared spectrum analysis.
Therefore, in the near-infrared spectrum analysis of water-bearing organic sample, how to deduct difficult point and emphasis that the interfere information caused by water becomes the breakthrough of near-infrared spectral analysis technology needs.
In addition, for Infrared spectroscopy, suitable method for making sample is the key that Infrared spectroscopy obtains correct information.At present, when carrying out Infrared spectroscopy to fluid sample, normally testing liquid sample being contained in sample cell and carrying out liquid phase Infrared spectroscopy, but the bubble in the thickness of sample cell and sample also can have an impact to analysis result.
Summary of the invention
The object of the present invention is to provide a kind of infrared spectrum analysis containing organic fluid sample, the method by the organism load in sample on microporous barrier, this load there is organic microporous barrier to be measured to be placed in infrared spectrometer analysis, be not only fluid sample and provide a kind of new method for making sample and infrared spectrum analysis; And when analyzing aqueous specimen, Infrared spectroscopy is carried out after dewatering by load there being organic microporous barrier, can effectively deduct the interfere information caused by water, overcome existing near-infrared spectrum analysis to be difficult to deduct the interfere information caused by water, and then the very difficult deficiency that aqueous specimen is analyzed.
The invention provides a kind of infrared spectrum analysis containing organic fluid sample, the method comprises the following steps:
(1) by containing the organism load in organic fluid sample on microporous barrier, described microporous barrier comprises matrix and grafting at least one grafted moiety on the matrix, described matrix is tygon, polypropylene or ethylene-propylene copolymer, described grafted moiety is selected from the group shown in the group shown in formula I and formula II
In formula I, R
1for C
8-C
20straight or branched alkyl;
In formula II, R
2and R
3be hydrogen or C separately
1-C
20straight or branched alkyl; And
(2) load there is described organic microporous barrier to be placed in infrared spectrometer and carry out Infrared spectroscopy.
Be provide a kind of new infrared spectrum sample preparation and analytical approach containing organic fluid sample according to method of the present invention.
In a preferred embodiment of the invention, when also containing water containing organic fluid sample, by by the organism load in this fluid sample on microporous barrier, and the water removed on microporous barrier, effectively can deduct the interfere information that the water in sample produces, thus validity and the accuracy of the Infrared spectroscopy of moisture and organic fluid sample can be improved, be applicable to analyze various moisture organism, be specially adapted to carry out rapid screening to the organism in sewage.
Accompanying drawing explanation
Fig. 1 is the near infrared light spectrogram that the embodiment of the present invention 1 obtains.
Fig. 2 is the first derivative spectrum figure that the embodiment of the present invention 1 obtains.
Fig. 3 is the near infrared light spectrogram that comparative example 1 of the present invention obtains.
Fig. 4 is the first derivative spectrum figure that comparative example 1 of the present invention obtains.
Fig. 5 is the near infrared light spectrogram that comparative example 2 of the present invention obtains.
Fig. 6 is the first derivative spectrum figure that comparative example 2 of the present invention obtains.
Fig. 7 is the near infrared light spectrogram that the embodiment of the present invention 2 obtains.
Fig. 8 is the first derivative spectrum figure that the embodiment of the present invention 2 obtains.
Embodiment
The invention provides a kind of infrared spectrum analysis containing organic fluid sample, the method comprise by containing the organism load in organic fluid sample on microporous barrier.
According to method of the present invention, described microporous barrier comprises matrix and grafting at least one grafted moiety on the matrix, described matrix is tygon, polypropylene or ethylene-propylene copolymer, and described grafted moiety is selected from the group shown in the group shown in formula I and formula II
In formula I, R
1for C
8-C
20straight or branched alkyl, such as: can be dodecyl, myristyl, cetyl, octadecyl or eicosyl;
In formula II, R
2and R
3be hydrogen or C separately
1-C
20straight or branched alkyl; Preferably, R
2and R
3be hydrogen or C separately
8-C
20straight or branched alkyl; More preferably, R
2for hydrogen, R
3for C
8-C
20straight or branched alkyl; Further preferably, R
2for hydrogen, R
3for C
8-C
12straight or branched alkyl.
The conventional various methods in this area can be adopted to be connected on matrix by described grafted moiety.Such as can by using matrix described in radiation exposure, form free radical on the matrix as activated centre, and acrylic acid is contacted with the activated centre on described matrix, with by free radical reaction by acrylic acid-grafted on described matrix, then by the matrix after grafting and R
1oH and/or
contact, to carry out esterification and/or amidation process, thus obtains the grafted moiety shown in formula I and/or formula II.
