CN106525551B - The preparation method of soluble organic fraction in a kind of artificial pollution test - Google Patents
The preparation method of soluble organic fraction in a kind of artificial pollution test Download PDFInfo
- Publication number
- CN106525551B CN106525551B CN201611050312.9A CN201611050312A CN106525551B CN 106525551 B CN106525551 B CN 106525551B CN 201611050312 A CN201611050312 A CN 201611050312A CN 106525551 B CN106525551 B CN 106525551B
- Authority
- CN
- China
- Prior art keywords
- soluble
- salt
- ion
- content
- filth
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
- 238000012360 testing method Methods 0.000 title claims abstract description 39
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 150000002500 ions Chemical class 0.000 claims abstract description 62
- 239000000203 mixture Substances 0.000 claims abstract description 31
- 150000003839 salts Chemical group 0.000 claims abstract description 19
- 238000000034 method Methods 0.000 claims description 24
- 150000001768 cations Chemical class 0.000 claims description 11
- 150000001450 anions Chemical class 0.000 claims description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 9
- 238000004458 analytical method Methods 0.000 claims description 8
- 238000001914 filtration Methods 0.000 claims description 8
- 238000005070 sampling Methods 0.000 claims description 8
- 229910021642 ultra pure water Inorganic materials 0.000 claims description 8
- 239000012498 ultrapure water Substances 0.000 claims description 8
- 239000007788 liquid Substances 0.000 claims description 7
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 5
- 238000010828 elution Methods 0.000 claims description 5
- 238000004090 dissolution Methods 0.000 claims description 4
- 239000012530 fluid Substances 0.000 claims description 4
- 238000004255 ion exchange chromatography Methods 0.000 claims description 4
- 238000010829 isocratic elution Methods 0.000 claims description 4
- 239000004570 mortar (masonry) Substances 0.000 claims description 4
- 125000002091 cationic group Chemical group 0.000 claims description 3
- 230000010355 oscillation Effects 0.000 claims description 3
- 230000008859 change Effects 0.000 claims description 2
- 238000001035 drying Methods 0.000 claims description 2
- 239000004615 ingredient Substances 0.000 abstract description 19
- 238000011109 contamination Methods 0.000 abstract description 15
- 238000010998 test method Methods 0.000 abstract description 3
- 229910052925 anhydrite Inorganic materials 0.000 description 18
- 239000012212 insulator Substances 0.000 description 18
- 229910019142 PO4 Inorganic materials 0.000 description 14
- 239000000243 solution Substances 0.000 description 11
- 239000011575 calcium Substances 0.000 description 10
- 238000011160 research Methods 0.000 description 8
- TWRXJAOTZQYOKJ-UHFFFAOYSA-L magnesium chloride Substances [Mg+2].[Cl-].[Cl-] TWRXJAOTZQYOKJ-UHFFFAOYSA-L 0.000 description 7
- 239000000126 substance Substances 0.000 description 7
- 150000003863 ammonium salts Chemical class 0.000 description 5
- 229910001629 magnesium chloride Inorganic materials 0.000 description 5
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 4
- 238000009422 external insulation Methods 0.000 description 4
- 238000002386 leaching Methods 0.000 description 4
- 230000009467 reduction Effects 0.000 description 4
- 238000004088 simulation Methods 0.000 description 4
- 159000000003 magnesium salts Chemical class 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 2
- 229910017677 NH4H2 Inorganic materials 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 239000001110 calcium chloride Substances 0.000 description 2
- 229910001628 calcium chloride Inorganic materials 0.000 description 2
- 159000000007 calcium salts Chemical class 0.000 description 2
- OSGAYBCDTDRGGQ-UHFFFAOYSA-L calcium sulfate Chemical compound [Ca+2].[O-]S([O-])(=O)=O OSGAYBCDTDRGGQ-UHFFFAOYSA-L 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 230000005611 electricity Effects 0.000 description 2
- 239000003480 eluent Substances 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 229910052731 fluorine Inorganic materials 0.000 description 2
- 239000011737 fluorine Substances 0.000 description 2
- 239000006210 lotion Substances 0.000 description 2
- 238000012423 maintenance Methods 0.000 description 2
- 230000007246 mechanism Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000010452 phosphate Substances 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 239000011780 sodium chloride Substances 0.000 description 2
- 239000013589 supplement Substances 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- 239000005995 Aluminium silicate Substances 0.000 description 1
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 235000012211 aluminium silicate Nutrition 0.000 description 1
- LFVGISIMTYGQHF-UHFFFAOYSA-N ammonium dihydrogen phosphate Chemical compound [NH4+].OP(O)([O-])=O LFVGISIMTYGQHF-UHFFFAOYSA-N 0.000 description 1
- 230000003373 anti-fouling effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- ZCCIPPOKBCJFDN-UHFFFAOYSA-N calcium nitrate Inorganic materials [Ca+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ZCCIPPOKBCJFDN-UHFFFAOYSA-N 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 230000002596 correlated effect Effects 0.000 description 1
- 230000000875 corresponding effect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 229910052602 gypsum Inorganic materials 0.000 description 1
- 239000010440 gypsum Substances 0.000 description 1
- XLYOFNOQVPJJNP-ZSJDYOACSA-N heavy water Substances [2H]O[2H] XLYOFNOQVPJJNP-ZSJDYOACSA-N 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000012266 salt solution Substances 0.000 description 1
- 238000009938 salting Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/38—Diluting, dispersing or mixing samples
Landscapes
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
The present invention provides a kind of preparation method of soluble-salt in artificial pollution.Nature filth sample composition is analyzed, determines the composition of salt, sequence, by Ca2+And SO4 2‑It is matched, remaining Ca2+Or SO4 2‑For use；By NH4 +With NO3 ‑It is matched, remaining NH4 +Or NO3 ‑For use；By remaining ion and residual ion in filth, matched according to the principle of " prepare soluble-salt and guarantee that its ion concentration sequence is basically unchanged "；According to above-mentioned pairing result configuration soluble-salt to get.The present invention not only contains soluble zwitterion in nature filth, and mass content sequence of the soluble zwitterion in filth is consistent with testing result.Compared to existing artificial pollution-test method, not only closer to the filthy ingredient after Natural contamination, but also simplicity is easy to get, easily operated.Step is simple and convenient to operate, is practical.
