CN113311102A - Method for measuring permanganate index in water - Google Patents
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- CN113311102A CN113311102A CN202110452725.4A CN202110452725A CN113311102A CN 113311102 A CN113311102 A CN 113311102A CN 202110452725 A CN202110452725 A CN 202110452725A CN 113311102 A CN113311102 A CN 113311102A
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N31/00—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods
- G01N31/16—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods using titration
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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
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Abstract
The invention relates to the technical field of substance analysis and detection, and discloses a method for determining permanganate index in water, which comprises the steps of absorbing 100mL of a sample which is fully shaken and uniformly mixed, placing the sample in a 250mL conical flask, adding 4.5-5.5 mL of sulfuric acid solution, adding 10mL of potassium permanganate solution with the concentration of 0.01mo1/L by using a burette, placing the conical flask in a boiling water bath for 40-107 min after shaking uniformly, wherein the boiling water bath duration of the sample is respectively as follows according to different heights of altitudes in Tibet in combination with different boiling points of the water bath: lasa, Shannan and Linzhi for 45 minutes; daily kart 55 minutes; changdall for 40 minutes; ali for 81 minutes; narcotine for 107 minutes; titrating a sample; blank test; calibrating; and (6) calculating a result. The method is suitable for measuring drinking water, source water and ground water in high-altitude areas of Tibet, the measuring range is 0.5-4.5 mg/L, and the water quality with serious pollution can still be measured after dilution.
Description
Technical Field
The invention relates to the technical field of substance analysis and detection, in particular to a method for measuring permanganate index in water (a non-standard method in plateau regions).
Background
The plateau is an important water source holding area and a supply area in China and also belongs to a typical ecological environment fragile area in China, the water quality condition of the plateau is influenced by natural geographic conditions such as landform, geology, climate and the like and human activities, the water quality of the plateau is not only a guarantee for the healthy development of a local ecological system, but also has direct influence on the safety of underground water quality, and therefore, the plateau is very important for monitoring the water environment of the plateau area. At present, water environment detection personnel in autonomous regions in Tibet are assiduously researching and discussing a permanganate index determination method suitable for plateau areas in the daily water quality detection process, and through years of tests of the inventor, the invention provides a method for determining the permanganate index in water.
Disclosure of Invention
Based on the problems, the invention provides a method for measuring the permanganate index in water (a nonstandard method in plateau regions), which is suitable for measuring drinking water, source water and ground water in Tibet high-altitude regions, and the measuring range is 0.5-4.5 mg/L.
In order to solve the technical problems, the invention provides the following technical scheme:
a method for measuring the permanganate index in water (a high-altitude area non-standard method) comprises the following steps:
s1: sucking 100mL of sample which is fully shaken and uniformly mixed, placing the sample in a 250mL conical flask, adding 4.5-5.5 mL of sulfuric acid solution, adding 10mL of potassium permanganate solution with the concentration of 0.01mo1/L by using a burette, placing the conical flask in a boiling water bath for 40-107 min after shaking uniformly, wherein the time of the sample boiling water bath is respectively as follows: lasa, Shannan, Linzhi 45min, Rike 55min, Changdu 40min, Ali 81min, and Naqu 107 min;
s2: titration of samples
Adding 10mL of sodium oxalate solution with the concentration of 0.01mo1/L into the erlenmeyer flask treated in the step S1 by using a clean tube until the solution becomes colorless, titrating the solution with potassium permanganate solution with the concentration of 0.01mo1/L until the solution in the erlenmeyer flask just appears pink when the solution is hot and the pink color is kept for 30S, and recording the volume of the potassium permanganate solution consumed at the moment;
s3: blank test
Replacing the sample in step S1 with 100mL of water containing no reducing substance, measured according to the procedures of step S1 and step S2, and recording the volume of the final back-dropped potassium permanganate solution;
s4: calibration
Adding 10mL of 0.01mo1/L sodium oxalate solution into the solution titrated in the step S3, continuously titrating the solution by using 0.01mo1/L potassium permanganate solution at the temperature of 80 ℃ until the solution just appears pink, and keeping the pink color for 30S, and recording the volume of the potassium permanganate solution consumed at the moment;
s5: calculation of results
Permanganate index IMnExpressed as milligrams oxygen consumed per liter of sample (O)2，mg/L) Calculated as follows (1):
V1represents the volume of potassium permanganate solution consumed during the sample titration in step S2; v2Represents the volume of potassium permanganate solution consumed during the calibration in step S4; c represents the concentration of sodium oxalate standard solution (4.6).
Further, the sulfuric acid solution in step S1 is prepared as follows: under the condition of continuous stirring, 100mL of sulfuric acid with the density of 1.84g/mL is slowly added into 300mL of water, and a plurality of drops of potassium permanganate solution with the concentration of 0.01mo1/L are added when the solution is hot until the solution is pink, thus obtaining the product.
