CN106018401A - Method for determining content of chlorine ions in water - Google Patents
Method for determining content of chlorine ions in water Download PDFInfo
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- CN106018401A CN106018401A CN201610489427.1A CN201610489427A CN106018401A CN 106018401 A CN106018401 A CN 106018401A CN 201610489427 A CN201610489427 A CN 201610489427A CN 106018401 A CN106018401 A CN 106018401A
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/75—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
- G01N21/77—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator
- G01N21/82—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator producing a precipitate or turbidity
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Abstract
The invention discloses a method for determining the content of chlorine ions in water. Turbidimetry method is adopted to determine the content of the chlorine ions in the water. The method comprises the following steps: adding silver ions into a water sample to be used as a precipitator, adding Arabic gum powder as a stabilizer, and uniformly shaking to obtain turbid liquid; and determining the turbidity of the turbid liquid, and calculating the content of the chlorine ions in the water according to the turbidity. By adopting the Arabic gum powder as the stabilizer, the method has the characteristics of good analysis data repeatability, simplicity and convenience in operation, high analysis speed, low detection lower limit and the like.
Description
Technical field
The present invention relates to the assay method of chloride ion content in a kind of water, belong to analysis field tests.
Background technology
The corrosion of metal material is had a great impact by chloride ion, can cause intercrystalline crack and the non-plastic fracture of metal structure, because of
This, the content of chloride ion is the important monitor control index of boiler plant.
At present, measure trace chlorine in water and mainly use a mole method, the chromatography of ions, spectrophotography and turbidimetry.Mole
Method mensuration chloride content is in the range of (5-100) mg/L, when chloride content is less than 5mg/L, uses the method inspection not measure
Muriatic content.Ion-chromatographic determination chloride ion is easy quickly, but ion chromatograph is expensive, considerably increases detection
Cost.Enrichment spectrophotography can be used for the analysis of trace chlorine in water, but the method use lead phosphate, sulfur cyanogen
Acid hydrargyrum and methanol are all noxious substances, and dangerous operation personnel's is healthy, and easily causes environmental pollution.The domestic people of having sets up
Mercuric sulfocyanate-ferric nitrate indirect spectrophotometric methods measure the trace chlorine in water, are (0.2～10) mg/L model at chloride ion content
In good linear relationship in enclosing, but the Mercuric sulfocyanate used is noxious substance equally, the health of harm operator and pollution ring
Border.
Summary of the invention
Present invention solves the technical problem that and be to provide the assay method of chloride ion content in the water of a kind of green, highly sensitive, can
Content with the trace chlorine in detection water outlet.
The technical scheme is that, it is provided that the assay method of chloride ion content in a kind of water, use in turbidimetry for Determination water chlorine from
Sub-content；Comprise the following steps: in water sample to be measured, addition silver ion is as precipitant, adds gum arabic powder as surely
Determine agent, shake up to obtain suspension；Measure the turbid luminosity of suspension, calculate the content of chloride ion in water according to turbid photometer.
Further, described stabilizer is to add with the form of Radix Acaciae senegalis amidin.
Further, in described suspension, the concentration of gum arabic powder is 10-14g/L.
The addition adding Radix Acaciae senegalis amidin in described suspension is 5mL, and the concentration of added gum arabic powder is
100g/L.With turbidimetry for Determination chloride ion accuracy it is crucial that improve precipitation stability.Add a certain amount of Radix Acaciae senegalis
Powder, can make the optical stability of suspension system significantly improve.This method determines Radix Acaciae senegalis in suspension by test
When the addition of powder is 5-7mL (50mL cuvette), the turbid luminosity of suspension is maximum and stable, i.e. Arabic tree in suspension
The concentration of rubber powder is 10-14g/L.
Further, the content of described Chloride Ion In Water to be measured is 0.2-5mg/L.This method is used to measure chloride ion in water
Time, in good linear relationship in the range of chloride ion content is (0.2～5) mg/L.And the method Monitoring lower-cut of the present invention is low,
In the range of chloride ion content is 0.2-2mg/L, degree of accuracy is the most fine.
Further, after described suspension stands 30 minutes, the more turbid luminosity of suspension is measured.From solution to be measured add Ah
Drawing uncle's natural gum powder solution to shake up the calculating time, measured the most turbid luminosity every 10 minutes, after 30min, the turbid luminosity of suspension reaches
To maximum, and can stablize 1h, therefore this method measures the turbid luminosity of suspension after using and adding gum arabic powder 30min.
Further, measuring the wavelength of light wave used by the turbid luminosity of suspension is 340nm.With blank solution as reference, to suspension
Carrying out all band scanning, it is known that at wavelength 340nm, the absorption of suspension is maximum, in order to obtain higher sensitivity, and we
Method uses 340nm as measuring wavelength.
