WO2011102273A1 - Method and device for detecting hydrogen sulfide - Google Patents

Abstract

Provided is a method for detecting hydrogen sulfide which is simpler than conventional methods. The method for detecting hydrogen sulfide comprises the steps of: introducing a flow gas into a diluent solvent in which a fuel oil containing hydrogen sulfide has been dissolved, while heating the diluent solvent; collecting the flow gas released from the diluent solvent, in a collection vessel; and determining the content of the hydrogen sulfide in the flow gas collected in the collection vessel, by means of a detection tube for hydrogen sulfide.

Description

Method and apparatus for detecting hydrogen sulfide

The present invention relates to a method and an apparatus for detecting hydrogen sulfide.

Fuel oil such as marine fuel contains hydrogen sulfide as an impurity. Hydrogen sulfide in fuel oil causes air pollution and damage deterioration of the internal combustion engine or combustion equipment. Therefore, it is necessary to remove hydrogen sulfide in fuel oil refining. And the technique which detects the hydrogen sulfide contained in fuel oil after the refinement | purification process of fuel oil or after refinement | purification is needed.

Conventionally, as a method for detecting hydrogen sulfide contained in fuel oil, a method standardized as IP 399/94 is known (see Non-Patent Document 1 below). In IP 399/94, nitrogen gas is continuously introduced into deoxygenated xylene while heating deoxygenated xylene in which fuel oil is dissolved. In the nitrogen gas released from the deoxygenated xylene, hydrogen sulfide and the like contained as impurities in the fuel oil are recovered. Nitrogen gas from which hydrogen sulfide has been recovered is introduced into the absorption liquid in the suction bottle. The absorbing solution contains reagents such as an amine test solution, ferric chloride, and ammonium hydrogen phosphate. Hydrogen sulfide in nitrogen gas is extracted into the absorbing solution. Transfer the absorbing solution containing hydrogen sulfide to the flask for absorbance measurement together with deoxygenated water. Then, hydrogen sulfide is quantified by methylene blue absorptiometry.

IP 399/94 measurement takes a long time of about 3 hours. IP 399/94 is a combination of a complex chemical reaction process using about 20 types of reagents and a methylene blue absorptiometry, and requires complicated operations. For this reason, the implementation of IP 399/94 requires a skilled professional to work for a long time. Furthermore, IP 399/94 is dangerous because it uses toxic chemicals such as cadmium hydroxide as a reagent.

In view of the above circumstances, the present inventors have sought a method for detecting hydrogen sulfide in fuel oil that is simpler than IP 399/94 and has the same accuracy as IP 399/94. The inventors have attempted to detect hydrogen sulfide by directly introducing a flow of nitrogen gas continuously released from xylene into the hydrogen sulfide detector tube.

In the detector tube method, it is necessary to measure the total volume of nitrogen gas that has passed through xylene and to control the volume of nitrogen gas introduced into the detector tube to an appropriate amount. However, it is not easy to control and measure the volume of nitrogen gas flowing through the xylene and flowing into the detector tube (flow rate of nitrogen gas). Therefore, when the flow of nitrogen gas is directly introduced into the detector tube, it is difficult to implement the detector tube method.

Also, if the flow rate of nitrogen gas is too small, a sufficient amount of nitrogen gas is not introduced into the detector tube, making it difficult to detect hydrogen sulfide. If the flow of nitrogen gas is too large, the gas pipe that introduces nitrogen gas into the detection pipe will come off the detection pipe. Since it is not easy to easily control the flow rate of nitrogen gas, these problems occur.

The present invention has been made in view of the above problems, and provides a hydrogen sulfide detection device for carrying out a hydrogen sulfide detection method simpler than before and a hydrogen sulfide detection method simpler than before. For the purpose.

In order to achieve the above object, the method for detecting hydrogen sulfide according to the present invention introduces a flow gas into the dilution solvent while heating the dilution solvent in which the fuel oil containing hydrogen sulfide is dissolved, and is released from the dilution solvent. A step of collecting the flow gas in a collector and measuring the content of hydrogen sulfide in the flow gas collected in the collector with a hydrogen sulfide detector tube is provided. That is, in the method for detecting hydrogen sulfide according to the present invention, the content of hydrogen sulfide in the fuel oil is measured by the detector tube method. The flow gas is a gas for expelling a detection target component such as hydrogen sulfide from the fuel oil.

In the present invention, it becomes possible to detect hydrogen sulfide in fuel oil more easily than in the past as described below.

IP 399/94 requires methylene blue absorptiometry. In addition, IP 399/94 requires a complicated chemical reaction process using a large number of reagents for methylene blue absorptiometry. Furthermore, IP 399/94 requires toxic chemicals such as cadmium hydroxide. In addition, in IP 399/94, it is necessary to remove oxygen that interferes with the color development of the absorbing solution from xylene. IP 399/94 also requires a step of recovering nitrogen gas released from the deoxygenated xylene into the absorbing solution.

On the other hand, the present invention does not require methylene blue absorptiometry. The present invention also eliminates the need for complicated chemical reaction processes that use a large number of reagents. Therefore, in the present invention, hydrogen sulfide in fuel oil can be detected more easily and more quickly than IP 399/94. Furthermore, in the present invention, hydrogen sulfide can be detected safely without using cadmium hydroxide. In the present invention, since no spectrophotometric method is used, it is not necessary to remove oxygen from xylene. The present invention is also simple in that the content of hydrogen sulfide in the flow gas can be measured with a detector tube without passing through the step of recovering the flow gas released from the diluting solvent into the absorbing solution.

In the present invention, the flow gas is not directly introduced into the hydrogen sulfide detector tube. In the present invention, the flow gas that has passed through the diluting solvent is collected in a collector. Therefore, in the present invention, the total volume of the flow gas that has passed through the diluting solvent can be measured easily and accurately. In the present invention, since the flow gas collected in the collector is collected in the hydrogen sulfide detector tube, the volume and volume of the flow gas collected in the detector tube can be controlled and measured easily and accurately.

In the method of directly introducing the flow gas into the hydrogen sulfide detector tube without using a collector, complicated operations and devices are required for controlling and measuring the flow rate of the flow gas flowing into the detector tube. However, in the present invention, since a collector is used, complicated operations and devices are not required for controlling and measuring the flow rate of the flow gas.

In the present invention, the fuel oil is at least one selected from the group consisting of sulfur dioxide, mercaptans, gasoline, acetylene, ethylene, ammonia, hydrogen chloride, nitrogen oxides, carbon monoxide, and carbon dioxide in addition to hydrogen sulfide. When impurities are contained, a step of measuring the content of the impurities in the flow gas collected in the collector with a detector tube corresponding to each impurity may be provided. Thus, the content of impurities other than hydrogen sulfide in the fuel oil can be measured.

