阅读说明：本技术 一种工业煤气中硫化物的检测方法 (Method for detecting sulfide in industrial gas ) 是由 夏云山 朱宏亮 于 2019-10-16 设计创作，主要内容包括：本发明公开了一种工业煤气中硫化物的检测方法,属于气体杂质检测技术领域,包括以下步骤：首先先用微量进样器抽取工业煤气中的样气并排空,如此重复2～3次后,抽取含有硫化物的100.0～200ml待检气体,再使用自动进样器等速进样；在此过程中利用高纯氮气作为载气,携带含有硫化物的待检气体,在一定色谱条件下通过装有固定相的色谱柱经色谱柱分离后,由火焰光度检测器测定,通过计算机记录火焰光度检测器得到的相应气相色谱,以色谱峰的保留时间进行定性分析,以色谱峰的面积进行定量分析。可以准确地检测出工业煤气中的硫化物的成分和含量,从而可通过不断地监测和改进,实现节能减排的目的。(The invention discloses a method for detecting sulfides in industrial gas, which belongs to the technical field of gas impurity detection and comprises the following steps: firstly, extracting sample gas in industrial coal gas by using a microsyringe and emptying, repeating the operation for 2-3 times, extracting 100.0-200 ml of sulfide-containing gas to be detected, and then carrying out constant-speed sample injection by using an automatic sampler; in the process, high-purity nitrogen is used as carrier gas, gas to be detected containing sulfide is carried, the gas is separated by a chromatographic column filled with a stationary phase under a certain chromatographic condition, the gas is measured by a flame photometric detector, a computer records corresponding gas chromatogram obtained by the flame photometric detector, qualitative analysis is carried out according to retention time of a chromatographic peak, and quantitative analysis is carried out according to the area of the chromatographic peak. The method can accurately detect the components and the content of the sulfide in the industrial gas, thereby realizing the purposes of energy conservation and emission reduction through continuous monitoring and improvement.)

1. The method for detecting the sulfide in the industrial gas is characterized by comprising the following steps of: firstly, extracting sample gas in industrial coal gas by using a microsyringe and emptying, repeating the operation for 2-3 times, extracting 100.0-200 ml of sulfide-containing gas to be detected, and then carrying out constant-speed sample injection by using an automatic sampler; in the process, high-purity nitrogen is used as carrier gas, gas to be detected containing sulfide is carried, the gas is separated by a chromatographic column filled with a stationary phase under a certain chromatographic condition, the gas is measured by a flame photometric detector, a computer records corresponding gas chromatogram obtained by the flame photometric detector, qualitative analysis is carried out according to retention time of a chromatographic peak, and quantitative analysis is carried out according to the area of the chromatographic peak.

2. The method for detecting sulfides in industrial gas according to claim 1, wherein the gas to be detected has an inlet flow rate of 0.3 to 0.5L/min.

3. The method for detecting sulfides in industrial gas according to claim 2, wherein the inlet flow rate of the high-purity nitrogen is 5 to 10L/min.

4. The method for detecting sulfides in industrial gas as claimed in claim 3, wherein the high-purity nitrogen and the gas to be detected are subjected to heat tracing in the sample introduction process, and the heat tracing temperature is 120-130 ℃.

5. The method for detecting sulfides in industrial gas according to claim 4, wherein the chromatographic column is located in a closed column box, a temperature control device and a temperature alarm device are arranged in the column box, the temperature control device controls the temperature in the column box to be kept at 120-130 ℃, and the temperature alarm device alarms when the temperature exceeds the range.

6. The method for detecting sulfides in industrial gas according to claim 5, wherein a humidity detector and a humidity alarm device are further arranged in the column box, the humidity detector detects that the humidity in the column box is 2-25% RH, and the humidity alarm device alarms when the humidity exceeds the range.

7. The method for detecting sulfides in industrial gas according to claim 1, wherein the gas to be detected and the high-purity nitrogen gas are filtered by a purifier during the sample injection process to remove solid particles in the gas to be detected and the high-purity nitrogen gas.

8. The method for detecting sulfides in industrial gas as claimed in claim 1, wherein the flame photometric detector detects by hydrogen combustion and uses air to support combustion, wherein the concentration of hydrogen in the combustion gas is 99.99%, and the concentration of air in the combustion-supporting gas is 99.9%.

Technical Field

The invention belongs to the field of detection methods of gas impurities, and particularly relates to a method for detecting sulfides in industrial gas.

Background

With the rapid development of Chinese economy, the environmental problems are increasingly prominent, and even the sustainable development of the economic society is restricted. With the increasing national exhaust emission standards of iron and steel enterprises, the emission of harmful gases in industrial gas after combustion is more and more concerned by various fields. The content of sulfide in the coal gas can be detected only by a pollution source environment monitoring method. The method is characterized in that a condition test is carried out by analyzing the content components of the industrial gas, comparing the detection results, eliminating interference components, optimizing the detection method and other measures, and finally the suitable detection method for the sulfide in the industrial gas is determined.

