CN201321856Y - Device for detecting hydrogen sulfide on oil drilling spot - Google Patents

Device for detecting hydrogen sulfide on oil drilling spot Download PDF

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Publication number
CN201321856Y
CN201321856Y CNU2008201237423U CN200820123742U CN201321856Y CN 201321856 Y CN201321856 Y CN 201321856Y CN U2008201237423 U CNU2008201237423 U CN U2008201237423U CN 200820123742 U CN200820123742 U CN 200820123742U CN 201321856 Y CN201321856 Y CN 201321856Y
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hydrogen sulfide
oil drilling
checkout gear
bottle
filtering flask
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CNU2008201237423U
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于爱民
王振德
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CHANGCHUN JIAA SMALL SWAN INSTRUMENT Co Ltd
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CHANGCHUN JIAA SMALL SWAN INSTRUMENT Co Ltd
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Abstract

The utility model discloses a portable device for detecting hydrogen sulfide on an oil drilling spot, and belongs to the field of chemical analysis devices. The detecting device comprises a detecting instrument and a preprocessing and separating box, wherein, the preprocessing and separating box includes a box body; an argon inlet, a gas flow indicator, an acquisition sample bottle, a filter bottle, a bubble absorption tube and a detection sample bottle are sequentially arranged in the box body according to airflow; and air passages in the fittings are communicated with each other through multi-section silicone tubes. The detecting instrument provided by the utility model is based on the colorimetric analysis method, substances like sulfur dioxide and sulfur trioxide of the free hydrogen sulfide in a sample are removed through a filter liquid, and the hydrogen sulfide is fixed by an absorption liquid and reacts with a color development reagent to generate a colored compound which selectively absorbs visible light, so that the operation is simple and convenient, the accuracy of the detection result is high, the visibility is good, and the content of the hydrogen sulfide gas during the petroleum gas exploring process can be quickly detected.

Description

The hydrogen sulfide on oil drilling site checkout gear
Technical field
The utility model belongs to chemical analysis instrument, relate to a kind of easy, sensitive, quick on-the-spot hydrogen sulfide detection method and detecting instrument, be specifically related to a kind of method and checkout gear that on-the-spot fast quantification detects the content of oil and gas exploitation process hydrogen sulfide gas that be used for.
Background technology
Hydrogen sulfide is a kind of colourless, poisonous gas that the rotten egg smell is arranged.Its density is 1.539 grams per liters, fusing point-85.5 ℃, boiling point-60.7 ℃.Hydrogen sulfide is slightly soluble in water, and its aqueous solution is hydrosulphuric acid.Unstable chemcial property can burn in air during igniting, has reproducibility.When the hydrogen sulfide that contains 0.1% in the air, will cause that people shed tears, eye shouting pain, runny nose, bottleneck throat burning heat sensation, or with headache, symptom such as dizzy, weak, nauseating.Check visible conjunctival congestion, can there be dried hello sound in lung, can recover in a short time after disengaging.Cough, uncomfortable in chest, blurred vision, eye chemosis and ulcer of the cornea appear in moderate intoxication person MMi sx, symptoms such as obvious headache, dizziness are arranged, and the slight disturbance of consciousness occurs, lung's news and dryness or moist gong sound.X line chest films showed lung marking strengthens or the sheet shade is arranged.
When sucking a large amount of hydrogen sulfide, stupor, pulmonary edema, respiratory and circulatory failure appear, and when sucking high concentration (1000mg/m ' more than), " lightning class death " can appear.On the industrial production, require the content of Air Hydrogen Sulfide must not surpass 0.01 mg/litre.