In the present invention, at least one of the detection tube for sulfurous acid gas or the detection tube for mercaptans is installed between the collector and the detection tube for hydrogen sulfide, and at least of the detection tube for sulfurous acid gas or the detection tube for mercaptans. It is preferable to measure the content of hydrogen sulfide in the flow gas that has passed through either of them with a hydrogen sulfide detector tube.

When the fuel oil contains not only hydrogen sulfide but also sulfite gas and mercaptans, not only hydrogen sulfide but also sulfite gas and mercaptans are recovered in the flow gas. Sulfurous acid gas and mercaptans have chemical properties similar to hydrogen sulfide. Therefore, when a flow gas containing sulfurous acid gas or mercaptans is directly collected in the hydrogen sulfide detector tube, sulfurous acid gas or mercaptans may be erroneously detected as hydrogen sulfide. As a result, the accuracy of measurement of the content of hydrogen sulfide in the flow gas may be reduced. In the present invention, the sulfurous acid gas in the flow gas is adsorbed by the detector tube for sulfurous acid gas, the mercaptans in the flow gas are adsorbed by the detector tube for mercaptans, and then the flow gas is introduced into the detector tube for hydrogen sulfide. Also good. As a result, in the present invention, the detection accuracy of hydrogen sulfide contained in the fuel oil is improved.

The hydrogen sulfide detection apparatus according to the present invention includes a test container for containing a diluted solvent in which fuel oil containing hydrogen sulfide is dissolved, a heater for heating the diluted solvent in the test container, and a flow gas in the diluted solvent in the test container. An introduction tube, a collector for collecting the flow gas in the test vessel, a hydrogen sulfide detector tube for measuring the content of hydrogen sulfide in the flow gas collected in the collector, and a test vessel A gas flow control mechanism that sucks the flow gas inside the collector and supplies the flow gas sucked into the collector to the hydrogen sulfide detection tube.

According to the detection apparatus according to the present invention, the hydrogen sulfide detection method according to the present invention can be easily implemented. That is, in the hydrogen sulfide detection apparatus according to the present invention, it is possible to measure the content of hydrogen sulfide in the fuel oil by the detection tube method.

In the hydrogen sulfide detection apparatus according to the present invention, since the detection tube method is used, hydrogen sulfide in fuel oil can be detected more easily and more quickly than IP 399/94.

The hydrogen sulfide detection device according to the present invention does not require a spectrophotometer necessary for the methylene blue absorptiometry. Further, the detection device according to the present invention does not require a mechanism for performing a complicated chemical reaction process using a large number of reagents. Therefore, the detection apparatus according to the present invention is simpler than the apparatus system for implementing IP 399/94 and can be downsized. Since IP 399/94 requires a spectrophotometer and a complicated chemical reaction process, it is difficult to implement IP 399/94 outdoors. On the other hand, the hydrogen sulfide detection device according to the present invention can be miniaturized and carried. Therefore, by using the hydrogen sulfide detection device according to the present invention, it is possible to easily detect hydrogen sulfide in the fuel oil in the field. Further, since the detection apparatus according to the present invention does not use the absorptiometry, a mechanism for removing oxygen from xylene is not required. In the present invention, since the collector is used, operations and devices for controlling and measuring the flow rate of the flow gas can be simplified as compared with the case where the flow gas is directly introduced into the hydrogen sulfide detector tube.

In the hydrogen sulfide detection device according to the present invention, the fuel oil is a group consisting of sulfur dioxide gas, mercaptans, gasoline, acetylene, ethylene, ammonia, hydrogen chloride, nitrogen oxide, carbon monoxide and carbon dioxide in addition to hydrogen sulfide. In the case of containing at least one impurity selected from the above, a detector tube for measuring the content of each impurity in the flow gas collected in the collector may be provided. That is, the hydrogen sulfide detection device may include a detection tube corresponding to each impurity. Thus, the content of impurities other than hydrogen sulfide in the fuel oil can be measured.

In the hydrogen sulfide detection apparatus according to the present invention, the hydrogen sulfide detector tube is preferably connected to the collector via at least one of a sulfurous acid gas detector tube and a mercaptan detector tube. That is, in the present invention, at least one of the sulfur dioxide gas detection tube and the mercaptans detection tube is installed between the collector and the hydrogen sulfide detection tube, and the sulfurous acid gas detection tube and the mercaptans detection tube. It is preferable to measure the content of hydrogen sulfide in the flow gas that has passed through at least one of the above with a hydrogen sulfide detector tube. This makes it possible to measure the content of hydrogen sulfide in the flow gas after removing sulfurous acid gas and mercaptans from the flow gas.

According to the present invention, it is possible to provide a hydrogen sulfide detection device for carrying out a hydrogen sulfide detection method simpler than before and a hydrogen sulfide detection method simpler than before.

It is a schematic diagram of the detection apparatus for enforcing the detection method of hydrogen sulfide concerning a first embodiment of the present invention. It is a schematic diagram of the detection apparatus for enforcing the detection method of hydrogen sulfide concerning a first embodiment of the present invention. It is a schematic diagram of the hydrogen sulfide detector tube used in the hydrogen sulfide detection method and detection device according to each embodiment of the present invention. It is a schematic diagram of the detection apparatus for enforcing the detection method of hydrogen sulfide concerning a first embodiment of the present invention. It is a schematic diagram of the hydrogen sulfide detection device according to the second embodiment of the present invention. It is a schematic diagram of the hydrogen sulfide detection device according to the third embodiment of the present invention. FIG. 7 is a schematic diagram of a plurality of detector tubes connected in series that can be used in place of the detector tube 64 shown in FIGS. 5 and 6.

Hereinafter, preferred embodiments of the present invention will be described in detail. However, the present invention is not limited to the following embodiments. In addition, the same code | symbol is attached | subjected about the same or equivalent element. In addition, although the positional relationship between the top, bottom, left and right is as shown in the drawing, the ratio of dimensions is not limited to that shown in the drawing. Moreover, as long as the detection value of hydrogen sulfide is consistent with IP 399/94, which is the conventional method, the conditions of each embodiment can be selected as appropriate.

[First embodiment]
In the first embodiment, a method for detecting hydrogen sulfide in fuel oil is performed using the detection apparatus shown in FIGS. The detection apparatus shown in FIGS. 1 to 3 may be composed of the following devices, for example.

