CN105203656A - Shandong area insulator dirtiness water-soluble negative ion ingredient testing method - Google Patents
Shandong area insulator dirtiness water-soluble negative ion ingredient testing method Download PDFInfo
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- CN105203656A CN105203656A CN201510582204.5A CN201510582204A CN105203656A CN 105203656 A CN105203656 A CN 105203656A CN 201510582204 A CN201510582204 A CN 201510582204A CN 105203656 A CN105203656 A CN 105203656A
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Abstract
The invention discloses a Shandong area insulator dirtiness water-soluble negative ion ingredient testing method. According to the method, an efficient negative ion exchange separation column IonPac AS18 is used, and water-soluble negative ions in a dirtiness sample are accurately and fast tested under the KOH gradient leaching condition. The experiment result shows that the method has the advantages that the quantity definition is precise; the repeatability is good; the requirement on the practical dirtiness accurate evaluation in the Shandong area insulator can be met. The method is simple, convenient and stable; the pertinency is good in the linear range; the accuracy is high; the interference by other factors is small; the sample consumption is low; the practical value is high.
Description
Technical field
The invention belongs to instrumental analysis field, particularly a kind of Shandong District insulator contamination water soluble anion method for measuring components.
Background technology
Industrial pollution and atmospheric pollution are on the rise, and cause operation pollution severity of insulators to aggravate thereupon, add the risk that pollution flashover accident appears in transmission line of electricity.
The filthy characteristic parameter of sign insulator conventional both at home and abroad at present mainly contains: equivalent salt density, pollution layer conductivity, leakage current and flashover field intensity etc.When assessing electric system external insulation pollution, usual measurement equivalent salt deposit density (equivalentsaltdepositdensity, ESDD) method assesses pollution degree, by measuring the size of cleaning pollution severity of insulators electrical conductivity of solution, be converted into the density of the NaCl of electric system external insulation surface attachment under standard temperature.Studied discovery in recent years, because of filthy component difference, use the larger difference existed between the pollution degree of equivalent salt density assessment and actual pollution degree, the actual effect causing external insulation design and day-to-day operation to be safeguarded is undesirable; The research of Mechanism of Contamination Flashover is also subject to the impact of filthy constituent analysis deficiency, causes the research of Mechanism of Contamination Flashover not enough.Therefore, the Flashover Characteristics of insulator can not being analyzed simply by the close value of salt, also must include chemical composition concrete for filth in research category, for more effectively carrying out antifouling work, needing to measure the main chemical compositions of filth.At present, the inorganic soluble cation constituent of generally acknowledging both at home and abroad has Na
+, K
+, NH
4 +, Mg
2+, Ca
2+, Zn
2+, Al
3+, Mn
2+, Cu
2+deng, inorganic soluble negative ion has Cl
-, NO
2 -, NO
3 -, F
-, SO
4 2-, HCO
3 -, CO
3 2-, PO
4 3-deng, the detection method of use concentrates on atomic absorption spectrophotometry, plasma emission spectrometry, the chromatography of ions etc.Day by day deep to the detection of insulator contamination composition at present, but few to the research and inquirement of detection method.The accuracy of detection method and accuracy affect the net result of insulator contamination composition, directly affect the measurement of Mechanism of Contamination Flashover research and pollution degree, are therefore extremely necessary to inquire into detection method and verify.
Capillary ion chromatography (capillaryionchromatography) is one of study hotspot of current ion chromatography system, there is sample and leacheate consumption is few, mass sensitivity is high, be easy to and the advantages such as mass spectrum, inductively coupled plasma spectrometry coupling, furtherd investigate in recent years and apply.
Shandong District insulator contamination is owing to being subject to the impact of local specific atmospheric environment and energy structure, filthy composition presents certain specificity, accuracy and the accuracy of detection method itself is limited in prior art, have impact on the accuracy of the net result of insulator contamination composition, cause evaluation result and actual pollution condition to there is larger difference, the actual effect causing external insulation design and day-to-day operation to be safeguarded is undesirable.