The present invention is not particularly limited with the kind of the ray producing activated centre for irradiating described matrix, the various rays that the polymer chain of tygon, polypropylene or ethylene-propylene copolymer can be made to produce free radical can commonly used for this area, such as: alpha ray, β ray, gamma-rays, x-ray or electron beam, gamma-rays is preferably.Suitable selection can be carried out according to the content of the grafted moiety on the matrix of expection with time of matrix described in radiation exposure, be as the criterion can guarantee that the content of the grafted moiety on the matrix that finally obtains can meet the demands.Usually, the time of irradiation can be 1 minute to 1 hour, is preferably 5 minutes to 30 minutes.
Can under normal conditions by acrylic acid and the substrate contact with activated centre, thus by acrylic acid-grafted on described matrix.Usually, can, at 40-80 DEG C, by acrylic acid and the activated substrate contact of described tool, the activated centre on the C=C in acrylic molecules structure and described matrix be reacted, thus by acrylic acid-grafted on described matrix.
The present invention is not particularly limited for the condition of described esterification and amidation process, carry out, as long as can guarantee that the content of microporous barrier Chinese style I and the grafted moiety shown in formula II finally obtained can meet actual requirement under the condition can commonly used in this area.Preferably, described esterification and described amidation process carry out under the existence of at least one dewatering agent.More preferably, described esterification and described amidation process are at N, N ' carry out under the existence of-dicyclohexylcarbodiimide, the extent of reaction of esterification and amidation process can be improved so further.
According to method of the present invention, the content of the grafted moiety in described microporous barrier can carry out suitable selection according to specific requirement.Usually, with the total amount of described microporous barrier for benchmark, the content of described matrix can be 65-99 % by weight, and the content of described grafted moiety can be 1-35 % by weight.Preferably, with the total amount of described microporous barrier for benchmark, the content of described matrix can be 70-90 % by weight, and the content of described grafted moiety can be 10-30 % by weight.
According to method of the present invention, as long as the material forming described microporous barrier meets previously described requirement, the average pore size in the hole in described microporous barrier and porosity are not particularly limited, the aperture that can have for the common microporous barrier with filtering function and porosity.
Described microporous barrier can adopt previously described material to be prepared by conventional various film build methods by conventional method, also can be commercially available.
According to method of the present invention, the various methods that this area can be adopted to commonly use by containing the organism load in organic fluid sample on described microporous barrier.Such as: can contact described with described microporous barrier containing organic fluid sample, the organism in sample is adsorbed on microporous barrier.Particularly, can make to flow through described microporous barrier containing organic fluid sample, flow through in the process of described microporous barrier described containing organic fluid sample, the described organism contained in organic fluid sample is adsorbed on microporous barrier; Also can be added drop-wise to described microporous barrier by containing organic fluid sample, the described organism contained in organic fluid sample is adsorbed on microporous barrier.
The present invention, for being not particularly limited containing the amount of organic fluid sample of contacting with described microporous barrier, is as the criterion with the requirement enabling the organic amount on the microporous barrier that finally obtains meet concrete testing tool.
Also comprise according to method of the present invention and have described organic microporous barrier to be placed in infrared spectrometer load to carry out Infrared spectroscopy.
Various types of infrared spectrometers that described infrared spectrometer can be commonly used for this area, without any restriction.Effectively can eliminate aquagenic interfere information in Infrared spectroscopy according to method of the present invention, be specially adapted to the occasion to carrying out near-infrared spectrum analysis containing water and organic fluid sample simultaneously.Therefore, described infrared spectrometer is preferably near infrared spectrometer.
Also comprise according to method of the present invention and the spectrogram that described Infrared spectroscopy obtains is converted into first derivative spectrum figure, the absorption peak in former spectrum and acromion can be shown like this, thus improve the accuracy analyzed further.The spectrogram that Infrared spectroscopy obtains by the various methods that this area can be adopted to commonly use is converted into first derivative spectrum figure, no longer describes in detail herein.