(Test container)
The test container is not particularly limited as long as it is a flask having a plurality of necks. For example, a three-necked round bottom flask 3 having a capacity of 100 mL may be used. Further, the main tube 4 and the side tubes 5 and 6 of the test container may have a fitting port so that they can be easily jointed with other instruments.

(Cooler)
The cooler is not particularly limited as long as the volatile component of the dilution solvent 14 contained in the flow gas can be cooled and liquefied, but the Erlin type cooler 10 can be preferably used. Or you may use the thing equivalent to this. The cooler may have a rubbing port so that it can be easily jointed with other instruments. The cooler 10 cools and liquefies the volatile component of the diluted solvent 14 contained in the flow gas, and prevents the diluted solvent 14 from being collected by the following collector.

(Connection pipe)
The connecting tube 9 connects the round bottom flask 3 and the cooling tube 10 and may have a fitting port. For example, the connecting tube 9 is used when the rounding flask 3 and the cooling tube 10 have different fitting diameters.

(Exhaust pipe)
The exhaust pipe 11 connects the upper part of the cooler 10 and the tedlar back 13. When the upper part of the cooler 10 is a matching port, the exhaust pipe 11 may have a matching port in order to joint with the upper part of the cooler 10.

(Introduction pipe)
The introduction pipe 2 introduces the flow gas into the diluting solvent. As the introduction tube 2, a thin glass tube can be preferably used. The tip of the introduction tube 2 is placed in a diluting solvent introduced into the three-necked round bottom flask 3.

(Water bath)
The water 7 in the water bath 8 is maintained at about 60 ± 2 ° C. by the heater.

(Diluted solvent)
The diluent solvent 14 is not particularly limited as long as it can dissolve the fuel oil, and examples thereof include xylene, toluene, dry solvent, ink solvent, and low-viscosity lubricating oil not containing hydrogen sulfide. In the first embodiment, xylene is used as a dilution solvent. What is necessary is just to use what was prescribed | regulated to JISK8271 as xylene.

(Collector)
The collector is not particularly limited as long as it can collect the flow gas containing hydrogen sulfide, but a Tedlar bag 13 made of polyvinyl fluoride can be preferably used.

(Flowmeter)
As the flow meter 1, a float type flow meter capable of adjusting the flow rate of the flow gas or a device having the same performance may be used. A preferable flow rate of the flow gas is about 200 ± 5 mL / min.

(Detection tube for hydrogen sulfide)
The detector tube is generally called a detector tube type gas measuring device. The detection tube is a cylinder type glass tube having a uniform inner diameter, which is tightly filled with a detection agent and sealed at both ends. When both ends of the detection tube are broken and connected to a gas collector (piston), and a certain amount of sample gas (flow gas) is sucked into the detection tube, the gas to be detected (hydrogen sulfide) contained in the sample gas becomes the detection agent. A chemical reaction occurs immediately, and the detection agent changes color from the entrance side of the detection tube. After the inhalation of the sample gas is completed, the position corresponding to the tip of the color change region of the detection agent is read with the density scale marked on the detection tube. Thereby, the content of the gas to be detected in the sample gas is quantified. The detection agent is obtained by adsorbing a reaction reagent that selectively reacts with a gas to be detected and colored to fine particles such as purified silica gel or alumina. As the hydrogen sulfide detection tube 20, a commercially available portable type may be used. The reaction reagent included in the hydrogen sulfide detector tube 20 is lead acetate. The hydrogen sulfide introduced into the hydrogen sulfide detector tube 20 reacts with lead acetate to produce lead sulfide, whereby the detection agent turns from white to brown. The measurement range of hydrogen sulfide with a commercially available detector tube for hydrogen sulfide is about 0.25 to 120 ppm.

(Detection method of hydrogen sulfide)
<Fuel oil collection>
As the fuel oil, those that do not easily volatilize at normal temperature are preferable, and those that do not volatilize even when heated at about 60 ° C. are particularly preferable. Examples of such fuel oil include marine fuel oil, light oil, A heavy oil, motor heavy oil, electric power heavy oil, heavy oil base material (cutback bottom), and the like. The method for detecting hydrogen sulfide according to the first embodiment is particularly suitable for the determination of hydrogen sulfide contained in marine fuel oil.

The fuel oil is preferably collected and prepared by a primary sample collection method and a secondary sample preparation method specified in JIS K 2251 (crude oil and petroleum products-sample collection method), or a method similar thereto.

In order to collect (sample) fuel oil from the sample container, a syringe or the like may be used. The sample collected in the syringe is used for measurement in the shortest possible time. When the sample container is opened, it is preferable to end the test within 4 hours in order to prevent the deterioration of the fuel oil.

If the viscosity of the fuel oil is high and the fuel oil cannot be taken with a syringe, the fuel oil is heated at the minimum temperature necessary to obtain the fluidity of the fuel oil. The heating temperature of the fuel oil is preferably around 40 ° C. It is not preferable to heat the fuel oil at a temperature higher than the heating temperature of the diluted solvent (for example, 60 ° C.) or to heat the fuel oil for a long time because it causes deterioration of the fuel oil.

After removing the lid of the sample container and collecting the fuel oil, it is better to replace the inside of the sample container with nitrogen gas and immediately cover the sample container to prevent the fuel oil from deteriorating.

<Preparation of detection device>
In the first embodiment, the cooling pipe 10 is attached to the main pipe 4 at the center of the test container 3 via the connection pipe 9. The introduction pipe 2 is connected to the side pipe 5, and the other side pipe 6 is plugged (glass stopper or rubber plug).

The test container 3 is installed at a position where the test container 3 is immersed in the water bath 8 or more.

Connect the flow gas main plug and the flow meter 1 with piping such as a flexible tube (not shown). Next, the outlet of the flow meter 1 and the introduction pipe 2 are connected by piping, and the combined exhaust pipe attached to the upper part of the cooler 10 and the Tedlar back 13 are connected by the exhaust pipe 11. The port of the exhaust pipe 11 on the side connected to the Tedlar back is previously adjusted to the diameter of the gas sampling port 12 of the Tedlar back.

As the flow gas, a gas that is inert to at least hydrogen sulfide and has a different chemical property from hydrogen sulfide may be used. As such a flow gas, nitrogen gas, inert gas, air, etc. are suitable. In addition, when air is used as the flow gas, it is preferable to pass air through a filter in order to remove impurities, dust, water, and the like in the air. As the nitrogen gas, a second-grade gas specified in JIS K 1107 or a gas having a purity equal to or higher than that may be used. Below, the case where nitrogen gas is used as a flow gas is demonstrated.

供給 Check the airtightness of the assembled test container 3 and Tedlar bag 13 by supplying nitrogen gas.