Disclosure of Invention

In view of this, the present application mainly provides a method for detecting sulfides in industrial gas, which can accurately detect the components and contents of sulfides in industrial gas, and provide a guidance for subsequent monitoring and improvement.

In order to achieve the purpose, the invention provides the following technical scheme:

the invention relates to a method for detecting sulfides in industrial gas, which comprises the following steps: firstly, extracting sample gas in industrial coal gas by using a microsyringe and emptying, repeating the operation for 2-3 times, extracting 100.0-200 ml of sulfide-containing gas to be detected, and then carrying out constant-speed sample injection by using an automatic sampler; in the process, high-purity nitrogen is used as carrier gas, gas to be detected containing sulfide is carried, the gas is separated by a chromatographic column filled with a stationary phase under a certain chromatographic condition, the gas is measured by a flame photometric detector, a computer records corresponding gas chromatogram obtained by the flame photometric detector, qualitative analysis is carried out according to retention time of a chromatographic peak, and quantitative analysis is carried out according to the area of the chromatographic peak.

Further, the gas inlet flow of the gas to be detected is 0.3-0.5L/min.

Further, the air inlet flow of the high-purity nitrogen is 5-10L/min.

Further, carrying out heat tracing on the high-purity nitrogen and the gas to be detected in the sample introduction process, wherein the heat tracing temperature is 120-130 ℃.

Further, the chromatographic column is positioned in a closed column box, a temperature control device and a temperature alarm device are arranged in the column box, the temperature control device controls the temperature in the column box to be kept at 120-130 ℃, and the temperature alarm device alarms when the temperature exceeds the range.

Further, a humidity detector and a humidity alarm device are further arranged in the column box, the humidity in the column box detected by the humidity detector is 2% -25% RH, and when the humidity exceeds the range, the humidity alarm device gives an alarm.

Further, the gas to be detected and the high-purity nitrogen gas are filtered by a purifier in the sample injection process, so that solid particles in the gas to be detected and the high-purity nitrogen gas are filtered.

Further, the flame photometric detector is used for detecting through hydrogen combustion and supporting combustion by air, wherein the concentration of hydrogen in combustion gas is 99.99%, and the concentration of air in combustion-supporting gas is 99.9%.

The invention has the beneficial effects that:

the invention relates to a method for detecting sulfides in industrial gas, which utilizes high-purity nitrogen as carrier gas to provide a carrier for gas to be detected, participates in the distribution process of a stationary phase and provides a driving force for the gas to be detected, so that the gas to be detected can be successfully detected. The invention carries the gas to be detected containing sulfide by high-purity nitrogen, after the gas is separated by a chromatographic column filled with a fixed phase under certain chromatographic conditions, the gas is measured by a flame photometric detector, a computer records the corresponding gas chromatogram obtained by the flame photometric detector, qualitative analysis is carried out by the retention time of a chromatographic peak, and quantitative analysis is carried out by the area of the chromatographic peak, thereby achieving the purpose of one-time detection and having higher detection efficiency and precision.

Drawings

For the purposes of promoting a better understanding of the objects, aspects and advantages of the invention, reference will now be made to the following detailed description taken in conjunction with the accompanying drawings in which:

FIG. 1 is a schematic diagram of the present invention.

Detailed Description

The embodiments of the present invention are described below with reference to specific embodiments, and other advantages and effects of the present invention will be easily understood by those skilled in the art from the disclosure of the present specification. The invention is capable of other and different embodiments and of being practiced or of being carried out in various ways, and its several details are capable of modification in various respects, all without departing from the spirit and scope of the present invention. It should be noted that the drawings provided in the following embodiments are only for illustrating the basic idea of the present invention in a schematic way, and the features in the following embodiments and examples may be combined with each other without conflict.

Wherein the showings are for the purpose of illustrating the invention only and not for the purpose of limiting the same, and in which there is shown by way of illustration only and not in the drawings in which there is no intention to limit the invention thereto; to better illustrate the embodiments of the present invention, some parts of the drawings may be omitted, enlarged or reduced, and do not represent the size of an actual product; it will be understood by those skilled in the art that certain well-known structures in the drawings and descriptions thereof may be omitted.

The same or similar reference numerals in the drawings of the embodiments of the present invention correspond to the same or similar components; in the description of the present invention, it should be understood that if there is an orientation or positional relationship indicated by terms such as "upper", "lower", "left", "right", "front", "rear", etc., based on the orientation or positional relationship shown in the drawings, it is only for convenience of description and simplification of description, but it is not an indication or suggestion that the referred device or element must have a specific orientation, be constructed in a specific orientation, and be operated, and therefore, the terms describing the positional relationship in the drawings are only used for illustrative purposes, and are not to be construed as limiting the present invention, and the specific meaning of the terms may be understood by those skilled in the art according to specific situations.