In the recovery process of oil and gas industry, the blowout phenomenon is very common, itself is not accident, is a kind of disaster phenomenon, and oil gas field causes the aspects such as content of natural gas also different because of the geological structure difference.Natural gas (natural gas) claim casing-head gas, oil gas, oil field gas again.During recover petroleum, have only gas to be called natural gas.The chemical compound and the physicochemical property thereof of natural gas vary in different localities, and wherein hydrogen sulfide is one of composition of raw natural gas.Country has all made relevant regulation at relevant problem in the exploitation of oil-gas field industry, as when hydrogen sulfide containing oil gas field carries out construction operation and production of hydrocarbons, all production operation personnel should accept the training of hydrogen sulfide protection; The hydrogen sulfide operation field should be installed the hydrogen sulfide warning system, and this system should be able to sound, light is reported to the police, and can be guaranteed that the personnel in entire job zone can both see and hear.Visitor and other non-regular dispatch personnel should be accepted interim safety education before entering the hydrogen sulfide hazardous area, and under the personnel's companion that was subjected to training, just allowed to enter the hazardous area.
Should install and fix the formula hydrogen sulfide detector at the position that hydrogen sulfide gas might appear in operation field, should be equipped with portable hydrogen sulfide detector in addition; In the obvious place of operating personnel marking signals such as wind vane, anemobiagraph should be installed.When piercing oil-gas Layer, should be according to the mensuration of field condition encryption to hydrogen sulfide in the drilling fluid.When in neotectonics, boring exploration well, should take corresponding hydrogen sulfide monitoring and preventive action.In view of this, in the exploitation of oil-gas field process, the detection of stink damp body burden is very necessary.And existing on-the-spot mensuration to hydrogen sulfide in the drilling fluid, disturbing factor is more, and the testing result deviation is bigger.
The utility model content
The purpose of this utility model is to provide a kind of checkout gear that can easy, quick, on-the-spot, quantitatively detect hydrogen sulfide content in the oil drilling.
For reaching above-mentioned purpose, the concrete content of the utility model is:
A kind of hydrogen sulfide on oil drilling site checkout gear, comprise detecting instrument, also comprise a pre-treatment separator box, described pre-treatment separator box comprises a casing, be provided with argon gas intake interface, gas flowmeter, collected specimens bottle, filtering flask and bubble absorption tube successively by the air-flow trend in the casing, and gas circuit is communicated with by the multistage silicone tube in these accessories.
Wherein, described collected specimens bottle inner bottom part is established a sample bottle filter, and the sample bottle strainer is communicated with by silicone tube with gas flowmeter by the air inlet that pipeline passes on the collected specimens bottle cap again, establishes a venthole on the collected specimens bottle cap in addition.
Wherein, described filtering flask inner bottom part is established a filtering flask strainer, the filtering flask strainer by pipeline pass on the filtering flask bottle cap air inlet again with the collected specimens bottle cap on venthole be communicated with by silicone tube, set out pore on the filtering flask bottle cap in addition.
Wherein, the venthole on the filtering flask bottle cap is communicated with bubble absorption tube inlet end by silicone tube, and the bubble absorption tube is also established outlet end.
Wherein, described detecting instrument is a miniaturization colorimetric detection instrument.The colorimetric detection instrument is provided with casing, is provided with the colorimetric pool lid at the upper surface of casing, and colorimetric pool lid lower room is provided with colorimetric pool.Described colorimetric pool is the rectangle cell body of a upper surface opening, and a side end face of colorimetric pool is provided with the super bright light emitting diode of 630nm, connects corresponding opposite side end face and is provided with photoelectric sensor; A colorimetric pool medial launder body space and a cuvette are complementary.
The distinguishing feature and the effect of the hydrogen sulfide on oil drilling site checkout gear that the utility model provides are:
1, detecting instrument is based on the colorimetric analysis method, free hydrogen sulfide is removed materials such as sulfur dioxide and sulfur trioxide through filtrate in the sample, it is liquid-solid fixed to be absorbed again, last and developer reaction generates colored compound to the selective absorption of visible light, easy and simple to handle, testing result degree of accuracy height, intuitive is good.
2, adopt Single-chip Controlling, have measurement, setting, record, preservation and data processing function.Be provided with the RS-232/USB interface,, and be provided with functions such as help, automaticity height with the PC on-line communication.
3, liquid crystal digital shows, the man-machine interactive operation.
4, colorimetric pool and cuvette all are used and adopt original design in the instrument, guarantee the instrument globality.
