CN106018698A - Method for qualitatively analyzing and detecting residual micromolecule monomer components of polycarboxylate superplasticizer - Google Patents
Method for qualitatively analyzing and detecting residual micromolecule monomer components of polycarboxylate superplasticizer Download PDFInfo
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- CN106018698A CN106018698A CN201610457482.2A CN201610457482A CN106018698A CN 106018698 A CN106018698 A CN 106018698A CN 201610457482 A CN201610457482 A CN 201610457482A CN 106018698 A CN106018698 A CN 106018698A
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- polycarboxylate water
- reducer
- polycarboxylate superplasticizer
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- 229920005646 polycarboxylate Polymers 0.000 title claims abstract description 65
- 239000000178 monomer Substances 0.000 title claims abstract description 35
- 238000000034 method Methods 0.000 title claims abstract description 13
- 239000008030 superplasticizer Substances 0.000 title abstract 10
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 claims abstract description 27
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims abstract description 27
- 238000004451 qualitative analysis Methods 0.000 claims abstract description 26
- 238000001514 detection method Methods 0.000 claims abstract description 24
- 238000004458 analytical method Methods 0.000 claims abstract description 18
- 238000005033 Fourier transform infrared spectroscopy Methods 0.000 claims abstract description 12
- 239000007788 liquid Substances 0.000 claims abstract description 12
- 239000007787 solid Substances 0.000 claims abstract description 7
- 238000000576 coating method Methods 0.000 claims abstract description 5
- 239000003638 chemical reducing agent Substances 0.000 claims description 59
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 33
- 150000003384 small molecules Chemical class 0.000 claims description 28
- 229910019142 PO4 Inorganic materials 0.000 claims description 12
- 239000010452 phosphate Substances 0.000 claims description 12
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims description 11
- 238000004949 mass spectrometry Methods 0.000 claims description 10
- 239000000243 solution Substances 0.000 claims description 10
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 8
- 238000000605 extraction Methods 0.000 claims description 8
- 239000007789 gas Substances 0.000 claims description 7
- 230000029087 digestion Effects 0.000 claims description 6
- 239000007791 liquid phase Substances 0.000 claims description 6
- 239000012925 reference material Substances 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- 238000000921 elemental analysis Methods 0.000 claims description 4
- 238000001819 mass spectrum Methods 0.000 claims description 4
- 229910052757 nitrogen Inorganic materials 0.000 claims description 4
- 239000008055 phosphate buffer solution Substances 0.000 claims description 4
- DFIWJEVKLWMZBI-UHFFFAOYSA-M sodium;dihydrogen phosphate;phosphoric acid Chemical compound [Na+].OP(O)(O)=O.OP(O)([O-])=O DFIWJEVKLWMZBI-UHFFFAOYSA-M 0.000 claims description 4
- 150000001732 carboxylic acid derivatives Chemical class 0.000 claims description 3
- 239000012159 carrier gas Substances 0.000 claims description 3
- 238000007405 data analysis Methods 0.000 claims description 3
- 125000000524 functional group Chemical group 0.000 claims description 3
- 238000002290 gas chromatography-mass spectrometry Methods 0.000 claims description 3
- 230000014759 maintenance of location Effects 0.000 claims description 3
- 239000012071 phase Substances 0.000 claims description 3
- 238000001228 spectrum Methods 0.000 claims description 3
- 238000006243 chemical reaction Methods 0.000 claims description 2
- XONPDZSGENTBNJ-UHFFFAOYSA-N molecular hydrogen;sodium Chemical compound [Na].[H][H] XONPDZSGENTBNJ-UHFFFAOYSA-N 0.000 claims 1
- 238000005516 engineering process Methods 0.000 abstract description 3
- 238000002329 infrared spectrum Methods 0.000 abstract 1
- 238000005457 optimization Methods 0.000 abstract 1
- 238000004128 high performance liquid chromatography Methods 0.000 description 6
- 239000002253 acid Substances 0.000 description 3
- 150000007513 acids Chemical class 0.000 description 3
- 238000005481 NMR spectroscopy Methods 0.000 description 2
- 238000004587 chromatography analysis Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000004817 gas chromatography Methods 0.000 description 2
- 238000002347 injection Methods 0.000 description 2
- 239000007924 injection Substances 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 210000003484 anatomy Anatomy 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 239000008366 buffered solution Substances 0.000 description 1