50 mL of diluted solvent 14 is weighed into a measuring cylinder, the stopper of the side tube 6 where the introduction tube 2 is not inserted is removed from the test container 3, the diluted solvent 14 is poured into the test container 3, and immediately the stopper of the side tube 6 is plugged. do.

<Fuel oil weighing>
Shake the sample container that has been heated to around 40 ° C in advance to homogenize the fuel oil in the sample container, remove the lid of the sample container, and quickly collect about 5 mL of fuel oil with the syringe 15 without a needle. To do. The amount of fuel oil collected in terms of weight may be 1.00 to 5.00 g. After collecting the fuel oil, the dirt attached around the syringe 15 is wiped off, and the weight W ₁ of the syringe 15 containing the fuel oil is measured. If the fuel oil has sufficiently high fluidity at room temperature, the fuel oil may be collected by the syringe 15 without heating.

∙ Immediately after collecting the fuel oil, purge the air in the sample container with nitrogen gas and quickly cover the sample container. Do not leave the sample container open.

<Flow gas collection>
After purging the inside of the round bottom flask 3 with nitrogen gas by the above method for 10 minutes, it is preferable to reduce the nitrogen gas flow rate so that the diluted solvent 14 does not spout during the fuel oil injection. In the first embodiment, the nitrogen gas flow rate is reduced from about 200 mL / min to about 10 mL / min, the side tube 6 of the round bottom flask 3 is unplugged, and the tip of the syringe 15 is inserted into the round bottom flask 3. Fuel oil is injected into the xylene 14 in the round bottom flask 3. The fuel oil is uniformly dissolved in xylene 14.

After the fuel oil is injected into the xylene 14, the side pipe 6 is immediately plugged, and the exhaust pipe 11 connected to the upper end of the cooler 10 is connected to the gas sampling port 12 of the Tedlar back 13 having a capacity of 3L. Immediately, the nitrogen gas flow rate is adjusted to 200 mL / min, and nitrogen gas is blown into the xylene 14 for 15 minutes while heating the xylene 14 to 60 ° C. in the water bath 8. By introducing nitrogen gas, hydrogen sulfide is driven out of the xylene 14 in which the fuel oil is dissolved. In other words, hydrogen sulfide or the like contained as an impurity in the fuel oil is recovered in the nitrogen gas released from the xylene 14 after being introduced into the xylene 14. While the nitrogen gas is continuously introduced into the xylene 14 for 15 minutes, the flow gas released from the xylene 14 is collected in the Tedlar bag 13. 3 L of nitrogen gas containing hydrogen sulfide is collected in the Tedlar bag 13.

The weight W2 of the syringe 15 after fuel oil injection is measured. From the following formula (1), the weight S _U (g) of the fuel oil dissolved in xylene 14 is calculated.
S _U = W ₁ −W ₂ (1)

After collecting 3 L of nitrogen gas in the Tedlar back 13, the Tedlar back 13 is removed from the exhaust pipe 11, and the gas sampling port 12 of the Tedlar back 13 is closed.

<Detection of hydrogen sulfide by detector tube method>
The both ends of the hydrogen sulfide detector tube 20 are folded with an attached cutter, the arrow written on the hydrogen sulfide detector tube 20 is directed to the gas collector 21, and the hydrogen sulfide detector tube 20 is inserted into the gas collector 21 and attached. Next, the following operations 1 and 2 are performed.

In operation 1, the piston handle (handle) of the gas sampling device 21 is completely pushed in to push out the air in the hydrogen sulfide detector tube 20 completely. And the front-end | tip of the detection tube 20 for hydrogen which faces the gas collector 21 and the other side is connected to the collection port 12 of the Tedlar back | bag 13 (refer FIG. 2).

In operation 2, the guide marks displayed on the main body of the gas collector 21 and the piston handle are adjusted to a gas sampling amount of 100 mL. The piston handle is pulled at a stroke until the stopper is applied, and the nitrogen gas in the Tedlar back 13 is sucked into the hydrogen sulfide detection tube 20 for a predetermined time. After completing the suction of the nitrogen gas, a value corresponding to the length of the color change region 22 of the hydrogen sulfide detection tube 20 is read from the scale marked on the hydrogen detection tube 20 (see FIG. 3). The value read from the scale corresponds to the hydrogen sulfide content A (volume ppm) in 100 mL of nitrogen gas.

If it is necessary to collect 100 mL or more of nitrogen gas, repeat steps 1 and 2 with the hydrogen detector tube 20 attached to the gas collector 21 to collect the required amount of nitrogen gas. In this case, the hydrogen sulfide content A is corrected as follows. For example, when a double amount (200 mL) of the reference sampling gas amount (100 mL) that is the basis of the detection tube display value is sampled in the hydrogen sulfide detection tube 20 by two suctions, 1/2 of the display value of the detection tube (100 mL / 200 mL) is the correct hydrogen sulfide content A.

The hydrogen sulfide content C (mass ppm) in the fuel oil is calculated by the following equation (2).
C = (M × V _U × A) / (V _S × S _U ) = (4.113 × A) / S _U (2)

In said formula (2), M is the molecular weight 34 (g) of hydrogen sulfide. V _U is a Tedlar bag 13 nitrogen gas collected in the (collector) volume (flow gas) (L). In the first embodiment, V _U is equal to the volume 3 L of the Tedlar back 13. A is the content (volume ppm) of hydrogen sulfide in 100 mL of nitrogen gas (flow gas) as described above, and is a value read from the hydrogen sulfide detector tube 20. Alternatively, A is the content of hydrogen sulfide corrected per 100 mL of nitrogen gas (flow gas). V _S is a volume of 24.8 (L) with an ideal volume of 1 mol at 1 atm (bar) and room temperature (25 ° C.). S _U is the weight S _U (g) of the fuel oil dissolved in xylene 14 (diluent solvent) as described above.

As described above, in the determination of hydrogen sulfide by the detection tube method, the volume V _{U of} the flow gas collected in the collector, the content A of hydrogen sulfide in 100 mL of the flow gas, and the fuel oil dissolved in the diluent solvent It is possible to determine the hydrogen sulfide content C in the fuel oil by measuring the weight _SU of each and using the above formula (2). In the first embodiment, it is possible to detect hydrogen sulfide in fuel oil more easily than IP 399/94 and with the same degree of accuracy as IP 399/94.