It is an object of the invention to overcome deficiency of the prior art, it is provided that chloride ion (particularly trace chlorine) in a kind of water
The assay method of content, the method utilizes silver ion to generate, with chloride ion, the silver nitride precipitation that dissolubility is the least, uses Arab tree
Rubber powder solution is made precipitation stabilizer and is formed suspension, with the turbid luminosity of this suspension of spectrophotometric determination, according to working curve side
Journey calculates the content of chloride ion in water outlet.The assay method of the present invention, have analytical data favorable reproducibility, simple to operation,
Analyze the features such as speed is fast, calibrating lower limit is low.
The present invention will be further explained below:
In turbidimetry for Determination water, the theoretical foundation of trace chlorine is as follows:
Turbidimetry is mainly used in measuring the deposit that can form suspended substance.When light beam passes through a medium containing particle in suspension,
Owing to particle in suspension is to scattering of light effect and selective absorption, make the strength reduction of transmission light.In turbidimetry, transmittance
With the mathematical expression that the relation object of suspended sediment concentration is similar to Lambert-Beer's law:
In formula (1), s is turbid luminosity (or turbid rate), represents the light intensity decays caused due to the scattering process of float；I0Divide with I
Wei incident intensity and transmitted intensity；B is optical path length；C is the concentration of particle in suspension；K is constant, cries the most again turbid
Degree coefficient, its value is relevant with the refractive index of the size of particle, shape, the wavelength of incident illumination, float and medium.
In determination of chloride ion, silver ion can generate the AgCl precipitation that dissolubility is the least, turbid luminosity size and Cl with chloride ion-Dense
Degree is directly proportional.The turbid luminosity of Accurate Determining float it is crucial that select suitably to precipitate stabilizer, making to be deposited in a period of time can be steady
Fixed distribution.Can the stability that solve AgCl precipitation be the key of Accurate Determining chloride ion content.It is used as precipitation stabilizer at present
Mainly have lower-molecular substance such as glycerol etc. and polymer substance such as glue number class, cellulose etc..Gum arabic powder is a kind of natural
Polymer substance, in water, solubilized becomes viscous liquid, can be used as precipitate stabilizer.
When analyzing, it is necessary to curve of first working, with turbid luminosity, the concentration of known float is mapped.
Compared with prior art, present invention have an advantage that
The stabilizer that a, employing gum arabic powder solution precipitate as AgCl, can make the optical stability of AgCl suspension system
Good and simple to operate, analytical data favorable reproducibility, accurately and reliably, and the gum arabic powder used be one sky to analytical data
Right macromolecule precipitation stabilizer, does not affect the healthy and free from environmental pollution of operating personnel.
B, this method use ultraviolet spectrometry protractor to measure turbid luminosity, and the content of chloride ion can be made in mensuration water relative to a mole method
Calibrating lower limit is substantially reduced.
Accompanying drawing explanation
Accompanying drawing represents the concentration c of known float chloride ion and the graph of a relation of turbid luminosity in embodiment 1.
Detailed description of the invention
The present invention is further illustrated with embodiment below in conjunction with the accompanying drawings.
Embodiment 1:
Take 0.0 successively, 2.0,4.0,6.0,8.0, the chloride ion standard solution of 10.0mL in 50mL color comparison tube, dilution
To 25mL, it is sequentially added into HNO3Solution, AgNO3Solution, shakes up；Add gummi arabicum pulveratum solution 5mL, dilution
To scale, shake up, to be not added with Cl-It is zero that the reference liquid of standard solution adjusts the turbid luminosity of instrument, at maximum wavelength, measures
The turbid luminosity A of solution, with the chloride ion content (mg) in standard solution as abscissa, corresponding turbid luminosity is vertical coordinate, draws
Working curve.
1, instrumentation condition is spectrophotometer: 752N spectrophotometer (Shanghai Precision Scientific Apparatus Co., Ltd)；Stone
English cuvette (5cm)；
2, condition determination
Mensuration wavelength is 340nm；The turbid luminosity of AgCl suspension is surveyed after adding gummi arabicum pulveratum 30min.
3, the drafting of working curve
According to above-mentioned experiment condition, measure known Cl-The turbid luminosity of content suspension, the results are shown in Table 1.
The known Cl of table 1-The measurement result of the turbid luminosity of content suspension
| Cl-Content, mg | 0 | 0.02 | 0.04 | 0.06 | 0.08 | 0.10 |
| Turbid luminosity | 0 | 0.148 | 0.306 | 0.465 | 0.594 | 0.767 |
With the chloride ion content (mg) in standard solution as abscissa, corresponding turbid luminosity is vertical coordinate, carries out linear regression, sees
Fig. 1.It will be seen from figure 1 that the correlation coefficient of chlorine ion concentration and turbid luminosity reaches 0.9995, illustrate in given scope,
Chlorine ion concentration and turbid luminosity are good linear relationship.Chlorine ion concentration and turbid photometric relationship figure, as shown in Figure 1.
4, sample analysis
Accurately pipette 25.0mL water sample in 50mL color comparison tube, be measured under these experimental conditions, record turbid luminosity.With
Mass concentration ρ represents chloride ion content, calculates the content of chloride ion in water by formula (2).
In formula:
The numerical value of V--volume of water sample, rises；
M--the numerical value of the quality of the chlorine checked in by standard curve, milligram.
