CN105259271A - Method for quantitatively testing total concentration of small molecules in composite insulator silicone rubber - Google Patents
Method for quantitatively testing total concentration of small molecules in composite insulator silicone rubber Download PDFInfo
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Abstract
The invention discloses a method for quantitatively testing the total concentration of small molecules in composite insulator silicone rubber. The method includes the following steps that 1, a composite insulator silicone rubber sample is selected, and small molecules in the silicone rubber sample are extracted till complete extraction; 2, extraction liquid merging is performed, and the volume is made constant after concentration; 3, extraction liquid is taken, a gas chromatograph is adopted for performing sample introduction to obtain a chromatogram of the silicone rubber sample, the peak position and retention time of each chromatographic peak are marked, and the peak area of each chromatographic peak is calculated; 4, an external standard substance is selected, a group of solutions with a concentration gradient are prepared, and a concentration-peak area standard curve of the external standard substance is made; 5, the concentration of each chromatographic peak is calculated according to the concentration-peak area standard curve of the external standard substance in the step 4 and the peak area of the corresponding chromatographic peak in the step 3, the concentrations of all the chromatographic peaks are added, and then the sum is the total concentration of the small molecules in the composite insulator silicone rubber. By means of the method, the total concentration of the small molecules in the composite insulator silicone rubber can be quantitatively tested.
Description
Technical field
The invention belongs to gas chromatographic technique field, be specifically related to a kind of method of quantitative test composite insulator silicon rubber small molecular total concentration.
Background technology
Insulator is often used in high voltage power transmission field, and the development experience of its manufactured materials pottery, glass and silicon rubber, be called porcelain insulator, glass insulator and composite insulator by people usually with the produced insulator of above material.
The time that composite insulator occurs the latest, performance is better than porcelain insulator and glass insulator, it have lightweight, hydrophobicity good, specific inductive capacity is high, the advantage of good flame resistance, and composite insulator can also recover gradually after losing hydrophobic nature, makes it have the universal prerequisite used.Meanwhile, the composite insulator use amount of China also increases year by year, has greatly the trend replacing porcelain insulator and glass insulator.But in the process of actual motion, due to the impact of the factor of the complex environments such as corona discharge, ultraviolet irradiation, acid and alkali corrosion, composite insulator easily occurs aging, and weakens gradually and lose hydrophobic nature.
Composite insulator after aging easily forms moisture film on surface, and the water soluble filth being deposited on its surface has just become good electrolyte, finally causes the generation of breakdown accident.Usually, a certain insulator puncture the paralysis that can cause whole piece circuit transmission line of electricity, bring great economic loss.
By consulting pertinent literature, the prevailing paradigm occurred for composite insulator hydrophobic rejuvenation is at present: Small molecular uncrosslinked in silicon rubber is moved to top layer by body layer.Therefore, the hydrophobic recovery capability of micromolecular measurement of concetration to assessment composite insulator is most important.But current existing method only rests on the stage of observational measurement, cannot obtain micromolecular Exact concentrations, realizing that the Small molecular concentration across comparison between different sample has the technical difficult problem being difficult to go beyond.Therefore, the accurate measurement being necessary for silicone rubber for composite insulator small molecular concentration provides a kind of method of science.
Gas chromatograph (GasChromatography, GC) is that a kind of difference of the boiling point of material, polarity and adsorption property that utilizes is to realize the chemical analysis instrument of the separation of potpourri.Typically, material in the gas phase transmission speed is fast, and therefore material can reach balance relatively easily between mobile phase and Stationary liquid.Add that the material of the optional phase that fixes is a lot of in addition, therefore gas chromatograph has the advantages that analysis speed is fast, efficiency is high.Adopt highly sensitive selective detector in recent years, it is had again advantages such as sensitivity for analysis is high, applied range.Simultaneously for the potpourri of complexity, the boiling point of potpourri can be utilized different, realize potpourri to be separated successively by temperature programme.By outstanding separating power, field is medium has a wide range of applications in industry, agricultural, national defence, scientific research etc. for gas chromatograph.
Common gas chromatograph is made up of following five big systems: air-channel system, sampling system, piece-rate system, temperature control system, detection record system.Sometimes in order to detect isolated material composition further, gas chromatography can also realize the coupling with other instruments, as mass spectrum, infrared spectrum etc.The coupling of gas chromatography here repeats no more.