According to method of the present invention, described containing organic fluid sample can for various need to carry out Infrared spectroscopy containing organic fluid sample, such as: various be liquid organism, containing organic liquid mixture.The present invention is not particularly limited containing the organism in organic fluid sample for described, can be common various organism.Preferably, described containing containing organic fluid sample is selected from ketone based compound (as C
3-C
20ketone), benzene compounds, alkane is (as C
1-C
20straight or branched alkane), halogenated hydrocarbons is (as C
1-C
20chlorohydrocarbon, C
1-C
20bromo-hydrocarbons) and aldehyde based compound (as C
1-C
20aldehyde) in one or more organism.
Method according to the present invention is specially adapted to the occasion needing to analyze the organism in moisture and organic fluid sample, also contains water namely containing organic fluid sample.The present invention is not particularly limited for the described content containing the water in organic fluid sample, can be various content.
Described containing organic fluid sample also containing water time, also comprise according to method of the present invention and remove load and have water on described organic microporous barrier.Removing load has the condition of the water on described organic microporous barrier can carry out suitable selection according to the content of water and described organic kind.Usually, can at the temperature of 25-40 DEG C, removing load has water on described organic microporous barrier.From the angle shortening the time of dewatering further, preferably described organic microporous barrier is had to purge with at least one non-active gas to load.Described non-active gas refers to and with water, described organism and microporous barrier, chemically interactive gas does not occur, the various non-active gas can commonly used for this area, such as: described non-active gas can be selected from nitrogen and group 0 element gas (as argon gas).
Pass through the organism load for liquid on microporous barrier according to method of the present invention, make liquid determinand can carry out Infrared spectroscopy with the method identical with solid determinand.The present invention is not particularly limited for the method for carrying out Infrared spectroscopy, and that can commonly use with this area under normal conditions carries out the method that solid matter is analyzed, and is not described in detail in this.
Method according to the present invention is specially adapted to adopt near infrared spectrometer to the occasion analyzed containing the organism in organic sewage.Particularly, described containing organic fluid sample can for come from chemical industry sewage, come from the sewage of petroleum industry or come from the sewage of hospital.
The present invention is described in detail below in conjunction with embodiment and comparative example.
In following examples and comparative example, the near infrared spectrometer of use is the near infrared spectrometer that to be purchased from the model of ThermoScientificTruProcess be AntarisII, and its resolution is 8cm
-1, sweep limit is 4000-10000cm
-1, scanning times is 64 times, adopts absorption mode.Adopt TQAnalyst software that the infrared spectrogram obtained is converted into first derivative spectrum figure.
Embodiment 1-2 is for illustration of method of the present invention.
Embodiment 1
(1) aqueous acetone solution being 49.6 % by weight by 0.2 milligram of concentration is added drop-wise on microporous barrier that (be purchased from Tianjin Beaune Jie Er Science and Technology Ltd., matrix is tygon, and grafted moiety is
the content of grafted moiety is 16 % by weight, and the content of matrix is 84 % by weight); Then microporous barrier is purged 30 minutes in room temperature (being 25 DEG C) with nitrogen, thus obtain the sample for Infrared spectroscopy.
(2) sample prepared by step (1) is placed near infrared spectrometer analysis.The spectrogram obtained as shown in Figure 1.
(3) spectrogram that step (2) obtains is converted into first derivative spectrum figure, as shown in Figure 2.
Comparative example 1
(1) be placed near infrared spectrometer by being equipped with the sample cell (sample cell specification is 0.2cm × 1cm × 3cm) that concentration is the acetone of 99.2 % by weight, carry out liquid near-infrared spectrum analysis, the infrared spectrogram obtained as shown in Figure 3.
(2) spectrogram that step (1) obtains is converted into first derivative spectrum figure, as shown in Figure 4.
Comparative example 2
(1) be placed near infrared spectrometer by being equipped with the sample cell (specification is with comparative example 1) that concentration is the acetone of 49.6 % by weight, carry out liquid near-infrared spectrum analysis, the infrared spectrogram obtained as shown in Figure 5.
(2) spectrogram that step (1) obtains is converted into first derivative spectrum figure, as shown in Figure 6.
Fig. 1 and Fig. 3 and Fig. 5 is compared, Fig. 2 and Fig. 4 and Fig. 6 is compared, can find out, effectively can eliminate the interfere information in sample according to method of the present invention, can clearly observe acetone and be positioned at 5660cm
-1characteristic absorption peak.
