CN110927003A - Method for detecting total sulfur in water - Google Patents

Method for detecting total sulfur in water Download PDF

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CN110927003A
CN110927003A CN201911112332.8A CN201911112332A CN110927003A CN 110927003 A CN110927003 A CN 110927003A CN 201911112332 A CN201911112332 A CN 201911112332A CN 110927003 A CN110927003 A CN 110927003A
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water
total sulfur
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coal
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崔海松
张同新
赵君君
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XUZHOU WEITIAN CHEMCIAL CO Ltd
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    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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    • G01N5/04Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid by removing a component, e.g. by evaporation, and weighing the remainder

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Abstract

A method for detecting total sulfur in water comprises the following steps: firstly, two parts of coal samples of intermediate medium with equal weight and constant total sulfur are selected, and the weight of the coal samples of intermediate medium is GMediumOne part of the sulfur content is measured by accurately measuring the medium dry base total sulfur S directly by GB/T214-2007 method for measuring total sulfur in coalMediumMixing the other coal sample with a water sample to be detected to obtain a water coal sample with the weight of GWater (W)The weight ratio of the coal sample to the water sample is 10: (3-5) placing the water-coal sample in a forced air drying oven with the internal temperature of 105-110 ℃, drying the water-coal sample in air flow until the quality is constant, and accurately measuring the total sulfur S of the water-coal sample drying base by adopting GB/T214-2007 method for measuring the total sulfur in coalMixing ofFinally, calculating to obtain the total sulfur content S in the water sampleWater (W)(ii) a Calculating the total sulfur content SWater (W)The formula of (a): sWater (W)=(GMedium*SMixing of‑GMedium*SMedium)/GWater (W). The detection method can accurately and reliably detect the total sulfur content in the water.