5, volume is little, in light weight, easy to use.
The utility model can fast detecting hydrogen sulfide gas in the oil and gas exploitation process content, can be used for on-the-spot mensuration to hydrogen sulfide in the drilling fluid.
Description of drawings
Fig. 1 is a detecting instrument external structure schematic diagram in the utility model checkout gear.
Fig. 2 is a pre-treatment separator box structural representation in the utility model checkout gear.
Fig. 3 is the colorimetric pool structural representation of detecting instrument in the utility model checkout gear.
Fig. 4 is a detecting instrument principle schematic in the utility model checkout gear.
The specific embodiment
The hydrogen sulfide on oil drilling site checkout gear that the utility model proposes is based in the sample free hydrogen sulfide remove materials such as sulfur dioxide and sulfur trioxide through filtrate after, it is liquid-solid fixed to be absorbed again, last and developer reaction generation colored compound, the technology of a kind of colorimetric analysis that the principle that visible light is absorbed selectively according to this compound is set up.
Below the effect forming and can produce with regard to the structure of the utility model hydrogen sulfide on oil drilling site checkout gear, conjunction with figs. is described in detail as follows with preferred embodiment:
The utility model checkout gear comprises detecting instrument 1 and pre-treatment separator box 2 two parts.Wherein, the sample of 2 pairs of collection in worksite of pre-treatment separator box carries out pre-treatment to obtain test sample, and 1 pair of test sample analysis of detecting instrument obtains testing result.
Wherein, as shown in Figure 1, external structure schematic diagram for detecting instrument 1, casing 19 is arranged, upper surface at casing 19 is provided with LCDs 11, a plurality of button 12 and colorimetric pool lid 13, and is disposed with power control switch 14, electrical socket 15 and RS-232 interface 16 below casing 19 back right side of face.
Be provided with colorimetric pool 3 below the colorimetric pool lid 13 of casing 19.As shown in Figure 3, colorimetric pool 3 is a rectangle cell body 31, upper surface opening and the sealing of other end, one end face of rectangle cell body 31 is provided with light source/monochromator 33, connect corresponding other end with light source/monochromator 33 and be provided with photoelectric detector 32, form single pass reaction colorimetric pool 3 with this, this colorimetric pool 3 is fixedly mounted in the corresponding space of casing 19, and the central space of colorimetric pool 3 cell bodies 31 is used for putting into the cuvette that test sample is housed when detecting.
Described light source/monochromator 33 is super bright light emitting diode, can adopt the Japanese super bright light emitting diode that day is inferior and Toyota Company produces, and luminance parameter is more than 1000mcd, and wavelength is 630nm; Described photoelectric detector 32 is a photoelectric sensor, adopted American TI Company to produce the integrated electro sensor, model can be a kind of among TSL201, TSL202, TSL203, TSL204, TSL205, TSL206, TSL207, TSL208, TSL209, TSL220, TSL230, TSL235, TSL245, TSL250, TSL251, TSL250, TSL253, TSL254, TSL255, TSL256, TSL257, TSL258, TSL259, TSL260, TSL261, the TSL262.Certainly, also can adopt other to have the integrated electro sensor of equal effect.
Colorimetric pool 3 is made by plastic material; The described colorimetric pool lid 13 of casing outer surface that places is connected on the host shell 19, can freely renovate, and when opening, cuvette can freely take out and be placed in the colorimetric pool 3, when colorimetric pool lid 13 closes, guarantees colorimetric pool 3 lucifuges.Described cuvette is standard quartz cuvette (or glass cuvette), is not described in detail in this.
Other configure microprocessor 18 in the detecting instrument 1, microprocessor 18 is electrically connected in a usual manner with light source/monochromator 33, photoelectric detector 32, power supply 14 and control button 12, display screen 11 etc., microprocessor 18 can be P51, the P52 series that PHILIPS Co. produces, its major parameter is 12 single-chip microcomputers, internal storage 64K wherein is equipped with colorimetric analysis software commonly used.As shown in Figure 4, the groundwork principle that has shown detecting instrument 1, wherein light source/monochromator 33, detected sample (being contained in the cuvette) and photoelectric detector 32 are in parallel with microprocessor 18, when power supply 14 was opened by switch 13 controls, detecting instrument 1 was started working and is obtained testing result and shows on display screen 11.
