CN106525551A - Method for preparing soluble salt in artificial pollution test - Google Patents
Method for preparing soluble salt in artificial pollution test Download PDFInfo
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- CN106525551A CN106525551A CN201611050312.9A CN201611050312A CN106525551A CN 106525551 A CN106525551 A CN 106525551A CN 201611050312 A CN201611050312 A CN 201611050312A CN 106525551 A CN106525551 A CN 106525551A
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- 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
Abstract
The invention provides a method for preparing a soluble salt in an artificial pollution test. The method comprises analyzing components of a natural pollutant sample to determine the composition of the salt, carrying out sorting, pairing Ca<2+> and SO4<2->, remaining the residual Ca<2+> and SO4<2-> for next use, pairing NH4<+> and NO3<->, remaining the residual NH4<+> and NO3<-> for next use, pairing other ions and the residual ions in the pollutant according to the principle of preparing soluble salts and ensuring that the ionic content order is essentially unchanged, and preparing a soluble salt according to the pairing results. The method utilizes soluble anions and cations in the natural pollutant and the order of the mass content of the soluble anions and cations in the pollutant is consistent with the test result. Compared with the existing artificial pollution test method, the method can produce a pollutant of which the components are close to those of a natural pollutant, utilizes simple and easily available raw materials, has simple processes, can be operated conveniently and has good practicality.
Description
Technical field
The invention belongs to electric power project engineering field, the preparation of soluble organic fraction in more particularly to a kind of artificial pollution test
Method.
Background technology
As ecological deterioration causes insulator dirty degree to increase, the serious safety and stablization for threatening power system.Current state
The parameter of inside and outside conventional sign 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 to study one of conventional evaluation criterion of insulator contamination degree.Research in recent years finds, filthy
Component difference cause equivalent salt density assessment pollution degree and actual pollution degree between there are greatest differences, cause external insulation design with
The actual effect that day-to-day operation is safeguarded is undesirable, and in insulator contamination, the difference of soluble component can cause insulator dielectric performance
There is bigger difference.Contribution of the different filth compositions to pollution layer conductivity is different from NaCl, using single filthy composition as can
Molten material can not intuitively find out contribution of this kind of material to pollution layer conductivity, additionally, with different filth composition ratios in soluble salt
Example changes, and the pollution flashover voltage for mixing soluble salt can also change.It is thus impossible to simply with salt density value studying insulation
The Flashover Characteristics of son, it is necessary to filthy specific chemical composition is included into research category, is more effectively to carry out antifouling work, is ground
Insulator contamination soluble component is studied carefully to studying external insulation performance and mechanism important in inhibiting.
Artificial pollution test can simulate Natural contamination process, test product surface is subject to artificial contamination and is sufficiently humidified so as to, and
The test that high voltage checks its electrical properties is applied to test product, is extensively applied in power external insulation research.Soluble-salt composition
And content is one of the principal element for affecting lending analysis, and affect artificial pollution test's equivalence key factor it
One.Insulator contamination test standard includes GB/T 4585-2004/IEC 60507 at present：1991、GB/T 22707-2008/
IEC61245：1993 and DL/T 859-2004.Solid layer method in these standards is all as saline solution, with one using NaCl
Fixed Kaolin or kieselguhr and water are mixed to form artificial pollution.Also have to study flashover voltage is being obtained with pollution degree relational expression
On the basis of, the referring factor such as the filthy composition of addition, filthy distribution, filthy composition are mainly considered with CaSO4For the divalent salts for representing.
This several method all considers the filthy actual composition of nature comprehensively, therefore, it is difficult to really realizing artificial pollution with filth naturally
Equivalence.
For this purpose, it has been proposed that by simulating nature filth salt composition, making selected soluble salts as close possible to institute
The natural filth situation of research area, but it is loaded down with trivial details due to testing, and standard disunity, practicality are poor.
The content of the invention
In order to overcome above-mentioned deficiency, the present invention to provide a kind of compound method of artificial pollution.By the determination of main component
With the determination of soluble salt point similarity, while the filthy reduction of nature being realized to greatest extent with equivalence, greatly improved and match somebody with somebody
Efficiency processed and accuracy, provide important experiment for research of the artificial pollution with the equivalence question of natural pollution test
Hold.
