CN106338554A - Method for determining salt spray concentration - Google Patents
Method for determining salt spray concentration Download PDFInfo
- Publication number
- CN106338554A CN106338554A CN201510407999.6A CN201510407999A CN106338554A CN 106338554 A CN106338554 A CN 106338554A CN 201510407999 A CN201510407999 A CN 201510407999A CN 106338554 A CN106338554 A CN 106338554A
- Authority
- CN
- China
- Prior art keywords
- concentration
- sample
- chloride ion
- fog
- standard curve
- 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.)
- Pending
Links
Abstract
The invention provides a method for determining salt spray concentration. The method comprises the following steps: a) collection of a salt spray sample, taking a mixing solution of deionized water or carbonate as absorption liquid, employing a porous glass tube for collecting the salt spray sample at the flow condition of lower than 0.5 L/min; simultaneously collecting a blank sample; b) ion chromatogram detection, pre-treating the sample, drafting a chloride ion standard curve and analyzing the salt spray sample as well as the blank sample according to the optimized ion chromatogram condition; and c) calculation on the salt spray concentration according to a formula. The method is suitable for detecting salt spray concentration of nuclear industry, aviation spaceflight and precision weapon production fields.
Description
Technical field
The invention belongs to surrounding air resist technology field, and in particular to a kind of assay method of concentration of saline fog, is particularly well-suited to the mensure of low concentration salt fog in various sophisticated product storage environments.
Background technology
Salt fog refers to that a kind of suspension contains muriatic liquid particle in an atmosphere, has a diameter larger than 40 μm little, mostly below 2 μm.It is mainly mutually is clashed into and bounced by wave a large amount of sea water foams of seashore generation and swept by air-flow to float towards and cause in the air.Due to containing substantial amounts of chloride ion in salt fog it has been found that salt fog has strong corrosion failure to act on to industrial products.In nuclear industry, Aero-Space and arms of precision production field, the salt mist environment that product is run in storage process is needed to carry out adapting to Journal of Sex Research, obtaining related salt mist environment data provides necessary precondition for carrying out the research of product Corrosion Protection further, and storing for product provides Data Source.For the assay method of salt fog, current GB law regulation gb/t10593.2-2012 " electric and electronic product ambient parameter measuring method part 2: salt fog ", it is 0.12mg/l using the concentration limit that spectrophotography records chloride ion.Assume sampling 20l, absorbing liquid volume is 20ml, the concentration limit obtaining chloride ion is 0.12mg/m3, the concentration limit of conversion salt fog is 0.22mg/m3.It will be apparent that the concentration limit of the method cannot meet the requirement of low concentration salt fog.Secondly spectrophotography needs to use the secondary pollution that the toxic reagents such as Mercuric sulfocyanate, ferric ammonium sulfate easily cause environment.
Content of the invention
The technical problem to be solved in the present invention is to provide a kind of assay method of concentration of saline fog.
The assay method of the concentration of saline fog of the present invention, in turn includes the following steps:
A). the collection of salt fog sample
Using deionized water or carbonic acid mixed salt solution as absorbing liquid, salt fog sample is gathered under less than 0.5l/min flow condition using fritted glass disk bubbler；Gather blank control sample simultaneously；
B). chromatography of ions detects
Sample is carried out after pretreatment, draw the analysis of chloride ion standard curve and salt fog sample, blank control sample with the chromatography of ions condition optimizing；
C). the calculating of concentration of saline fog
Concentration of saline fog is calculated according to formula (1):
………………………… …………………………(1)
In formula:
scSalt fog content, unit is every cube of milligram (mg/m3)；
[cl-] chlorine ion concentration in absorbing liquid, unit is milligrams per liter (mg/l)；
The cumulative volume of v absorbing liquid, unit is milliliter (ml)；
Q air sampler inspiratory flow rate, unit is Liter Per Minute (l/min)；
In the t sampling time, unit is minute (min)；
1.8065 being empirical.
When deionized water in step a is as salt fog absorbing liquid, its resistance is more than 18.0
mω.
Carbonic acid mixed salt solution in step a is less than 10 for concentration-3The sodium carbonate of mol/l and the mixed solution of sodium bicarbonate.