Certainly the utility model also can pass through RS-232/USB interface and PC on-line communication, and analysis result is shown by PC.Microprocessor 18 also can pass through RS-232/USB interface and computer on-line communication, and the setting of data, collection, analysis and processing procedure can be finished by operating computer, and the information after will handling shows by computer display screen or printer.
Detecting instrument 1 available in the utility model is not limited to the structure of above-mentioned introduction, and can adopt any commercial being suitable for to be carried to on-the-spot colorimetric detection instrument.
The pre-treatment separator box 2 of the utility model checkout gear is for realizing the corollary apparatus of collected specimens pre-treatment, the test sample that becomes detecting instrument 1 to use with the sample treatment with collection in worksite.As shown in Figure 2, sample pre-treatments case 2 comprises a casing 21, be provided with argon gas intake interface 27, gas flowmeter 26, collected specimens bottle 24, filtering flask 23, bubble absorption tube 22 and test sample bottle 25 successively by the air-flow trend in the casing 21, gas circuit is communicated with by multistage silicone tube 28 in these accessories; Wherein, collected specimens bottle 24 inner bottom parts are established a sample bottle filter 241, and sample bottle strainer 241 is communicated with by silicone tube 28 with gas flowmeter 26 by the air inlet 242 that pipeline 29 passes on collected specimens bottle 24 bottle caps again; Filtering flask 23 inner bottom parts are established a filtering flask strainer 231, filtering flask strainer 231 by pipeline 29 pass on filtering flask 23 bottle caps air inlet 232 again with collected specimens bottle 24 bottle caps on venthole 243 be communicated with by silicone tube 28; Set out pore 233 in addition on filtering flask 23 bottle caps, be communicated with bubble absorption tube 22 inlet ends 222 by silicone tube 28, the outlet end 223 of bubble absorption tube 22 connects test sample bottle 25.
Here, casing 21 is preferably vehicle-mounted standard semiconductor refrigeration case (commercially available), in the utility model, mainly adopts its function of temperature control, also can adopt other devices with same function; Bubble absorption tube 22 is the business-like patented product of applicant (referring to patent 200410058158.0), and sample bottle strainer 241 and filtering flask strainer 231 are commercially available product (new Asia, Shanghai purifies device factory); Test sample bottle 25 can be cylindric bottle with cover, and is provided with containing mark, is advisable with 10ml.
Utilize above checkout gear, and, can implement on-the-spot the detection hydrogen sulfide on oil drilling site in conjunction with detection method described below.
This detection method is by measuring with sulphion (S 2-) sulfide concentration of meter also obtains the hydrogen sulfide content of test sample.
The method principle: reducing substances and colorimetry-turbidity etc. are interference measurement all, and most of sample is by isolating H under acid condition 2S can eliminate interference.Sulfur dioxide in the testing sample drilling fluid, sulfide and barium chloride reaction generate the barium sulfite precipitation, and the free hydrogen sulfide in the solution does not react with barium chloride, from solution, dissociate out, thereby eliminated the interference of the hydrogen sulfide that sulfur dioxide and sulfide detects need.
BaCl 2+ Na 2SO 3-----BaSO 3(precipitation)+Nacl
At Fe 3+Exist down, to amino N, N dimethylaniline and S 2-Reaction generates methylene blue, and the chromogenic reaction formula is as follows:
Figure Y20082012374200071
In the utility model hydrogen sulfide detection method, need to use following reagent:
One: 1.0 milliliter of glacial acetic acid of hydrogen sulfide reagent, sodium acetate 0.6 gram, barium chloride 0.250 gram is loaded in the plastics square vase, is diluted with water to 50ml and mixes until dissolving fully.Hydrogen sulfide reagent one is used for filtering flask 23, uses 1ml at every turn, and its effect is to make sample and barium chloride reaction generate barium sulfite precipitation sulfur dioxide and other sulfide to remove interference measurement in the sample.