As existing water solublity filth composition is with Ca2+And SO4 2-Based on, and in XRD results, judge Gypsum Fibrosum (CaSO4·
2H2O presence), therefore the present invention proposes one kind particularly for such CaSO4For the natural filthy process side of main component
Method, the method realize such filthy reduction and equivalence naturally to greatest 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 to study Mechanism of Contamination Flashover, reducing pollution flashover accident.
To achieve these goals, the present invention is adopted the following technical scheme that：
The compound method of soluble-salt in a kind of artificial pollution, including：
1) nature filth sample composition is analyzed, the content of zwitterion is ranked up；
2) by Ca2+And SO4 2-Matched, remaining Ca2+Or SO4 2-It is stand-by；
3) by NH4 +With NO3 -Matched, remaining NH4 +Or NO3 -It is stand-by；
4) by remaining ion and residual ion in filth, according to " preparing and soluble-salt and ensure its ion concentration order base
This is constant " principle matched；
5) according to above-mentioned pairing result configuration soluble-salt, obtain final product.
Preferably, the concrete grammar of described " prepare soluble-salt and ensure that its ion concentration is basically unchanged " is：
A. using remaining ion and residual ion cationic and anion-content highest ion as a category feature ion；
B. by Na+、Mg2+、Cl-、K+、F-Matched with a category feature ion, constituted corresponding soluble-salt；
C. unpaired ion in filth is carried out matching, constitutes soluble-salt；If pairing after, still suffer from it is unpaired from
Son, can adopt Na+、Mg2+、Cl-、K+、F-Or the arbitrary ion in residual ion is matched with which, soluble-salt is constituted；
D. it is true respectively according to " percentage composition of unique ion in the filthy sample of originating in above-mentioned soluble-salt "
The proportioning I of fixed each soluble-salt；
E. further according to " a category feature ion concentration is consistent or close with analysis experimental result, and other zwitterion contents are suitable
Sequence is consistent with testing result " principle the proportioning of soluble-salt is adjusted, obtain proportioning II；
F. soluble-salt is prepared according to proportioning II, is obtained final product.
In the present invention, " remaining ion " is referred to：Ca is removed in filthy composition2+、SO4 2-、NH4 +Or NO3 -Ion in addition.
In the present invention, " residual ion " is referred to：In filthy composition Jing above-mentioned steps 2), 3) match after, remaining Ca2+、
SO4 2-、NH4 +Or NO3 -。
In the present invention be used for pairing each ion initial content according to naturally filth sample composition in each ion content
It is determined that.
Research shows：Such CaSO of Shandong District4Typically at least to contain Ca in the natural filth of main component2+With
SO4 2-、NH4 +、Na+、Mg2+、Cl-、NO3 -、K+、F-Plasma and content is relatively stable, therefore, in the present invention, prioritizing selection is above-mentioned
Ion is matched with a category feature ion.
It is furthermore preferred that in step d, the adjustment is concretely comprised the following steps：
According to the content sequence of test result cationic, the soluble-salt content of the composition of proportioning I is adjusted；According to
The content sequence of anion in test result, is adjusted to the proportion of composing of each salt in the soluble-salt of the composition of said ratio I；
Or according to the content sequence of anion in test result, the soluble-salt content of the composition of proportioning I is adjusted；
According to the content sequence of test result cationic, the proportion of composing of each salt in the soluble-salt of the composition of said ratio I is carried out
Adjustment.
