CN101887014A - Method for identifying white oil-doped silicone sealant - Google Patents
Method for identifying white oil-doped silicone sealant Download PDFInfo
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- CN101887014A CN101887014A CN 201010200499 CN201010200499A CN101887014A CN 101887014 A CN101887014 A CN 101887014A CN 201010200499 CN201010200499 CN 201010200499 CN 201010200499 A CN201010200499 A CN 201010200499A CN 101887014 A CN101887014 A CN 101887014A
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- white oil
- silicone sealant
- sealant
- silicone
- doped
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- 239000004590 silicone sealant Substances 0.000 title claims abstract description 66
- 238000000034 method Methods 0.000 title claims abstract description 23
- 230000008961 swelling Effects 0.000 claims abstract description 26
- 238000012512 characterization method Methods 0.000 claims abstract description 14
- 238000012360 testing method Methods 0.000 claims abstract description 10
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 44
- 239000002904 solvent Substances 0.000 claims description 18
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 8
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 claims description 6
- 238000010521 absorption reaction Methods 0.000 claims description 4
- 239000012298 atmosphere Substances 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 3
- 238000000605 extraction Methods 0.000 claims description 3
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 3
- 239000001301 oxygen Substances 0.000 claims description 3
- 229910052760 oxygen Inorganic materials 0.000 claims description 3
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 claims description 3
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 claims description 2
- 239000003292 glue Substances 0.000 abstract description 19
- 239000007788 liquid Substances 0.000 abstract 2
- 239000003921 oil Substances 0.000 description 63
- 239000000565 sealant Substances 0.000 description 26
- 229920001296 polysiloxane Polymers 0.000 description 15
- 239000013464 silicone adhesive Substances 0.000 description 14
- 239000012530 fluid Substances 0.000 description 12
- 208000016261 weight loss Diseases 0.000 description 12
- 230000004580 weight loss Effects 0.000 description 12
- 238000011156 evaluation Methods 0.000 description 9
- 125000001181 organosilyl group Chemical group [SiH3]* 0.000 description 8
- 238000001757 thermogravimetry curve Methods 0.000 description 8
- 239000002994 raw material Substances 0.000 description 7
- 239000005662 Paraffin oil Substances 0.000 description 4
- 238000004458 analytical method Methods 0.000 description 4
- 239000011521 glass Substances 0.000 description 4
- 239000002480 mineral oil Substances 0.000 description 4
- 235000010446 mineral oil Nutrition 0.000 description 4
- 125000003944 tolyl group Chemical group 0.000 description 4
- 238000005033 Fourier transform infrared spectroscopy Methods 0.000 description 3
- 239000000470 constituent Substances 0.000 description 3
- 230000008595 infiltration Effects 0.000 description 3
- 238000001764 infiltration Methods 0.000 description 3
- 229920002545 silicone oil Polymers 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 208000027418 Wounds and injury Diseases 0.000 description 2
- 229920005549 butyl rubber Polymers 0.000 description 2
- 230000006378 damage Effects 0.000 description 2
- JZZIHCLFHIXETF-UHFFFAOYSA-N dimethylsilicon Chemical compound C[Si]C JZZIHCLFHIXETF-UHFFFAOYSA-N 0.000 description 2
- 238000002329 infrared spectrum Methods 0.000 description 2
- 208000014674 injury Diseases 0.000 description 2
- IOLCXVTUBQKXJR-UHFFFAOYSA-M potassium bromide Chemical compound [K+].[Br-] IOLCXVTUBQKXJR-UHFFFAOYSA-M 0.000 description 2
- 238000010998 test method Methods 0.000 description 2
- 238000002411 thermogravimetry Methods 0.000 description 2
- -1 wherein: 1 Substances 0.000 description 2
- 238000004566 IR spectroscopy Methods 0.000 description 1
- 150000001335 aliphatic alkanes Chemical class 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000005253 cladding Methods 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 125000000113 cyclohexyl group Chemical group [H]C1([H])C([H])([H])C([H])([H])C([H])(*)C([H])([H])C1([H])[H] 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000011256 inorganic filler Substances 0.000 description 1
- 229910003475 inorganic filler Inorganic materials 0.000 description 1
- 239000005344 low-emissivity glass Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 238000012113 quantitative test Methods 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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Abstract
The invention discloses a method for identifying a white oil-doped silicone sealant, which comprises the following steps of: (1), performing a swelling or extracting test on the silicone sealant to obtain a swelling liquid or an extract, then performing infrared characterization on the swelling liquid or the extract to determine qualitatively that the silicone sealant contains the white oil; (2), performing thermal gravimetric characterization on the silicone sealant to determine quantitatively that the silicone sealant contains the white oil; and (3), identifying the white oil-doped silicone sealant according to two characterization results in the step (1) and the step (2). By using the method, users can identify poor glues and unqualified glues quickly and correctly in the process of using the silicone sealant; by using the method, the silicone sealant which contains a small amount of white oil can be identified correctly; and the silicone sealant which cannot be identified by testing volatile matters and smelling can be identified accurately by using the method.