Hydrogen sulfide reagent two: A reagent-NaOH 3.0 grams are dissolved in 50 ml waters, and solid all is loaded in the plastics square vase after the dissolving; Cadmium sulfate 0.05 gram of B reagent-8 crystallization water and ammonium alcohol polyvinyl phosphate 0.10 gram.Getting the A reagent of 1ml and B reagent during use mixes in an empty bottle and adds water to the 10ml groove.Hydrogen sulfide reagent two is used for bubble absorption tube 22, uses 10ml at every turn.
Hydrogen sulfide reagent three: P-aminodimethylaniline hydrochloride 1.25 grams add 125 milliliters of the concentrated sulfuric acids, and water is settled to 250 milliliters then.Hydrogen sulfide reagent three is used for adding test sample as developer.
Hydrogen sulfide reagent four: ammonium ferric sulfate 31.25 grams add 6.25 milliliters of the concentrated sulfuric acids, and water is settled to 250 milliliters then.Hydrogen sulfide reagent four-function is adjusted the environment of chromogenic reaction in adding test sample.
After checkout gear and reagent is ready to, implement following operation:
Sample pre-treatments: use pre-treatment separator box 2.Load onto a certain amount of collection in worksite sample (space is left on collected specimens bottle 24 tops) in the collected specimens bottle 24, by intake interface 27 logical argon gas in pre-treatment separator box 2, (the adjustments of gas flow velocity also is stabilized in 2000 ml/min to argon gas through gas flowmeter 26 backs, ventilation and timing 10 minutes), lead in the collected specimens bottle 24 on the sample bottle strainer 241 by silicone tube, argon gas enters in the sample solution of collection, and the mist disengaging liquid level that carries in the collected specimens solution gathers collected specimens bottle 24 upper spaces, overflow from venthole 243, enter in the filtering flask 23 by silicone tube, enter hydrogen sulfide reagent one solution in the filtering flask 23 after coming out by filtering flask strainer 231, at this moment, hydrogen sulfide reagent one and the mist generation chemical reaction that enters in the filtering flask 23 have precipitation to generate; The gas effusion liquid level that chemical reaction does not take place in the filtering flask 23 gathers filtering flask 23 upper spaces, overflow from venthole 233, enter in the bubble absorption tube 22 by silicone tube 28, mix with the hydrogen sulfide reagent two in the plastics bubble absorption tube 22, obtain specimen solution after the concurrent biochemical reaction and be stored in the bubble absorption tube 22, put into cuvette by liquid outlet 223 during detection.
Sample detection: use detecting instrument 1.The cuvette that test sample solution at first will be housed is placed in the colorimetric pool 3, close colorimetric pool lid 13 then, opening power and light source/monochromator 33, the light transmission cuvette that light source/monochromator 33 sends is received by photoelectric detector 32, photoelectric detector 32 detected signals are passed to and are transferred to microprocessor 18, carry out data analysis by microprocessor 18 result is outputed on the display screen 11.
1, the preparation of test sample: get the blank bottle of 10ml and add 1 milliliter of hydrogen sulfide reagent two, and add the water benefit, mix (can use the ultrasonic wave assist in dissolving) and promptly get blank solution to 10 milliliters.
Pipette each 0.4 milliliter of hydrogen sulfide reagent three with pipettor and add respectively in 10ml test sample bottle and the blank bottle of 10ml, screw bottle cap, fluctuate 3 times, and then add hydrogen sulfide reagent four each 0.2 milliliter, screw bottle cap, fluctuate 3 times; Place at ambient temperature at last chromogenic reaction took place in 10 minutes.
2, colour developing-measuring operation
1). blank measure: take off the blank bottle cap of 10ml, with 3 milliliters of plastic suction pipes blank solution is sucked in the infrared quartz cuvette, clean the cuvette outer wall, cuvette is put into the instrument colorimetric pool, cover colorimetric pool lid 3, " measurement " project of selection is operated by the prompting of instrument, carries out blank sample and measures.