Summary of the invention
For solving the problem, the present invention has carried out systematically investigating to the source of Shandong District insulator contamination and diffusion, when adopting capillary ion chromatography to analyze filthy composition, chances on: except the F appeared in the newspapers in the insulator contamination of Shandong District
-, Cl
-, SO
4 2-, NO
3 -, PO
4 3-also detected C outward
2o
4 2-, and not containing NO
2 -.Experiment confirms, insulator contamination complicated component, especially water soluble ingredient is tightly detected, and is the one of the main reasons causing the larger difference existed between the evaluation result of existing Shandong District insulator pollution situation and actual conditions.For addressing this problem, present invention discusses capillary ion chromatography and being separated the application process detecting insulator water soluble anion, and by C
2o
4 2-as one of evaluation index, exchange separating column IonPacAS18, under KOH gradient conditions, quickly and accurately to F in filthy sample with high-efficiency anion
-, Cl
-, NO
2 -, Br
-, NO
3 -, SO
4 2-, C
2o
4 2-, PO
4 3-measure.Experimental result shows, the method is quantitatively accurate, and favorable reproducibility, can meet the requirement to the actual pollution condition accurate evaluation of Shandong District insulator.
For achieving the above object, the present invention adopts following technical proposals:
A kind of Shandong District insulator contamination water soluble anion method for measuring components, comprises the following steps: adopt capillary ion chromatography to measure the peak area of negative ion in negative ion mixed standard solution, Criterion curve, described negative ion comprises F
-, Cl
-, NO
2 -, Br
-, NO
3 -, SO
4 2-, C
2o
4 2-, PO
4 3-;
Shandong District insulator contamination is carried out pre-service, obtains pre-service insulator contamination liquid to be measured;
Capillary ion chromatography is adopted to measure the peak area of negative ion in pre-service insulator contamination liquid to be measured, according to the typical curve of peak area and foundation, obtain the concentration of insulator contamination water soluble anion Shandong District, Shandong District insulator contamination water soluble anion.
Preferably, described preprocessing process is:
Insulator contamination is sieved, dries, be dissolved in ultrapure water, obtain mixed liquor A;
By mixed liquor A water bath sonicator, filtration, obtain mixed liquid B;
Mixed liquid B is carried out wash-out, obtains pre-service core pump cleaning fluid to be measured.
Preferably, the leacheate in described capillary ion chromatography is potassium hydroxide solution.Because the affinity of KOH to Stationary liquid is less than Na
2cO
3and NaHCO
3, select KOH leacheate that various negative ion can be made to reach better separation.
Preferably, the concentration of described potassium hydroxide solution is 1-50mmol/L.For strengthening F
-separating effect, use ICS-5000 capillary ion chromatography instead, adjustment gradient elution program: first low concentration 1mmol/L drip washing, the Gradient Elution Method being progressively elevated to 30mmol/L afterwards ensure F
-thorough separation; Because of PO
4 3-retention is the strongest, should adopt high concentration drip washing, therefore the follow-up 50mmol/L that brought up to by eluent concentration, accelerates PO
4 3-drip washing speed.
Preferably, the type of elution that described capillary ion chromatography measures is gradient elution.
Gradient condition of the present invention is divided into double teacher, and the first stage, leacheate is constant; Subordinate phase, eluent concentration linearly raises; Phase III, eluent concentration linearly raises, and increase rate is different from subordinate phase; Fourth stage, leacheate is constant; Five-stage: eluent concentration is down to first stage concentration.This elution requirement significantly can shorten disengaging time, improves peak shape, and target substance have also been obtained good separation.Preferred gradient elution program is: 0 ~ 2min, 1mmol/L; 2 ~ 35min, 1 ~ 30mmol/L; 35 ~ 40min, 30 ~ 50mmol/L; 40 ~ 45min, 50mmol/L; 45 ~ 48min, 1mmol/L.