Description
Technical field
The invention belongs to electric power project engineering field, in particular to the preparation of soluble organic fraction in a kind of artificial pollution test
Method.
Background technique
Since environmental degradation causes insulator dirty degree to increase, the safety and stablization of electric system are seriously threatened.State at present
The parameter of inside and outside common characterization insulator contamination feature mainly has: equivalent salt density, pollution layer conductivity, leakage current and flashover field
It is strong etc., wherein equivalent salt density is one of the common evaluation criterion for studying insulator contamination degree.It is in recent years the study found that filthy
There are greatest differences between the pollution degree and practical pollution degree that component difference assesses equivalent salt density, cause external insulation design with
The actual effect of day-to-day operation maintenance is undesirable, and the difference of soluble component will lead to insulator dielectric performance in insulator contamination
There is bigger difference.Different filth ingredients are different from NaCl to the contribution of pollution layer conductivity, and being used as using single filthy ingredient can
Molten substance cannot intuitively find out contribution of such substance to pollution layer conductivity, in addition, with filth ingredient ratios different in soluble salt
Example changes, and the pollution flashover voltage for mixing soluble salt can also change.It is thus impossible to simply study insulation with salt density value
The Flashover Characteristics of son, it is necessary to filthy specific chemical component is included in research category, more effectively to carry out antifouling work, ground
Insulator contamination soluble component is studied carefully to research external insulation performance and mechanism important in inhibiting.
Artificial pollution test can simulate Natural contamination process, make test product surface by artificial contamination and be sufficiently humidified so as to, and
The test that high voltage examines its electrical properties is applied to test product, is widely applied in power external insulation research.Soluble-salt ingredient
And content be influence lending analysis one of principal element, and influence artificial pollution test's equivalence key factor it
One.Insulator contamination testing standard includes GB/T 4585-2004/IEC 60507:1991, GB/T 22707-2008/ at present
IEC61245:1993 and DL/T 859-2004.Solid layer method in these standards is all using NaCl as salting liquid, with one
Fixed kaolin or diatomite and water are mixed to form artificial pollution.Also research is obtaining flashover voltage and pollution degree relational expression
On the basis of, it adds referring factors, the filthy ingredients such as filthy ingredient, filthy distribution and mainly considers with CaSO4For the divalent salts of representative.
For these types of method all without the practical composition for considering nature filth comprehensively, therefore, it is difficult to really realize artificial pollution and filth naturally
Equivalence.
Thus, it is thus proposed that by simulation nature filth salt composition, make selected soluble salts as close possible to institute
The natural filthy situation of research area, but due to testing cumbersome, standard disunity, practicability is poor.
Summary of the invention
In order to overcome above-mentioned deficiency, the present invention provides a kind of preparation method of artificial pollution.Pass through the determination of main component
Divide the determination of similarity with soluble salt, while realizing the reduction and equivalence of nature filth to the maximum extent, greatly improved and match
Efficiency processed and accuracy, the research for artificial pollution and the equivalence question of natural pollution test provide important experiment branch
It holds.
Since existing water-soluble filthy ingredient is with Ca2+And SO4 2-Based on, and gypsum (CaSO is determined in XRD result4·
2H2O presence), therefore the invention proposes one kind particularly for such CaSO4Naturally filthy processing side as main component
Method, this method realizes such filthy reduction and equivalence naturally to the maximum extent, and then artificial pollution and nature is substantially improved
Filthy equivalence, while the accuracy of the insulator external insulation state evaluating result of artificial pollution test's acquisition is substantially improved,
Reference is provided for research Mechanism of Contamination Flashover, reduction pollution flashover accident.
To achieve the goals above, the present invention adopts the following technical scheme:
The preparation method of soluble-salt in a kind of artificial pollution, comprising:
1) nature filth sample composition is analyzed, the content of zwitterion is ranked up；
2) by Ca2+And SO4 2-It is matched, remaining Ca2+Or SO4 2-For use；
3) by NH4 +With NO3 -It is matched, remaining NH4 +Or NO3 -For use；
4) by remaining ion and residual ion in filth, according to " preparing soluble-salt and guarantee its ion concentration sequence base
This is constant " principle matched；
5) according to above-mentioned pairing result configuration soluble-salt to get.