The chromatography of ions condition of described optimization is:
Anion chromatographic column；
Leacheate component and concentration: 3.0 ~ 4.0mmol/lna2co3/1.0~1.5mmol/lnahco3 ；
Regenerated liquid: 0.05% ~ 1.0% sulfuric acid solution；
Drip washing flow velocity: 0.6 ml/min ~ 1.0ml/min；
Sample size: 100 l ~ 500 l.
The drafting of described chloride ion standard curve comprises the following steps: configures serial chloride ion standard curve concentration first, it is directly injected into ion chromatograph, the response value of measurement chloride ion, using chloride ion peak area as vertical coordinate, corresponding chlorine ion concentration, as abscissa, is drawn and is obtained standard curve.
When described salt fog sample, the analysis experiment of blank control sample, deducted after the peak area of blank using chloride ion peak area in sample, then the concentration of the chloride ion in liquid of being absorbed by chloride ion standard curve in step b.
The invention has the advantage that salt fog is detected using the method for the present invention, quickly, accurately, safety, using consistent with ion chromatograph leacheate component, as salt fog absorbing liquid, its absorption efficiency reaches more than 95.0 for the sodium carbonate of its concentration order of magnitude lower and sodium bicarbonate mixed liquor；Ion chromatography completes the once mensure of salt fog sample within 6 minutes, continuous mode does not increase any chemical toxic reagent, not generation environment pollution, when sample size is 100 μ l, detection limit reaches 1.0 μ g/l, aqueous phase micropore filter is installed it is achieved that the online pretreatment of sample, its concentration of saline fog method measurement range is 0.001 ~ 10.0mg/m3, it is particularly well-suited to the mensure of low concentration salt fog in various sophisticated product storage environments.
Specific embodiment
The assay method of the concentration of saline fog of the present invention, in turn includes the following steps:
A). the collection of sample
1). the deionized water of 18.0 m ω is more than as salt fog absorbing liquid using resistance, is injected after 10ml or 20ml absorbing liquid to clean fritted glass disk bubbler with the syringe demarcated, fritted glass disk bubbler two ends are stoppered with little stopper；Fritted glass disk bubbler using two series connection is acquired, and the salt fog being beneficial in environment is fully absorbed；
2). air sampler is sequentially connected with surge flask, fritted glass disk bubbler, after detecting that each junction is air tight, opens air sampler, the flow velocity pumping less than 0.5l/min, gather 20 l salt fog samples, simultaneously record temperature, humidity and air pressure；
3). after the completion of sampling, close air sampler switch, successively the connection between air sampler, surge flask and absorption tube is disconnected, solution in two fritted glass disk bubblers is transferred to volumetric flask constant volume, numbering respectively, treat that ion chromatograph analysis is used, record corresponding sampling time, sampling optimization information；
4). control experiment
The fritted glass disk bubbler that will be equipped with absorbing liquid carries to sampled point, and in addition to being not connected to air sampler collection air sample, remaining operates same sample, as the blank of sample；
B). sample pretreatment
Using online method, directly in ion chromatograph injection port, micropore filter is installed；
C). chromatography of ions testing conditions
Analytical tool: ion chromatograph；
Leacheate component and concentration: 3.0 ~ 4.0mmol/lna2co3/1.0~1.5mmol/lnahco3
Regenerated liquid: (0.05% ~ 1.0%) sulfuric acid solution；
Drip washing flow velocity: (0.6 ~ 1.0) ml/min；
Sample size: 100 l ~ 500 l
D). the analytical procedure of sample
1). the drafting of standard curve
Take six 100ml volumetric flasks, note people's 0.00ml, 0.005ml, 0.05ml, 0.10ml, 0.50ml, 1.0ml concentration is the chloride ion standard solution of 100mg/l respectively, plus deionized water is diluted to 100ml, obtain 0.00mg/l, 0.005 mg/l, 0.05
mg/l、0.10 mg/l、0.50
Mg/l, the chloride ion standard curve concentration of 1.0 mg/l, after each volumetric flask shakes up, it is directly injected into ion chromatograph, the response value of measurement chloride ion, obtain peak area and the retention time of chloride ion standard curve, using chloride ion peak area as vertical coordinate, corresponding chlorine ion concentration, as abscissa, is drawn and is obtained standard curve；
2). the mensure of salt fog in sample
With step 1). the testing conditions determination sample of the ion chromatograph of middle bioassay standard curve and blank control sample；After in determination sample, chloride ion peak area deducts the peak area of blank, by step 1). standard curve is absorbed the concentration (mg/l) of chloride ion in liquid；
E). the calculating of concentration of saline fog
The computing formula of concentration of saline fog is as follows:
………………………… …………………………(1)
In formula:
scSalt fog content, unit is every cube of milligram (mg/m3)；
[cl-] chlorine ion concentration in absorbing liquid, unit is milligrams per liter (mg/l)；
The cumulative volume of v absorbing liquid, unit is milliliter (ml)；
Q air sampler inspiratory flow rate, unit is Liter Per Minute (l/min)；
In the t sampling time, unit is minute (min)；
1.8065 being empirical.