Preferably, in described capillary ion chromatography: rejector electric current 11mA; Column temperature: 30 DEG C; Flow velocity: 10 μ L/min; Sampling volume: 0.4 μ L; Chromatographic column: IonPacAG18Capillary guard column (50 × 0.4mm), IonPacAS18Capillary analytical column (250 × 0.4mm).
Preferably, F in described negative ion mixed standard solution
-mass concentration is 0.1mg/L ~ 10mg/L.
Preferably, C in described negative ion mixed standard solution
2o
4 2-mass concentration be 0.1mg/L ~ 10mg/L.
Preferably, the recovery of standard addition of described Shandong District insulator contamination water soluble anion method for measuring components is 88.2 ~ 101.0%, and related coefficient is 0.9991 ~ 0.9999; In 0.1 ~ 10mg/L concentration range, the detection limit (S/N=3) of negative ion is 0.22 ~ 24.27 μ g/L.
Beneficial effect:
The System Discussion application process of capillary ion chromatography in insulator contamination water soluble anion detects herein, separating column IonPacAS18 is exchanged with high-efficiency anion, under KOH gradient conditions, quickly and accurately the water-soluble negative ion in filthy sample is measured.Experimental result shows, does not detect NO in the insulator contamination of Shandong District
3 -, except the F appeared in the newspapers
-, Cl
-, SO
4 2-, NO
3 -, PO
4 3-detected C outward
2o
4 2-.Carried out repeatability, sample determination and recovery testu to the method, result is satisfied.
Accompanying drawing explanation
The degree such as Fig. 1 ICS-2000 is separated filthy sample design sketch.Wherein, 1.F
-; 2.Cl
-; 3.SO
4 2-; 4.PO
4 3-.
Fig. 2 ICS-5000 capillary ion chromatography gradient separations standard solution chromatogram (each ion concentration is 0.1mg/L)
Wherein, 1.F
-; 2.Cl
-; 3.NO
2 -; 4.Br
-; 5.NO
3 -; 6.SO
4 2-; 7.C
2o
4 2-; 8.PO
4 3-.
Fig. 3 sample 1 separate colors spectrogram, wherein, 1.F
-; 2.Cl
-; 3.NO
3 -; 4.SO
4 2-; 5.C
2o
4 2-; 6.PO
4 3-.
Embodiment
Mode by the following examples further illustrates the present invention, but does not therefore limit the present invention among described scope of embodiments.In the following example, the experiment of unreceipted actual conditions and detection method, conventionally select with condition.
When existing Anionic recognition method is used for the filthy composition of Shandong District, usually can only measure wherein containing F
-, Cl
-, Br
-, NO
3 -, SO
4 2-, PO
4 3-ion, but when using above-mentioned ion to carry out insulator Pollution, the larger difference that evaluation result and actual pollution condition exist, the actual effect causing external insulation design and day-to-day operation to be safeguarded is undesirable, for this reason, carried out systematically investigating to the source of Shandong District insulator contamination and diffusion in the present invention, period chances on due to the special energy structure in Shandong District and atmospheric environment, generally containing a certain amount of C in the insulator contamination of this area
2o
4 2-, and by further testing proof: by C
2o
4 2-be classified as one of filthy assessment of scenario index, effectively can improve the accuracy of evaluation result, meet relevant design and day-to-day operation maintenance requirement, reach Expected Results.
The invention provides a kind of Shandong District insulator contamination water soluble anion method for measuring components,
Comprise the following steps: adopt capillary ion chromatography to measure the peak area of negative ion in negative ion mixed standard solution, Criterion curve, described negative ion comprises F
-, Cl
-, NO
2 -, Br
-, NO
3 -, SO
4 2-, C
2o
4 2-, PO
4 3-;
Shandong District insulator contamination is carried out pre-service, obtains pre-service insulator contamination liquid to be measured;
Capillary ion chromatography is adopted to measure the peak area of negative ion in pre-service insulator contamination liquid to be measured, according to the typical curve of peak area and foundation, obtain the concentration of insulator contamination water soluble anion Shandong District, Shandong District insulator contamination water soluble anion.