- 239000004566 building material Substances 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 1
- 239000004568 cement Substances 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 239000004035 construction material Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 125000004435 hydrogen atom Chemical class [H]* 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000004452 microanalysis Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 230000003595 spectral effect Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
-
- 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
- G01N21/35—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
- G01N21/3577—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light for analysing liquids, e.g. polluted water
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/88—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86
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- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Biochemistry (AREA)
- Analytical Chemistry (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Spectroscopy & Molecular Physics (AREA)
- Engineering & Computer Science (AREA)
- Food Science & Technology (AREA)
- Medicinal Chemistry (AREA)
- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
Abstract
The invention discloses a method for qualitatively analyzing and detecting residual micromolecule monomer components of a polycarboxylate superplasticizer. The method comprises steps as follows: (1) a polycarboxylate superplasticizer sample is dried, a solid sample is obtained and subjected to element analysis test, element analysis data are obtained, and the variety of elements in the polycarboxylate superplasticizer sample is qualitatively analyzed; (2) the polycarboxylate superplasticizer sample is subjected to Fourier transform infrared spectroscopy scanning with a coating method, and an infrared spectrum of the polycarboxylate superplasticizer sample is obtained; (3) the polycarboxylate superplasticizer sample is extracted with ethyl acetate, and an obtained extracting solution is tested with a high-performance liquid chromatograph; (4) the polycarboxylate superplasticizer sample is extracted with acetonitrile, GC-MS (gas chromatograph-mass spectrometer) data of an obtained extracting solution are obtained with a GC-MS. The qualitative analysis and detection method is a method for qualitatively analyzing the residual micromolecule monomer components of the polycarboxylate superplasticizer and provides technical support for performance optimization and technology improvement of the polycarboxylate superplasticizer sample.
Description
Technical field
The invention belongs to construction material detection technique field, be specifically related to a kind of polycarboxylate water-reducer residual small molecule monomer group
The qualitative analysis detection method divided.
Background technology
Polycarboxylate water-reducer is a kind of concrete admixture of current building materials aspect large usage quantity, and it has the spy of a series of excellence
Property: high water-reducing rate, minimum yield and the preferable compatibility of cement etc..In the evolution of polycarboxylate water-reducer,
People are devoted to find the product that performance is more excellent, and the anatomy to its crucial unknown component is particularly important with detection.
The instrument conventional currently for the component analysis research of unknown material has: gas chromatograph, high performance liquid chromatograph, gas
Phase combined gas chromatography mass spectrometry, nuclear magnetic resonance, NMR, scanning electron microscope, transmission electron microscope, atomic force microscope etc..Instrument means make
Unknown structure obtains with functional study and develops rapidly.Polycarboxylate water-reducer is the macromolecular compound of a kind of complicated component, single
Instrument has certain limitation to the detection of its component.Component analysis to polycarboxylate water-reducer at present there is no document patent report
Road.The present invention combines elementary analysis, Fourier transform infrared spectroscopy, high performance liquid chromatography, gas chromatography combined with mass spectrometry technology
Polycarboxylate water-reducer is remained the qualitative analysis of small molecule monomer component.
Summary of the invention
It is an object of the invention to overcome prior art defect, it is provided that a kind of polycarboxylate water-reducer residual small molecule monomer component
Qualitative analysis detection method.