Preferably, described " prepare soluble-salt and guarantee that its ion concentration is basically unchanged " method particularly includes:
A. using cation in remaining ion and residual ion and the highest ion of anion-content as a kind of characteristic ion；
B. by Na+、Mg2+、Cl-、K+、F-It is matched with a kind of characteristic ion, forms corresponding soluble-salt；
C. ion unpaired in filth matched, form soluble-salt；If pairing after, there are still it is unpaired from
Na can be used in son+、Mg2+、Cl-、K+、F-Or any ion in residual ion is matched with it, forms soluble-salt；
D. true respectively according to " percentage composition of the unique ion in source in the filthy sample in above-mentioned soluble-salt "
The proportion I of fixed each soluble-salt；
E. further according to " a kind of characteristic ion content and analysis experimental result are consistent or close, other zwitterion contents are suitable
Sequence is consistent with testing result " principle the proportion of soluble-salt is adjusted, obtain proportion II；
F. according to proportion II prepare soluble-salt to get.
" remaining ion " refers in the present invention: Ca is removed in filthy ingredient2+、SO4 2-、NH4 +Or NO3 -Ion in addition.
" residual ion " refers in the present invention: through above-mentioned steps 2 in filthy ingredient), 3) match after, remaining Ca2+、
SO4 2-、NH4 +Or NO3 -。
For the initial content of each ion of pairing according to the content of each ion in naturally filthy sample composition in the present invention
It determines.
Research shows that: such CaSO of Shandong District4Naturally generally at least contain Ca in filth as main component2+With
SO4 2-、NH4 +、Na+、Mg2+、Cl-、NO3 -、K+、F-Therefore plasma and content is relatively stable preferentially selects above-mentioned in the present invention
Ion is matched with a kind of characteristic ion.
It is furthermore preferred that in step d, the specific steps of the adjustment are as follows:
According to content sequence cationic in test result, the soluble-salt content formed to proportion I is adjusted；According to
The content sequence of anion in test result is adjusted the composition ratio of each salt in the soluble-salt of the composition of said ratio I；
Or the content sequence according to anion in test result, the soluble-salt content formed to proportion I are adjusted；
According to content sequence cationic in test result, the composition ratio of each salt is carried out in the soluble-salt formed to said ratio I
Adjustment.
Preferably, the specific steps of the analysis nature filth sample composition are as follows:
(1) it is the true integrality for guaranteeing sample, filth is swept down using hard hair brush, is accepted, is wrapped with pan paper,
It is fitted into dedicated valve bag and stores immediately.Before test, filthy sample is first crossed into 150 meshes, be placed in baking oven, 105 DEG C
Drying for 24 hours, then with agate mortar is ground.It accurately weighs 0.2g filth sample to be dissolved in 60ml ultrapure water, 80 DEG C of water bath sonicator vibrations
It swings 30min and promotes water-soluble composition dissolution in sample, stand 30min, quantitative filter paper filtering, filtered fluid is settled to ultrapure water
100ml.Solution is into first crossing 0.22 μm of filtering head before ion chromatography；
(2) anion-content in sample, the technological parameter of the IC test are as follows: IonPac AG18 are measured
Capillary guard column (50 × 0.4mm), IonPac AS18 Capillary analytical column (250 × 0.4mm)；Leacheate: EG-
KOH capillary elutes the KOH solution that liquid generator generates, gradient elution: 0~2min, 1mmol/L；2~35min, 1~
30mmol/L；35~40min, 30~50mmol/L；40~45min, 50mmol/L；45~48min, 1mmol/L.Suppressor electricity
Flow 11mA；Column temperature: 30 DEG C；Flow velocity: 10 μ L/min；Sampling volume: 0.4 μ L；
(3) cations location parameter: IonPac CG16 Capillary guard column (50 × 0.4mm, the U.S.
Thermo Fisher company), (250 × 0.4mm, U.S. Thermo Fisher are public for IonPac CS16 Capillary analytical column
Department)；Leacheate: EG-MSA capillary elutes the MSA solution that liquid generator generates, isocratic elution: 35min, flow 20mmol/
L, 10 μ L/min of flow velocity.Suppressor electric current 7mA；Sampling volume: 0.4 μ L；Column temperature: 30 DEG C.
Now studies have shown that: in the filthy ingredient of Shandong District, Ca2+With SO4 2-Mass content than about in 1:2 or so, with
CaSO4Middle Ca2+With SO4 2-Mass ratio 1:2.4 it is very close.In addition, it can clearly be seen that CaSO in XRD analysis result4Peak, i.e.,
Contain CaSO in the naturally filthy chemical component of insulator4.Consider based on the above reasons, by Ca2+With SO4 2-Pairing, further really
Determine CaSO4Mass content.Extra Ca2+Or SO4 2-Soluble-salt can be formed with remaining ion, supplement its quality.
A large number of experiments proves, Ca in Shandong District filth water soluble ingredient2+、NH4 +、SO4 2-、NO3 -For content higher four
Kind ion.For ammonium salt (NH4 +), consider NH4 +Content Ca is only second in water-soluble cationic2+, therefore content is selected first
Higher anion is matched with it, i.e., selects the NO of anion mass content second first3 -It is paired, can according to situation according to
NH4 +Or NO3 -Content calculate NH4NO3Quality, remaining NH4 +Or NO3 -Soluble-salt can be formed with remaining ion, supplement it
Quality.
As a result, in artificial pollution soluble-salt, CaSO4With NH4NO3It is main component determining first.Remaining ion according to
The principle prepared soluble-salt and guarantee that its ion concentration is basically unchanged is matched.Can continue according to anion or cation
Content sequence carries out soluble-salt pairing.
Heretofore described " soluble-salt " is water-soluble salt.
The present invention also provides the artificial pollution soluble-salts of any of the above-described method preparation.
