CN209961681U

CN209961681U - Novel sealed acidizing aeration hydrogen sulfide determinator

Info

Publication number: CN209961681U
Application number: CN201920167915.XU
Authority: CN
Inventors: 谢素梅; 陈嘉浩; 翟家骥; 郝永刚; 李椿方
Original assignee: 谢素梅; 陈嘉浩
Current assignee: BEIJING XIANQU WEIFENG TECHNOLOGY DEVELOPMENT Co.,Ltd.
Priority date: 2019-01-31
Filing date: 2019-01-31
Publication date: 2020-01-17
Anticipated expiration: 2029-01-31

Abstract

The utility model discloses a novel sealed acidizing aeration hydrogen sulfide apparatus, which is suitable for the determination of sulfide content in samples such as environment, chemical industry and the like. The instrument comprises a circulating pump (5), a gas lower pipeline (2), a gas left pipeline (6), a gas right pipeline (4), a gas-liquid separation cover (11), a peristaltic pump (9), an absorption pressure-resistant bottle (1), a right releasing agent liquid path (8), a left releasing agent liquid path (10) and an electric control part. The device is also provided with a gas-liquid separation cover (11) and a sample bottle gas-liquid separation cover (12), so that the liquid in the sample bottle and the absorption bottle can not enter a circulating pipeline while the integral sealing of the system is ensured. The design of integral sealing ensures that hydrogen sulfide is not lost due to incomplete absorption, an external gas source is not required to be added, and the device has high precision and accuracy and is simple to operate. If a six-channel mode is used, the analysis efficiency can be greatly improved.

Description

Novel sealed acidizing aeration hydrogen sulfide determinator

Technical Field

The utility model is suitable for a sulphide content's survey in samples such as environment, petroleum, chemical industry, energy, like water, soil, solid waste, oil, coal etc..

Background

In the fields of environment, petroleum, chemical industry, energy and the like, trace to trace sulfides are usually contained, and the sulfides are extremely toxic and can be released under the condition of carbonation, so that the sulfides are necessary to be measured in the fields of surface water, seawater, domestic drinking water, soil, solid wastes, petroleum, coal and the like. In these samples, the water sample often has interference factors such as color and turbidity, and petroleum and other solid samples can not be directly measured. The pretreatment technology is usually an acidification aeration absorption method at present.

In the GB 5749-2006 standard, the sulfide is the sensory property and general chemical index in the water quality unconventional index, and the limit value is 0.02 mg/L. In the standard detection method GB/T5750.5-2006, the aeration separation method only stipulates the precision and accuracy of 0.08mg/L and above. At the limit or lower, absorption recovery is not good.

In the GB 3838-2002 standard, sulfide is a basic item of surface water environmental quality standard, and the limit values of the water quality from the I class to the V class are 0.05, 0.1, 0.2, 0.5 and 1.0mg/L in sequence. In the standard detection method GB/T16489-1996, the aeration separation method only stipulates the precision and accuracy of four groups of samples of 0.148-0.600 mg/L. It cannot be absorbed and recovered well even at or below the detection limit.

In the GB 3097-1997 standard, sulfide is one of the seawater quality items, and the limit values of the seawater quality from the first type to the fourth type are 0.02, 0.05, 0.10 and 0.25mg/L in sequence. In 18.1 of its standard detection method GB 17378-2007, the aeration separation method only stipulates the repeatability and reproducibility of a 0.427mg/L sample. It cannot be absorbed and recovered well even at or below the detection limit.

The traditional aeration separation method adopts nitrogen purging, has complex device, low automation degree of acidification and the like, complex operation and higher requirement on operators. In addition, in the aeration process, the gas-liquid mass transfer of the bubbles and the liquid has certain resistance, so that incomplete absorption is caused, and the precision and the accuracy are difficult to ensure.

SUMMERY OF THE UTILITY MODEL

The utility model discloses use sealed acidizing aeration to absorb as the principle, provide a hydrogen sulfide content measurement appearance sealed, circulation and small, solved the technical problem that above-mentioned exists.

For solving the problem of measuring the content of sulfide, the utility model discloses sulfide content measuring instrument has following part: the device comprises a circulating pump, a lower gas pipeline, a right gas pipeline, a left gas pipeline, a gas-liquid separation cover, a peristaltic pump, an absorption pressure-resistant bottle, a left releasing agent liquid path, a right releasing agent liquid path and an electric control part. The circulating pump is made of a material which does not react with hydrogen sulfide chemically and is driven by a brushless motor. The lower gas pipeline, the left gas pipeline and the right gas pipeline are made of chemical inert materials for hydrogen sulfide integrally. The gas-liquid separation cover is made of chemical inert materials to hydrogen sulfide, is machined by a numerical control machine, and has a gas-liquid separation effect. The peristaltic pump automatically adds the release agent to the sample bottle, which is driven by a brush motor. The absorption pressure-resistant bottle is made of high borosilicate, high-density polypropylene, polytetrafluoroethylene and the like. The electric control part adopts MOS tube circulation time delay switch to control the circulation time.

