CN110907586A - Method for measuring content of sulfite in water - Google Patents

Method for measuring content of sulfite in water Download PDF

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Publication number
CN110907586A
CN110907586A CN201911322122.1A CN201911322122A CN110907586A CN 110907586 A CN110907586 A CN 110907586A CN 201911322122 A CN201911322122 A CN 201911322122A CN 110907586 A CN110907586 A CN 110907586A
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Prior art keywords
sulfite
sample
water
concentration
measuring
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林新艳
俞晓明
顾承伟
王红玲
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Jiangsu Taijie Zhibang Testing Technology Co Ltd
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Jiangsu Taijie Zhibang Testing Technology Co Ltd
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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/96—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation using ion-exchange
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02—Column chromatography
    • G01N30/60—Construction of the column

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  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
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  • Analytical Chemistry (AREA)
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  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
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  • Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)

Abstract

The invention discloses a method for measuring the content of sulfite in water, which comprises the following steps: using a mixed solution of sodium carbonate and sodium bicarbonate as an eluent, and adopting Dionex IonPacTMThe AS22 anion analytical column and the conductivity detector are used for measuring the content of sulfite by ion chromatography.

Description

Method for measuring content of sulfite in water
The technical field is as follows:
the invention belongs to the technical field of analysis and test, and particularly relates to a method for measuring sulfite content in water.
Background art:
with the rapid development of modern industry, the harm of acid rain formed by sulfur dioxide pollution to the environment is larger and larger, after the sulfur dioxide enters a water body, the sulfur dioxide exists in the water in a dynamic balance of sulfite and bisulfite, and has a certain poisoning effect on fishes and aquatic organisms in the water, and the reducing property of the sulfur dioxide can quickly consume dissolved oxygen in the water to deteriorate the water quality. In addition, the sulfite can be mutually converted with sulfur in different forms in the water body on one hand, and can be converted into sulfur dioxide on the other hand, and then the sulfur dioxide enters the atmosphere through gas-liquid exchange. Therefore, the concentration of sulfite in the water body is an important index of sulfur and related environmental problems, and has important significance for analyzing and determining the concentration of sulfite in water.
Currently, the detection of sulfite is carried out by an iodometry method, a colorimetric method, a distillation-alkali titration method, an ion chromatography method and the like, and the iodometry method, the colorimetric method and the distillation-alkali titration method are long in time consumption and low in precision, so that the ion chromatography method is a better method. The chromatographic column of the ion chromatograph used in the method is AS22, and is a special column for analyzing various anions (fluoride ions, chloride ions, nitrate ions, nitrite ions, sulfate ions, phosphate ions, bromide ions and the like) in the domestic drinking water.
The invention content is as follows:
the invention aims to overcome the defects in the prior art, and provides a method for measuring the content of sulfite in water, which is simple and convenient to operate, high in analysis speed and low in cost.
In order to achieve the purpose, the invention provides a method for measuring the content of sulfite in water, wherein the method takes a mixed solution of sodium carbonate and sodium bicarbonate as an eluent and adopts Dionex IonPacTMThe AS22 anion analytical column and the conductivity detector are used for measuring the content of sulfite by ion chromatography.
The method provided by the invention comprises the following steps: drawing a standard curve, collecting a sample, measuring the sample and calculating the concentration of sulfite.
The drawing of the standard curve comprises the following steps: (1) preparing standard secondary mother liquor: taking 0.1mL of sulfite standard solution into a 10mL volumetric flask, adding ultrapure water to constant volume and mixing uniformly. This was 100. mu.g/mL of sulfite standard secondary mother liquor. (2) Preparing a standard curve solution: transferring 0.125mL, 0.250mL, 0.625mL, 0.500mL, 1.00mL of sulfite standard secondary mother liquor into 25mL, 10mL volumetric flasks respectively to prepare standard curve solutions of 0.5. mu.g/mL, 1.0. mu.g/mL, 2.5. mu.g/mL, 5.0. mu.g/mL, 10. mu.g/mL. Mixing and performing on-machine analysis. (3) Drawing a standard curve: adjusting an ion chromatograph to an optimal determination state according to the operation conditions of the instrument, sequentially determining a standard series according to the sequence of the concentration of the standard solution from low to high, repeatedly determining each concentration for 3 times, and drawing a standard curve according to the peak area average value to the corresponding concentration of the sulfite.
The collecting of the sample comprises:
after sample collection, 0.1% formaldehyde must be added for fixation. The collected sample should be analyzed as soon as possible, if the measurement cannot be carried out in time, the sample should be filtered by an air-extracting and filtering device, and then refrigerated below 4 ℃ and stored away from light.
The determination of the sample comprises:
the clean water sample without interfering substances such as hydrophobic compounds, heavy metals or transition metal ions can be directly sampled after being filtered by an air-extracting and filtering device; or injecting sample with disposable injector with water system microporous membrane syringe filter. For a complex water quality sample containing interfering substances, a corresponding pretreatment column is required to be used for effectively removing the sample and then injecting the sample. Injecting the sample into an ion chromatograph to determine the concentration of sulfite according to the chromatographic conditions and steps which are the same as those for drawing a standard curve, and carrying out qualitative retention time and quantitative peak area determination.