The concrete technical scheme of the present invention is as follows:
The qualitative analysis detection method of a kind of polycarboxylate water-reducer residual small molecule monomer component, comprises the following steps:
(1) polycarboxylate water-reducer sample is dried process, obtains its solid sample, the solid sample of gained is carried out
Elementary analysis is tested, and obtains its Elemental analysis data, and qualitative analysis goes out the element kind in polycarboxylate water-reducer sample, above-mentioned
The digestion condition of elementary analysis is 1000 DEG C～2000 DEG C；
(2) using coating method to carry out Fourier transform infrared spectroscopy scanning in polycarboxylate water-reducer sample, sweep limits is
4000～400cm-1, scanning times is 30～35 times, and resolution is 3.5～4.5cm-1, obtain the red of polycarboxylate water-reducer sample
External spectrum figure, the functional group of qualitative polycarboxylate water-reducer sample；
(3) adopting and be extracted with ethyl acetate polycarboxylate water-reducer sample, gained extract uses high performance liquid chromatograph test,
Flowing is methanol and phosphatic mixed liquor mutually, and its percentage by weight ratio is methanol: phosphate solution=5～12:100～80,
Phosphate solution be pH be the sodium dihydrogen phosphate-phosphate buffer solution of 2.0～4.0, the residual obtaining polycarboxylate water-reducer sample is little
Molecule monomer component high-efficient liquid phase chromatogram；The reference material of residual small molecule monomer uses test condition same as described above to carry out
High performance liquid chromatograph is tested, and occurs if any the retention time component consistent with the reference material of any residual small molecule monomer, then
Can residual small molecule monomer in qualitative polycarboxylate water-reducer sample；The volume of above-mentioned ethyl acetate is polycarboxylate water-reducer sample
0.1～1.0 times of volume；
(4) using acetonitrile extraction polycarboxylate water-reducer sample, gained extract uses gas chromatograph-mass spectrometer to obtain it
CG-MS data, carry out the extraction of the pure spectrogram of gaschromatographic mass spectrometry, to the residual small molecule monomer in mass spectrometric data storehouse
Standard mass spectrum is screened, the residual small molecule monomer in qualitative polycarboxylate water-reducer sample；The volume of above-mentioned acetonitrile is poly-
0.1～0.5 times of carboxylic acid water reducer sample volume.
In a preferred embodiment of the invention, the molecular weight of described polycarboxylate water-reducer sample is 3～50,000, converts
Rate is 85%～100%.
In a preferred embodiment of the invention, the digestion condition of the elementary analysis of described step (1) is 1400 DEG C.
In a preferred embodiment of the invention, the sweep limits of described Fourier transform infrared spectroscopy scanning is
4000～400cm-1, scanning times is 32 times, and resolution is 4cm-1。
In a preferred embodiment of the invention, the chromatographic column used by high performance liquid chromatograph of described step (3) is
C18 post.
In a preferred embodiment of the invention, described mobile phase methanol and phosphatic weight percent are methanol:
Phosphate=8:92；
In a preferred embodiment of the invention, described phosphate solution be pH be 3.0 sodium dihydrogen phosphate-phosphoric acid delay
Dissolved liquid；
In a preferred embodiment of the invention, the makings condition of the gas chromatograph-mass spectrometer of described step (4)
For: HP-Innowax, 30m*0.25mm*0.25um, temperature: detector 300 DEG C, injection port 120 DEG C, shunting is entered
Sample, carrier gas is nitrogen, and flow velocity is 1.5mL/min, and split ratio is 30:1.
The invention has the beneficial effects as follows:
1, the qualitative analysis detection method first elemental analyser of the present invention carries out elementary analysis survey to polycarboxylate water-reducer sample
Examination, recycling Fourier transform infrared spectrometer polycarboxylate water-reducer sample is scanned, then by high performance liquid chromatography,
Gaschromatographic mass spectrometry is to its further analysis, it is achieved the qualitative analysis of polycarboxylate water-reducer residual small molecule monomer component, is not required to
Want complicated sample making course, detect sensitive, favorable reproducibility.