Description

Method for detecting total sulfur in water
Technical Field
The invention belongs to the technical field of detection of sulfur in environment, and particularly relates to a method for detecting total sulfur in water.
Background
Total sulfur is a generic term for organic, inorganic, and elemental sulfur. In industrial production, sulfur has more or less influence on enterprises, so that the sulfur content in water and waste water for enterprises is widely concerned. The sulfur in the water body exists in the form of sulfur compounds, the sulfur compounds have strong chemical action on a plurality of metal ions in metabolism in organisms, for example, sulfide in the sulfur compounds has strong corrosion action on plant rhizomes, and even the concentration of the sulfide in the drinking water is as low as 0.07 mu g/L, the sulfur compounds can influence the taste of the water. When the concentration of sulfide in the water body reaches 0.15 mu g/L, the growth of newly released fry and the survival of roe are influenced. The sulfide in water is easy to escape into the air to generate odor, has high toxicity, and can react with human cytochrome, oxidase and disulfide bonds in the substances to influence the oxidation process of cells, so that the oxygen deficiency of cell tissues is caused, and the life of a human is endangered. The sulfide in water can release hydrogen sulfide, and the hydrogen sulfide can corrode metal and can be oxidized into sulfuric acid by microorganisms in sewage to corrode a sewer and the like. Other forms of sulfur compounds are also important hazardous substances for water pollution and water ecosystems.
At present, most of the existing detection technologies aim at measuring compounds of a certain class of sulfur, but an accurate and reliable detection method for total sulfur in water is lacked.
Disclosure of Invention
The invention aims to provide a method for detecting total sulfur in water, which can accurately and reliably detect the total sulfur content in water.
In order to achieve the aim, the invention provides a method for detecting total sulfur in water, which comprises the following steps:
firstly, two parts of coal samples of intermediate medium with equal weight and constant total sulfur are selected, and the weight of the coal samples of intermediate medium is GMediumOne part of the sulfur content is measured by accurately measuring the medium dry base total sulfur S directly by GB/T214-2007 method for measuring total sulfur in coalMediumMixing the other coal sample with a water sample to be detected to obtain a water coal sample with the weight of GWater (W)The weight ratio of the coal sample to the water sample is 10: (3-5) placing the water-coal sample in an air-blast drying box with the internal temperature of 105-110 ℃, drying the water-coal sample in air flow until the quality is constant, and then accurately measuring the total sulfur S of the dry basis of the water-coal sample by adopting GB/T214-2007 method for measuring the total sulfur in coalMixing ofFinally, calculating the total sulfur content S in the water sample by a material balance methodWater (W)(ii) a Calculating the total sulfur content SWater (W)The formula of (a): sWater (W)=(GMedium*SMixing of-GMedium*SMedium)/GWater (W)
Further, adding a certain amount of hydrogen peroxide when the other coal sample is mixed with a water sample to be detected, wherein the mass ratio of the hydrogen peroxide to the water sample is 1: 2.
preferably, the hydrogen peroxide is industrial hydrogen peroxide meeting the national standard GB/T1616-.
Preferably, the weight ratio of the coal sample to the water sample is 10: 4.
preferably, the water coal sample is dried in a forced air drying oven with an internal temperature of 108 ℃.
The invention discloses a method for determining total sulfur in water, which is simple and feasible to operate and reliable in resultMixing ofWith medium-drying base of total sulfur SMediumAccurately obtaining the total sulfur content S in the water sample by the differenceWater (W)The measurement result is accurate, the operation is simple and convenient, and the measurement result meets the precision requirement; in addition, the method has no requirement on a water sample, and can be widely applied to water sample detection in the environment.
Detailed Description
The present invention will be described in further detail with reference to examples.
Example one
A method for detecting total sulfur in water comprises the following steps:
firstly, two parts of coal samples of intermediate medium with equal weight and constant total sulfur are selected, and the weight of the coal samples of intermediate medium is GMedium100g, one part of the sulfur is directly and accurately measured according to GB/T214-2007 method for measuring total sulfur in coalMedium0.32%, mixing another coal sample with the water sample to be detected to obtain water coal sample, and preventing S2-The hydrolysis volatilization prevents the loss of sulfur dioxide and other gas sulfides in the drying process, and adds a certain amount of hydrogen peroxide into the water sample, wherein the mass ratio of the hydrogen peroxide to the water sample is 1: 2, the hydrogen peroxide is industrial hydrogen peroxide meeting the national standard GB/T1616-Water (W)30g, the weight ratio of the coal sample to the water sample is 10: 3, placing the water coal sample in a blast drying oven with the internal temperature of 105 ℃,drying in air flow until the mass is constant, and accurately measuring the total sulfur S of the dry base of the water coal sample according to GB/T214-2007 method for measuring the total sulfur in coalMixing of0.36 percent, and finally calculating the total sulfur content S in the water sample by a material balance methodWater (W)=0.133%。
Example two
A method for detecting total sulfur in water comprises the following steps:
firstly, two parts of coal samples of intermediate medium with equal weight and constant total sulfur are selected, and the weight of the coal samples of intermediate medium is GMedium100g, one part of the sulfur is directly and accurately measured according to GB/T214-2007 method for measuring total sulfur in coalMedium0.32%, mixing another coal sample with the water sample to be detected to obtain water coal sample, and preventing S2-The hydrolysis volatilization prevents the loss of sulfur dioxide and other gas sulfides in the drying process, and adds a certain amount of hydrogen peroxide into the water sample, wherein the mass ratio of the hydrogen peroxide to the water sample is 1: 2, the hydrogen peroxide is industrial hydrogen peroxide meeting the national standard GB/T1616-Water (W)The weight ratio of the coal sample to the water sample is 10: 4, placing the water coal sample in a blast drying oven with the internal temperature of 108 ℃, drying the water coal sample in air flow until the quality is constant, and then accurately measuring the total sulfur S of the dry base of the water coal sample by using GB/T214-2007 method for measuring the total sulfur in coalMixing of0.372%, and finally calculating the total sulfur content S in the water sample by a material balance methodWater (W)=0.130%。
EXAMPLE III
A method for detecting total sulfur in water comprises the following steps:
firstly, two parts of coal samples of intermediate medium with equal weight and constant total sulfur are selected, and the weight of the coal samples of intermediate medium is GMedium100g, one part of the sulfur is directly used for accurately measuring the medium dry base total sulfur S according to GB/T214-2007 determination method of total sulfur in coalMedium0.32%, mixing another coal sample with the water sample to be detected to obtain water coal sample, and preventing S2-Hydrolyzing and volatilizing to prevent loss of sulfur dioxide and other gas sulfide during drying, and adding certain amount of hydrogen peroxide and peroxyThe mass ratio of the hydrogen hydride to the water sample is 1: 2, the hydrogen peroxide is industrial hydrogen peroxide meeting the national standard GB/T1616-Water (W)The weight ratio of the coal sample to the water sample is 50 g: 5, placing the water coal sample in an air-blast drying oven with the internal temperature of 110 ℃, drying the water coal sample in air flow until the quality is constant, and then accurately measuring the total sulfur S of the dry basis of the water coal sample according to GB/T214-2007 method for measuring the total sulfur in coalMixing of0.385 percent, and finally calculating the total sulfur content S in the water sample by a material balance methodWater (W)=0.130%。
Accuracy and reliability verification
GB/T214-2007 determination method of total sulfur in coal is adopted to accurately measure medium dry base total sulfur SMediumThe concentration of the standard water sample is 0.32%, four groups of standard water samples of total sulfur with different concentration levels are selected as shown in the following table 1, the precision is calculated according to the measurement result by adopting the method, and the detection result is shown in the following table 1.
TABLE 1 detection results and measurement errors of different water samples
Figure BDA0002273083260000031
Figure BDA0002273083260000041
As can be seen from Table 1, the relative standard deviation of the method of the invention is very small, the precision is very good, and the measurement result meets the precision requirement; in addition, the method has no requirement on a water sample, and can be widely applied to water sample detection in the environment.