The present invention also provides above-mentioned artificial pollution soluble salt solutions answering in the artificial pollution test of insulator
With.Since preparation method of the invention is simple, good with filthy equivalence naturally, insulator can be widely used in
Artificial pollution test.
Method of the invention is suitable for the insulator contamination of any material, any grade.
The present invention also provides above-mentioned artificial pollution soluble-salt AC system high-tension insulator artificial pollution
Application in test.
The present invention also provides above-mentioned artificial pollution soluble-salt direct current system high-tension insulator artificial pollution
Application in test.
The present invention also provides above-mentioned artificial pollution soluble-salts in the artificial of high-voltage alternating system composite insulator
Application in pollution test.
Beneficial effects of the present invention
(1) present invention provides a kind of preparation method of artificial pollution soluble-salt.Method provided by the invention can be maximum
Realize to limit the reduction and equivalence of nature filth soluble-salt.
(2) present invention retains the filthy existing principal component of nature, and residual ion is carried out soluble-salt pairing.
(3) present invention not only contains soluble zwitterion in nature filth, and soluble zwitterion is in filth
Mass content sequence it is consistent with testing result.Compared to existing artificial pollution-test method, not only closer to Natural contamination
Filthy ingredient afterwards, and simplicity is easy to get, it is easily operated.
(4) the different kinds of ions mass content after present invention pairing can realize the mass content base with each ion in filth naturally
This is consistent.
(5) preparation method of the present invention is simple, confecting efficiency is high, practical, easy to spread.
(6) have a wide range of application, the transmission line of electricity suitable for the various charged species of various grades.
Specific embodiment
Feature of present invention and other correlated characteristics are described in further detail by the following examples, in order to the same industry
The understanding of technical staff:
Embodiment 1
By taking the operation insulator contamination ingredient obtained in the transmission tower that certain base often pollution flashover occurs as an example:
Wherein certain part of filthy sample component analyzes result such as table 1, intends preparing 10g artificial pollution:
The filthy sample component of certain part of table 1 analyzes result
| Ion title | Ca2+ | NH4 + | K+ | Na+ | Mg2+ |
| Mass percent (%) | 7.59 | 0.71 | 0.27 | 0.18 | 0.12 |
| Ion title | SO4 2- | NO3 - | Cl- | F- | PO4 3- |
| Mass percent (%) | 17.61 | 1.52 | 0.35 | 0.35 | 0.11 |
Calculating process is as follows:
(1) as can be seen from the above results, Ca2+With SO4 2-Mass content ratio be 1:2.3, with CaSO4Middle Ca2+With SO4 2-
Mass ratio 1:2.4 it is very close.With SO4 2-Mass content calculate 10g artificial pollution in CaSO4Quality be 2.49g, this
When Ca2+Content is 7.32%, almost the same with 1 result of table.
(2) NH is selected4NO3As soluble ammonium salt.With NH4 +Mass content calculate 10g artificial pollution in NH4NO3Matter
Amount is 0.32g, at this time NO3 -Content be 2.48%.
(3) MgCl is selected2As soluble magnesium salt.With Mg2+Mass content calculate 10g artificial pollution in MgCl2Matter
Amount is 0.05g, at this time Cl-Content be 0.37%.
(4) selection KF provides F-And K+.With K+Mass content calculate 10g artificial pollution in KF quality be 0.04g, this
When F-Content is 0.13%.Lower than nature filth content.Simultaneous selection NaF and KF is as fluorine-containing salts, respectively with Na+Contain with the amount of K
The quality that amount calculates NaF and KF in 10g artificial pollution is respectively 0.03g and 0.04g, at this time F-Content is 0.27%, is still below
Naturally filthy content.0.05gKF, 0.04gNaF are chosen, then F-Content rises to 0.34%, consistent with naturally filthy content.This
When K+Content is 0.34%, Na+Content is 0.22%.
(5) common water-soluble substances NH is taken4H2PO4Phosphate is provided.With PO4 3-Mass content calculate 10g artificial pollution
Middle NH4H2PO4Quality be 0.01g.NH at this time4H2PO4And NH4NO3NH is provided simultaneously4 +, final NH4 +Content be 0.74%.
The preparation program for obtaining 10g artificial pollution by above procedure is as follows:
Table 2 is according to filthy composition analysis result simulation artificial pollution Initial Composition proportion
| Title | CaSO4 | NH4NO3 | MgCl2 | KF | NaF | NH4H2PO4 |
| Quality (g) | 2.49 | 0.32 | 0.05 | 0.05 | 0.04 | 0.01 |
It is matched according to above, each mass of ion content such as table 3:
Each mass of ion content in 3 artificial pollution of table proportion
| Ion title | Ca2+ | NH4 + | K+ | Na+ | Mg2+ |
| Mass percent (%) | 7.32 | 0.74 | 0.34 | 0.22 | 0.12 |
| Ion title | SO4 2- | NO3 - | Cl- | F- | PO4 3- |
| Mass percent (%) | 17.61 | 2.48 | 0.37 | 0.34 | 0.11 |
Contrast table 3 and table 1 are as can be seen that the program not only contains all soluble zwitterions, and soluble yin
Mass content of the cation in filth and filth naturally are almost the same.Compared to existing artificial pollution test's method, not only more
Close to the filthy ingredient after Natural contamination, and simplicity is easy to get, easily operated.