Description
Technical field
The present invention relates to a kind of Quality Identification of silicone sealant, be specifically related to utilize infrared spectrum and thermogravimetric to identify a kind of method of white oil-doped silicone sealant.
Background technology
Less than 20 years, but because the individual character and the aesthetic feature of its distinctness formed colorful and changeful urban look to glass curtain wall in the rise of China and development.And be used for the silicone weather resistant fluid sealant of curtain wall bonding, because of its good cohesiveness and weatherability play an important role at the building curtain wall fit on.Yet along with popularizing of glass curtain wall, its product yield increases fast, also to have occurred curtain wall on market very different with the quality of fluid sealant thereupon, and in recent years along with the construction market price competition intensifies, the tendency of high price lattice lightweight has appearred in many companies, in some building curtain wall engineering even adopt the silicone sealant that fills white oil that price is ultralow, quality is low in a large number, be called for short white oil glue.Because white oil is a kind of low molecule mineral oil, be filled in and be easy in the glue vapor away, time one length can make fluid sealant structuring occur, glass joint seal glue cracking, the inefficacy of double glazing unit piece oil impregnate etc. will appear like this, and may jeopardize the be bonded and sealed quality accident of assembling safety of cladding glass, make us the safety and the permanance of curtain wall are very worried.
If containing the silicone sealant of white oil is used for will occurring behind the double glazing double glazing salient point, trickling and at the rainbow phenomena of low emissivity glass, double glazing is caused very big injury.When white oil glue uses in double glazing, can be the sealing of first road of double glazing that butyl rubber dissolves away, will make double glazing salient point, the trickling phenomenon of leakage, water inlet, butyl rubber occur like this.
By above elaboration, we know if mixed in the silicone adhesive behind the white oil can and in use cause very big injury to the quality of glue, can differentiate out by the method for smell, survey fugitive constituent for the silicone adhesive that white oil content is high, Quality Identification for silicone sealant, GB 16776～2005 (structural silicone sealant for building) is defined in carries out fugitive constituent and measures under 90 ± 2 ℃ the condition, it is specification product that regulation is not more than 10% silicone adhesive.The scope of stipulating in this standard is too big, if added a spot of white oil in the silicone adhesive, as then surveying to come out less than 5% o'clock.
Summary of the invention
The technical problem to be solved in the present invention is can not detect at the silicone sealant that has added a small amount of white oil, and a kind of authentication method of white oil-doped silicone sealant is provided.