Preferably, it is described to analyze concretely comprising the following steps for nature filth sample composition：
(1) be ensure sample true integrity, filth is swept down using hard hair brush, with pan paper accept, wrap,
Deposit in loading special valve bag immediately.Before test, filthy sample is crossed into 150 mesh sieves first, be placed in baking oven afterwards, 105 DEG C
Drying 24h, then ground with agate mortar.Accurately weigh 0.2g filth samples to be dissolved in 60ml ultra-pure waters, 80 DEG C of water bath sonicators shake
Swing 30min and promote water-soluble composition dissolving in sample, stand 30min, quantitative filter paper is filtered, and filtrate is settled to ultra-pure water
100ml.Solution first crosses 0.22 μm of filtering head before entering chromatography of ions；
(2) anion-content in determination sample, the technological parameter of IC test is：IonPac AG18
Capillary guard columns (50 × 0.4mm), IonPac AS18 Capillary analytical columns (250 × 0.4mm)；Leacheate：EG-
The KOH solution that KOH capillary tube drip washing liquid generator is produced, 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
Stream 11mA；Column temperature：30℃；Flow velocity：10μL/min；Sampling volume：0.4μL；
(3) cations location parameter：IonPac CG16 Capillary guard columns (50 × 0.4mm, the U.S.
Thermo Fisher companies), (250 × 0.4mm, Thermo Fisher are public in the U.S. for IonPac CS16 Capillary analytical columns
Department)；Leacheate：The MSA solution that EG-MSA capillary tube drip washing liquid generator is produced, isocratic drip washing：35min, flow are 20mmol/
L, 10 μ L/min of flow velocity.Suppressor electric current 7mA；Sampling volume：0.4μL；Column temperature：30℃.
Now there are some researches show：In the filthy composition of Shandong District, Ca2+With SO4 2-Mass content ratio about 1:2 or so, with
CaSO4Middle Ca2+With SO4 2-Mass ratio 1:2.4 is very close.Additionally, it can clearly be seen that CaSO in XRD analysis result4Peak, i.e.,
Contain CaSO in the naturally filthy chemical composition of insulator4.Considered based on above reason, by Ca2+With SO4 2-Pairing, further really
Determine CaSO4Mass content.Unnecessary Ca2+Or SO4 2-Soluble-salt can be constituted with remaining ion, supplement its quality.
Lot of experiments proves, Ca in Shandong District filth water soluble ingredient2+、NH4 +、SO4 2-、NO3 -For content it is higher four
Plant ion.For ammonium salt (NH4 +), it is considered to NH4 +Content Ca is only second in water-soluble cationic2+, therefore content is selected first
Higher anion is matched with which, i.e., select the NO of anion mass content second first3 -It is paired, can according to situation according to
NH4 +Or NO3 -Cubage NH4NO3Quality, remaining NH4 +Or NO3 -Soluble-salt can be constituted with remaining ion, supplement which
Quality.
Thus, in artificial pollution soluble-salt, CaSO4With NH4NO3It is the main component for determining first.Remaining ion according to
Prepare soluble-salt and ensure that the principle 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.
Present invention also offers artificial pollution soluble-salt prepared by any of the above-described method.
Present invention also offers above-mentioned artificial pollution soluble salt solutions answering in the artificial pollution test of insulator
With.As the preparation method of the present invention is simple, and the equivalence of filth naturally it is good, therefore, it can be widely used in insulator
Artificial pollution test.
The method of the present invention is applied to any material, the insulator contamination of any grade.
Present invention also offers artificial pollution of the above-mentioned artificial pollution soluble-salt in AC system high-tension insulator
Application in test.
Present invention also offers artificial pollution of the above-mentioned artificial pollution soluble-salt in straight-flow system high-tension insulator
Application in test.
Present invention also offers above-mentioned artificial pollution soluble-salt is 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 compound method of artificial pollution soluble-salt.The method that the present invention is provided can be maximum
Reduction and the equivalence of nature filth soluble-salt are realized limit.
(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 solubility zwitterion in nature filth, and solubility zwitterion is in filth
Mass content order it is consistent with testing result.Compared to existing artificial pollution-test method, not only closer to Natural contamination
Filthy composition afterwards, and simplicity is easy to get, it is easy to operate.
(4) the different kinds of ions mass content after present invention pairing is capable of achieving 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, it is easy to promote.
(6) applied range, it is adaptable to the transmission line of electricity of the various charged species of various grades.