The fuel oil is not only hydrogen sulfide but also at least one selected from the group consisting of sulfurous acid gas (sulfur dioxide), mercaptans, gasoline, acetylene, ethylene, ammonia, hydrogen chloride, nitrogen oxides, carbon monoxide, and carbon dioxide May also be included. In the first embodiment, the content of sulfurous acid gas in the nitrogen gas collected in the Tedlar bag 13 may be measured using a sulfurous acid gas detection tube. The mercaptan content in the nitrogen gas collected in the Tedlar bag 13 may be measured using a detection tube for mercaptans. The gasoline content in the nitrogen gas collected in the Tedlar bag 13 may be measured using a gasoline detection tube. You may measure content of acetylene in the nitrogen gas collected by the tedlar back | bag 13 using the detection tube for acetylene. You may measure ethylene content in the nitrogen gas collected by the Tedlar back | bag 13 using the detector tube for ethylene. You may measure the content of ammonia in the nitrogen gas collected by the Tedlar bag 13 using the ammonia detection tube. The hydrogen chloride content in the nitrogen gas collected in the Tedlar bag 13 may be measured using a hydrogen chloride detector tube. You may measure the content of the nitrogen oxide in the nitrogen gas collected by the Tedlar back | bag 13 using the detection tube for nitrogen oxides. The carbon monoxide content in the nitrogen gas collected in the Tedlar bag 13 may be measured using a carbon monoxide detector tube. You may measure the content of the carbon dioxide in the nitrogen gas collected by the Tedlar bag 13 using the carbon dioxide detection tube. According to the detector tube method, not only hydrogen sulfide but also the above impurities can be quantified easily. Sulfurous acid gas detector tube, mercaptan detector tube, gasoline detector tube, acetylene detector tube, ethylene detector tube, ammonia detector tube, hydrogen chloride detector tube, nitrogen oxide detector tube, carbon monoxide detector A commercially available detector tube may be used as the tube and the detector tube for carbon dioxide.

In addition to hydrogen sulfide detector tube 20, sulfurous acid gas detector tube, mercaptans detector tube, gasoline detector tube, acetylene detector tube, ethylene detector tube, ammonia detector tube, hydrogen chloride detector tube, nitrogen oxidation At least one of the object detector tube, the carbon monoxide detector tube, and the carbon dioxide detector tube may be connected to the tedlar back 13. That is, a plurality of types of gas detection tubes may be connected to the tedlar back 13 in parallel.

In the first embodiment, as shown in FIG. 4, a sulfurous acid gas detection tube 42 and a mercaptan detection tube 41 may be installed between the tedlar back 13 and the hydrogen sulfide detection tube 20. That is, the tedlar back 13, the sulfurous acid gas detection tube 42, the mercaptan detection tube 41, and the hydrogen sulfide detection tube 20 may be connected in series in this order. Thereby, after removing sulfurous acid gas and mercaptans which inhibit detection of hydrogen sulfide from nitrogen gas, hydrogen sulfide in nitrogen gas can be quantified. As a result, the detection accuracy of hydrogen sulfide in the fuel oil is improved. In FIG. 4, the sulfurous acid gas detection tube 42 and the mercaptan detection tube 41 may be interchanged.

[Second Embodiment]
A hydrogen sulfide detection device according to a second embodiment of the present invention and a hydrogen sulfide detection method using the detection device will be described.

(Detection device)
As shown in FIG. 5, the hydrogen sulfide detection device 50 according to the second embodiment includes, as main components, a test vessel 56, a heater 54, an introduction tube 51, a collector 59, a detection tube 64, and hydrogen sulfide. A detection tube 20 and a gas flow control mechanism 61 are provided. The insides of the test vessel 56, the collector 59, the gas pipes 62, 65, 66, the detection pipe 64, and the hydrogen sulfide detection pipe 20 can be hermetically sealed.

The test container 56 includes a sample introduction port 53. A heater 54 and a thermocouple 55 are installed in the test container 56. The leading end of the introduction tube 51 is disposed in the test container 56, and the inside of the test container 56 is vented to the atmosphere through the introduction tube 51. A filter 52 is installed in the middle of the introduction pipe 51. The filter 52 has a function of removing dust in the gas introduced into the test container 56 through the introduction pipe 51.

The gas pipe 57 connects the test container 56 and the collector 59. An electromagnetic valve 58 for opening and closing the gas pipe 57 is installed in the middle of the gas pipe 57. The gas pipe 62 connects the collector 59 and the detection pipe 64. An electromagnetic valve 63 that opens and closes the gas pipe 62 is installed in the middle of the gas pipe 62. The gas pipe 65 connects the end of the detection pipe 64 opposite to the electromagnetic valve 63 and the hydrogen sulfide detection pipe 20. A gas pipe 66 is connected to the end of the hydrogen sulfide detection pipe 20 opposite to the gas pipe 65. The gas pipe 66 communicates with the atmosphere. The detection tube 64 is for detecting components other than hydrogen sulfide contained in the flow gas.

The gas flow control mechanism 61 has a piston 60 disposed in the collector 59 and a flow rate control motor that moves the piston 60. The gas flow control mechanism 61 opens the electromagnetic valve 58, closes the electromagnetic valve 63, and moves the piston 60 disposed in the collector 59 to suck the flow gas in the test container 56 into the collector 59. To do. The gas flow control mechanism 61 closes the electromagnetic valve 58, opens the electromagnetic valve 63, discharges the flow gas sucked into the collector 59 from the gas pipe 62, and supplies it to the hydrogen sulfide detection pipe 20. Thus, the flow rate of the flow gas is controlled by the gas flow control mechanism 61. A step of sucking the flow gas in the test container 56 into the collector 59 by the gas flow control mechanism 61 and a step of supplying the flow gas sucked into the collector 59 to the hydrogen sulfide detection tube 20 side. Can be automated.

(Detector tube)
What is necessary is just to use the same thing as 1st embodiment as a detection tube. In the second embodiment, by supplying a certain amount of sample gas (flow gas) from the collector 59 to the hydrogen sulfide detection tube 20, the content of the gas to be detected in the sample gas is quantified.

(Detection method of hydrogen sulfide)
The method for detecting hydrogen sulfide in fuel oil is performed using the detection device 50 in the following procedure.

<Fuel oil collection>
In the second embodiment, fuel oil may be collected by the same method as in the first embodiment. As the fuel oil, the same fuel oil as that used in the first embodiment may be used. The hydrogen sulfide detection device of the present invention is particularly suitable for the determination of hydrogen sulfide contained in marine fuel oil.

<Fuel oil weighing>
The fuel oil was collected with a syringe in the first embodiment and the same method, measuring the weight W ₁ of the syringe containing the fuel oil.