Composite insulator is in the process of high temperature vulcanized refining, crosslinking degree is relevant with many factors, this just determines the (silane-Dn of such as ring-type of uncrosslinked Small molecular in finished product, Dn is 2n methyl ring n siloxane, for cyclosiloxane Small molecular and Dn, the test upper limit of gas chromatography is generally n=20 or 21) existence.Meanwhile, composite insulator, under arms in process, is subject to the impact of various ageing environment, chain-breaking reaction can occurs and generate Small molecular.These micromolecular existence, have impact on the hydrophobic restorability of composite insulator silicon rubber to a great extent.Therefore, accurately measure composite insulator silicon rubber small molecular concentration high voltage power transmission field tool is of great significance.
Summary of the invention
Technical matters to be solved by this invention is to provide a kind of method of quantitative test composite insulator silicon rubber small molecular total concentration, the method adopts vapor-phase chromatography, utilize the boiling point of composite insulator silicon rubber small molecular potpourri different, realize Small molecular to be separated successively by the temperature programme in GC, adopt quantified by external standard method, realize the quantitative test of composite insulator silicon rubber small molecular total concentration.
Above-mentioned technical matters to be solved by this invention is achieved through the following technical solutions: a kind of method of quantitative test composite insulator silicon rubber small molecular total concentration, comprises the following steps:
(1) choose composite insulator silicon rubber sample, drying after cleaning, adopt the Small molecular in solvent extraction process extraction silicon rubber sample, repeatedly extracting is complete to extraction;
(2) extract of repeatedly extracting is merged, constant volume after concentrated;
(3) get extract after constant volume, adopt gas chromatograph sampling, obtain the chromatogram of silicon rubber sample, mark peak position and the retention time of each chromatographic peak in chromatogram, and calculate the peak area of each chromatographic peak;
(4) choose external standard, prepare the solution that one group has concentration gradient, adopt the gas chromatograph condition sample introduction of same step (3), make the concentration-peak area typical curve of external standard;
(5) according to the concentration-peak area typical curve of external standard in step (4), and the peak area of each chromatographic peak in step (3), calculate the concentration of each chromatographic peak, the concentration of each chromatographic peak is added, is composite insulator silicon rubber small molecular total concentration.
In the method for above-mentioned quantitative test composite insulator silicon rubber small molecular total concentration:
Preferably adopt normal hexane during cleaning in step (1), when adopting solvent extraction process to extract, described solvent is preferably normal hexane.
In step (1), repeatedly silicon rubber sample, to when extracting complete, when after the Small molecular that first time adopts in solvent extraction process extraction silicon rubber sample, is carried out vacuum drying, obtains quality m by extracting
1, and then repeat to adopt the Small molecular step in solvent extraction process extraction silicon rubber sample, and silicon rubber sample is carried out vacuum drying, obtain quality m
2, as (m
2-m
1) value when being tending towards constant, then the Small molecular in silicon rubber sample is extracted out completely.
Vacuum drying temperature is preferably 70 DEG C ~ 90 DEG C, and the vacuum drying time is preferably 18 ~ 48h, is more preferred from 24h.
In step (3) ~ step (4), gas chromatograph adopts Agilent-6890 gas chromatograph, and the parameters of this gas chromatograph is preferably: chromatographic column: HP-5; Injector temperature: 280 DEG C; Split ratio: 10:1; Heating schedule: initial temperature 50 DEG C, retains 3min, is then warming up to 200 DEG C with the speed of 20 DEG C/min, then retains 0.5min; FID:280 DEG C, sample size: 1 μ L.
The retention time of the some chromatographic peaks in step (4) in the retention time of this external standard of selection demand fulfillment of external standard and the chromatogram of the middle silicon rubber sample of step (3) is identical.
Described external standard is preferably D4, D5 or D6.Wherein D4 is octamethylcy-clotetrasiloxane, and D5 is decamethylcyclopentaandoxane, and D6 is ten diformazan basic ring six siloxane.
Step chooses external standard in (4), prepare one group when there is the solution of concentration gradient, the following condition of concentration demand fulfillment of external standard: in step (3) silicon rubber sample chromatogram in the chromatographic peak identical with described external standard retention time concentration should this group there is the solution of concentration gradient between maximum concentration and least concentration.