FIG. 1 is a schematic diagram of a method for detecting sulfides in industrial gas, comprising the following steps: firstly, extracting and emptying sample gas in industrial coal gas by using a micro-sampler, repeating the operation for 2-3 times, completely draining the original impure gas in the sampler, then extracting 100.0-200 ml of gas to be detected containing sulfide, and then carrying out constant-speed sampling by using an automatic sampler; in the process, high-purity nitrogen is used as carrier gas, gas to be detected containing sulfide is carried, the gas is separated by a chromatographic column filled with a stationary phase under a certain chromatographic condition, the gas is measured by a flame photometric detector, a computer records corresponding gas chromatogram obtained by the flame photometric detector, qualitative analysis is carried out according to retention time of a chromatographic peak, and quantitative analysis is carried out according to the area of the chromatographic peak. The invention uses high-purity nitrogen as carrier gas to provide carrier for gas to be detected, and the carrier participates in the distribution process of stationary phase, and provides driving force for the gas to be detected, so that the gas to be detected can be detected smoothly. The invention carries the gas to be detected containing sulfide by high-purity nitrogen, after the gas is separated by a chromatographic column filled with a fixed phase under a certain chromatographic condition, the gas is measured by a flame photometric detector, a computer records the corresponding gas chromatogram obtained by the flame photometric detector, qualitative analysis is carried out by the retention time of a chromatographic peak, and quantitative analysis is carried out by the area of the chromatographic peak, thus achieving the purpose of simultaneously detecting the type and the content of the gas at one time, and having higher detection efficiency and precision.

In the present embodiment, the flame photometric detector is a detector which is used in a gas chromatograph and has high selectivity and high sensitivity to phosphorus-containing and sulfur-containing compounds. When the sample is burnt in a hydrogen-rich flame, the phosphorus-containing organic compound mainly emits light with the wavelength of 526nm in the form of HPO fragments, and the sulfur-containing compound emits characteristic light with the wavelength of 394nm in the form of S2 molecules. The photomultiplier converts the optical signal into an electrical signal, and the electrical signal is amplified and recorded by a micro-current. The sensitivity of such detectors can reach tens to hundreds of coulombs per gram, and the detection limit of flame photometric detectors can reach 10-12g/S (for P) or 10-11g/S (for S). Meanwhile, the ratio of the response value of the detector to organophosphorus and organosulfur to the response value of hydrocarbon can reach 104, so that a large number of solvent peaks and interference of hydrocarbons can be eliminated, the detector is very beneficial to analysis of trace phosphorus and sulfur, and is a main tool for detecting sulfur-containing pollutants.

In the embodiment, the gas inflow rate of the gas to be detected is 0.3-0.5L/min, preferably 0.5L/min. The gas inflow rate of the high-purity nitrogen is 5-10L/min, preferably 10L/min, and the high-purity nitrogen is adapted by adopting the proper gas inflow rate, so that the detection stability can be improved, the interference of impurity gas is reduced, and the detection precision can be submitted.

In the embodiment, high-purity nitrogen and gas to be detected are subjected to heat tracing in the sample introduction process, the heat tracing temperature is 120-130 ℃, the chromatographic column is located in a closed column box, a temperature control device and a temperature alarm device are arranged in the column box, the temperature control device controls the temperature in the column box to be kept at 120-130 ℃, and the temperature alarm device gives an alarm when the temperature exceeds the range. Because hydrogen sulfide is a gas which is easily soluble in water and has reducibility, the hydrogen sulfide is unstable and is easily decomposed by heating; sulfur dioxide is a stable, readily water-soluble, oxidizing gas. Under appropriate conditions, redox chemical reaction occurs, however, sulfur is liquefied at 119 ℃, so that the whole device including transportation and chromatographic separation processes is carried out at a temperature of 119 ℃ to reduce interference caused by the reaction.

In this embodiment, still be provided with moisture detector and humidity alarm device in the post case, moisture detector detects the interior humidity of post case and is 2% ~ 25% RH, surpasss this scope, and humidity alarm device reports to the police, through controlling suitable humidity, reduces the influence of water in the air to components and parts in the post case.

In this embodiment, examine gas and high-purity nitrogen gas and advance kind in-process and pass through the clarifier filtration earlier, the solid particle in the gas and the high-purity nitrogen gas are examined in the filtering, reduce the influence of solid casing to follow-up separation and combustion process.

In the embodiment, the flame photometric detector is used for detecting through hydrogen combustion and supporting combustion by air, wherein the concentration of hydrogen in combustion gas is 99.99%, the influence of other impurity gases on the detection result during combustion is reduced, and the concentration of air in combustion-supporting gas is 99.9%.

Finally, the above embodiments are only intended to illustrate the technical solutions of the present invention and not to limit the present invention, and although the present invention has been described in detail with reference to the preferred embodiments, it will be understood by those skilled in the art that modifications or equivalent substitutions may be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions, and all of them should be covered by the claims of the present invention.