Technical scheme of the present invention is: a kind of authentication method of white oil-doped silicone sealant, and its step is as follows:
(1) silicone sealant is carried out swelling or extraction test, obtain swelling solution or extract, then swelling solution or extract are carried out IR Characterization, if at 710～732cm
～1, 1370～1390cm
～1, 2915～2935cm
～1, 2950～2970cm
～1, 1450～1470cm
～1At least three absorption peaks of middle appearance can qualitatively judge and contain white oil in the silicone sealant;
(2) silicone sealant is carried out thermogravimetric and characterize,, can quantitatively judge and contain white oil in the silicone sealant if weightlessness occurs at 120～160 ℃;
(3) comprehensive step (1) and (2) two kinds of characterization results of step are identified white oil-doped silicone sealant.
The used solvent of described swell test is any one in toluene, acetone, tetrahydrofuran or the cyclohexane.
The method that thermogravimetric characterizes in the described step (3) is for to be raised to 200～220 ℃ in 20～50 ℃ of intensification scopes with 50～160 ℃/min under the condition of nitrogen atmosphere, and under this temperature, kept 2～5 minutes, the heating rate with 50～160 ℃/min is raised to 800～900 ℃ in the atmosphere of oxygen then.
The invention provides a kind of method that a kind of dialogue factice is identified, silicone sealant is carried out swelling or extraction test, the spacing of its cross-linked network is increased, thereby the plastifier of not participating in reaction is bubbled out, if having added white oil in the silicone sealant will bubble out from cross-linked network, can carry out infrared scan to its swelling solution subsequently, can measure whether contain white oil in the silicone adhesive in the plastifier so qualitatively.
Utilize the method for thermogravimetric analysis that silicone sealant is carried out heat analysis,, and in the atmosphere of nitrogen, carry out heat analysis, contain how many white oils in the evaluation silicone sealant that can be quantitative from the curve of thermal weight loss according to certain heating rate.
The invention has the beneficial effects as follows: the present invention utilizes infrared spectrum and two kinds of analytical instrument of thermal weight loss to unite to identify, both can test qualitatively also and can carry out quantitative test to it.Helping more accurate dialogue factice identifies.The present invention can make us in the process of using silicone sealant those glue inferior, defective glue be carried out fast, identify accurately.The present invention can identify that the fluid sealant that can not identify for survey fugitive constituent, smelling uses the method accurately to identify accurately to the white oil that contains minute quantity in the silicone sealant.
Description of drawings
Fig. 1 is not for containing white oil silicone sealant and the TG curve that contains 6% silicone sealant, wherein: 1, silicone sealant, 2, contain 6% white oil silicone adhesive;
Fig. 2 is the TG curve of white oil;
Fig. 3 is not for to contain the silicone sealant of white oil and the TG curve of the silicone sealant that contains different white oil content, wherein: 1, silicone sealant 2, contain 1% white oil silicone adhesive 3, contain 2% silicone adhesive 4, contain 3% silicone adhesive 5, contain 4% silicone adhesive 6, contain 5% silicone adhesive 7, contain 6% silicone adhesive 8, contain 10% silicone adhesive;
Fig. 4 is the FTIR spectrogram of white oil;
Fig. 5 is the FTIR spectrogram of methyl-silicone oil;
Fig. 6 is the FTIR spectrogram of white oil, methyl-silicone oil and the swelling solution that contains the white oil silicone sealant, wherein: 1, white oil 2, dimethyl silicon oil 3, fluid sealant swelling solution.
Embodiment
Evaluation to the silicone sealant that contains white oil amount 1%
Get a certain amount of sample glue it is put into conical flask or 7 days solvent toluene of swelling.
Utilize Nicolet is10 type infrared spectrometer that U.S. Thermo scientific company produces that the swelling solution of silicone sealant is carried out infrared analysis, method with pressing potassium bromide troche is carried out, before infrared test, earlier window is placed under the infrared lamp and toasts, solvent toluene is vapored away, in test, can remove the interference of toluene like this, and then obtain collection of illustrative plates more accurately.