The present invention adopts the peak area of negative ion in Determination Anion by Ion Chromatography mixed standard solution, Criterion curve, and described negative ion comprises F
-, Cl
-, NO
2 -, Br
-, NO
3 -, SO
4 2-, C
2o
4 2-, PO
4 3-.
In the present invention, described negative ion mixed standard solution is F
-, Cl
-, NO
2 -, Br
-, NO
3 -, SO
4 2-, C
2o
4 2-, PO
4 3-hybrid standard uses liquid.Described negative ion mixed standard solution (100mg/L) and C
2o
4 2-(1000mg/L) standard solution purchased from American o2si company, F
-, Cl
-, NO
3 -, SO
4 2-, PO
4 3-(1000mg/L) standard solution is purchased from national non-ferrous metal and electronic material Institute of Analysis, then is diluted to standard working solution with ultrapure water step by step.Shandong certain transmission line of electricity domestic taken from by insulator contamination sample, and experimental water is the ultrapure water that resistivity is greater than 18.2M Ω cm.
Embodiment 1
1 experimental section
Instrument and reagent
DionexICS-5000 capillary type ion chromatograph is (containing degree pumps such as DP-5 capillary level, EG-KOH kapillary leacheate generator, kapillary electric conductivity detector, AS-AP automatic sampler), Chromeleon6.8 chromatographic work station (ThermoFisher company), ACES-300 capillary suppressor, CRD200 kapillary carbon dioxide remover; DionexICS-2000 analytic type ion chromatograph (EG-KOH leacheate generator, electric conductivity detector), Chromeleon6.0 chromatographic work station (ThermoFisher company); Electric heating constant-temperature blowing drying box (BinderFD53); Ultrasonic cleaning machine (Fauna of Kunshan, Jiangsu KQ-500DE); 0.22 μm of miillpore filter.
Negative ion mixed standard solution (100mg/L) and C
2o
4 2-(1000mg/L) standard solution purchased from American o2si company, F
-, Cl
-, NO
3 -, SO
4 2-, PO
4 3-(1000mg/L) standard solution is purchased from national non-ferrous metal and electronic material Institute of Analysis, then is diluted to standard working solution with ultrapure water step by step.Shandong certain transmission line of electricity domestic taken from by insulator contamination sample, and experimental water is the ultrapure water that resistivity is greater than 18.2M Ω cm.
1.1 chromatographic condition
Chromatographic column: IonPacAG18Capillary guard column (50 × 0.4mm), IonPacAS18Capillary analytical column (250 × 0.4mm); Leacheate: the KOH solution that EG-KOH kapillary leacheate generator produces, gradient elution: 0 ~ 2min, 1mmol/L; 2 ~ 35min, 1 ~ 30mmol/L; 35 ~ 40min, 30 ~ 50mmol/L; 40 ~ 45min, 50mmol/L; 45 ~ 48min, 1mmol/L.Rejector electric current 11mA; Column temperature: 30 DEG C; Flow velocity: 10 μ L/min; Sampling volume: 0.4 μ L.
1.2 sample pre-treatments
First filthy sample is crossed 150 mesh standard sieves, be placed in baking oven, 105 DEG C dry 24h.The filthy sample accurately taking 0.1g is dissolved in 60ml ultrapure water, and 80 DEG C of water bath sonicator vibration 30min promote that in sample, water-soluble composition dissolves, and leaves standstill 30min, and quantitative filter paper filters, and filtered fluid ultrapure water is settled to 100ml.Solution first crosses 0.22 μm of filtering head before entering chromatography of ions.