Tool of the present invention has the following advantages:
(1) the inventive method adopts vapor-phase chromatography, utilize the boiling point of composite insulator silicon rubber small molecular potpourri different, realize Small molecular to be separated successively by the temperature programme in GC, and adopt quantified by external standard method, the quantitative test of composite insulator silicon rubber small molecular total concentration can be realized;
(2) accuracy of the inventive method energy is high, and operability is good, has stronger using value, accurately can measure the Small molecular concentration in composite insulator silicon rubber, has stronger using value and very important meaning for high voltage power transmission field.
(3) the present invention is that the hydrophobic recovery capability assessing silastic material provides one measuring method comparatively reliably.
Accompanying drawing explanation
Fig. 1 is the variation diagram of quality along with extraction times of silicon rubber sample in embodiment 2;
Fig. 2 is the chromatogram GC figure of composite insulator silicon rubber sample in embodiment 2;
Fig. 3 is the concentration-peak area canonical plotting of the external standard being external standard foundation with D4 in embodiment 2;
Fig. 4 is the concentration-peak area canonical plotting of the external standard being external standard foundation with D5 in embodiment 3;
Fig. 5 is the concentration-peak area canonical plotting of the external standard being external standard foundation with D6 in embodiment 4.
Embodiment
Following examples are used for illustrating and implementing the present invention, belong to the protection domain of invention, and those skilled in the art all can realize object of the present invention according to above disclosed content.
Embodiment 1
The method of the quantitative test composite insulator silicon rubber small molecular total concentration that the present embodiment provides, comprises the following steps:
(1) composite insulator silicon rubber sample, is got, be placed in vacuum drying chamber with normal hexane cleaning and dry, dried sample is placed in extractor normal hexane extracting extraction, after extracting, silicon rubber sample is placed in the dry 18 ~ 48h of vacuum drying chamber, 24h is better, and weighs and obtain quality m
1, vacuum drying chamber design temperature interval is: 70 DEG C ~ 90 DEG C;
(2), circulation step (1) obtains quality silicon rubber quality m
2, as (m
2-m
1) value when being tending towards constant, think that the Small molecular in silicon rubber sample is all extracted;
(3), the extract distillation and concentration obtained is settled to 10mL;
(4), by the extract sample introduction in gas chromatography (GC) after concentrated, constant volume, single injected sampling amount is 1 μ L, obtains the chromatogram of sample, marks peak position and retention time; Carry software by gas chromatography to carry out integration to chromatographic peak and obtain peak area corresponding to each peak; Wherein in step (3) silicon rubber sample chromatogram in the chromatographic peak identical with described external standard retention time concentration should this group there is the solution of concentration gradient between maximum concentration and least concentration.
(5), external standard is selected, general choice criteria: the retention time of external standard chromatographic peak identically with the some peaks retention time in silicon rubber extract chromatogram (for silicon rubber sample, must select D usually
4, D
5or D
6a certain).The external standard hexane solution of preparation at least 4 variable concentrations, and in gas chromatography sample introduction, obtain chromatogram and quadrature, making the concentration-peak area typical curve of external standard.
(6), repeat step (5), adjustment external standard concentration, until the concentration at corresponding external standard retention time peak is between Cmax and Cmin in silicon rubber drawing liquid concentrate; And make new concentration-peak area typical curve according to the external standard concentration after adjustment, and by mathematic(al) representation that the matching of orign software obtains between the two:
y＝f(x)
Wherein x represents concentration, and y represents peak area;
(7), calculated the micromolecular concentration of corresponding external standard retention time in extract by 1. formula, then the peak area of comparison chromatogram obtains other Small molecular relative concentrations, finally each micromolecular concentration summation is obtained total concentration.
The parameter of the Agilent-6890 gas chromatograph in step (4), (5) and (6) is as follows:
Chromatographic column: HP-5;
Injector temperature: 280 DEG C
Split ratio: 10:1;
Heating schedule: initial temperature 50 DEG C, retains 3min, is then warming up to 200 DEG C with the speed of 20 DEG C/min, then retains 0.5min;
FID：280℃；
Sample size: 1 μ L.