Acid or other releasing agents are added into the sample bottle by the peristaltic pump, hydrogen sulfide in the sample bottle is released in a molecular state, and then the hydrogen sulfide is blown out by bubbling and aeration of the circulating pump and is absorbed by the absorbing agent in the absorption pressure-resistant bottle, and the unabsorbed hydrogen sulfide is continuously circulated until the hydrogen sulfide is completely absorbed. The release agent is added into the peristaltic pump and the circulation time is controlled by two MOS pipe circulation delay switches respectively.

Drawings

FIG. 1 is a schematic view of the single-channel sealed aeration separation hydrogen sulfide content measuring instrument of the utility model.

Fig. 2 is a schematic view of the gas-liquid separation cover of the present invention.

Fig. 3 is a schematic view of the gas-liquid separation cover of the sample bottle of the present invention.

In the figure: 1. an absorption pressure-resistant bottle; 2. a gas lower pipeline; 3. a sample bottle; 4. a gas right pipeline; 5. a circulation pump; 6. a gas left line; 7. a release agent bottle; 8. the right release agent liquid path; 9. a peristaltic pump; 10. the left release agent liquid path; 11. a gas-liquid separation cover; 12. and a gas-liquid separation cover of the sample bottle.

Detailed Description

Single-channel sealed acidification aeration separation hydrogen sulfide content tester-methylene blue determination mode

N, N-diethyl-p-phenylenediamine solution: 0.75g of N, N-diethyl-p-phenylenediamine hydrochloride was weighed out, dissolved in 900mL of purified water, and 100mL of sulfuric acid (1+1) was added. Stored in brown bottles, if the color turns red, it needs to be reconfigured.

Sodium hydroxide (0.1 mol/L): 4g of sodium hydroxide are weighed and dissolved in 1000mL of water.

Ferric chloride solution: 10g of ferric chloride hexahydrate is weighed, dissolved in 900mL of pure water, and 100mL of sulfuric acid (1+1) is added.

Releasing agent: (1+3) hydrochloric acid.

As shown in FIG. 1, 10mL of sodium hydroxide (0.1mol/L) was precisely transferred to an absorption pressure bottle 1, and 0.00, 2.00, 4.00, 6.00, 8.00, and 10.00mL of a sulfide standard solution having a concentration of 2.00mg/L were sequentially sucked into a sample bottle 3 to draw a standard curve. The circulation pump 5 is started and at the same time the peristaltic pump 9 is started to add the release agent. The circulation pump 5 was turned on for 5 minutes at a flow rate of 1L/min. The peristaltic pump 9 was on for 10 seconds at a flow rate of 60 mL/min. After complete absorption, 10.00mL of N, N-diethyl-p-phenylenediamine solution and 5.00mL of ferric chloride solution are added into an absorption pressure bottle 1, uniformly shaken and placed for 20min, and then color comparison is carried out at 665 nm. The method draws a standard curve y of 0.0177x +0.0057 and a linear correlation coefficient R²＝0.9985。

Directly absorbing 0.00, 2.00, 4.00, 6.00, 8.00 and 10.00mL of sulfide standard solution with the concentration of 2.00mg/L, adding 10.00mL of N, N-diethyl-p-phenylenediamine solution and 5.00mL of ferric chloride solution,shaking, standing for 20min, and performing color comparison at 665 nm. The method draws a standard curve y of 0.0178x +0.0015 and a linear correlation coefficient R²＝0.9994。

The standard curves configured by the two methods are not different, and the fact that the adopted system is not different from the non-adopted system is proved.

Then, 500mL of tap water was taken in, 1mL of EDTA solution and 2mL of ascorbic acid solution were added, and the blank value was measured to be 0.00 mg/L. 2.00mL of a 2.00mg/L sulfide standard solution (corresponding to a sulfide concentration level of 0.004 mg/L) was added, and the circulation pump 5 was turned on for 15 minutes at a flow rate of 6L/min. The peristaltic pump 9 was on for 30 seconds at a flow rate of 60 mL/min. The precision relative standard deviation is 2.6 percent and the recovery rate is 93.9 to 100.0 percent after 6 times of parallel measurement.