Wherein, naturally filthy method for measuring components is as follows:
For the true integrality for guaranteeing sample, filth is swept down using hard hair brush, is accepted, is wrapped with pan paper, with
It is fitted into dedicated valve bag and stores.Before test, filthy sample is first crossed into 150 meshes, be placed in baking oven, 105 DEG C baking
It does for 24 hours, then ground with agate mortar.It accurately weighs 0.2g filth sample to be dissolved in 60ml ultrapure water, 80 DEG C of water bath sonicator oscillations
30min promotes water-soluble composition dissolution in sample, stands 30min, quantitative filter paper filtering, and filtered fluid is settled to 100ml with ultrapure water.
Solution is into first crossing 0.22 μm of filtering head before ion chromatography.
Measure the anion-content in sample, the technological parameter of the IC test are as follows: IonPac AG18 Capillary is protected
Guard post (50 × 0.4mm), IonPac AS18 Capillary analytical column (250 × 0.4mm)；Leacheate: EG-KOH capillary leaching
The KOH solution that eluent generator generates, gradient elution: 0~2min, 1mmol/L；2~35min, 1~30mmol/L；35~
40min, 30~50mmol/L；40~45min, 50mmol/L；45~48min, 1mmol/L.Suppressor electric current 11mA；Column temperature:
30℃；Flow velocity: 10 μ L/min；Sampling volume: 0.4 μ L.
Cations location parameter: IonPac CG16 Capillary guard column (50 × 0.4mm, U.S. Thermo
Fisher company), IonPac CS16 Capillary analytical column (250 × 0.4mm, Thermo Fisher company, the U.S.)；Leaching
Washing lotion: EG-MSA capillary elutes the MSA solution that liquid generator generates, isocratic elution: 35min, flow 20mmol/L, flow velocity
10μL/min.Suppressor electric current 7mA；Sampling volume: 0.4 μ L；Column temperature: 30 DEG C.
The detection of the soluble filthy concentration of insulator surface is limited to 0.001mmol/l in the present invention.
Embodiment 2
By taking the more complicated filthy sample of a ingredient as an example, chemical composition analysis result is as follows:
The filthy sample component of certain part of table 4 analyzes result
Calculating process is as follows:
(1) as can be seen from the above results, Ca2+With SO4 2-Mass content ratio be 1:1.94, compare CaSO4Middle Ca2+With
SO4 2-Mass ratio 1:2.4 high, show except CaSO4It is outer that there are also other calcium salts.With SO4 2-Mass content calculate 10g artificial pollution
Middle CaSO4Quality be 1.31g, at this time Ca2+Content is 3.85%, lower than the Ca in filth naturally2+Content 4.75%.
(2) NH is selected4NO3As soluble ammonium salt.With NH4 +Mass content calculate 10g artificial pollution in NH4NO3Matter
Amount is 0.16g, at this time NO3 -Content be 1.24%, lower than naturally filth in NO3 -Content 2.22%.
(3) Ca (NO is added3)2, with NO3 -Residual mass calculates Ca (NO3)2Content is 0.13g.Contain 1.31g simultaneously
CaSO4With 0.13g Ca (NO3)2When Ca2+Content is 4.17%, slightly below the actually detected value in table 4.It is appropriate to increase CaSO4With
Ca(NO3)2Content, by CaSO4Mass adjust- ment be 1.5g, Ca (NO3)2Mass adjust- ment is 0.15g, then Ca2+Content is
4.78%, it is consistent with actually detected value.SO at this time4 2-Content is 10.59%, NO3 -Content is 2.37%.
(4) MgCl is selected2As soluble magnesium salt.With Mg2+Mass content calculate 10g artificial pollution in MgCl2Matter
Amount is 0.08g, at this time Cl-Content be 0.60%.
(5) selection NaF provides F-And Na+.With Na+Mass content calculate the quality of NaF in 10g artificial pollution and be
0.06g, at this time F-Content is 0.27%.Lower than nature filth content.Simultaneous selection NaF and KF is as fluorine-containing salts, respectively with Na+
And K+Amount content to calculate the quality of NaF and KF in 10g artificial pollution be respectively 0.06g and 0.02g, F at this time-Content is
0.34%, it is still below nature filth content.0.03gKF, 0.07gNaF are chosen, then F-Content rises to 0.41%, with natural dirt
Dirty content is consistent.Na at this time+Content is 0.38%, K+Content is 0.20%.
(6) because of C2O4 2-And PO4 3-Content it is lower, in preparation program may be selected both soluble ammonium salt, Ji Nengti
For required anion, and it not will increase dramatically NH4 +Quality.Select water solubility (NH4)2C2O4C is provided2O4 2-, with C2O4 2-'s
Mass content calculates (NH in 10g artificial pollution4)2C2O4Quality be 0.03g.
(7) common water-soluble substances NH is taken4H2PO4Phosphate is provided.With PO4 3-Mass content calculate 10g artificial pollution
Middle NH4H2PO4Quality be 0.002g.NH at this time4H2PO4、(NH4)2C2O4And NH4NO3NH is provided simultaneously4 +, final NH4 +Contain
Amount is 0.45%.