2, the qualitative analysis detection method of the present invention uses ethyl acetate, acetonitrile that polycarboxylate water-reducer sample carries out extraction richness
Collection processes, and carries out high performance liquid chromatography, gaschromatographic mass spectrometry test, reaches to separate the effect concentrated, it is simple to analyze detection.
3, the qualitative analysis detection method of the present invention uses four kinds of instruments to enter polycarboxylic acids sample the unknown monomer component the most simultaneously
Row qualitative analysis, multiple instrument data combines, and data are reliably enriched, and makes this method for qualitative analysis more accurate.
4, qualitative point of qualitative analysis detection method offer a kind of polycarboxylate water-reducer residual small molecule monomer component of the present invention
Analysis method, optimizes for polycarboxylate water-reducer properties of sample, and process modification provides technical support.
Detailed description of the invention
Below by way of detailed description of the invention technical scheme it is further detailed and describes.
Embodiment 1
It is desirable to provide the method for qualitative analysis of a kind of polycarboxylate water-reducer residual small molecule monomer component, embodiment is with certain
As a example by polycarboxylate water-reducer sample (hereinafter referred to as sample 1).The sample 1 used is the polycarboxylic acids that certain commercially available company produces
Water reducer, index meets GB 8076-2008 " concrete admixture " requirement.
(1) elementary analysis
Take 105 DEG C of oven for drying of sample 1 10g, 1400 DEG C of High-temperature Digestions, carry out unit at Vario EL Cube elemental analyser
Element analyzes test, obtains the Elemental analysis data of sample 1, show that its element type contains carbon, hydrogen, oxygen and nitrogen.
(2) Fourier transform infrared spectroscopy scanning analysis
Use coating method to carry out Fourier transform infrared spectroscopy scanning, take appropriate amount of sample 1, under infrared lamp, be uniformly applied to window
On, treat the most dried, carry out Fourier transform infrared spectroscopy (sweep limits 4000～400cm-1；Scanning times: 32
Secondary；Resolution 4cm-1) scanning, obtain the collection of illustrative plates of sample 1.Illustrate that sample 1 shows the characteristic absorption peak of carboxyl；
(3) efficient liquid phase chromatographic analysis
Take sample 1 10g to add in 20mL centrifuge tube, add the ethyl acetate solution of 5mL, shake up, in centrifuge tube from
Heart 10min.Centrifuge tube upper liquid carries out efficient liquid phase chromatographic analysis.Wherein, chromatographic column selects C18, and flowing is methanol mutually
-phosphate buffered solution (pH is 3.0), flow velocity is 1.0mL/min, and detection wavelength is 220nm, and sample size is 20uL.
By high performance liquid chromatography spectrogram and the high performance liquid chromatography spectrogram comparison in addition of sample 1 of standard substance, subtract with qualitative polycarboxylic acids
The constituent of water preparation.By comparison, can qualitative go out sample 1 inner residual small molecule monomer component.
(4) gaschromatographic mass spectrometric analysis
Take sample 1 10g and add in 20mL centrifuge tube, add the acetonitrile solution of 2mL, shake up, centrifugal 10min in centrifuge tube.
Centrifuge tube upper liquid carries out gaschromatographic mass spectrometric analysis, uses the detection of gas chromatography thermal conductivity detector alkalescence to analyze.Wherein color
Spectral condition is HP-Innowax, 30m*0.25mm*0.25um, temperature: detector 300 DEG C, injection port 120 DEG C, shunting
Formula sample introduction, carrier gas is nitrogen, and flow velocity is 1.5mL/min, and split ratio is 30:1.Obtain the gaschromatographic mass spectrometry figure of sample 1,
Then carry out the extraction of the pure spectrogram of gaschromatographic mass spectrometry, standard mass spectrum in mass spectrometric data storehouse screened, qualitative go out sample
Residual small molecule monomer component in product 1.