The calculation of the concentration of sulfite comprises: the calculation formula for the concentration of sulfite in the sample is:
C＝C1×f-C0
c-concentration of sulfite in Water in milligrams per liter (mg/L)
C1Reading by the instrument the concentration of sulphite in the sample solution in milligrams per litre (mg/L)
C0Concentration of sulfite in the laboratory blank in milligrams per liter (mg/L)
f is the dilution factor.
Description of the drawings:
FIG. 1 is a test chart of sulfite concentration.
The specific implementation mode is as follows:
the following describes in detail specific embodiments of the present invention. It should be understood that the detailed description and specific examples, while indicating the present invention, are given by way of illustration and explanation only, not limitation.
Example 1: determining the concentration of sulfite in a water
Using a mixed solution of sodium carbonate and sodium bicarbonate as an eluent, and adopting Dionex IonPacTMThe AS22 anion analytical column and the conductivity detector are used for measuring the content of sulfite by ion chromatography.
The method comprises the following steps: drawing of standard curve
(1) Preparing standard secondary mother liquor: taking 1mL of sulfite standard solution into a 10mL volumetric flask, adding ultrapure water to constant volume and mixing uniformly. This was 100. mu.g/mL of sulfite standard secondary mother liquor.
(2) Preparing a standard curve solution: transferring 0.125mL, 0.250mL, 0.625mL, 0.500mL, 1.00mL of sulfite standard secondary mother liquor into 25mL, 10mL volumetric flasks respectively to prepare standard curve solutions of 0.5. mu.g/mL, 1.0. mu.g/mL, 2.5. mu.g/mL, 5.0. mu.g/mL, 10. mu.g/mL. Mixing and performing on-machine analysis.
(3) Drawing a standard curve: adjusting an ion chromatograph to an optimal determination state according to the operation conditions of the instrument, sequentially determining a standard series according to the sequence of the concentration of the standard solution from low to high, repeatedly determining each concentration for 3 times, and drawing a standard curve according to the peak area average value to the corresponding concentration of the sulfite.
Step two: collection of samples
After sample collection, 0.1% formaldehyde must be added for fixation. The collected sample should be analyzed as soon as possible, if the measurement cannot be carried out in time, the sample should be filtered by an air-extracting and filtering device, and then refrigerated below 4 ℃ and stored away from light.
Step three: determination of samples
(1) Determination of samples
The clean water sample without interfering substances such as hydrophobic compounds, heavy metals or transition metal ions can be directly sampled after being filtered by an air-extracting and filtering device; or injecting sample with disposable injector with water system microporous membrane syringe filter. For a complex water quality sample containing interfering substances, a corresponding pretreatment column is required to be used for effectively removing the sample and then injecting the sample. Injecting the sample into an ion chromatograph to determine the concentration of sulfite according to the chromatographic conditions and steps which are the same as those for drawing a standard curve, and carrying out qualitative retention time and quantitative peak area determination.
FIG. 1 is a test chart of sulfite concentration.
(2) Determination of detection Limit
Because the blank has no sulfite, 2-5 times of the estimated detection limit is taken, and a standard solution with fixed concentration is continuously injected into a 7-needle sample, and the detection limit measurement result of the sulfite is shown in the following table:
serial number Values read from the curves/(mg/L)
1 0.4338
2 0.4402
3 0.4229
4 0.4485
5 0.4224
6 0.4308
7 0.4139
Standard deviation/(mg/L) 0.0092
t value 3.143
Detection limit/(mg/L) 0.029
Lower limit of measurement/(mg/L) 0.116
Therefore, the detection limit of the method for measuring the content of the sulfite is 0.029 mu g/mL.
(3) Determination of precision
Under the above operating conditions, after the baseline of the apparatus is stabilized, the low, medium and high concentration standard solutions are measured in parallel 6 times, and the relative standard deviation is calculated, and the results are shown in the following table:
serial number Low concentration/(mg/L) Intermediate concentration/(mg/L) High concentration/(mg/L)
1 0.4338 2.3308 10.0875
2 0.4402 2.3248 9.3779
3 0.4229 2.2707 10.16344
4 0.4485 2.2721 10.4984
5 0.4224 2.0785 10.1560
6 0.4308 2.1250 10.1643
Mean value/(mg/L) 0.4331 2.2337 10.0746
Standard deviation/(mg/L) 0.0101 0.1063 0.3709
Relative standard deviation/%) 2.3 4.8 3.7
The precision of the low, medium and high concentration measurements of the sulfite content thus obtained were 2.3%, 4.8% and 3.7%, respectively.
(4) Determination of accuracy
And (3) performing a standard adding recovery test on the actually measured sample to obtain the accuracy of 97.5%, 99.0% and 98.5% respectively.
Step four: calculation of the sulfite concentration
The calculation formula for the concentration of sulfite in the sample is:
C＝C1×f-C0
c-concentration of sulfite in Water in milligrams per liter (mg/L)
C1Reading by the instrument the concentration of sulphite in the sample solution in milligrams per litre (mg/L)
C0Concentration of sulfite in the laboratory blank in milligrams per liter (mg/L)
f is the dilution factor.
By the method, the content of the sulfite in the water sample is measured, the detection limit is 0.029mg/L, the measurement lower limit is 0.116mg/L, the precision of low, medium and high concentration is respectively 2.3%, 4.8% and 3.7%, and the accuracy obtained by adding standard recovery tests on the actually measured sample is respectively 97.5%, 99.0% and 98.5%. Thus, by ion chromatography, in Dionex IonPacTMUnder the conditions of AS22 anion analytical column and conductivity detector, the method for measuring the content of sulfite in water is feasible.