2). sample in measurement: take out cuvette, outwell blank solution, with small amount of sample solution rinse cuvette, with 3 milliliters of plastic suction pipes sample solution is transferred in the cuvette again, cuvette is put into the instrument colorimetric pool, cover colorimetric pool lid 3, option is operated by the prompting of instrument, draws the result of sample in measurement.
Though the utility model is described by previous embodiment, but still can change its form and details, make not breaking away under the spirit of the present utility model.Aforementioned is the most rational using method of the utility model, one of the mode that can specifically implement for the utility model only, but not as limit.

Claims (7)

1, a kind of hydrogen sulfide on oil drilling site checkout gear, comprise detecting instrument, it is characterized in that, also comprise a pre-treatment separator box, described pre-treatment separator box comprises a casing, be provided with argon gas intake interface, gas flowmeter, collected specimens bottle, filtering flask and bubble absorption tube successively by the air-flow trend in the casing, and gas circuit is communicated with by the multistage silicone tube in these accessories.
2, hydrogen sulfide on oil drilling site checkout gear as claimed in claim 1, it is characterized in that, described collected specimens bottle inner bottom part is established a sample bottle filter, the sample bottle strainer is communicated with by silicone tube with gas flowmeter by the air inlet that pipeline passes on the collected specimens bottle cap again, establishes a venthole on the collected specimens bottle cap in addition.
3, hydrogen sulfide on oil drilling site checkout gear as claimed in claim 1 or 2, it is characterized in that, described filtering flask inner bottom part is established a filtering flask strainer, the filtering flask strainer by pipeline pass on the filtering flask bottle cap air inlet again with the collected specimens bottle cap on venthole be communicated with by silicone tube, set out pore on the filtering flask bottle cap in addition.
4, hydrogen sulfide on oil drilling site checkout gear as claimed in claim 3 is characterized in that, the venthole on the filtering flask bottle cap is communicated with bubble absorption tube inlet end by silicone tube, and the bubble absorption tube is also established outlet end.
5, hydrogen sulfide on oil drilling site checkout gear as claimed in claim 1 or 2 is characterized in that, described detecting instrument is a miniaturization colorimetric detection instrument.
6, hydrogen sulfide on oil drilling site checkout gear as claimed in claim 5 is characterized in that, the colorimetric detection instrument is provided with casing, is provided with the colorimetric pool lid at the upper surface of casing, and colorimetric pool lid lower room is provided with colorimetric pool.
7, hydrogen sulfide on oil drilling site checkout gear as claimed in claim 6, it is characterized in that, wherein said colorimetric pool is the rectangle cell body of a upper surface opening, and a side end face of colorimetric pool is provided with the super bright light emitting diode of 630nm, connects corresponding opposite side end face and is provided with photoelectric sensor; A colorimetric pool medial launder body space and a cuvette are complementary.
CNU2008201237423U 2008-11-18 2008-11-18 Device for detecting hydrogen sulfide on oil drilling spot Expired - Lifetime CN201321856Y (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106596902A (en) * 2017-01-20 2017-04-26 上海出入境检验检疫局工业品与原材料检测技术中心 Portable full-automatic apparatus for testing hydrogen sulfide in petroleum products
CN114577793A (en) * 2022-05-07 2022-06-03 北京大学 Multi-scene hydrogen sulfide gas content online monitoring method and monitoring device

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106596902A (en) * 2017-01-20 2017-04-26 上海出入境检验检疫局工业品与原材料检测技术中心 Portable full-automatic apparatus for testing hydrogen sulfide in petroleum products
CN106596902B (en) * 2017-01-20 2023-01-20 上海海关工业品与原材料检测技术中心 Portable full-automatic petroleum product hydrogen sulfide tester
CN114577793A (en) * 2022-05-07 2022-06-03 北京大学 Multi-scene hydrogen sulfide gas content online monitoring method and monitoring device

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