The preparation program for obtaining 10g artificial pollution by above procedure is as follows:
Table 5 is according to filthy composition analysis result simulation artificial pollution Initial Composition proportion
It is matched according to above, each mass of ion content such as table 6:
Each mass of ion content in 6 artificial pollution of table proportion
| Ion title | Ca2+ | NH4 + | Na+ | K+ | Mg2+ | |
| Mass percent (%) | 4.78 | 0.45 | 0.38 | 0.2 | 0.2 | |
| Ion title | SO4 2- | NO3 - | Cl- | F- | C2O4 2- | PO4 3- |
| Mass percent (%) | 10.59 | 2.37 | 0.6 | 0.41 | 0.24 | 0.02 |
Contrast table 6 and table 4 are as can be seen that the program not only contains all soluble zwitterions, and soluble yin
Mass content of the cation in filth and filth naturally are almost the same.Compared to existing artificial pollution test's method, not only more
Close to the filthy ingredient after Natural contamination, and simplicity is easy to get, easily operated.
Embodiment 3
Certain converter station is in light filthy area, and water soluble salt content is relatively fewer.The dirt of maintenance acquisition in 2015 and 2016
Dirty sample, soluble-salt ingredient are almost the same.Pole II sample composition is analyzed as follows within 2016:
Certain the converter station pole of table 7 II filth sample composition analyzes result
| Ion title | Ca2+ | NH4 + | Na+ | K+ | Mg2+ |
| Mass percent (%) | 1.95 | 0.54 | 0.26 | 0.15 | 0.11 |
| Ion title | SO4 2- | NO3 - | Cl- | F- | C2O4 2- |
| Mass percent (%) | 3.95 | 1.93 | 0.59 | 0.12 | 0.17 |
(1) as can be seen from the above results, Ca2+With SO4 2-Mass content ratio be 1:2.03, compare CaSO4Middle Ca2+With
SO4 2-Mass ratio 1:2.4 it is slightly higher, show except CaSO4It is outer that there are also other calcium salts.With SO4 2-Mass content calculate 10g it is manually dirty
Dirty middle CaSO4Quality be 0.56g, at this time Ca2+Content is 1.65%, the slightly below naturally Ca in filth2+Content 1.95%.
(2) MgCl is selected2As soluble magnesium salt.With Mg2+Mass content calculate 10g artificial pollution in MgCl2Matter
Amount is 0.04g, at this time Cl-Content be 0.30%, be lower than actually detected value.
(3) CaCl is added2So that Ca2+Mass content and table 7 it is consistent, quality is with Ca2+Content (1.95%-1.65%
=0.30%) it calculates.CaCl need to be added20.08g.Contain 0.04g MgCl simultaneously2With 0.08g CaCl2When, Cl-Content be
0.81%.
(4) NH is selected4NO3As soluble ammonium salt.With NH4 +Mass content calculate 10g artificial pollution in NH4NO3Matter
Amount is 0.24g, at this time NO3 -Content be 1.86%, with it is naturally filthy in NO3 -Content is almost the same.
(5) selection NaF provides F-And Na+.With Na+Mass content calculate the quality of NaF in 10g artificial pollution and be
0.05g, at this time F-Content is 0.23%, though more slightly higher than actually detected value, the mass content sequence in anion is constant.
(6) water solubility K is selected2C2O4C is provided2O4 2-And K+, with K+Mass content calculate 10g artificial pollution in K2C2O4's
Quality is 0.03g.C at this time2O4 2-Content is 0.16%, almost the same with mass content in filth naturally.
The preparation program for obtaining 10g artificial pollution by above procedure is as follows:
Table 8 is according to filthy composition analysis result simulation artificial pollution Initial Composition proportion
| Title | CaSO4 | NH4NO3 | CaCl2 | MgCl2 | NaF | K2C2O4 |
| Quality (g) | 0.56 | 0.24 | 0.08 | 0.04 | 0.05 | 0.03 |
It is matched according to above, each mass of ion content such as table 9:
Each mass of ion content in 9 artificial pollution of table proportion
| Ion title | Ca2+ | NH4 + | Na+ | K+ | Mg2+ |
| Mass percent (%) | 1.95 | 0.54 | 0.26 | 0.15 | 0.11 |
| Ion title | SO4 2- | NO3 - | Cl- | F- | C2O4 2- |
| Mass percent (%) | 3.95 | 1.86 | 0.81 | 0.23 | 0.16 |
Contrast table 9 and table 7 are as can be seen that the program not only contains all soluble zwitterions, and soluble yin
Mass content of the cation in filth and filth naturally are almost the same.Compared to existing artificial pollution test's method, not only more
Close to the filthy ingredient after Natural contamination, and simplicity is easy to get, easily operated.
Naturally filthy method for measuring components described in three above example is as follows:
For the true integrality for guaranteeing sample, filth is swept down using hard hair brush, is accepted, is wrapped with pan paper, with
It is fitted into dedicated valve bag and stores.Before test, filthy sample is first crossed into 150 meshes, be placed in baking oven, 105 DEG C baking
It does for 24 hours, then ground with agate mortar.It accurately weighs 0.2g filth sample to be dissolved in 60ml ultrapure water, 80 DEG C of water bath sonicator oscillations
30min promotes water-soluble composition dissolution in sample, stands 30min, quantitative filter paper filtering, and filtered fluid is settled to 100ml with ultrapure water.
Solution is into first crossing 0.22 μm of filtering head before ion chromatography.
Measure the anion-content in sample, the technological parameter of the IC test are as follows: IonPac AG18 Capillary is protected
Guard post (50 × 0.4mm), IonPac AS18 Capillary analytical column (250 × 0.4mm)；Leacheate: EG-KOH capillary leaching
The KOH solution that eluent generator generates, gradient elution: 0~2min, 1mmol/L；2~35min, 1~30mmol/L；35~
40min, 30~50mmol/L；40~45min, 50mmol/L；45~48min, 1mmol/L.Suppressor electric current 11mA；Column temperature:
30℃；Flow velocity: 10 μ L/min；Sampling volume: 0.4 μ L.