<Flow gas collection>
About 50 mL of diluted solvent 14 is weighed into a measuring cylinder and introduced into the test container 56 from the sample introduction port 53. The diluent solvent 14 is not particularly limited as long as it can dissolve the fuel oil, and examples thereof include xylene, toluene, dry solvent, ink solvent, and low-viscosity lubricating oil not containing hydrogen sulfide.

When xylene or toluene is used as the diluting solvent 14, the detection device 50 includes a cooler (reverter) for liquefying and recovering the volatile content of the diluting solvent contained in the flow gas flowing in the gas pipe 57 by cooling. A trap may be provided. The cooler is not particularly limited. For example, an Erlin type cooler can be used. However, in order to reduce the size of the detection device 50, it is preferable to omit the cooler and the trap. Therefore, in order to reduce the size of the detection device 50, it is preferable to use a diluting solvent (a solvent having a high melting point) that is less volatile than xylene and toluene.

The inside of the test vessel 56 and the collector 59 is purged with the flow gas introduced from the introduction pipe 51. As the flow gas, a gas that is inert to at least hydrogen sulfide and has a different chemical property from hydrogen sulfide may be used. As such a flow gas, nitrogen gas, inert gas, air, etc. are suitable. Nitrogen gas may be supplied from a gas cylinder. The air may be used as the air. When air is used as the flow gas, it is preferable to pass air through the filter 52 to remove impurities, dust, water, and the like in the air. As the nitrogen gas, a second-grade gas specified in JIS K 1107 or a gas having a purity equal to or higher than that may be used.

The fuel oil in the syringe is injected from the sample inlet 53 into the diluent solvent 14 in the test container 56. Using the heater 54 and the thermocouple 55, the dilution solvent 14 is heated to about 60 ± 2 ° C., and the fuel oil is uniformly dissolved in the dilution solvent 14. The type of the heater 54 is not particularly limited as long as it has a function of heating the diluted solvent 14 in the test container 56. For example, a throw-in heater as shown in FIG. Alternatively, the test container 56 may be heated with an aluminum block or the like instead of the throw-in heater. When injecting the fuel oil, the flow rate of the flow gas may be reduced from 200 mL / min to about 10 mL / min so that the diluted solvent 14 does not spout out.

Measuring the weight W ₂ of the syringe after the fuel oil injection. From the following formula (1), the weight S _U (g) of the fuel oil dissolved in the diluent solvent 14 is calculated.
S _U = W ₁ −W ₂ (1)

With the electromagnetic valve 58 opened and the electromagnetic valve 63 closed, the piston 60 of the gas flow control mechanism 61 is moved to increase the volume of the collector 59. As a result, the flow gas introduced from the introduction pipe 51 is blown into the dilution solvent 14 for about 15 minutes. By introducing the flow gas, hydrogen sulfide is expelled from the diluted solvent 14 in which the fuel oil is dissolved. In other words, hydrogen sulfide or the like contained as an impurity in the fuel oil is recovered in the flow gas released from the diluted solvent 14 after being introduced into the diluted solvent 14. The flow gas released from the diluted solvent 14 is collected in the collector 59. The volume V _U of the flow gas was collected in the collector 59 is measured. The volume V _U corresponds to the volume of the collector 59 controlled by the piston 60 of the gas flow control mechanism 61. The flow rate of the flow gas blown into the diluted solvent 14 may be controlled by the gas flow control mechanism 61. A preferable flow rate of the flow gas is about 200 ± 5 mL / min.

<Detection of hydrogen sulfide by detector tube method>
After collecting the flow gas volume V _U in the collector 59, closes the electromagnetic valve 58, with open solenoid valve 63 to move the piston 60 of the gas flow control mechanism 61, the volume of the collector 59 Decrease. As a result, the flow gas collected by the collector 59 is supplied into the hydrogen sulfide detection tube 20 via the gas pipe 62, the detection pipe 64, and the gas pipe 65. The amount of flow gas supplied to the hydrogen sulfide detection tube 20 may be controlled to about 100 mL by the gas flow control mechanism 61, for example.

After supplying the flow gas into the hydrogen sulfide detector tube 20, a value corresponding to the length of the discoloration region 22 of the hydrogen sulfide detector tube 20 is read from the scale marked on the hydrogen detector tube 20 (see FIG. 3). ). The value read from the scale corresponds to the hydrogen sulfide content A (volume ppm) in 100 mL of the flow gas collected in the collector 59.

Note that a flow gas of 100 mL or more may be supplied into the hydrogen detection tube 20. In this case, the hydrogen sulfide content A is corrected as follows. For example, when a double amount (200 mL) of the reference sampling gas amount (100 mL) that is the basis of the detection tube display value is supplied into the hydrogen sulfide detection tube 20, it is ½ of the display value of the detection tube (100 mL / 200 mL). Is the correct hydrogen sulfide content A.

The flow gas introduced into the hydrogen sulfide detector tube 20 is released to the atmosphere through the gas tube 66. The diluted solvent 14 and the fuel oil introduced into the test container 56 are sucked into the waste liquid tank 68 through the pipe 67 and discharged outside the apparatus through the pipe 69. In the same manner, the cleaning liquid introduced from the sample introduction port 53 into the test container 56 may be sucked into the waste liquid tank 68 and discharged out of the apparatus.

The hydrogen sulfide content C (mass ppm) in the fuel oil is calculated by the following equation (2).
C = (M × V _U × A) / (V _S × S _U ) = (4.113 × A) / S _U (2)

In said formula (2), M is the molecular weight 34 (g) of hydrogen sulfide. V _U is the volume (L) of the flow gas collected in the collector 59. A is the content (volume ppm) of hydrogen sulfide in 100 mL of the flow gas as described above, and is a value read from the hydrogen sulfide detector tube 20. Alternatively, A is the hydrogen sulfide content corrected per 100 mL of flow gas. V _S is a volume of 24.8 (L) with an ideal volume of 1 mol at 1 atm (bar) and room temperature (25 ° C.). S _U is the weight S _U (g) of the fuel oil dissolved in the diluent solvent 14 as described above.

As described above, in the second embodiment, it is possible to detect hydrogen sulfide in fuel oil more easily than IP 399/94 and with the same accuracy as IP 399/94. Further, the hydrogen sulfide detection device 50 according to the second embodiment can be made smaller than the device system for implementing IP 399/94.

The detector tube 64 is a detector tube for sulfurous acid gas, a detector tube for mercaptans, a detector tube for gasoline, a detector tube for acetylene, a detector tube for ethylene, a detector tube for ammonia, a detector tube for hydrogen chloride, a detector tube for nitrogen oxides, Any of a carbon monoxide detector tube and a carbon dioxide detector tube may be used.