Embodiment 2
The method of the quantitative test composite insulator silicon rubber small molecular total concentration that the present embodiment provides, comprises the following steps:
(1) silicon rubber sample 25g is got, silicon rubber specification is 2cm × 2cm × 1mm, be placed in vacuum drying chamber with normal hexane cleaning and dry, vacuum drying chamber design temperature is: 75 DEG C, drying time 8h, dried sample is placed in Soxhlet extractor normal hexane extracting extraction, after extracting, silicon rubber sample is placed in the dry 24h of vacuum drying chamber, and weighs and obtain quality m
1;
(2) circulation step (1) obtains quality silicon rubber quality m
2, as (m
2-m
1) value when being tending towards constant, think that the Small molecular in silicon rubber sample is all extracted, as shown in fig. 1;
(3) with Rotary Evaporators, extract is concentrated into below 10mL, and then gets normal hexane with glue head dropper extract is settled to 10mL;
(4) then sample introduction in Agilent-6890 gas chromatograph, arranges supremacy clause of the present invention, chromatographic column: HP-5; Injector temperature: 280 DEG C; Split ratio: 10:1; Heating schedule: initial temperature 50 DEG C, retains 3min, is then warming up to 200 DEG C with the speed of 20 DEG C/min, then retains 0.5min; FID:280 DEG C, sample size: 1 μ L, obtains the chromatogram of extract, marks peak position and the retention time of chromatographic peak, and the retention time at first peak is 7.131min (D
4retention time), as shown in Figure 2.The peak area being calculated this peak by gas chromatography special software is 10.93865, obtains the peak area ratio of peak area with this peak at other peak, as following table 1 simultaneously.
The retention time of the peak area of each chromatographic peak of table 1, peak area and with external standard D
4peak area ratio
| Sequence number | Retention time | Peak area | (D relatively 4) peak area ratio |
| 1 | 7.131 | 10.939 | 1.000 |
| 2 | 8.586 | 4.076 | 0.373 |
| 3 | 9.848 | 4.778 | 0.437 |
| 4 | 10.94 | 3.583 | 0.328 |
| 5 | 11.758 | 3.831 | 0.350 |
| 6 | 12.593 | 3.748 | 0.343 |
| 7 | 13.708 | 8.107 | 0.741 |
| 8 | 14.805 | 50.233 | 4.592 |
| 9 | 15.458 | 118.424 | 10.826 |
| 10 | 16.183 | 206.985 | 18.922 |
| 11 | 17.03 | 289.700 | 26.484 |
| 12 | 18.055 | 329.859 | 30.155 |
| 13 | 19.345 | 340.393 | 31.118 |
| 14 | 20.997 | 355.111 | 32.464 |
| 15 | 23.139 | 400.146 | 36.581 |
(5) D is selected
4for external standard, following 6 concentration gradients (10 of preparation
-5mol/L): 0.5,1,3,7,20,30, by the D of each concentration gradient
4normal hexane is sample introduction in the gas chromatograph of the same terms, obtains external standard D
4chromatogram, as shown in Figure 3, the expression formula obtaining concentration (x) and peak area (y) with origin matching is:
y＝0.63807x+0.20502
The value of a, b that table 2Origin simulates and standard deviation thereof
| Numerical value | Standard deviation | |
| b | 0.20502 | 0.15725 |
| a | 0.63807 | 0.01098 |
(6) D in extract is obtained by above formula
4concentration be 16.822 × 10
-5mol/L, then by other materials and D
4relative peak area ratio obtain its concentration and be: n
2, n
3, n
4n
15, summation n
1+ n
2+ n
3+ n
4+ ... + n
15=N, N are the total concentration of silicon rubber small molecular.
Silicon rubber Small molecular total concentration result of calculation in table 3 the present embodiment
| Concentration (10 -5mol/L) | |
| n 1 | 16.822 |
| n 2 | 6.268 |
| n 3 | 7.348 |
| n 4 | 5.511 |
| n 5 | 5.892 |
| n 6 | 5.764 |
| n 7 | 12.468 |
| n 8 | 77.251 |
| n 9 | 182.119 |
| n 10 | 318.312 |
| n 11 | 445.516 |
| n 12 | 507.274 |
| n 13 | 523.474 |
| n 14 | 546.108 |
| n 15 | 615.366 |
| N | 3275.493 |
Embodiment 3
Step (1) arrives (3) with embodiment 2.