Specific embodiment
By the following examples feature of present invention and other correlated characteristics are described in further detail, in order to the same industry
The understanding of technical staff：
Embodiment 1
By taking the operation insulator contamination composition obtained in the transmission tower that pollution flashover often occurs in -yl Jing as an example：
Wherein certain part filthy sample component analysis result such as table 1, intends preparing 10g artificial pollutions：
The filthy sample component analysis result of 1 certain part of table
| 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 is very close.With SO4 2-Mass content calculate 10g artificial pollutions in CaSO4Quality be 2.49g, this
When Ca2+Content is 7.32%, basically identical with 1 result of table.
(2) select NH4NO3As solubility ammonium salt.With NH4 +Mass content calculate 10g artificial pollutions in NH4NO3Matter
Measure as 0.32g, now NO3 -Content be 2.48%.
(3) select MgCl2As soluble magnesium salt.With Mg2+Mass content calculate 10g artificial pollutions in MgCl2Matter
Measure as 0.05g, now Cl-Content be 0.37%.
(4) KF is selected to provide F-And K+.With K+Mass content calculate 10g artificial pollutions in KF quality be 0.04g, this
When F-Content is 0.13%.Less than naturally filthy content.NaF and KF is selected simultaneously as fluorine-containing salts, respectively with Na+Contain with the amount of K
Amount calculates the quality of NaF and KF in 10g artificial pollutions and is respectively 0.03g and 0.04g, now 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) take common water-soluble substanceses NH4H2PO4Phosphate is provided.With PO4 3-Mass content calculate 10g artificial pollutions
Middle NH4H2PO4Quality be 0.01g.Now NH4H2PO4And NH4NO3NH is provided simultaneously4 +, final NH4 +Content be 0.74%.
The preparation program that 10g artificial pollutions are obtained by above procedure is as follows：
Table 2 simulates artificial pollution Initial Composition proportioning according to filthy composition analysis result
| Title | CaSO4 | NH4NO3 | MgCl2 | KF | NaF | NH4H2PO4 |
| Quality (g) | 2.49 | 0.32 | 0.05 | 0.05 | 0.04 | 0.01 |
According to above proportioning, its each mass of ion content such as table 3：
Each mass of ion content in 3 artificial pollution proportioning of table
| 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 of solubility zwitterion, and solubility is cloudy
Mass content of the cation in filth is basically identical with naturally filthy.Compared to existing artificial pollution test's method, not only more
It is easy to get close to the filthy composition after Natural contamination, and simplicity, it is easy to operate.
Wherein, naturally filthy method for measuring components is as follows：
To ensure the true integrity of sample, filth is swept down using hard hair brush, accepted with pan paper, wrapped, with
Deposit in loading special valve bag.Before test, filthy sample is crossed into 150 mesh sieves first, be placed in baking oven afterwards, 105 DEG C of bakings
Dry 24h, then ground with agate mortar.Accurately weigh 0.2g filth samples to be dissolved in 60ml ultra-pure waters, 80 DEG C of water bath sonicator vibrations
30min promotes water-soluble composition dissolving in sample, stands 30min, and quantitative filter paper is filtered, and filtrate ultra-pure water is settled to 100ml.
Solution first crosses 0.22 μm of filtering head before entering chromatography of ions.
Anion-content in determination sample, the technological parameter of IC test is：IonPac AG18 Capillary are protected
Guard post (50 × 0.4mm), IonPac AS18 Capillary analytical columns (250 × 0.4mm)；Leacheate：EG-KOH capillary tubies drench
The KOH solution that eluent generator is produced, 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：10μL/min；Sampling volume：0.4μL.
Cations location parameter：IonPac CG16 Capillary guard columns (50 × 0.4mm, U.S. Thermo
Fisher companies), IonPac CS16 Capillary analytical columns (250 × 0.4mm, Thermo Fisher companies of the U.S.)；Drench
Washing liquid：The MSA solution that EG-MSA capillary tube drip washing liquid generator is produced, isocratic drip washing：35min, flow is 20mmol/L, flow velocity
10μL/min.Suppressor electric current 7mA；Sampling volume：0.4μL；Column temperature：30℃.
The detection of insulator surface solubility filth concentration in the present invention is limited to 0.001mmol/l.