The fuel oil is not only hydrogen sulfide but also at least one selected from the group consisting of sulfurous acid gas (sulfur dioxide), mercaptans, gasoline, acetylene, ethylene, ammonia, hydrogen chloride, nitrogen oxides, carbon monoxide, and carbon dioxide May also be included. In the second embodiment, the sulfurous acid gas content in the flow gas collected in the collector 59 may be measured using a sulfurous acid gas detection tube. The mercaptan content in the flow gas collected by the collector 59 may be measured using a detection tube for mercaptans. You may measure the gasoline content in the flow gas collected by the collector 59 using the gasoline detection tube. You may measure content of acetylene in the flow gas collected by the collector 59 using the detector tube for acetylene. You may measure ethylene content in the flow gas collected by the collector 59 using the ethylene detector tube. You may measure the content of ammonia in the flow gas collected by the collector 59 using the ammonia detection tube. The hydrogen chloride content in the flow gas collected in the collector 59 may be measured using a hydrogen chloride detector tube. You may measure the content of the nitrogen oxide in the flow gas collected by the collector 59 using the detection tube for nitrogen oxides. The carbon monoxide content in the flow gas collected in the collector 59 may be measured using a carbon monoxide detector tube. The carbon dioxide content in the flow gas collected in the collector 59 may be measured using a carbon dioxide detector tube. According to the detector tube method, not only hydrogen sulfide but also the above impurities can be quantified easily. Sulfurous acid gas detector tube, mercaptan detector tube, gasoline detector tube, acetylene detector tube, ethylene detector tube, ammonia detector tube, hydrogen chloride detector tube, nitrogen oxide detector tube, carbon monoxide detector A commercially available detector tube may be used as the tube and the detector tube for carbon dioxide.

The detection tube 64 is preferably one of a detection tube for sulfurous acid gas and a detection tube for mercaptans. Further, between the gas pipe 62 and the hydrogen sulfide detection pipe 20, both the sulfurous acid gas detection pipe and the mercaptans detection pipe may be installed as the detection pipe 64. That is, the collector 59, the sulfurous acid gas detector tube, the mercaptan detector tube, and the hydrogen sulfide detector tube 20 may be connected in series in this order. Thereby, after removing sulfurous acid gas and mercaptans which inhibit detection of hydrogen sulfide from the flow gas, hydrogen sulfide in the flow gas can be quantified. As a result, the detection accuracy of hydrogen sulfide in the fuel oil is improved. The sulfurous acid gas detector tube and the mercaptan detector tube may be interchanged. For example, as shown in FIG. 7, instead of the detection tube 64, a detection tube 64a for mercaptans, a detection tube 64b for sulfurous acid gas, and another detection tube 64c (such as a detection tube for carbon monoxide) connected in series. May be used. Each detection tube is connected to each other by a gas tube 40. However, the arrangement order of the detector tubes is not limited to that shown in FIG.

In addition to hydrogen sulfide detector tube 20, sulfurous acid gas detector tube, mercaptans detector tube, gasoline detector tube, acetylene detector tube, ethylene detector tube, ammonia detector tube, hydrogen chloride detector tube, nitrogen oxidation The collector 59 may be directly connected to at least one of the object detector tube, the carbon monoxide detector tube, and the carbon dioxide detector tube. That is, a plurality of types of gas detection tubes may be connected to the collector 59 in parallel. Alternatively, a plurality of types of gas detection tubes may be connected to the branched gas tube 62 in parallel.

[Third embodiment]
A hydrogen sulfide detection device according to a third embodiment of the present invention and a hydrogen sulfide detection method using the detection device will be described. Below, the description regarding the matter which is common in 3rd embodiment and 2nd embodiment is abbreviate | omitted, and both difference is demonstrated.

As shown in FIG. 6, the hydrogen sulfide detection device 50a according to the third embodiment includes a small test tube 56a as a collector. The detection device 50a includes a cylindrical heater 54a surrounding the test tube 56a. The temperature in the test tube 56a can be freely controlled by the heater 54a. In the detection device 50 a, an electromagnetic three-way cock 58 a is installed in the middle of the gas pipe 57 instead of the solenoid valve. The three-way cock 58a is connected to an air sampling pipe 51a different from the introduction pipe 51. The three-way cock 58a has the same function as the electromagnetic valve 58 in the second embodiment. When detecting hydrogen sulfide in fuel oil with the detection device 50a of the third embodiment, the air sampling pipe 51a is always shut off by the three-way cock 58a. The test tube 56a is detachable from the detection device 50a. After putting the diluted solvent 14 and the fuel oil into the test tube 56a removed from the detection device 50a, the test tube 56a is attached to the detection device 50a, and detection of hydrogen sulfide in the fuel oil is started in the same manner as in the second embodiment. To do. After detection of hydrogen sulfide, the test tube 56a is removed from the detection device 50a, and the diluted solvent 14 and fuel oil in the test tube 56a are discarded.

In the detection device 50a of the third embodiment, when the atmosphere is directly sucked into the collector 59, hydrogen sulfide and other harmful components in the atmosphere can be detected by the hydrogen sulfide detector tube 20 or the detector tube 64. That is, the detection device 50a has a function of detecting hydrogen sulfide in fuel oil and a function of detecting harmful components in the atmosphere. When detecting harmful components in the atmosphere with the detection device 50a, the test tube 56a and the collector 59 are shut off by the three-way cock 58a. The air introduced from the air sampling tube 51a is sucked into the collector 59 via the three-way cock 58a. When detecting harmful components in the atmosphere, the test tube 56a may be removed from the detection device 50a in order to increase detection accuracy.

The detection devices of the second embodiment and the third embodiment described above may be used in the laboratory or in the field. In particular, since the inspection device 50a of the third embodiment includes a small test tube 56a as a test container, it is easier to miniaturize than the second embodiment and can be easily carried in the field. Therefore, according to the hydrogen sulfide inspection apparatus 50a according to the third embodiment, hydrogen sulfide in the fuel oil and harmful components in the atmosphere can be easily detected in the field. For example, the inspection apparatus 50a of the third embodiment can be brought into a tanker, and hydrogen sulfide in fuel oil loaded on the tanker can be detected on the tanker. When hydrogen sulfide is detected in the field, nitrogen gas in a portable cylinder or air may be used as the flow gas.

Hereinafter, the present invention will be described in more detail with reference to examples, but the present invention is not limited to these examples.

Example 1
In Example 1, the content of hydrogen sulfide in six types of fuel oils A to F was quantified using the apparatus system shown in FIGS. In Example 1, the content of hydrogen sulfide in each fuel oil was determined twice.