Six-channel sealed aeration separation hydrogen sulfide content tester-conductivity mode

Lead nitrate solution: the concentration of lead nitrate was 20mg/L, and a standard titration solution of hydrochloric acid was added to make the concentration 1.5. mu. mol/L.

Releasing agent: a citric acid solution of 200g/L at pH 4.00.

Precisely transferring 50.00mL of lead nitrate solution into an absorption pressure-resistant bottle 1, and sequentially sucking 0.00mL, 2.00mL, 4.00 mL, 6.00 mL, 8.00 mL and 10.00mL of sulfide standard solution with the concentration of 10.00mg/L into a sample bottle 3 for drawing a standard curve. The circulation pump 5 is started and at the same time the peristaltic pump 9 is started to add the release agent. The circulation pump 5 was turned on for 5 minutes at a flow rate of 1L/min. The peristaltic pump 9 was on for 10 seconds at a flow rate of 60 mL/min. The method draws a standard curve y of 0.3832x +25.9234 and a linear correlation coefficient R²＝0.9951。

Then 50.00mL of industrial wastewater is absorbed, 1mL of EDTA solution and 2mL of ascorbic acid solution are added, and six times of parallel determination are carried out, the average value is 0.064mg/L, and the precision is 1.0%.

The above-mentioned embodiments are only for describing the preferred embodiments of the present invention, and are not intended to limit the scope of the present invention, and various modifications and improvements made by those skilled in the art without departing from the design spirit of the present invention should fall into the protection scope defined by the claims of the present invention.

Claims

1. The utility model provides a novel sealed acidizing aeration hydrogen sulfide apparatus, a serial communication port, the device includes circulating pump (5), gaseous lower pipeline (2), gaseous left side pipeline (6), gaseous right side pipeline (4), gas-liquid separation lid (11), peristaltic pump (9), absorb withstand voltage bottle (1), right release agent liquid way (8), left release agent liquid way (10) and automatically controlled part, peristaltic pump (9) are squeezed into sample bottle (3) with release agent bottle (7) in the liquid, circulating pump (5) are through gaseous lower pipeline (2), gaseous left side pipeline (6) and gaseous right side pipeline (4) provide gaseous circulation power, the trace hydrogen sulfide that will release is brought into and absorbs withstand voltage bottle (1), the hydrogen sulfide that does not absorb is absorbed by the absorption liquid in withstand voltage absorption bottle (1) through gaseous pipeline circulation many times.

2. The apparatus for determining the hydrogen sulfide in the sealed acidification aeration according to the claim 1, wherein the circulating pump (5) is made of a material which does not react with the hydrogen sulfide, and the circulating pump (5) is driven by a brushless motor.

3. The novel sealed acidification aeration hydrogen sulfide determinator as claimed in claim 1, wherein the gas lower pipeline (2), the gas right pipeline (4) and the gas left pipeline (6) are all made of materials which do not react with hydrogen sulfide, wherein the gas lower pipeline (2) is arranged below the liquid level of the sample solution at one end of the sample bottle (3), and the gas lower pipeline (2) is arranged above the liquid level of the absorption liquid at one end of the absorption pressure-resistant bottle (1); one end of the gas right pipeline (4) at the sample bottle is positioned on the liquid level of the sample solution, and the other end of the gas right pipeline (4) is connected with the inlet end of the circulating pump (5); one end of the left gas pipeline (6) at the absorption pressure-resistant bottle (1) is below the liquid level of the absorption liquid, and the other end of the left gas pipeline (6) is connected with the outlet end of the circulating pump (5).

4. The novel sealed acidification aeration hydrogen sulfide determinator as claimed in claim 1, wherein the gas-liquid separation cover (11) is made of a material chemically inert to hydrogen sulfide, the gas-liquid separation cover (11) is provided with a chute, and the port of the gas lower pipeline (2) is higher than the bottom surface of the gas-liquid separation cover (11) to have a gas-liquid separation function and prevent a solution in the bottle from entering the circulating pipeline.

5. The novel sealed acidification aeration hydrogen sulfide determinator as claimed in claim 1, wherein a peristaltic pump (9) automatically adds a releasing agent into the sample bottle (3), the peristaltic pump (9) is driven by a brush motor, a right releasing agent liquid path (8) is arranged below the solution liquid level at one end of the releasing agent bottle (7), and the other end of the right releasing agent liquid path (8) is connected with the inlet end of the peristaltic pump (9); the left releasing agent liquid path (10) is arranged on the liquid level of the sample solution at one end of the sample bottle (3), and the other end of the left releasing agent liquid path (10) is connected with the outlet end of the peristaltic pump (9).