Embodiment 2
By taking the complex filthy sample of a composition as an example, its chemical composition analysis result is as follows：
The filthy sample component analysis result of 4 certain part of table
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 is high, shows except CaSO4There are outward other calcium salts.With SO4 2-Mass content calculate 10g artificial pollutions
Middle CaSO4Quality be 1.31g, now Ca2+Content is 3.85%, less than the Ca in filth naturally2+Content 4.75%.
(2) select NH4NO3As solubility ammonium salt.With NH4 +Mass content calculate 10g artificial pollutions in NH4NO3Matter
Measure as 0.16g, now NO3 -Content be 1.24%, less than naturally filth in NO3 -Content 2.22%.
(3) Ca (NO are 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.Now SO4 2-Content is 10.59%, NO3 -Content is 2.37%.
(4) select MgCl2As soluble magnesium salt.With Mg2+Mass content calculate 10g artificial pollutions in MgCl2Matter
Measure as 0.08g, now Cl-Content be 0.60%.
(5) NaF is selected to provide F-And Na+.With Na+Mass content calculate 10g artificial pollutions in the quality of NaF be
0.06g, now F-Content is 0.27%.Less than naturally filthy content.NaF and KF is selected simultaneously as fluorine-containing salts, respectively with Na+
And K+Amount cubage 10g artificial pollutions in the quality of NaF and KF be respectively 0.06g and 0.02g, now F-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.Now Na+Content is 0.38%, K+Content is 0.20%.
(6) because of C2O4 2-And PO4 3-Content it is relatively low, in preparation program may be selected the solubility ammonium salt of the two, Ji Nengti
For required anion, NH will not be significantly increased again4 +Quality.From water solublity (NH4)2C2O4C is provided2O4 2-, with C2O4 2-'s
Mass content calculates (NH in 10g artificial pollutions4)2C2O4Quality be 0.03g.
(7) take common water-soluble substanceses NH4H2PO4Phosphate is provided.With PO4 3-Mass content calculate 10g artificial pollutions
Middle NH4H2PO4Quality be 0.002g.Now NH4H2PO4、(NH4)2C2O4And NH4NO3NH is provided simultaneously4 +, final NH4 +Contain
Measure as 0.45%.
The preparation program that 10g artificial pollutions are obtained by above procedure is as follows：
Table 5 simulates artificial pollution Initial Composition proportioning according to filthy composition analysis result
According to above proportioning, its each mass of ion content such as table 6：
Each mass of ion content in 6 artificial pollution proportioning of table
| 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 of solubility zwitterion, and solubility is cloudy
Mass content of the cation in filth is basically identical with naturally filthy.Compared to existing artificial pollution test's method, not only more
It is easy to get close to the filthy composition after Natural contamination, and simplicity, it is easy to operate.
Embodiment 3
, in light filth area, water soluble salt content is relatively fewer for certain current conversion station.The dirt of maintenance collection in 2015 and 2016
Dirty sample, its soluble-salt composition are basically identical.Pole II sample compositions are analyzed as follows within 2016：
Certain the current conversion station pole of table 7 II filth sample composition analysis results
| 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 is slightly higher, shows except CaSO4There are outward other calcium salts.With SO4 2-Mass content calculate 10g it is manually dirty
Dirty middle CaSO4Quality be 0.56g, now Ca2+Content is 1.65%, slightly below naturally filth in Ca2+Content 1.95%.
(2) select MgCl2As soluble magnesium salt.With Mg2+Mass content calculate 10g artificial pollutions in MgCl2Matter
Measure as 0.04g, now Cl-Content be 0.30%, less than actually detected value.
(3) add CaCl2So that Ca2+Mass content it is consistent with table 7, its quality is with Ca2+Content (1.95%-1.65%
=0.30%) calculate.CaCl need to be added20.08g.Contain 0.04g MgCl simultaneously2With 0.08g CaCl2When, Cl-Content be
0.81%.