(4) sample introduction in Agilent-6890 gas chromatograph, arranges supremacy clause of the present invention, obtains the chromatogram of extract, marks peak position and the retention time of chromatographic peak, and the retention time at second peak is 8.586min (D
5retention time).The peak area being calculated this peak by gas chromatography special software is 4.076, obtains the peak area ratio of peak area with this peak at other peaks, as following table 4 simultaneously.
The retention time of the peak area of each chromatographic peak of table 4, peak area and with external standard D
4peak area ratio
| Sequence number | Retention time | Peak area | (D relatively 5) peak area ratio |
| 1 | 7.131 | 10.939 | 2.684 |
| 2 | 8.586 | 4.076 | 1.000 |
| 3 | 9.848 | 4.778 | 1.172 |
| 4 | 10.94 | 3.583 | 0.879 |
| 5 | 11.758 | 3.831 | 0.940 |
| 6 | 12.593 | 3.748 | 0.920 |
| 7 | 13.708 | 8.107 | 1.989 |
| 8 | 14.805 | 50.233 | 12.324 |
| 9 | 15.458 | 118.424 | 29.054 |
| 10 | 16.183 | 206.985 | 50.781 |
| 11 | 17.03 | 289.700 | 71.075 |
| 12 | 18.055 | 329.859 | 80.927 |
| 13 | 19.345 | 340.393 | 83.512 |
| 14 | 20.997 | 355.111 | 87.122 |
| 15 | 23.139 | 400.146 | 98.171 |
(5) D5 is selected to be external standard, following 6 concentration gradients (10 of preparation
-5mol/L): 0.5,1,3,7,20,30, by the D5 normal hexane of each concentration gradient sample introduction in the gas chromatograph of the same terms, obtain the chromatogram of external standard D5, as shown in Figure 4, obtaining concentration (x) with origin matching with the expression formula of peak area (y) is:
y＝0.6411x+0.26911
The value of a, b that table 5Origin simulates and standard deviation thereof
| Numerical value | Standard deviation | |
| b | 0.26911 | 0.11186 |
| a | 0.6411 | 0.00781 |
(6) concentration obtaining D5 in extract by above formula is 5.938 × 10
-5mol/L, then obtain its concentration by other materials with the relative peak area ratio of D5 and be: n
2, n
2, n
3, n
4n
15, summation n
1+ n
2+ n
3+ n
4+ ... + n
15=N, N are the total concentration of silicon rubber small molecular.
Silicon rubber Small molecular total concentration result of calculation in table 6 the present embodiment
| Concentration (10 -5mol/L) | |
| n 1 | 15.936 |
| n 2 | 5.938 |
| n 3 | 6.961 |
| n 4 | 5.220 |
| n 5 | 5.581 |
| n 6 | 5.460 |
| n 7 | 11.810 |
| n 8 | 73.180 |
| n 9 | 172.523 |
| n 10 | 301.540 |
| n 11 | 422.041 |
| n 12 | 480.545 |
| n 13 | 495.891 |
| n 14 | 517.333 |
| n 15 | 582.941 |
| N | 3102.901 |
Embodiment 4
Step (1) arrives (3) with embodiment 2.
(4) sample introduction in Agilent-6890 gas chromatograph, arranges supremacy clause of the present invention, with embodiment 2, obtains the chromatogram of extract, marks peak position and the retention time of chromatographic peak, and the retention time at second peak is 9.848min (D
6retention time).The peak area being calculated this peak by gas chromatography special software is 4.787, obtains the peak area ratio of peak area with this peak at other peaks, as following table 7 simultaneously.