Described step a). middle employing concentration is less than 10-3The sodium carbonate of mol/l and the mixed solution of sodium bicarbonate are as salt fog absorbing liquid.
Described step b). in the micropore filter aperture directly installed in ion chromatograph injection port be 0.20 μm or 0.45 μm, realize the online method of pretreatment sample.
Described chromatography of ions large volume sample injection amount is 100 ~ 500 l, or adopts pre-concentration input mode, and volume is more than 500 l.
In order to overcome the detection limit for height of salt fog analysis method in prior art, salt fog absorption efficiency is low, there is the deficiency of secondary environmental pollution, and the present invention provides a kind of assay method of concentration of saline fog.The present invention adopts using deionized water or low concentration carbonate as the absorbing liquid of salt fog, gathers about 20 l salt fog samples to connect less than 0.5l/min flow velocity, realizes the chromatography of ions advanced instrument analysis method to the online pretreatment of salt fog sample.
Salt fog in certain product storage condition of embodiment 1 measures
1. the collection of salt fog sample: sampled point (temperature: 20 DEG C in certain product storage condition, air pressure 101.2kpa), 2 are connected with the absorption tube of 0.10mmol/l sodium bicarbonate absorbing liquid equipped with 10ml 0.32mmol/l sodium carbonate and is connected with air sampler, surge flask, open sampler, with the flow velocity pumping of 0.4l/min, sampling time 60min.Solution in two absorption tubes is transferred to 10ml volumetric flask constant volume respectively, gathers blank sample simultaneously.
2. salt fog sample pretreatment and analysis
Injection port installs 0.45 μm of aqueous phase micropore filter, realizes the online pretreatment of salt fog sample.
Chromatography of ions testing conditions: 761 type ion chromatographs, leacheate component and concentration: 3.2mmol/lna are led in Switzerland ten thousand2co3/1.0mmol/lnahco3, regenerated liquid: 0.05% sulfuric acid solution, drip washing flow velocity: 0.7ml/min, sample size: 100 l.
1) precision of sample measures: carries out ion chromatography to six parallel sample collecting, calculate the concentration of saline fog in the sample of collection with above-mentioned formula (1), the results are shown in Table 1, it is 7.3% requirement being less than chemical laboratory control quality 10.0% that Duplicate Samples measure relative standard deviation (rsd).
Table 1 parallel sample salt fog measurement result
2) mensure of method accuracy: in order to investigate the accuracy of the assay method of salt fog in certain product storage condition further, a certain amount of chloride ion standard solution is added after sampling in absorbing liquid, carry out recovery testu, measure actual recovery of standard addition between 95.5% ~ 101.0%, meet the requirement that chemical laboratory controls quality 95.0% ~ 105.0%.Analysis result is shown in Table 2.
Table 2 sample salt fog recovery of standard addition measurement result
3) chromatography of ions Specification Curve of Increasing
Serial chloride ion normal concentration and peak area numerical value as shown in table 3, can be drawn according to table 3 and obtain chloride ion standard curve.
The standard curve concentration of table 3 chloride ion and peak area
Embodiment 2
Specific implementation step is same as Example 1, and its difference is to replace carbonate as the absorbing liquid of salt fog using deionized water.
The inventive method is not limited to this embodiment, all can implement and have described good result described in the inventive method content.