The TGA that utilizes Switzerland's plum Teller～Francesco Toldo company to produce carries out heat analysis to silicone sealant, concrete test method is for to be raised to 200～220 ℃ in 20～50 ℃ of intensification scopes with 50～160 ℃/min under the condition of nitrogen atmosphere, and under this temperature, kept 2～5 minutes, plastifier is volatilized, in the atmosphere of oxygen, be raised to 800～900 ℃ then organosilicon and inorganic filler branch taken off with the heating rate of 50～160 ℃/min.
Infared spectrum to swelling solution is analyzed, and it and methyl-silicone oil, the infrared of white oil are compared, and 1260cm all occurred as can be seen on the spectrogram of dimethyl silicon oil and fluid sealant swelling solution from three's figure
～1Si～the CH at place
3Absorption peak and 1130～1000cm
～1Si～O～Si the absorption peak at place, and 710～732cm has also appearred on the spectrogram of fluid sealant swelling solution
～1Alkane skeletal vibration (n＞4), it is open chain CH in the alkane
2C～H plane wobble frequency; And at 1370～1390cm
～1The peak at place is CH
3CH symmetric curvature vibration peak, at 1450～1470cm
～1The place is CH
2Scissoring vibration or CH
3Antisymmetry flexural vibrations peak, and at 2950～2970cm
～1CH
3The asymmetric stretching vibration peak of C～H and 2915～2935cm
～1Open chain CH
2The asymmetric vibration peak of stretching of C～H.Therefore, can judge and in the swelling solution of fluid sealant, have white oil (being saturated paraffin oil).
From the TGA curve as can be seen: curve 1 is the thermogravimetric curve of silicone sealant, its weightless starting point is about 400 ℃, has the good heat endurance energy, and curve 2 is the fluid sealant weight-loss curves that contain white oil, and its curve has two steps in the weightless district of organism, and first step is weightless 160 ℃ of beginnings, this is because have paraffin oil in the fluid sealant, it is a kind of easy infiltration, volatile micromolecule mineral oil, and only 160～230 ℃ of flash-points are 0.94% at this weightless massfraction.Second step is organosilyl weight-loss curve, and it just begins weightlessness about 400 ℃.Therefore we can clearly find out the difference of two kinds of glue heat resistances from two weight-loss curves.The heat resistance of white oil glue is far smaller than silicone adhesive.
Can draw by above two kinds of test methods: Infrared spectroscopy can draw whether contain white oil in the silicone sealant qualitatively, and what thermogravimetric analysis then can be quantitative analyzes how much content of white oil has in the silicone sealant.In conjunction with two kinds of methods, we can draw this more accurately, authentication method effectively.
Embodiment 2: contain the evaluation of the silicone sealant of white oil amount 2%
Raw material: white oil content is 2% silicone structure sealant; Solvent is a toluene.
Get a certain amount of sample glue it put into conical flask or swelling 7 days, or in the extracting instrument extracting 24h, solvent toluene, IR Characterization qualitatively judges in the silicone sealant and contains white oil with embodiment 1.
From the TGA curve as can be seen: white oil content is that 2% silicone structure sealant has two steps in the weightless district of organism, first step is weightless 130 ℃ of beginnings, this is because have paraffin oil in the fluid sealant, it is a kind of easy infiltration, volatile micromolecule mineral oil, only 160～230 ℃ of flash-points are 1.91% at this weightless massfraction.Second step is organosilyl weight-loss curve, and it just begins weightlessness about 400 ℃.
Embodiment 3: contain the evaluation of the silicone sealant of white oil amount 3%
Raw material: white oil content is 3% silicone structure sealant; Solvent is a toluene.
Get a certain amount of sample glue it put into conical flask or swelling 7 days, or in the extracting instrument extracting 24h, solvent toluene, IR Characterization qualitatively judges in the silicone sealant and contains white oil with embodiment 1.
From the TGA curve as can be seen: white oil content is that 3% silicone structure sealant has two steps in the weightless district of organism, first step is weightless 160 ℃ of beginnings, this is because have paraffin oil in the fluid sealant, it is a kind of easy infiltration, volatile micromolecule mineral oil, only 160～230 ℃ of flash-points are 2.92% at this weightless massfraction.Second step is organosilyl weight-loss curve, and it just begins weightlessness about 400 ℃.