Further, when the sample is obtained after diluting the original sample, the calculation result in step S5 is calculated according to the following formula (2):
V0represents the volume of potassium permanganate solution consumed in the step S3 blank test; v3Represents the volume of the sample taken during the measurement steps S1 and S2; f represents the proportion of distilled water in the volume for measuring 100mL when the sample is diluted; v1Represents the volume of potassium permanganate solution consumed during the sample titration in step S2; v2Represents the volume of potassium permanganate solution consumed during the calibration in step S4; c represents the concentration of sodium oxalate standard solution (4.6).
Compared with the prior art, the invention has the beneficial effects that: the method is suitable for measuring drinking water, source water and ground water in high-altitude areas of Tibet, the measuring range is 0.5-4.5 mg/L, and the water quality with serious pollution can still be measured after dilution.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail below with reference to examples, and the exemplary embodiments and descriptions thereof are only used for explaining the present invention and are not used as limitations of the present invention.
Example (b):
unless otherwise stated, the reagents used in this example were analytically pure reagents meeting national or professional standards and distilled water or water of equivalent purity, and deionized water was not used.
The preparation of the reagents concerned (plateau area nonstandard method) is as follows:
(1) the preparation method of the water without reducing substances comprises the following steps: placing 1L of distilled water in an all-glass distiller, adding 10mL of sulfuric acid (sulfuric acid in (3) below) and a small amount of potassium permanganate solution (4.6.1), distilling, discarding 100mL of primary distillate, and storing the rest distillate in a narrow-mouth bottle with a glass plug;
(2) sulfuric acid (H)2SO4): the density is 1.84 g/mL;
(3) sulfuric acid, 1+3 solution: with continuous stirring, 100mL of (2) sulfuric acid was slowly added to 300mL of water, and a few drops of potassium permanganate solution (0.01mo1/L) were added while hot until the solution appeared pink;
(4) sodium hydroxide, 500g/L solution: weighing 50g of sodium hydroxide, dissolving in water and diluting to 100 mL;
(5) sodium oxalate stock solution, concentration C (1/2 Na)2C2O4) 0.1mo 1/L: 0.6705g of sodium oxalate (Na) which is dried for 2 hours at 120 ℃ and cooled are weighed2C2O4) Dissolving in water, transferring into a 100mL volumetric flask, diluting with water to marked line, mixing, and storing at 4 ℃;
(6) sodium oxalate standard solution, concentration C1(1/2 Na)2C2O4) 0.01mo 1/L: sucking 10.00mL of the sodium oxalate stock solution into a 100mL volumetric flask, diluting the sodium oxalate stock solution with water to a marked line, and uniformly mixing;
(7) standard stock solution of potassium permanganate, concentration C2(1/2 KMnO)4) About 0.1mo 1/L: weighing 3.2g of potassium permanganate, dissolving in water, diluting to 1000mL, heating the solution in a water bath at 90-95 ℃ for two hours, and cooling; after two days of storage, the clear liquid is poured out and stored in a brown bottle;
(8) standard solution of potassium permanganate, concentration C3(1/2KMnO4) About 0.01mo 1/L: 100mL of the above potassium permanganate standard stock solution is taken in a 1000mL volumetric flask, diluted with water to the marked line and mixed well, the solution can be stored for several months in the dark, and the concentration is calibrated on the day of use.
Commonly used laboratory instruments and the following: a water bath or equivalent heating device (of sufficient volume and power); acid burette, 25 mL. Note: new glassware must be cleaned with an acidic potassium permanganate solution.
And (3) sample preservation: and (3) adding sulfuric acid in the step (3) after sampling to ensure that the pH of the sample is 1-2 and the sample is analyzed as soon as possible. If the preservation time exceeds 6 hours, the product needs to be placed in a dark place and preserved at 0-5 ℃, and the preservation time cannot exceed 2 days.