Claims (6)
1. a kind of assay method of concentration of saline fog is it is characterised in that in turn include the following steps:
A). the collection of salt fog sample
Using deionized water or carbonic acid mixed salt solution as absorbing liquid, salt fog sample is gathered under less than 0.5l/min flow condition using fritted glass disk bubbler；Gather blank control sample simultaneously；
B). chromatography of ions detects
Sample is carried out after pretreatment, draw the analysis of chloride ion standard curve and salt fog sample, blank control sample with the chromatography of ions condition optimizing；
C). the calculating of concentration of saline fog
Concentration of saline fog is calculated according to formula (1):
………………………………….…………………(1)
In formula:
scSalt fog content, unit is every cube of milligram (mg/m3)；
[cl-] chlorine ion concentration in absorbing liquid, unit is milligrams per liter (mg/l)；
The cumulative volume of v absorbing liquid, unit is milliliter (ml)；
Q air sampler inspiratory flow rate, unit is Liter Per Minute (l/min)；
In the t sampling time, unit is minute (min)；
1.8065 being empirical.
2. concentration of saline fog according to claim 1 assay method it is characterised in that: the resistance value of the deionized water in step a be more than 18.0 m ω.
3. concentration of saline fog according to claim 1 assay method it is characterised in that: the carbonic acid mixed salt solution in step a for concentration be less than 10-3The sodium carbonate of mol/l and the mixed solution of sodium bicarbonate.
4. the assay method of concentration of saline fog according to claim 1 is it is characterised in that the chromatography of ions condition of described optimization is:
Anion chromatographic column；
Leacheate component and concentration: 3.0 ~ 4.0mmol/lna2co3/1.0~1.5mmol/lnahco3 ；
Regenerated liquid: 0.05% ~ 1.0% sulfuric acid solution；
Drip washing flow velocity: 0.6
ml/min ~1.0ml/min；
Sample size: 100 l ~ 500 l.
5. the assay method of concentration of saline fog according to claim 1, it is characterized in that, the drafting of described chloride ion standard curve comprises the following steps: configures serial chloride ion standard curve concentration first, it is directly injected into ion chromatograph, the response value of measurement chloride ion, using chloride ion peak area as vertical coordinate, corresponding chlorine ion concentration, as abscissa, is drawn and is obtained standard curve.
6. the assay method of concentration of saline fog according to claim 1, it is characterized in that: when described salt fog sample, the analysis experiment of blank control sample, deducted after the peak area of blank using chloride ion peak area in sample, then the concentration of the chloride ion in liquid of being absorbed by chloride ion standard curve in step 1.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510407999.6A CN106338554A (en) | 2015-07-14 | 2015-07-14 | Method for determining salt spray concentration |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510407999.6A CN106338554A (en) | 2015-07-14 | 2015-07-14 | Method for determining salt spray concentration |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN106338554A true CN106338554A (en) | 2017-01-18 |
Family
ID=57826620
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510407999.6A Pending CN106338554A (en) | 2015-07-14 | 2015-07-14 | Method for determining salt spray concentration |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106338554A (en) |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107290256A (en) * | 2017-06-15 | 2017-10-24 | 国网福建省电力有限公司 | A kind of concentration of saline fog method for automatic measurement and device |
| CN109682651A (en) * | 2019-01-31 | 2019-04-26 | 上海交通大学 | A kind of collection device and detection method of portable coastal building surface chloride ion |
| CN110441412A (en) * | 2019-07-16 | 2019-11-12 | 中国石油化工股份有限公司 | A kind of detection method and device for facing micro hydrogen chloride in hydrogen production device gas phase |
| WO2020207046A1 (en) * | 2019-04-09 | 2020-10-15 | 中国电器科学研究院股份有限公司 | Device for online detection of atmospheric salt content and detection method |
| CN112763384A (en) * | 2020-12-09 | 2021-05-07 | 中国电器科学研究院股份有限公司 | Online salt spray concentration rapid monitoring method and device based on particle size distribution spectrum |
| CN116990202A (en) * | 2023-09-25 | 2023-11-03 | 哈尔滨工程大学 | Online salt fog concentration measurement simulation device and method |
-
2015
- 2015-07-14 CN CN201510407999.6A patent/CN106338554A/en active Pending
Non-Patent Citations (4)
| Title |
|---|