Embodiment 4: contain the evaluation of the silicone sealant of white oil amount 4%
Raw material: white oil content is 4% silicone structure sealant; Solvent is an acetone.
Get a certain amount of sample glue it put into conical flask or swelling 7 days, or in the extracting instrument extracting 24h, solvent toluene, IR Characterization qualitatively judges in the silicone sealant and contains white oil with embodiment 1.
From the TGA curve as can be seen: white oil content is that 4% silicone structure sealant has two steps in the weightless district of organism, first step is weightless 150 ℃ of beginnings, weightless massfraction at this is 3.87%, second step is organosilyl weight-loss curve, and it just begins weightlessness about 400 ℃.
Embodiment 5: contain the evaluation of the silicone sealant of white oil amount 5%
Raw material: white oil content is 5% silicone structure sealant; Solvent is a tetrahydrofuran.
Get a certain amount of sample glue it put into conical flask or swelling 7 days, or in the extracting instrument extracting 24h, solvent toluene, IR Characterization qualitatively judges in the silicone sealant and contains white oil with embodiment 1.
From the TGA curve as can be seen: white oil content is that 5% silicone structure sealant has two steps in the weightless district of organism, first step is weightless 130 ℃ of beginnings, weightless massfraction at this is 4.62%, second step is organosilyl weight-loss curve, and it just begins weightlessness about 400 ℃.
Embodiment 6: contain the evaluation of the silicone sealant of white oil amount 6%
Raw material: white oil content is 6% silicone structure sealant; Solvent is a cyclohexane.
Get a certain amount of sample glue it put into conical flask or swelling 7 days, or in the extracting instrument extracting 24h, solvent toluene, IR Characterization qualitatively judges in the silicone sealant and contains white oil with embodiment 1.
From the TGA curve as can be seen: white oil content is that 6% silicone structure sealant has two steps in the weightless district of organism, first step is weightless 140 ℃ of beginnings, weightless massfraction at this is 5.53%, second step is organosilyl weight-loss curve, and it just begins weightlessness about 400 ℃.
Embodiment 7: contain the evaluation of the silicone sealant of white oil amount 7%
Raw material: white oil content is 7% silicone structure sealant; Solvent is a toluene.
Get a certain amount of sample glue it put into conical flask or swelling 7 days, or in the extracting instrument extracting 24h, solvent toluene, IR Characterization qualitatively judges in the silicone sealant and contains white oil with embodiment 1.
From the TGA curve as can be seen: white oil content is that 7% silicone structure sealant has two steps in the weightless district of organism, first step is weightless 150 ℃ of beginnings, weightless massfraction at this is 6.68%, second step is organosilyl weight-loss curve, and it just begins weightlessness about 400 ℃.
Embodiment 8: contain the evaluation of the silicone sealant of white oil amount 10%
Raw material: white oil content is 10% silicone structure sealant; Solvent is a toluene.
Get a certain amount of sample glue it put into conical flask or swelling 7 days, or in the extracting instrument extracting 24h, solvent toluene, IR Characterization qualitatively judges in the silicone sealant and contains white oil with embodiment 1.
From the TGA curve as can be seen: white oil content is that 10% silicone structure sealant has two steps in the weightless district of organism, first step is weightless 160 ℃ of beginnings, weightless massfraction at this is 9.23%, second step is organosilyl weight-loss curve, and it just begins weightlessness about 400 ℃.
Claims (3)
1. the authentication method of a white oil-doped silicone sealant, it is characterized in that: its step is as follows:
(1) silicone sealant is carried out swelling or extraction test, obtain swelling solution or extract, then swelling solution or extract are carried out IR Characterization, if at 710～732cm
～1, 1370～1390cm
～1, 2915～2935cm
～1, 2950～2970cm
～1, 1450～1470cm
～1At least three absorption peaks of middle appearance can qualitatively judge and contain white oil in the silicone sealant;
(2) silicone sealant is carried out thermogravimetric and characterize,, can quantitatively judge and contain white oil in the silicone sealant if weightlessness occurs at 120～160 ℃;
(3) comprehensive step (1) and (2) two kinds of characterization results of step are identified white oil-doped silicone sealant.