By elemental microanalysis method, fourier transform infrared spectroscopy, high performance liquid chromatography, GC-MS to sample
1 is analyzed, can qualitative go out sample 1 residual small molecule monomer component.
Those of ordinary skill in the art understand, when technical scheme change in following ranges, remain able to obtain and
The technique effect that above-described embodiment is same or like, still falls within protection scope of the present invention:
A kind of qualitative analysis detection method of polycarboxylate water-reducer residual small molecule monomer component, described polycarboxylate water-reducer sample
Molecular weight be 3～50,000, conversion ratio is 85%～100%.Specifically include following steps:
(1) polycarboxylate water-reducer sample is dried process, obtains its solid sample, the solid sample of gained is carried out
Elementary analysis is tested, and obtains its Elemental analysis data, and qualitative analysis goes out the element kind in polycarboxylate water-reducer sample, above-mentioned
The digestion condition of elementary analysis is 1000 DEG C～2000 DEG C；
(2) using coating method to carry out Fourier transform infrared spectroscopy scanning in polycarboxylate water-reducer sample, sweep limits is
4000～400cm-1, scanning times is 30～35 times, and resolution is 3.5～4.5cm-1, obtain the red of polycarboxylate water-reducer sample
External spectrum figure, the functional group of qualitative polycarboxylate water-reducer sample；
(3) adopting and be extracted with ethyl acetate polycarboxylate water-reducer sample, gained extract uses high performance liquid chromatograph test,
Flowing is methanol and phosphatic mixed liquor mutually, and its percentage by weight ratio is methanol: phosphate solution=5～12:100～80,
Phosphate solution be pH be the sodium dihydrogen phosphate-phosphate buffer solution of 2.0～4.0, the residual obtaining polycarboxylate water-reducer sample is little
Molecule monomer component high-efficient liquid phase chromatogram；The reference material of residual small molecule monomer uses test condition same as described above to carry out
High performance liquid chromatograph is tested, and occurs if any the retention time component consistent with the reference material of any residual small molecule monomer, then
Can residual small molecule monomer in qualitative polycarboxylate water-reducer sample；The volume of above-mentioned ethyl acetate is polycarboxylate water-reducer sample
0.1～1.0 times of volume；
(4) using acetonitrile extraction polycarboxylate water-reducer sample, gained extract uses gas chromatograph-mass spectrometer to obtain it
CG-MS data, carry out the extraction of the pure spectrogram of gaschromatographic mass spectrometry, to the residual small molecule monomer in mass spectrometric data storehouse
Standard mass spectrum is screened, the residual small molecule monomer in qualitative polycarboxylate water-reducer sample；The volume of above-mentioned acetonitrile is poly-
0.1～0.5 times of carboxylic acid water reducer sample volume.
The above, only presently preferred embodiments of the present invention, therefore the scope that the present invention implements can not be limited according to this, i.e. depend on
The equivalence change that the scope of the claims of the present invention and description are made with modify, all should still belong in the range of the present invention contains.