The embodiment provides a method for measuring the permanganate index in water, which comprises the following steps:
s1: sucking 100mL of a sample which is fully shaken and uniformly mixed (or taking a proper amount of the sample, diluting the sample with water to 100mL), putting the sample into a 250mL conical flask, adding 4.5-5.5 mL of sulfuric acid solution, adding 10mL of potassium permanganate solution with the concentration of 0.01mo1/L into a burette, shaking uniformly, and putting the conical flask into a boiling water bath for 40-107 min (the water bath boils, timing is started, and the time of the boiling water bath of the sample is 45min for Lasa, south China and Linzhi, 55min for Nick, 40min for Changdu, 81min for Ali and 107min for Naqu); the sulfuric acid solution in this step is configured as follows: under the condition of continuous stirring, slowly adding 100mL of sulfuric acid with the density of 1.84g/mL into 300mL of water, and adding a plurality of drops of potassium permanganate solution with the concentration of 0.01mo1/L until the solution is pink, thus obtaining the product;
s2: titration of samples
Adding 10mL of sodium oxalate solution with the concentration of 0.01mo1/L into the erlenmeyer flask treated in the step S1 by using a clean tube until the solution becomes colorless, titrating the solution with potassium permanganate solution with the concentration of 0.01mo1/L until the solution in the erlenmeyer flask just appears pink when the solution is hot and the pink color is kept for 30S, and recording the volume of the potassium permanganate solution consumed at the moment;
s3: blank test
Replacing the sample in step S1 with 100mL of water containing no reducing substance, measured according to the procedures of step S1 and step S2, and recording the volume of the final back-dropped potassium permanganate solution;
s4: calibration
Adding 10mL of 0.01mo1/L sodium oxalate solution into the solution titrated in the step S3, continuously titrating the solution by using 0.01mo1/L potassium permanganate solution at the temperature of 80 ℃ until the solution just appears pink, and keeping the pink color for 30S, and recording the volume of the potassium permanganate solution consumed at the moment;
note: the water level of the boiling water bath is higher than the liquid level in the conical flask; secondly, the sample amount is 1/2-1/3 of the amount of the potassium permanganate standard solution which is remained after heating oxidation, if the solution red is removed during heating, the potassium permanganate is not enough, the sample is taken again, and the sample is diluted and then measured; ③ when the temperature is lower than 60 ℃ during titration, the reaction speed is slow, therefore, the temperature is about 80 ℃; fourthly, the bath temperature of boiling water is 98 ℃, and when data are reported in a plateau area, the boiling point of water needs to be injected;
s5: calculation of results
Permanganate index IMnExpressed as milligrams oxygen consumed per liter of sample (O)2mg/L) as calculated by the following formula (1):
V1represents the volume (mL) of potassium permanganate solution consumed upon sample titration in step S2; v2Represents the volume (mL) of potassium permanganate solution consumed in the calibration of step S4; c represents the concentration of the sodium oxalate standard solution (0.01mo 1/L).
The concentration range of the sample measured in this embodiment is 0.5-4.5 mg/L, and for the sample with serious contamination concentration exceeding the detection range, the sample can be diluted to 100mL, and when the sample is obtained after dilution of the original sample, the result in step S5 is calculated according to the following formula (2):
V0represents the volume (mL) of potassium permanganate solution consumed in the step S3 blank test; v3Represents the volume (mL) of the sample taken at the time of the measurement in steps S1 and S2; f represents the proportion of distilled water in the volume of 100mL of the sample to be measured when the sample is diluted (for example, when 10mL of the sample is diluted to 100mL with water
)；V1Represents the volume of potassium permanganate solution consumed during the sample titration in step S2; v2Represents the volume of potassium permanganate solution consumed during the calibration in step S4; c represents the concentration of the sodium oxalate standard solution (0.01mo 1/L).
When the concentration of chloride ions in the sample is higher than 300mg/L, oxidizing some organic matters and inorganic reducing substances in the sample by potassium permanganate in an alkaline medium, and analyzing the steps as follows: a sample (100 mL) was aspirated (or an appropriate amount thereof was diluted with water to 100mL), the sample was placed in a 250mL Erlenmeyer flask, 0.5mL of the above sodium hydroxide solution was added thereto, the mixture was shaken, 10mL of a potassium permanganate solution was added via a burette, the Erlenmeyer flask was placed in a boiling water bath for 45. + -. 2min (water bath boiling, start timing), the mixture was taken out, 10. + -. 0.5mL of the sulfuric acid solution of the above (3) was added thereto, the shaking was carried out, the following procedure was the same as the above step S2, and the expression of the analysis result was the same as the above calculation.
The above is an embodiment of the present invention. The embodiments and specific parameters in the embodiments are only for the purpose of clearly illustrating the process of verifying the invention and are not intended to limit the scope of the invention, which is defined by the claims, and all the equivalent structural changes made by applying the content of the specification of the invention should be covered by the scope of the invention.