Embodiment 2
(1) aqueous solution being the toluene of 5mg/L by 0.2 milligram of concentration is added drop-wise on microporous barrier that (be purchased from Tianjin Beaune Jie Er Science and Technology Ltd., matrix is polypropylene, and grafted moiety is
the content of grafted moiety is 25 % by weight, and the content of matrix is 75 % by weight); Then microporous barrier is purged 30 minutes in room temperature (being 25 DEG C) with nitrogen, thus obtain the sample for Infrared spectroscopy.
(2) sample prepared by step (1) is placed near infrared spectrometer analysis.The spectrogram obtained as shown in Figure 7.
(3) spectrogram that step (2) obtains is converted into first derivative spectrum figure, as shown in Figure 8.
Can clearly observe toluene from Fig. 7 and Fig. 8 and be positioned at 5760cm
-1characteristic absorption peak.
Claims (8)
1., containing an infrared spectrum analysis for organic fluid sample, the method comprises the following steps:
(1) by containing the organism load in organic fluid sample on microporous barrier, described microporous barrier comprises matrix and grafting at least one grafted moiety on the matrix, described matrix is tygon, polypropylene or ethylene-propylene copolymer, described grafted moiety is selected from the group shown in the group shown in formula I and formula II
In formula I, R
1for C
8-C
20straight or branched alkyl;
In formula II, R
2and R
3be hydrogen or C separately
1-C
20straight or branched alkyl; And
(2) load there is described organic microporous barrier to be placed in infrared spectrometer and carry out Infrared spectroscopy.
Wherein, before the method is also included in and has described organic microporous barrier to carry out Infrared spectroscopy load, removing load has water on described organic microporous barrier.
2. method according to claim 1, wherein, with the total amount of described microporous barrier for benchmark, the content of described matrix is 65-99 % by weight, and the content of described grafted moiety is 1-35 % by weight.
3. method according to claim 1 and 2, wherein, in formula II, R
2for hydrogen, R
3for C
8-C
20straight or branched alkyl.
4. method according to claim 1, wherein, described containing organic fluid sample also containing water.
5. method according to claim 1, wherein, at 25-40 DEG C, removing load has water on described organic microporous barrier.
6. method according to claim 1, wherein, the method also comprises the spectrogram obtained by described Infrared spectroscopy is converted into first derivative spectrum figure.
7. according to the method in claim 1,2 and 4-6 described in any one, wherein, described infrared spectrometer is near infrared spectrometer.
8. according to the method in claim 1,2 and 4-6 described in any one, wherein, describedly contain one or more organism be selected from ketone based compound, benzene compounds, alkane, halogenated hydrocarbons and aldehyde based compound containing organic fluid sample.
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Citations (2)
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| CN1171412A (en) * | 1996-06-19 | 1998-01-28 | 希尔斯股份公司 | Hydrophilic coating surfaces of polymeric substrates |
| CN102512999A (en) * | 2006-04-11 | 2012-06-27 | 麻省理工学院 | Fouling resistant membranes formed with polyacrylonitrile graft copolymers |
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| JP2011080013A (en) * | 2009-10-09 | 2011-04-21 | Mitsui Chemicals Inc | Fine polyolefin particles and modified fine polyolefin particles, resin composition containing them, and application of them |
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2012
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1171412A (en) * | 1996-06-19 | 1998-01-28 | 希尔斯股份公司 | Hydrophilic coating surfaces of polymeric substrates |
| CN102512999A (en) * | 2006-04-11 | 2012-06-27 | 麻省理工学院 | Fouling resistant membranes formed with polyacrylonitrile graft copolymers |
Non-Patent Citations (2)
| Title |
|---|
| Chemical and electrical characterization of virgin and protein-fouled polycarbonate track-etched membranes by FTIR and streaming-potential measurements;K.J. Kim 等;《Journal of Membrane Science》;19971231;第134卷;199-208 * |
| Flux enhancement for polypropylene microporous membrane in a SMBR by the immobilization of poly(N-vinyl-2-pyrrolidone) on the membrane surface;Hai-Yin Yu 等;《Journal of Membrane Science》;20060104;第279卷;148-155 * |
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Inventor after: Gui Ping Inventor after: He Qin Inventor after: Li Mengmeng Inventor after: Wei Jincheng Inventor after: Wang Wan Inventor after: Wang Qunjie Inventor before: Gui Ping Inventor before: He Qin Inventor before: Li Mengmeng Inventor before: Wang Wan Inventor before: Wang Qunjie |
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