In Example 1, 5 mL of fuel oil was dissolved in 50 mL of xylene in a round bottom flask. While heating xylene to 60 ° C., 200 mL / min of nitrogen gas was introduced into xylene, and nitrogen gas released from xylene was collected in a 3 L Tedlar bag. The hydrogen sulfide content A per 100 mL of nitrogen gas collected in the Tedlar bag was measured with a hydrogen sulfide detector tube (manufactured by Gastec Corporation, model number: 4LL). Using the weight S _U of 5 mL of fuel oil, 3 L of the total volume of nitrogen gas collected in the Tedlar bag, and the hydrogen sulfide content A per 100 mL of nitrogen gas, the above formula (2) gives the hydrogen sulfide content in the fuel oil. The content C was calculated.

Table 1 shows the content of hydrogen sulfide in the fuel oils A to F obtained in Example 1.

(Comparative Example 1)
In Comparative Example 1, the content of hydrogen sulfide in the six types of fuel oils A to F was quantified by IP 399/94. In Comparative Example 1, the content of hydrogen sulfide in each fuel oil was determined twice. Table 1 shows the content of hydrogen sulfide in the fuel oils A to F obtained in Comparative Example 1.

As shown in Table 1, it was confirmed that the content of hydrogen sulfide in each fuel oil measured in Example 1 substantially coincided with the measurement result of Comparative Example 1.

(Example 2)
In Example 2, as shown in FIG. 4, the sulfurous acid gas detector tube and the mercaptan detector tube were installed between the Tedlar bag and the hydrogen sulfide detector tube. That is, in Example 2, the tedlar back, the sulfurous acid gas detector tube, the mercaptan detector tube, and the hydrogen sulfide detector tube were connected in series in this order. In Example 2, the sulfurous acid gas content in the fuel oil G was determined using a sulfurous acid gas detector tube (manufactured by Gastec Corporation, model number: 5 Lb). Moreover, in Example 2, the content of mercaptans in the fuel oil G was determined using a detection tube for mercaptans (manufactured by Gastec Corporation, model number: 70L). The content of mercaptans in the fuel oil G is a conversion value on the assumption that the mercaptans correspond to methyl mercaptan or ethyl mercaptan. In Example 2, the content of hydrogen sulfide in the fuel oil G was determined using a hydrogen sulfide detector tube (manufactured by Gastec Corporation, model number: 4LL). Except for the above, the same method as in Example 1 was adopted in Example 2.

The content of hydrogen sulfide in the fuel oil G was less than 1 mg / kg. The content of sulfurous acid gas in the fuel oil G was less than 2 mg / kg. The content of mercaptans in the fuel oil G was 3 mg / kg.

As described above, in Example 2, the contents of hydrogen sulfide, sulfurous acid gas, and mercaptans in the fuel oil G could be quantified.

According to the method and apparatus for detecting hydrogen sulfide according to the present invention, hydrogen sulfide in fuel oil such as marine fuel can be detected more easily than before.

DESCRIPTION OF SYMBOLS 1 ... Flow meter, 2 ... Introducing tube, 3 ... Test container (three-necked round bottom flask), 4 ... Main tube, 5, 6 ... Side tube, 7 ... Water, 8 ..Water bath, 9 ... connecting pipe, 10 ... cooler, 11 ... exhaust pipe, 12 ... gas sampling port, 13 ... Tedlar bag, 14 ... diluting solvent, 15 ... Syringe, 20 ... hydrogen sulfide detector tube, 21 ... gas collector, 22 ... discoloration region, 41 ... mercaptan detector tube, 42 ... sulfurous acid gas detector tube, 50, 50a・ ・ ・ Hydrogen sulfide detection device, 51 ・ ・ ・ Introducing pipe, 51 a ・ ・ ・ Air sampling pipe, 52 ・ ・ ・ Filter, 53 ・ ・ ・ Sample inlet, 54 ・ ・ ・ Throw-in type heater, 54 a ・ ・ ・Cylindrical heater, 55... Thermocouple, 56... Test container, 56 a... Test tube, 40, 57, 62, 65, 66 ..Gas pipe, 58, 63 ... solenoid valve, 58a ... three-way cock, 59 ... collector, 60 ... piston, 61 ... gas flow control mechanism, 64, 64a, 64b, 64c ... detection tube, 67,69 ... piping, 68 ... waste liquid tank.

Claims (6)

1. The flow gas is introduced into the dilution solvent while heating the dilution solvent in which the fuel oil containing hydrogen sulfide is heated, and the flow gas released from the dilution solvent is collected in a collector, and the collection is performed. Measuring the content of the hydrogen sulfide in the flow gas collected in a vessel with a hydrogen sulfide detector tube,
   How to detect hydrogen sulfide.
2. The fuel oil contains at least one impurity selected from the group consisting of sulfurous acid gas, mercaptans, gasoline, acetylene, ethylene, ammonia, hydrogen chloride, nitrogen oxides, carbon monoxide, and carbon dioxide,
   Measuring the content of the impurities in the flow gas collected in the collector with a detector tube corresponding to the impurities,
   The method for detecting hydrogen sulfide according to claim 1.
3. At least one of a detection tube for sulfurous acid gas or a detection tube for mercaptans is installed between the collector and the detection tube for hydrogen sulfide, and at least one of the detection tube for sulfurous acid gas or the detection tube for mercaptans Measuring the hydrogen sulfide content in the flow gas that has passed through the hydrogen sulfide detector tube;
   The method for detecting hydrogen sulfide according to claim 1 or 2.
4. A test vessel containing a diluent solvent in which fuel oil containing hydrogen sulfide is dissolved;
   A heater for heating the dilution solvent in the test container;
   An introduction pipe for introducing a flow gas into the diluent solvent in the test container;
   A collector for collecting the flow gas in the test container;
   A hydrogen sulfide detector tube for measuring the content of hydrogen sulfide in the flow gas collected in the collector;
   A gas flow control mechanism for sucking the flow gas in the test container into the collector and supplying the flow gas sucked into the collector to the hydrogen sulfide detector tube;
   An apparatus for detecting hydrogen sulfide.
5. The fuel oil contains at least one impurity selected from the group consisting of sulfurous acid gas, mercaptans, gasoline, acetylene, ethylene, ammonia, hydrogen chloride, nitrogen oxides, carbon monoxide and carbon dioxide,
   Comprising a detector tube for measuring the content of the impurities in the flow gas collected in the collector;
   The hydrogen sulfide detection device according to claim 4.
6. The hydrogen sulfide detector tube is connected to the collector via at least one of a sulfurous acid gas detector tube or a mercaptan detector tube,
   The hydrogen sulfide detection device according to claim 4 or 5.

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