2 results and discussion
The selection of 2.1 chromatographic systems and leacheate program optimization
Because the affinity of KOH to Stationary liquid is less than Na
2cO
3and NaHCO
3, select KOH leacheate that various negative ion can be made to reach better separation, select DionexEG leacheate generator to produce KOH online as leacheate herein.First adopt the degree drip washing such as DionexICS-2000 analytic type chromatography of ions, 38mM, the separating effect figure of filthy sample is shown in Fig. 1.Shown can be found out by Fig. 1 solid circles, F
-be separated by impurity effect, do not reach complete separating effect.In addition, Cl
-with SO
4 2-there is a less not qualitative peak (as in Fig. 1, dotted line circle shows) centre, is tentatively judged as NO
2 -, be NO
2 -typical curve, retention time is 4.89min, and the retention time average out to 4.83min at unknown peak in three samples, be therefore judged to be NO
2 -.
For strengthening F
-separating effect, use ICS-5000 capillary ion chromatography instead, adjustment gradient elution program: first low concentration 1mmol/L drip washing, the Gradient Elution Method being progressively elevated to 30mmol/L afterwards ensure F
-thorough separation; Because of PO
4 3-retention is the strongest, should adopt high concentration drip washing, therefore the follow-up 50mmol/L that brought up to by eluent concentration, accelerates PO
4 3-drip washing speed.The condition of gradient elution of final optimization pass is shown in 1.2 joints.Under this chromatographic condition, survey component single injected sampling and both can ensure peak shape and degree of separation, component can be made again to go out peak at Best Times.Fig. 2 is the chromatogram of ICS-5000 capillary ion chromatography gradient separations mixed standard solution.
Get five parts of insulator contamination samples through 1.3 joint pre-treatments, under above-mentioned chromatographic condition, adopt external standard method to carry out quantitative test, sample 1 separate colors spectrogram is shown in Fig. 3.As can be seen from Fig. 3, NO
2 -characteristic peak (retention time 16.16min) near there is no any peak occur, show to there is no water-soluble NO in this sample
2 -.And collect tens of parts of insulator contamination samples and detect, NO
2 -characteristic peak (retention time 16.16min) near all occur without any peak, show to there is no water-soluble nitrite in collected Shandong District electric transmission line isolator filth.In addition, after signal is amplified, NO
3 -with SO
4 2-between have an obvious peak (as shown in circle in Fig. 3 accompanying drawing), according to experience infer may be CO
3 2-or HCO
3 -; In the degree elution methods such as ICS-2000 analytic type 38mM, CO
3 2-or HCO
3 -go out peak position just also at Cl
-with SO
4 2-between, with NO
2 -retention time very close, cause misjudgment, in Fig. 1, No. 3 peaks may be CO thus
3 2-or HCO
3 -.Due to chromatography of ions standard measure CO
3 2-or HCO
3 -accuracy is poor, and titrimetry also has no indicator discoloration, therefore cannot determine its content.Meanwhile, the method detects in insulator contamination to there is a certain amount of C
2o
4 2-(in Fig. 3 shown in No. 5 peaks), may due to SO in the degree chromatographies of ions such as ICS-2000
4 2-peak is too large, is masked.
2.2 linear relationships, the range of linearity and detection limit
Investigate the linear relationship of 8 kinds of anion concentrations and peak area.Precision measures standard reserving solution, preparation mass concentration is respectively 0.1,0.5,1.0,2.0,5.0, the mixed standard solution of 10.0mg/L.Each concentration determination 3 times, take peak area as ordinate, titer mass concentration is horizontal ordinate, Criterion working curve, and linear equation, related coefficient and detection limit are in table 1.The wherein mass concentration (mg/L) of y to be peak area (μ Smin), x be component, related coefficient all between 0.9991 ~ 0.9999, linearly better.In 0.1 ~ 10mg/L concentration range, the detection limit (S/N=3) of 8 kinds of negative ion is between 0.22 ~ 24.27 μ g/L.
Table 1 linear equation, related coefficient and detection limit
Table1Linearequation,correlationcoefficientandlimitofdetection
2.3 repeated
Draw the negative ion mixed standard solution to be measured of appropriate 0.5mg/L, repeat sample introduction 7 times, record chromatogram, relative standard deviation is in table 2.The relative standard deviation of retention time all below 0.03%, the relative standard deviation scope of peak area 0.07 ~ 0.38%, the relative standard deviation scope 0.12 ~ 0.27% of peak height.