| 国家技术监督局: "《GB 10593-90 电工电子产品环境参数测量方法 盐雾》", 1 August 1990 * |
| 李士永: "工作场所空气中多种酸性气体同时测定的离子色谱法", 《中华劳动卫生职业病杂志》 * |
| 田小萌: "离子色谱法测定空气中氟化氢氯化氢和硫酸", 《环境监测管理与技术》 * |
| 陶志红: "离子色谱法测定环境空气中氯化氢含量", 《漳州师范学院学报（自然科学版）》 * |
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107290256A (en) * | 2017-06-15 | 2017-10-24 | 国网福建省电力有限公司 | A kind of concentration of saline fog method for automatic measurement and device |
| CN107290256B (en) * | 2017-06-15 | 2023-07-28 | 国网福建省电力有限公司 | Automatic salt fog concentration measuring method and device |
| CN109682651A (en) * | 2019-01-31 | 2019-04-26 | 上海交通大学 | A kind of collection device and detection method of portable coastal building surface chloride ion |
| WO2020207046A1 (en) * | 2019-04-09 | 2020-10-15 | 中国电器科学研究院股份有限公司 | Device for online detection of atmospheric salt content and detection method |
| US11878298B2 (en) | 2019-04-09 | 2024-01-23 | China National Electric Apparatus Research Institute Co., Ltd. | Device for online detection of atmospheric salt fog content and detection method thereof |
| CN110441412A (en) * | 2019-07-16 | 2019-11-12 | 中国石油化工股份有限公司 | A kind of detection method and device for facing micro hydrogen chloride in hydrogen production device gas phase |
| CN112763384A (en) * | 2020-12-09 | 2021-05-07 | 中国电器科学研究院股份有限公司 | Online salt spray concentration rapid monitoring method and device based on particle size distribution spectrum |
| CN112763384B (en) * | 2020-12-09 | 2021-11-30 | 中国电器科学研究院股份有限公司 | Online salt spray concentration rapid monitoring method and device based on particle size distribution spectrum |
| CN116990202A (en) * | 2023-09-25 | 2023-11-03 | 哈尔滨工程大学 | Online salt fog concentration measurement simulation device and method |
| CN116990202B (en) * | 2023-09-25 | 2024-01-09 | 哈尔滨工程大学 | Online salt fog concentration measurement simulation device and method |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN106338554A (en) | Method for determining salt spray concentration | |
| CN106908564B (en) | The method for measuring lithium in smoke-free tobacco product, sodium, ammonia, potassium, magnesium, calcium content simultaneously | |
| CN102590383A (en) | Method for determining content of potassium, sodium, calcium and magnesium in cigarette paper simultaneously | |
| CN101968436B (en) | Quantitative analysis method for measuring trace nickel in water by microwave digestion-flame atomic absorption spectrometry (FAAS) | |
| Al-Horr et al. | A continuous analyzer for soluble anionic constituents and ammonium in atmospheric particulate matter | |
| CN102818864A (en) | Passive sampling detection method of formaldehyde in environment | |
| CN109142612A (en) | The measuring method of TMSP in lithium battery electrolytes | |
| CN102331462B (en) | Method for measuring ammonia content in water base adhesive for tobaccos | |
| CN113899822A (en) | Method for determining purity of lithium hexafluorophosphate based on ion chromatography technology | |
| CN103776931B (en) | The assay method of the ethamine in workplace air | |
| CN103675125B (en) | Test device for sampling efficiency of volatile organic compounds in air | |
| CN104865175A (en) | Method for detecting concentration of PM2.5 (particulate matter) in air | |
| CN104730162B (en) | A kind of measure the ion chromatographic method of trace anion content in iron phosphate | |
| CN107328877A (en) | A kind of method of N methyl diethanolamine contents in LC-MS analysis water | |
| CN207933311U (en) | A kind of purification devices of chromatographically pure Loprazolam | |
| CN109613168A (en) | The method for monitoring sulfur dioxide concentration in gas attack chamber on-line | |
| CN110887930A (en) | Method for measuring oxalic acid content in workplace | |
| CN102539557B (en) | Method for analyzing and detecting methoxyacetic acid | |
| CN104807911A (en) | Method for testing glycidol in air and waste gas | |
| CN110411961A (en) | A kind of apparatus and method measuring underwater trace cyanide | |
| CN104749304A (en) | Method for determining concentrations of cyanide ion and sulfide ion in desulphurization solution | |
| CN103472169B (en) | Method for measuring content of bromide ions in brine by gas chromatography | |
| CN203117142U (en) | Device for detecting content of formaldehyde in food | |
| CN105588887B (en) | Chloride test working solution and detection method and application in Power Plant Water Vapor | |
| CN103091371A (en) | Detection method and detection device for content of formaldehyde in foods |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| WD01 | Invention patent application deemed withdrawn after publication | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20170118 |