Embodiment 2:
Accurately pipette 25.0mL electrothermal stove water water sample in 50mL color comparison tube, be measured under these experimental conditions, record
Turbid luminosity is 0.052.Calculate with the formula of embodiment 1, represent that the chlorine ion concentration in water is for 0.28 with mass concentration ρ
mg/L。
Embodiment 3:
1.0mg/L Cl is added in electrothermal stove water water sample-Standard solution 5.00mL, is measured under these experimental conditions, meter
The recovery of standard addition drawn is 98.24%.
Embodiment 4:
Preparation Cl-Concentration is the solution of 1.0mg/L, accurately pipettes this solution 25.0mL in 50mL color comparison tube, in above-mentioned experiment
Under the conditions of be measured, the turbid luminosity recorded is 0.186.Calculate with the formula of embodiment 1, represent in water with mass concentration ρ
Chlorine ion concentration be 0.981mg/L.
Embodiment 5:
Preparation Cl-Concentration is the solution of 2.0mg/L, accurately pipettes this solution 25.0mL in 50mL color comparison tube, in above-mentioned experiment
Under the conditions of be measured, the turbid luminosity recorded is 0.385.Calculate with the formula of embodiment 1, represent in water with mass concentration ρ
Chlorine ion concentration be 2.03mg/L.
Comparative example:
Add a certain amount of precipitation stabilizer, the optical stability of suspension system can be made to improve.It is used as precipitation stabilizer at present
Mainly have lower-molecular substance such as glycerol etc. and polymer substance such as glue number class, cellulose etc..In experimentation, applicant tastes
Tween-60 has been selected in examination, and PVA solution is as precipitation stabilizer, the turbid luminosity of the suspension measured and the line of chloride ion content
Sexual relationship is the most bad.
Claims (6)
1. the assay method of chloride ion content in a water, it is characterised in that use chloride ion content in turbidimetry for Determination water；Comprise the following steps: in water sample to be measured, add silver ion as precipitant, add gum arabic powder as stabilizer, shake up to obtain suspension；Measure the turbid luminosity of suspension, calculate the content of chloride ion in water according to turbid photometer.
2. assay method as claimed in claim 1, it is characterised in that described stabilizer is to add with the form of Radix Acaciae senegalis amidin.
3. assay method as claimed in claim 1 or 2, it is characterised in that in described suspension, the concentration of gum arabic powder is 10-14 g/L.
4. assay method as claimed in claim 1 or 2, it is characterised in that the content of described Chloride Ion In Water to be measured is 0.2-5mg/L.
5. assay method as claimed in claim 1 or 2, it is characterised in that after described suspension stands 30 minutes, then measure the turbid luminosity of suspension.
6. assay method as claimed in claim 1 or 2, it is characterised in that measuring the wavelength of light wave used by the turbid luminosity of suspension is 340nm.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610489427.1A CN106018401A (en) | 2016-06-29 | 2016-06-29 | Method for determining content of chlorine ions in water |
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| CN201610489427.1A CN106018401A (en) | 2016-06-29 | 2016-06-29 | Method for determining content of chlorine ions in water |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107064033A (en) * | 2017-04-28 | 2017-08-18 | 攀钢集团研究院有限公司 | The Quick qualitative detection method and fast quantitative measurement method for detecting of chlorion |
| CN108072622A (en) * | 2017-12-29 | 2018-05-25 | 新津海天水务有限公司 | Chlorion rapid detection method in a kind of tap water |
| CN112730403A (en) * | 2020-12-29 | 2021-04-30 | 中国南方电网有限责任公司超高压输电公司柳州局 | Portable measuring device for chlorine and chloride content in atmosphere and gas measuring method thereof |
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| CN104198488A (en) * | 2014-09-24 | 2014-12-10 | 山西翔宇化工有限公司 | Method for measuring content of free chlorine ions in phenylamine |
| CN105403523A (en) * | 2015-10-27 | 2016-03-16 | 遵宝钛业有限公司 | Method for determining chlorine in titanium sponge, titanium and titanium alloy |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104198488A (en) * | 2014-09-24 | 2014-12-10 | 山西翔宇化工有限公司 | Method for measuring content of free chlorine ions in phenylamine |
| CN105403523A (en) * | 2015-10-27 | 2016-03-16 | 遵宝钛业有限公司 | Method for determining chlorine in titanium sponge, titanium and titanium alloy |
Non-Patent Citations (2)
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107064033A (en) * | 2017-04-28 | 2017-08-18 | 攀钢集团研究院有限公司 | The Quick qualitative detection method and fast quantitative measurement method for detecting of chlorion |
| CN108072622A (en) * | 2017-12-29 | 2018-05-25 | 新津海天水务有限公司 | Chlorion rapid detection method in a kind of tap water |
| CN112730403A (en) * | 2020-12-29 | 2021-04-30 | 中国南方电网有限责任公司超高压输电公司柳州局 | Portable measuring device for chlorine and chloride content in atmosphere and gas measuring method thereof |
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