(4) select NH4NO3As solubility ammonium salt.With NH4 +Mass content calculate 10g artificial pollutions in NH4NO3Matter
Measure as 0.24g, now NO3 -Content be 1.86%, with it is naturally filthy in NO3 -Content is basically identical.
(5) NaF is selected to provide F-And Na+.With Na+Mass content calculate 10g artificial pollutions in the quality of NaF be
0.05g, now F-Content is 0.23%, though more slightly higher than actually detected value, the mass content order in anion is constant.
(6) from water solublity K2C2O4C is provided2O4 2-And K+, with K+Mass content calculate 10g artificial pollutions in K2C2O4's
Quality is 0.03g.Now C2O4 2-Content is 0.16%, basically identical with mass content in filth naturally.
The preparation program that 10g artificial pollutions are obtained by above procedure is as follows：
Table 8 simulates artificial pollution Initial Composition proportioning according to filthy composition analysis result
| Title | CaSO4 | NH4NO3 | CaCl2 | MgCl2 | NaF | K2C2O4 |
| Quality (g) | 0.56 | 0.24 | 0.08 | 0.04 | 0.05 | 0.03 |
According to above proportioning, its each mass of ion content such as table 9：
Each mass of ion content in 9 artificial pollution proportioning of table
| 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 of solubility zwitterion, and solubility is cloudy
Mass content of the cation in filth is basically identical with naturally filthy.Compared to existing artificial pollution test's method, not only more
It is easy to get close to the filthy composition after Natural contamination, and simplicity, it is easy to operate.
Described in three above example, naturally filthy method for measuring components is as follows：
To ensure the true integrity of sample, filth is swept down using hard hair brush, accepted with pan paper, wrapped, with
Deposit in loading special valve bag.Before test, filthy sample is crossed into 150 mesh sieves first, be placed in baking oven afterwards, 105 DEG C of bakings
Dry 24h, then ground with agate mortar.Accurately weigh 0.2g filth samples to be dissolved in 60ml ultra-pure waters, 80 DEG C of water bath sonicator vibrations
30min promotes water-soluble composition dissolving in sample, stands 30min, and quantitative filter paper is filtered, and filtrate ultra-pure water is settled to 100ml.
Solution first crosses 0.22 μm of filtering head before entering chromatography of ions.
Anion-content in determination sample, the technological parameter of IC test is：IonPac AG18 Capillary are protected
Guard post (50 × 0.4mm), IonPac AS18 Capillary analytical columns (250 × 0.4mm)；Leacheate：EG-KOH capillary tubies drench
The KOH solution that eluent generator is produced, 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：10μL/min；Sampling volume：0.4μL.
Cations location parameter：IonPac CG16 Capillary guard columns (50 × 0.4mm, U.S. Thermo
Fisher companies), IonPac CS16 Capillary analytical columns (250 × 0.4mm, Thermo Fisher companies of the U.S.)；Drench
Washing liquid：The MSA solution that EG-MSA capillary tube drip washing liquid generator is produced, isocratic drip washing：35min, flow is 20mmol/L, flow velocity
10μL/min.Suppressor electric current 7mA；Sampling volume：0.4μL；Column temperature：30℃.
The detection of insulator surface solubility filth concentration in the present invention is limited to 0.001mmol/l.
Finally it should be noted that the foregoing is only the preferred embodiments of the present invention, this is not limited to
Bright, although being described in detail to the present invention with reference to the foregoing embodiments, for a person skilled in the art, which is still
Technical scheme described in previous embodiment can be modified, or equivalent is carried out to which part.It is all at this
Within bright spirit and principle, any modification, equivalent substitution and improvements made etc. should be included in protection scope of the present invention
Within.Although the above-mentioned specific embodiment to the present invention is described, not limiting the scope of the invention, institute
Category art personnel should be understood that on the basis of technical scheme those skilled in the art need not pay wound
The various modifications made by the property made work or deformation are still within protection scope of the present invention.