Table 2 repeated experiment (n=7)
Table2Repeatabilityofdetection(n＝7)
2.4 sample determinations and recovery of standard addition
Get five parts of insulator contamination samples through 1.3 joint pre-treatments, under 1.2 joint chromatographic conditions, adopt external standard method to carry out quantitative test, because of SO in sample
4 2-and NO
3 -content is higher, and dilute ten times and measure, all the other ions all measure with original concentration, and concrete outcome is in table 4.
Table 4 sample solution assay result (n=3)
Table4Analyticalresultsofsamples(n＝3)
N.d.: represent and do not detect
For the accuracy of the method for inspection, choose the recovery testu that No. 1 sample solution makes 3 variable concentrations levels, because of SO
4 2-with NO
3 -content is comparatively large, and do recovery testu after diluting ten times, the recovery is in table 5.Result shows, recovery of standard addition is in 88.2 ~ 101.0% scopes.According to general knowledge known in this field, as the content≤1mg/L of tested component, the allowing of the recovery is limited to 80% ~ 120%; As the content 1 ~ 100mg/L of tested component, the allowing of the recovery is limited to 90% ~ 110%, and therefore this experimental result is satisfied, can be applied to the mensuration of the water-soluble anion-content of filthy sample.
3 conclusions
(1) capillary ion chromatography technology is applied to and detects insulator contamination water soluble anion composition by this research, and this method is easy, stable, and in the range of linearity, correlativity is good, accuracy is high, little by other factors interference, amount of samples is few, has higher practical value.
(2) this method can detect the F in the filth of insulator water dissolubility simultaneously
-, Cl
-, SO
4 2-, NO
3 -, PO
4 3-, C
2o
4 2-, gradient elution: 0 ~ 2min, 1mmol/L; 2 ~ 35min, 1 ~ 30mmol/L; 35 ~ 40min, 30 ~ 50mmol/L; 40 ~ 45min, 50mmol/L; 45 ~ 48min, 1mmol/L.Flow velocity: 10 μ L/min; Sampling volume: 0.4 μ L.Experiment shows, not containing NO in the water-soluble filth of Shandong District electric transmission line isolator
2 -, may CO be contained
3 2-, HCO
3 -deng
(3) to capillary ion chromatography carry out linear relationship, detection limit, repeatability, mark-on reclaim angularly test and discuss, related coefficient between 0.9991 ~ 0.9999, linearly better.In 0.1 ~ 10mg/L concentration range, the detection limit (S/N=3) of negative ion is between 0.22 ~ 24.27 μ g/L.Recovery of standard addition is in 88.2 ~ 101.0% scopes.This research provides new method for insulator contamination water soluble anion composition detection, has higher practical value and application prospect.
As seen from the above embodiment, the invention provides a kind of Shandong District insulator contamination water soluble anion method for measuring components, comprise the following steps: the peak area adopting negative ion in Determination Anion by Ion Chromatography mixed standard solution, Criterion curve, described negative ion comprises F
-, Cl
-, NO
2 -, Br
-, NO
3 -, SO
4 2-, C
2o
4 2-, PO
4 3-; Insulator contamination sample is carried out pre-service, obtains pre-service insulator contamination liquid to be measured; Adopt the peak area of negative ion in ion-chromatographic determination pre-service insulator contamination liquid to be measured, according to the typical curve of peak area and foundation, obtain the concentration of negative ion in pre-service insulator contamination liquid to be measured.The present invention is that the mensuration of anion-content in pre-service insulator contamination liquid to be measured provides method foundation; Method provided by the invention is simple to operate, reappearance is better.