Cations location parameter: IonPac CG16 Capillary guard column (50 × 0.4mm, U.S. Thermo
Fisher company), IonPac CS16 Capillary analytical column (250 × 0.4mm, Thermo Fisher company, the U.S.)；Leaching
Washing lotion: EG-MSA capillary elutes the MSA solution that liquid generator generates, isocratic elution: 35min, flow 20mmol/L, flow velocity
10μL/min.Suppressor electric current 7mA；Sampling volume: 0.4 μ L；Column temperature: 30 DEG C.
The detection of the soluble filthy concentration of insulator surface is limited to 0.001mmol/l in the present invention.
Finally it should be noted that the foregoing is only a preferred embodiment of the present invention, it is not limited to this hair
It is bright, although the present invention is described in detail referring to the foregoing embodiments, for those skilled in the art, still
It can modify to technical solution documented by previous embodiment, or part is equivalently replaced.It is all in this hair
Within bright spirit and principle, any modification, equivalent replacement, improvement and so on should be included in protection scope of the present invention
Within.Above-mentioned, although specific embodiments of the present invention have been described, and it is not intended to limit the protection scope of the present invention, institute
Category field technical staff should be understood that based on the technical solutions of the present invention those skilled in the art do not need to pay wound
The various modifications or changes that the property made labour can be made are still within protection scope of the present invention.
Claims (4)
1. the preparation method of soluble-salt in a kind of artificial pollution, comprising:
1) nature filth sample composition is analyzed, the content of zwitterion is ranked up；
2) by Ca2+And SO4 2-It is matched, remaining Ca2+Or SO4 2-For use；
3) by NH4 +With NO3 -It is matched, remaining NH4 +Or NO3 -For use；
4) by remaining ion and residual ion in filth, according to " preparing soluble-salt and guarantee its ion concentration sequence substantially not
The principle of change " is matched；
5) according to above-mentioned pairing result configuration soluble-salt to get；
Described " prepare soluble-salt and guarantee that its ion concentration is basically unchanged " method particularly includes:
A. using cation in remaining ion and residual ion and the highest ion of anion-content as a kind of characteristic ion；
B. by Na+、Mg2+、Cl-、K+、F-It is matched with a kind of characteristic ion, forms corresponding soluble-salt；
C. ion unpaired in filth matched, form soluble-salt；If after pairing, there are still unpaired ion,
Using Na+、Mg2+、Cl-、K+、F-Or any ion in residual ion is matched with it, forms soluble-salt；
D. it is determined respectively according to " percentage composition of the unique ion in source in the filthy sample in above-mentioned soluble-salt " each
The proportion I of soluble-salt；
E. further according to " a kind of characteristic ion content and analysis experimental result it is consistent or close, other zwitterion content sequences with
Testing result is consistent " principle the proportion of soluble-salt is adjusted, obtain proportion II；
F. according to proportion II prepare soluble-salt to get.
2. the method as described in claim 1, which is characterized in that in step d, the specific steps of the adjustment are as follows:
According to content sequence cationic in test result, the soluble-salt content formed to proportion I is adjusted；According to test
As a result the content sequence of middle anion is adjusted the composition ratio of each salt in the soluble-salt of the composition of said ratio I.
3. the method as described in claim 1, which is characterized in that in step d, the specific steps of the adjustment are as follows:
According to the content sequence of anion in test result, the soluble-salt content formed to proportion I is adjusted；According to test
As a result the content sequence of cation in is adjusted the composition ratio of each salt in the soluble-salt of the composition of said ratio I.
4. the method according to claim 1, which is characterized in that described to analyze the specific of nature filth sample composition
Step are as follows:
(1) it is the true integrality for guaranteeing sample, filth is swept down using hard hair brush, is accepted, is wrapped with pan paper, immediately
It is fitted into dedicated valve bag and stores；Before test, filthy sample is first crossed into 150 meshes, be placed in baking oven, 105 DEG C drying
For 24 hours, then with agate mortar it grinds；It accurately weighs 0.2g filth sample to be dissolved in 60ml ultrapure water, 80 DEG C of water bath sonicator oscillations
30min promotes water-soluble composition dissolution in sample, stands 30min, quantitative filter paper filtering, and filtered fluid is settled to 100 with ultrapure water
ml；Solution is into first crossing 0.22 μm of filtering head before ion chromatography；
(2) anion-content in sample, the technological parameter of IC test are as follows: IonPac AG18 Capillary guard column are measured
50 × 0.4mm, 250 × 0.4mm of IonPac AS18 Capillary analytical column；Leacheate: EG-KOH capillary leacheate occurs
The KOH solution that device generates, gradient elution: 0~2min, 1mmol/L；2~35min, 1~30mmol/L；35~40min, 30~
50mmol/L；40~45min, 50mmol/L；45~48min, 1mmol/L；Suppressor electric current 11mA；Column temperature: 30 DEG C；Flow velocity:
10μL/min；Sampling volume: 0.4 μ L；
(3) cations location parameter: IonPac CG16 Capillary 50 × 0.4mm of guard column, U.S. Thermo
Fisher company, IonPac CS16 Capillary 250 × 0.4mm of analytical column, Thermo Fisher company, the U.S.；Elution