Claims (3)
1. A method for measuring the permanganate index in water is characterized by comprising the following steps:
s1: sucking 100mL of sample which is fully shaken and uniformly mixed, placing the sample in a 250mL conical flask, adding 4.5-5.5 mL of sulfuric acid solution, adding 10mL of potassium permanganate solution with the concentration of 0.01mo1/L by using a burette, placing the conical flask in a boiling water bath for 40-107 min after shaking uniformly, wherein the time of the sample boiling water bath is respectively as follows: lasa, Shannan, Linzhi 45min, Rike 55min, Changdu 40min, Ali 81min, and Naqu 107 min;
s2: titration of samples
Adding 10mL of sodium oxalate solution with the concentration of 0.01mo1/L into the erlenmeyer flask treated in the step S1 by using a clean tube until the solution becomes colorless, titrating the solution with potassium permanganate solution with the concentration of 0.01mo1/L until the solution in the erlenmeyer flask just appears pink when the solution is hot and the pink color is kept for 30S, and recording the volume of the potassium permanganate solution consumed at the moment;
s3: blank test
Replacing the sample in step S1 with 100mL of water containing no reducing substance, measured according to the procedures of step S1 and step S2, and recording the volume of the final back-dropped potassium permanganate solution;
s4: calibration
Adding 10mL of 0.01mo1/L sodium oxalate solution into the solution titrated in the step S3, continuously titrating the solution by using 0.01mo1/L potassium permanganate solution at the temperature of 80 ℃ until the solution just appears pink, and keeping the pink color for 30S, and recording the volume of the potassium permanganate solution consumed at the moment;
s5: calculation of results
Permanganate index IMnExpressed as milligrams oxygen consumed per liter of sample (O)2mg/L) as calculated by the following formula (1):
V1represents the volume of potassium permanganate solution consumed during the sample titration in step S2; v2Represents the volume of potassium permanganate solution consumed during the calibration in step S4; c represents the concentration of the sodium oxalate standard solution.
2. The method for determining the permanganate index in water according to claim 1, wherein the sulfuric acid solution in step S1 is configured as follows: under the condition of continuous stirring, 100mL of sulfuric acid with the density of 1.84g/mL is slowly added into 300mL of water, and a plurality of drops of potassium permanganate solution with the concentration of 0.01mo1/L are added when the solution is hot until the solution is pink, thus obtaining the product.
3. The method according to claim 1, wherein the result of step S5 is calculated according to the following formula (2) when the sample is diluted from the original sample:
V0represents the volume of potassium permanganate solution consumed in the step S3 blank test; v3Represents the volume of the sample taken during the measurement steps S1 and S2; f represents the proportion of distilled water in the volume for measuring 100mL when the sample is diluted; v1Represents the volume of potassium permanganate solution consumed during the sample titration in step S2; v2Represents the volume of potassium permanganate solution consumed during the calibration in step S4; c represents the concentration of the sodium oxalate standard solution.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105372385A (en) * | 2015-12-15 | 2016-03-02 | 广西大学 | Method for rapidly measuring permanganate index in water |
| CN109270192A (en) * | 2018-12-02 | 2019-01-25 | 太湖流域水文水资源监测中心（太湖流域水环境监测中心） | Pretreating device, method and purposes for the detection of aquatic products sulfa antibiotics |
| CN110133178A (en) * | 2019-06-14 | 2019-08-16 | 上海安杰环保科技股份有限公司 | The permanganate index analyzer for having environment adaption function |
| CN111489080A (en) * | 2020-04-10 | 2020-08-04 | 中国科学院南京地理与湖泊研究所 | Method for representing reducing substance quantity of lake and reservoir water body by CDOM absorption |
| CN112179899A (en) * | 2020-10-09 | 2021-01-05 | 蒙自海关综合技术中心 | Method for detecting total iron content in iron ore |
-
2021
- 2021-04-26 CN CN202110452725.4A patent/CN113311102A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105372385A (en) * | 2015-12-15 | 2016-03-02 | 广西大学 | Method for rapidly measuring permanganate index in water |
| CN109270192A (en) * | 2018-12-02 | 2019-01-25 | 太湖流域水文水资源监测中心（太湖流域水环境监测中心） | Pretreating device, method and purposes for the detection of aquatic products sulfa antibiotics |
| CN110133178A (en) * | 2019-06-14 | 2019-08-16 | 上海安杰环保科技股份有限公司 | The permanganate index analyzer for having environment adaption function |
| CN111489080A (en) * | 2020-04-10 | 2020-08-04 | 中国科学院南京地理与湖泊研究所 | Method for representing reducing substance quantity of lake and reservoir water body by CDOM absorption |
| CN112179899A (en) * | 2020-10-09 | 2021-01-05 | 蒙自海关综合技术中心 | Method for detecting total iron content in iron ore |
Non-Patent Citations (6)
| Title |
|---|
| 吴凤芝等: "西藏地区高锰酸盐指数测定方法探讨", 《西藏科技》 * |
| 吴振德，李大虎: "《环境监测技术方法概论——环境监测基础知识》", 30 September 2008 * |
| 国家环保总局: "《GB11892-1989 水质高锰酸盐指数的测定》", 31 December 1989 * |
| 张金艳: "酸性法测定高锰酸盐指数原理解析", 《环境科学导刊》 * |
| 李红科等: "不同处理方式对高原地表水中高锰酸盐指数测定结果的影响", 《西藏科技》 * |
| 陈周杰等: "浅谈高海拔地区(西宁)水浴锅加热温度和时间对测定高锰酸盐指数的影响", 《青海环境》 * |
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