The retention time of the peak area of each chromatographic peak of table 7, peak area and with external standard D
4peak area ratio
| Sequence number | Retention time | Peak area | (D relatively 6) peak area ratio |
| 1 | 7.131 | 10.939 | 2.289 |
| 2 | 8.586 | 4.076 | 0.853 |
| 3 | 9.848 | 4.778 | 1.000 |
| 4 | 10.94 | 3.583 | 0.750 |
| 5 | 11.758 | 3.831 | 0.802 |
| 6 | 12.593 | 3.748 | 0.784 |
| 7 | 13.708 | 8.107 | 1.697 |
| 8 | 14.805 | 50.233 | 10.513 |
| 9 | 15.458 | 118.424 | 24.785 |
| 10 | 16.183 | 206.985 | 43.320 |
| 11 | 17.03 | 289.700 | 60.632 |
| 12 | 18.055 | 329.859 | 69.037 |
| 13 | 19.345 | 340.393 | 71.242 |
| 14 | 20.997 | 355.111 | 74.322 |
| 15 | 23.139 | 400.146 | 83.748 |
(5) D6 is selected to be external standard, following 6 concentration gradients (10 of preparation
-5mol/L): 0.5,1,3,7,20,30, by the D6 normal hexane of each concentration gradient sample introduction in the gas chromatograph of the same terms, obtain the chromatogram of external standard D6, as shown in Figure 5, obtaining concentration (x) with origin matching with the expression formula of peak area (y) is:
y＝0.64965x+0.26788
The value of a, b that table 8Origin simulates and standard deviation thereof
| Numerical value | Standard deviation | |
| b | 0.26788 | 0.10883 |
| a | 0.64965 | 0.0076 |
(6) concentration obtaining D6 in extract by above formula is 6.942 × 10
-5mol/L, then obtain its concentration by other materials with the relative peak area ratio of D6 and be: n
2, n
3, n
4n
15, summation n
1+ n
2+ n
3+ n
4+ ... + n15=N, N are the total concentration of silicon rubber small molecular.
Silicon rubber Small molecular total concentration result of calculation in table 9 the present embodiment
| Concentration (10 -5mol/L) | |
| n 1 | 15.894 |
| n 2 | 5.922 |
| n 3 | 6.942 |
| n 4 | 5.206 |
| n 5 | 5.566 |
| n 6 | 5.446 |
| n 7 | 11.779 |
| n 8 | 72.988 |
| n 9 | 172.069 |
| n 10 | 300.748 |
| n 11 | 420.932 |
| n 12 | 479.283 |
| n 13 | 494.589 |
| n 14 | 515.974 |
| n 15 | 581.409 |
| N | 3094.748 |
Above embodiment is only for setting forth the present invention, and protection scope of the present invention is not only confined to above embodiment.Those skilled in the art, according to above content disclosed by the invention and scope that each parameter is got, all can realize object of the present invention.
Claims (8)
1. a method for quantitative test composite insulator silicon rubber small molecular total concentration, is characterized in that comprising the following steps:
(1) choose composite insulator silicon rubber sample, drying after cleaning, adopt the Small molecular in solvent extraction process extraction silicon rubber sample, repeatedly extracting is complete to extraction;
(2) extract of repeatedly extracting is merged, constant volume after concentrated;
(3) get extract after constant volume, adopt gas chromatograph sampling, obtain the chromatogram of silicon rubber sample, mark peak position and the retention time of each chromatographic peak in chromatogram, and calculate the peak area of each chromatographic peak;
(4) choose external standard, prepare the solution that one group has concentration gradient, adopt the gas chromatograph condition sample introduction of same step (3), make the concentration-peak area typical curve of external standard;
(5) according to the concentration-peak area typical curve of external standard in step (4), and the peak area of each chromatographic peak in step (3), calculate the concentration of each chromatographic peak, the concentration of each chromatographic peak is added, is composite insulator silicon rubber small molecular total concentration.
2. the method for quantitative test composite insulator silicon rubber small molecular total concentration according to claim 1, is characterized in that: adopt normal hexane during cleaning in step (1), and when adopting solvent extraction process to extract, described solvent is normal hexane.
3. the method for quantitative test composite insulator silicon rubber small molecular total concentration according to claim 1, it is characterized in that: in step (1) repeatedly extracting to when extracting complete, when after the Small molecular that first time adopts in solvent extraction process extraction silicon rubber sample, silicon rubber sample is carried out vacuum drying, obtains quality m
1, and then repeat to adopt the Small molecular step in solvent extraction process extraction silicon rubber sample, and silicon rubber sample is carried out vacuum drying, obtain quality m
2, as (m
2-m
1) value when being tending towards constant, then the Small molecular in silicon rubber sample is extracted out completely.
4. the method for quantitative test composite insulator silicon rubber small molecular total concentration according to claim 3, is characterized in that: vacuum drying temperature is 70 DEG C ~ 90 DEG C, and the vacuum drying time is 18 ~ 48h.