The detection method for Shandong District insulator contamination water soluble anion that the present invention sets up is one of key point ensureing the actual pollution condition accurate evaluation of insulator, which ensure that external insulation design and day-to-day operation are safeguarded and can be produced a desired effect.
The above is only the preferred embodiment of the present invention; it should be pointed out that for those skilled in the art, under the premise without departing from the principles of the invention; can also make some improvements and modifications, these improvements and modifications also should be considered as protection scope of the present invention.
Claims (10)
1. a Shandong District insulator contamination water soluble anion method for measuring components, it is characterized in that, comprise the following steps: adopt capillary ion chromatography to measure the peak area of negative ion in negative ion mixed standard solution, Criterion curve, described negative ion comprises F
-, Cl
-, NO
2 -, Br
-, NO
3 -, SO
4 2-, C
2o
4 2-, PO
4 3-;
Shandong District insulator contamination is carried out pre-service, obtains pre-service insulator contamination liquid to be measured;
Capillary ion chromatography is adopted to measure the peak area of negative ion in pre-service insulator contamination liquid to be measured, according to the typical curve of peak area and foundation, obtain the concentration of insulator contamination water soluble anion Shandong District, Shandong District insulator contamination water soluble anion.
2. assay method according to claim 1, is characterized in that, described preprocessing process is:
Insulator contamination is sieved, dries, be dissolved in ultrapure water, obtain mixed liquor A;
By mixed liquor A water bath sonicator, filtration, obtain mixed liquid B;
Mixed liquid B is carried out wash-out, obtains pre-service core pump cleaning fluid to be measured.
3. assay method according to claim 1, is characterized in that, the leacheate in described capillary ion chromatography is potassium hydroxide solution.
4. assay method according to claim 3, is characterized in that, the concentration of described potassium hydroxide solution is 1-50mmol/L.
5. assay method according to claim 1, is characterized in that, the type of elution that described capillary ion chromatography measures is gradient elution.
6. assay method according to claim 5, is characterized in that, described gradient elution program is: 0 ~ 2min, 1mmol/L; 2 ~ 35min, 1 ~ 30mmol/L; 35 ~ 40min, 30 ~ 50mmol/L; 40 ~ 45min, 50mmol/L; 45 ~ 48min, 1mmol/L.
7. assay method according to claim 1, is characterized in that, in described capillary ion chromatography: rejector electric current 11mA; Column temperature: 30 DEG C; Flow velocity: 10 μ L/min; Sampling volume: 0.4 μ L; Chromatographic column: IonPacAG18Capillary guard column (50 × 0.4mm), IonPacAS18Capillary analytical column (250 × 0.4mm).
8. assay method according to claim 1, is characterized in that, F in described negative ion mixed standard solution
-mass concentration is 0.1mg/L ~ 10mg/L.
9. assay method according to claim 1, is characterized in that, C in described negative ion mixed standard solution
2o
4 2-mass concentration be 0.1mg/L ~ 10mg/L.
10., according to the arbitrary described Shandong District insulator contamination water soluble anion method for measuring components of claim 1-9, it is characterized in that, the recovery of standard addition of described detection method is 88.2 ~ 101.0%, and related coefficient is 0.9991 ~ 0.9999; In 0.1 ~ 10mg/L concentration range, the detection limit (S/N=3) of negative ion is 0.22 ~ 24.27 μ g/L.
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| CN106442798A (en) * | 2016-11-04 | 2017-02-22 | 长沙理工大学 | Accurate determination method for high-temperature decomposition products of humic acid organic matters |
| CN106442798B (en) * | 2016-11-04 | 2018-12-14 | 长沙理工大学 | A kind of accurate measuring method of humic-acid kind organic matter high-temperature decomposition product |
| CN109085268A (en) * | 2018-08-15 | 2018-12-25 | 青岛博正检验技术有限公司 | The measuring method of inorganic anion in a kind of product salt |
| CN113109480A (en) * | 2021-04-22 | 2021-07-13 | 山东电力研究院 | Method for detecting soluble salt component in atmospheric sediment and application thereof |
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