Claims (3)

1. A method for measuring the content of sulfite in water is characterized in that a mixed solution of sodium carbonate and sodium bicarbonate is used as an eluent, and Dionex IonPac is adoptedTMThe AS22 anion analytical column and the conductivity detector are used for measuring the content of sulfite by ion chromatography.
2. The method of claim 1, comprising the steps of: drawing a standard curve, collecting a sample, measuring the sample and calculating the concentration of sulfite.
3. The method of claim 2, wherein the sample is determined using a Dionex IonPacTMAnd (3) carrying out ion chromatography determination on the AS22 anion analytical column and a conductivity detector, and carrying out qualitative retention time and quantitative peak area.
CN201911322122.1A 2019-12-20 2019-12-20 Method for measuring content of sulfite in water Pending CN110907586A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111999130A (en) * 2020-08-31 2020-11-27 重庆惠能标普科技有限公司 Anti-oxidation absorption liquid for collecting sulfur dioxide and preparation method thereof
CN114460028A (en) * 2020-11-09 2022-05-10 上海梅山钢铁股份有限公司 Method for detecting content of calcium sulfate in sintering desulfurization and denitrification ash

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104407078A (en) * 2014-11-26 2015-03-11 中山出入境检验检疫局检验检疫技术中心 Pretreatment method for sample to be detected by sulfur dioxide residue detection method
CN106645460A (en) * 2016-11-08 2017-05-10 同济大学 Method for quickly and accurately determining sulfite, sulfate and thiosulfate anion in biogas slurry
CN107478734A (en) * 2017-06-29 2017-12-15 河北工业大学 The chromatography of ions detection method of sulfate radical and inferior sulfate radical is determined in a kind of desulfurization seawater simultaneously
CN110470785A (en) * 2019-09-26 2019-11-19 苏州金宏气体股份有限公司 The detection method of sulfur dioxide and sulfate in boron trifluoride

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104407078A (en) * 2014-11-26 2015-03-11 中山出入境检验检疫局检验检疫技术中心 Pretreatment method for sample to be detected by sulfur dioxide residue detection method
CN106645460A (en) * 2016-11-08 2017-05-10 同济大学 Method for quickly and accurately determining sulfite, sulfate and thiosulfate anion in biogas slurry
CN107478734A (en) * 2017-06-29 2017-12-15 河北工业大学 The chromatography of ions detection method of sulfate radical and inferior sulfate radical is determined in a kind of desulfurization seawater simultaneously
CN110470785A (en) * 2019-09-26 2019-11-19 苏州金宏气体股份有限公司 The detection method of sulfur dioxide and sulfate in boron trifluoride

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111999130A (en) * 2020-08-31 2020-11-27 重庆惠能标普科技有限公司 Anti-oxidation absorption liquid for collecting sulfur dioxide and preparation method thereof
CN114460028A (en) * 2020-11-09 2022-05-10 上海梅山钢铁股份有限公司 Method for detecting content of calcium sulfate in sintering desulfurization and denitrification ash

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Application publication date: 20200324