2. according to the authentication method of the described white oil-doped silicone sealant of claims 1, it is characterized in that: the used solvent of described swell test is any one in toluene, acetone, tetrahydrofuran or the cyclohexane.
3. according to the authentication method of the described white oil-doped silicone sealant of claims 1, it is characterized in that: the method that thermogravimetric characterizes in the described step (3) is for to be raised to 200～220 ℃ in 20～50 ℃ of intensification scopes with 50～160 ℃/min under the condition of nitrogen atmosphere, and under this temperature, kept 2～5 minutes, the heating rate with 50～160 ℃/min is raised to 800～900 ℃ in the atmosphere of oxygen then.
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|---|---|---|---|
| CN 201010200499 CN101887014B (en) | 2010-06-13 | 2010-06-13 | Identification method of white oil-doped silicone sealant |
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|---|---|---|---|
| CN 201010200499 CN101887014B (en) | 2010-06-13 | 2010-06-13 | Identification method of white oil-doped silicone sealant |
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| Publication Number | Publication Date |
|---|---|
| CN101887014A true CN101887014A (en) | 2010-11-17 |
| CN101887014B CN101887014B (en) | 2012-04-25 |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103743889A (en) * | 2013-12-25 | 2014-04-23 | 辽宁省产品质量监督检验院 | Kit for rapidly detecting hydrocarbons plasticizer in silicone sealant and application thereof |
| CN103743645A (en) * | 2013-07-19 | 2014-04-23 | 中国石油化工股份有限公司 | Method for controlling quality of polymer for reservoir oil displacement using thermal gravimetric analysis technology |
| CN103760300A (en) * | 2013-12-25 | 2014-04-30 | 辽宁省产品质量监督检验院 | Butyl rubber test paper and preparation method |
| CN103822985A (en) * | 2014-03-12 | 2014-05-28 | 中国建筑科学研究院 | Chemical identifying method of white oil doped silicone sealant |
| CN106483209A (en) * | 2016-09-06 | 2017-03-08 | 中国建筑科学研究院 | Method for measuring silicone sealant |
| CN107290243A (en) * | 2017-05-25 | 2017-10-24 | 常州第六元素材料科技股份有限公司 | A kind of accurate measurement method of graphene content in graphene slurry |
| CN107722305A (en) * | 2017-10-17 | 2018-02-23 | 辽宁省产品质量监督检验院（辽宁省建筑材料监督检验院） | A kind of standard butyl rubber solution |
| CN109060711A (en) * | 2018-08-28 | 2018-12-21 | 中蓝晨光成都检测技术有限公司 | A method of calculating white oil content in white oil-doped organosilicon product |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103743645A (en) * | 2013-07-19 | 2014-04-23 | 中国石油化工股份有限公司 | Method for controlling quality of polymer for reservoir oil displacement using thermal gravimetric analysis technology |
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| CN103760300B (en) * | 2013-12-25 | 2015-09-09 | 辽宁省产品质量监督检验院 | A kind of butyl rubber test paper and preparation method |
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| CN107290243A (en) * | 2017-05-25 | 2017-10-24 | 常州第六元素材料科技股份有限公司 | A kind of accurate measurement method of graphene content in graphene slurry |
| CN107722305A (en) * | 2017-10-17 | 2018-02-23 | 辽宁省产品质量监督检验院（辽宁省建筑材料监督检验院） | A kind of standard butyl rubber solution |
| CN109060711A (en) * | 2018-08-28 | 2018-12-21 | 中蓝晨光成都检测技术有限公司 | A method of calculating white oil content in white oil-doped organosilicon product |
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