Claims (8)
1. the qualitative analysis detection method of a polycarboxylate water-reducer residual small molecule monomer component, it is characterised in that: bag
Include following steps:
(1) polycarboxylate water-reducer sample is dried process, obtains its solid sample, the solid sample of gained is carried out
Elementary analysis is tested, and obtains its Elemental analysis data, and qualitative analysis goes out the element kind in polycarboxylate water-reducer sample, above-mentioned
The digestion condition of elementary analysis is 1000 DEG C～2000 DEG C；
(2) using coating method to carry out Fourier transform infrared spectroscopy scanning in polycarboxylate water-reducer sample, sweep limits is
4000～400cm-1, scanning times is 30～35 times, and resolution is 3.5～4.5cm-1, obtain the red of polycarboxylate water-reducer sample
External spectrum figure, the functional group of qualitative polycarboxylate water-reducer sample；
(3) adopting and be extracted with ethyl acetate polycarboxylate water-reducer sample, gained extract uses high performance liquid chromatograph test,
Flowing is methanol and phosphatic mixed liquor mutually, and its percentage by weight ratio is methanol: phosphate solution=5～12:100～80,
Phosphate solution be pH be the sodium dihydrogen phosphate-phosphate buffer solution of 2.0～4.0, the residual obtaining polycarboxylate water-reducer sample is little
Molecule monomer component high-efficient liquid phase chromatogram；The reference material of residual small molecule monomer uses test condition same as described above to carry out
High performance liquid chromatograph is tested, and occurs if any the retention time component consistent with the reference material of any residual small molecule monomer, then
Can residual small molecule monomer in qualitative polycarboxylate water-reducer sample；The volume of above-mentioned ethyl acetate is polycarboxylate water-reducer sample
0.1～1.0 times of volume；
(4) using acetonitrile extraction polycarboxylate water-reducer sample, gained extract uses gas chromatograph-mass spectrometer to obtain it
CG-MS data, carry out the extraction of the pure spectrogram of gaschromatographic mass spectrometry, to the residual small molecule monomer in mass spectrometric data storehouse
Standard mass spectrum is screened, the residual small molecule monomer in qualitative polycarboxylate water-reducer sample；The volume of above-mentioned acetonitrile is poly-
0.1～0.5 times of carboxylic acid water reducer sample volume.
2. qualitative analysis detection method as claimed in claim 1, it is characterised in that: described polycarboxylate water-reducer sample
Molecular weight is 3～50,000, and conversion ratio is 85%～100%.
3. qualitative analysis detection method as claimed in claim 1, it is characterised in that: the elementary analysis of described step (1)
Digestion condition be 1400 DEG C.
4. qualitative analysis detection method as claimed in claim 1, it is characterised in that: described Fourier transform infrared spectroscopy
The sweep limits of scanning is 4000～400cm-1, scanning times is 32 times, and resolution is 4cm-1。
5. qualitative analysis detection method as claimed in claim 1, it is characterised in that: the efficient liquid phase of described step (3)
Chromatographic column used by chromatograph is C18 post.
6. qualitative analysis detection method as claimed in claim 1, it is characterised in that: described mobile phase methanol and phosphate
Weight percent be methanol: phosphate=8:92.
7. qualitative analysis detection method as claimed in claim 1, it is characterised in that: described phosphate solution is that pH is
Sodium dihydrogen phosphate-the phosphate buffer solution of 3.0.
8. qualitative analysis detection method as claimed in claim 1, it is characterised in that: the gas chromatogram of described step (4)
The makings condition of GC-MS is: HP-Innowax, 30m*0.25mm*0.25um, temperature: detector 300 DEG C, enters
120 DEG C of sample mouth, shunting sample introduction, carrier gas is nitrogen, and flow velocity is 1.5mL/min, and split ratio is 30:1.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112326587A (en) * | 2020-12-18 | 2021-02-05 | 兰州交通大学 | Polycarboxylic acid water reducing agent analysis and identification method |
| CN115452998A (en) * | 2022-09-28 | 2022-12-09 | 煤炭科学技术研究院有限公司 | Method for determining hydraulic transmission medium components in water sample |
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| 王江雪等: ""聚羧酸减水剂中小分子单体残留量的测定"", 《广州化工》 * |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112326587A (en) * | 2020-12-18 | 2021-02-05 | 兰州交通大学 | Polycarboxylic acid water reducing agent analysis and identification method |
| CN112326587B (en) * | 2020-12-18 | 2023-09-05 | 兰州交通大学 | Polycarboxylate water reducer analysis and identification method |
| CN115452998A (en) * | 2022-09-28 | 2022-12-09 | 煤炭科学技术研究院有限公司 | Method for determining hydraulic transmission medium components in water sample |
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