5. the method for quantitative test composite insulator silicon rubber small molecular total concentration according to claim 1, it is characterized in that: in step (3) ~ step (4), gas chromatograph adopts Agilent-6890 gas chromatograph, and the parameters of this gas chromatograph is: chromatographic column: HP-5; Injector temperature: 280 DEG C; Split ratio: 10:1; Heating schedule: initial temperature 50 DEG C, retains 3min, is then warming up to 200 DEG C with the speed of 20 DEG C/min, then retains 0.5min; FID:280 DEG C, sample size: 1 μ L.
6. the method for quantitative test composite insulator silicon rubber small molecular total concentration according to claim 1, is characterized in that: the retention time of the some chromatographic peaks in step (4) in the retention time of this external standard of selection demand fulfillment of external standard and the chromatogram of the middle silicon rubber sample of step (3) is identical.
7. the method for quantitative test composite insulator silicon rubber small molecular total concentration according to claim 6, is characterized in that: described external standard is D4, D5 or D6.
8. the method for the quantitative test composite insulator silicon rubber small molecular total concentration according to claim 6 or 7, it is characterized in that: step chooses external standard in (4), prepare one group when there is the solution of concentration gradient, the following condition of concentration demand fulfillment of external standard: in step (3) silicon rubber sample chromatogram in the chromatographic peak identical with described external standard retention time concentration should this group there is the solution of concentration gradient between maximum concentration and least concentration.
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| CN115112794A (en) * | 2022-06-22 | 2022-09-27 | 青岛中海博睿检测技术服务有限公司 | Method for measuring content of dibutylamine in rubber product |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2011102903A1 (en) * | 2010-02-18 | 2011-08-25 | Bima Limited | Immobilised-bead immunomultiplex assay |
| CN104111288A (en) * | 2014-06-19 | 2014-10-22 | 广东电网公司电力科学研究院 | Method for measuring siloxane small molecules in composite insulator silicone rubber |
| CN104237299A (en) * | 2014-08-11 | 2014-12-24 | 广东电网公司电力科学研究院 | Thermal analysis method for measuring contents of polydimethylsiloxane (PDMS), SiO2 and aluminum hydroxide (ATH) in silicone rubber composite insulator |
| CN104713844A (en) * | 2015-03-30 | 2015-06-17 | 武汉大学 | Method for evaluating composite insulator silicone rubber aging degree based on Fourier infrared spectroscopy |
-
2015
- 2015-11-13 CN CN201510777616.4A patent/CN105259271A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2011102903A1 (en) * | 2010-02-18 | 2011-08-25 | Bima Limited | Immobilised-bead immunomultiplex assay |
| CN104111288A (en) * | 2014-06-19 | 2014-10-22 | 广东电网公司电力科学研究院 | Method for measuring siloxane small molecules in composite insulator silicone rubber |
| CN104237299A (en) * | 2014-08-11 | 2014-12-24 | 广东电网公司电力科学研究院 | Thermal analysis method for measuring contents of polydimethylsiloxane (PDMS), SiO2 and aluminum hydroxide (ATH) in silicone rubber composite insulator |
| CN104713844A (en) * | 2015-03-30 | 2015-06-17 | 武汉大学 | Method for evaluating composite insulator silicone rubber aging degree based on Fourier infrared spectroscopy |
Non-Patent Citations (5)
| Title |
|---|
| T. TANAKA 等: "Polymer Nanocomposites as Dielectrics and Electrical Insulation-perspectives for Processing Technologies,Material Characterization and Future Applications", 《 TRANSACTIONS ON DIELECTRICS AND ELECTRICAL INSULATION》 * |
| 张彬 等: "纯中定剂作外标气相色谱法测定火药内的中定剂含量", 《理化检验（化学分册）》 * |
| 景治中 等: "有机硅橡胶裂解产物气相色谱-质谱联用分析", 《分析测试学报》 * |
| 袁丽凤 等: "气相色谱法测定橡胶制品中短链氯化石蜡含量", 《理化检验（化学分册）》 * |
| 邓冰: "GC-PFPD法测定炼厂气中微量硫化物", 《石油化工技术与经济》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115112794A (en) * | 2022-06-22 | 2022-09-27 | 青岛中海博睿检测技术服务有限公司 | Method for measuring content of dibutylamine in rubber product |
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