Claims (5)

1. A method for detecting total sulfur in water is characterized by comprising the following steps:
firstly, two parts of coal samples of intermediate medium with equal weight and constant total sulfur are selected, and the weight of the coal samples of intermediate medium is GMediumOne part of the sulfur content is measured by accurately measuring the medium dry base total sulfur S directly by GB/T214-2007 method for measuring total sulfur in coalMediumMixing another coal sample with the water sample to be detected to obtain a water coal sample and waterSample weight of GWater (W)The weight ratio of the coal sample to the water sample is 10: (3-5) placing the water-coal sample in an air-blast drying box with the internal temperature of 105-110 ℃, drying the water-coal sample in air flow until the quality is constant, and accurately measuring the total sulfur S of the dry basis of the water-coal sample according to GB/T214-2007 method for measuring the total sulfur in coalMixing ofFinally, calculating the total sulfur content S in the water sample by a material balance methodWater (W)(ii) a Calculating the total sulfur content SWater (W)The formula of (a): sWater (W)=(GMedium*SMixing of-GMedium*SMedium)/GWater (W)
2. The method for detecting total sulfur in water according to claim 1, wherein a certain amount of hydrogen peroxide is added when another coal sample is mixed with a water sample to be detected, and the mass ratio of the hydrogen peroxide to the water sample is 1: 2.
3. the method for detecting total sulfur in water as claimed in claim 2, wherein the hydrogen peroxide is industrial hydrogen peroxide meeting national standard GB/T1616-2014.
4. The method for detecting total sulfur in water according to claim 1 or 2, wherein the weight ratio of the coal sample to the water sample is 10: 4.
5. the method for detecting the total sulfur in the water according to claim 1 or 2, wherein the water coal sample is dried in an air-blast drying oven with the internal temperature of 108 ℃.
CN201911112332.8A 2019-11-14 2019-11-14 Method for detecting total sulfur in water Pending CN110927003A (en)

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