Claims (7)
1. in a kind of artificial pollution soluble-salt compound method, including：
1) nature filth sample composition is analyzed, the content of zwitterion is ranked up；
2) by Ca2+And SO4 2-Matched, remaining Ca2+Or SO4 2-It is stand-by；
3) by NH4 +With NO3 -Matched, remaining NH4 +Or NO3 -It is stand-by；
4) by remaining ion and residual ion in filth, according to " preparing soluble-salt and ensure its ion concentration order substantially not
The principle of change " is matched；
5) according to above-mentioned pairing result configuration soluble-salt, obtain final product.
2. the method for claim 1, it is characterised in that described " to prepare soluble-salt and ensure that its ion concentration is basic
It is constant " concrete grammar be：
A. using remaining ion and residual ion cationic and anion-content highest ion as a category feature ion；
B. by Na+、Mg2+、Cl-、K+、F-Matched with a category feature ion, constituted corresponding soluble-salt；
C. unpaired ion in filth is carried out matching, constitutes soluble-salt；If after pairing, still suffering from unpaired ion,
Na can be adopted+、Mg2+、Cl-、K+、F-Or the arbitrary ion in residual ion is matched with which, soluble-salt is constituted；
D. determined according to " percentage composition of unique ion in the filthy sample of originating in above-mentioned soluble-salt " respectively each
The proportioning I of soluble-salt；
E. further according to " a category feature ion concentration with analysis experimental result it is consistent or close, other zwitterion content sequences with
Testing result is consistent " principle the proportioning of soluble-salt is adjusted, obtain proportioning II；
F. soluble-salt is prepared according to proportioning II, is obtained final product.
3. method as claimed in claim 2, it is characterised in that in step d, the adjustment are concretely comprised the following steps：
According to the content sequence of test result cationic, the soluble-salt content of the composition of proportioning I is adjusted；According to test
As a result the content sequence of middle anion, is adjusted to the proportion of composing of each salt in the soluble-salt of the composition of said ratio I；
Or according to the content sequence of anion in test result, the soluble-salt content of the composition of proportioning I is adjusted；According to
The content sequence of test result cationic, is adjusted to the proportion of composing of each salt in the soluble-salt of the composition of said ratio I.
4. the method as described in any one of claim 1-3, it is characterised in that the naturally filthy sample composition of the analysis it is concrete
Step is：
(1) be ensure sample true integrity, filth is swept down using hard hair brush, with pan paper accept, wrap, immediately
Deposit in loading special valve bag.Before test, filthy sample is crossed into 150 mesh sieves first, be placed in baking oven afterwards, 105 DEG C of drying
24h, then ground with agate mortar.Accurately weigh 0.2g filth samples to be dissolved in 60ml ultra-pure waters, 80 DEG C of water bath sonicator vibrations
30min promotes water-soluble composition dissolving in sample, stands 30min, and quantitative filter paper is filtered, and filtrate ultra-pure water is settled to 100ml.
Solution first crosses 0.22 μm of filtering head before entering chromatography of ions；
(2) anion-content in determination sample, the technological parameter of IC test is：IonPac AG18 Capillary are protected
Guard post (50 × 0.4mm), IonPac AS18 Capillary analytical columns (250 × 0.4mm)；Leacheate：EG-KOH capillary tubies drench
The KOH solution that eluent generator is produced, 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：10μL/min；Sampling volume：0.4μL；
(3) cations location parameter：IonPac CG16 Capillary guard columns (50 × 0.4mm, U.S. Thermo
Fisher companies), IonPac CS16 Capillary analytical columns (250 × 0.4mm, Thermo Fisher companies of the U.S.)；Drench
Washing liquid：The MSA solution that EG-MSA capillary tube drip washing liquid generator is produced, isocratic drip washing：35min, flow is 20mmol/L, flow velocity
10μL/min；.Suppressor electric current 7mA；Sampling volume：0.4μL；Column temperature：30℃.
5. the artificial pollution soluble-salt that prepared by any one of claim 1-4 methods described.
6. application of the artificial pollution soluble-salt described in claim 5 in the artificial pollution test of insulator.
7. the artificial pollution soluble-salt described in claim 5 AC system high-tension insulator artificial pollution test,
The artificial pollution test of straight-flow system high-tension insulator, in the artificial pollution test of high-voltage alternating system composite insulator
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