Liquid: EG-MSA capillary elutes the MSA solution that liquid generator generates, isocratic elution: 35min, flow 20mmol/L, flow velocity 10
μL/min；Suppressor electric current 7mA；Sampling volume: 0.4 μ L；Column temperature: 30 DEG C.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611050312.9A CN106525551B (en) | 2016-11-24 | 2016-11-24 | The preparation method of soluble organic fraction in a kind of artificial pollution test |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611050312.9A CN106525551B (en) | 2016-11-24 | 2016-11-24 | The preparation method of soluble organic fraction in a kind of artificial pollution test |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN106525551A CN106525551A (en) | 2017-03-22 |
| CN106525551B true CN106525551B (en) | 2019-04-09 |
Family
ID=58357949
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201611050312.9A Active CN106525551B (en) | 2016-11-24 | 2016-11-24 | The preparation method of soluble organic fraction in a kind of artificial pollution test |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106525551B (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107677580A (en) * | 2017-08-28 | 2018-02-09 | 国网山东省电力公司电力科学研究院 | The method and pollution level of the filthy simulation in power transmission and transforming equipment operation area determine method |
| CN108845044A (en) * | 2018-05-03 | 2018-11-20 | 山东滨州智源生物科技有限公司 | The detection method of sodium content in a kind of sulfobutyl ether betadex sodium |
Family Cites Families (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0655769A1 (en) * | 1993-11-17 | 1995-05-31 | Hewlett-Packard Company | Method and apparatus for preparing an electrospray ion source sample |
| CN102288515A (en) * | 2011-07-29 | 2011-12-21 | 武汉大学 | Insulator dirt on-site sampling and contamination degree measuring method |
| CN102735582A (en) * | 2012-06-01 | 2012-10-17 | 华南理工大学 | Method for measuring contamination degree of surface of electric power insulator |
| CN103674990B (en) * | 2013-09-29 | 2016-08-17 | 广州供电局有限公司 | High-tension insulator filth method for measuring components |
| CN104181148A (en) * | 2014-08-29 | 2014-12-03 | 国家电网公司 | Method for determining soluble contamination components of insulators |
| CN104215551A (en) * | 2014-09-24 | 2014-12-17 | 南方电网科学研究院有限责任公司 | Method for testing natural pollution characteristics of high-voltage external-insulation device |
| CN105974284A (en) * | 2016-06-27 | 2016-09-28 | 中国电力科学研究院 | External insulation configuration method for EHV (extra-high voltage) icing region |
-
2016
- 2016-11-24 CN CN201611050312.9A patent/CN106525551B/en active Active
Also Published As
| Publication number | Publication date |
|---|---|
| CN106525551A (en) | 2017-03-22 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Zhou et al. | Characterizing and sourcing ambient PM2. 5 over key emission regions in China I: Water-soluble ions and carbonaceous fractions | |
| CN106525551B (en) | The preparation method of soluble organic fraction in a kind of artificial pollution test | |
| CN102565595B (en) | Method for judging aging degree of umbrella skirt of composite insulator | |
| Xu et al. | Kinetic determination of sedimentation for GMZ bentonite colloids in aqueous solution: Effect of pH, temperature and electrolyte concentration | |
| CN106786506B (en) | A kind of transmission line of electricity routing resource based on dunghill constituent analysis | |
| CN106442036B (en) | The preparation method of soluble-salt in a kind of artificial pollution | |
| CN104215551A (en) | Method for testing natural pollution characteristics of high-voltage external-insulation device | |
| CN107677580A (en) | The method and pollution level of the filthy simulation in power transmission and transforming equipment operation area determine method | |
| CN103196802B (en) | A kind of measuring method of filler sheet layer material radius-thickness ratio | |
| CN109030703A (en) | A kind of method of content of halogen in Oxygen Bomb Combustion-sulfate by ion chromatography cable nonmetallic materials | |
| Zhang et al. | Study on the flashover performance of various types of insulators polluted by nitrates | |
| CN109142865A (en) | Consider the frequency domain spectra discrimination method of paper oil insulation interfacial polarization equivalent circuit parameter | |
| CN103674990B (en) | High-tension insulator filth method for measuring components | |
| Derylo-Marczewska | Analysis of the adsorption equilibrium for the system dilute aqueous solution of dissociating organic substance-activated carbon | |
| CN102116767B (en) | Method for simultaneously measuring K, Ca and Mg in tobacco | |
| CN117538697A (en) | Artificial pollution simulation method for insulator considering pollution source property | |
| CN105203656A (en) | Shandong area insulator dirtiness water-soluble negative ion ingredient testing method | |
| Feilat et al. | ESDD-and DDDG-based assessment of insulator pollution levels in Oman | |
| CN105067745B (en) | Method for detecting dirty components through ion pairing based on fuzzy clustering | |
| Sacco et al. | Electrolyte viscosities in hexamethylphosphotriamide at 25° C | |
| CN111025091B (en) | Intelligent evaluation method for uneven damp state of urban distribution network cable | |
| Roger et al. | Effect of ionic condensation and interactions between humic substances on their mobility: An experimental and simulation study | |
| Loginova et al. | Microwave dielectric properties of aqueous solutions of potassium and cesium fluorides | |
| CN110905454B (en) | Hydrate reservoir interwell electricity dynamic monitoring simulation experiment device | |
| JP2018205125A (en) | Method and device for measuring soil corrosion speed |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |