CN108318550A - The detection device and detection method of hydrogen sulfide in a kind of fluid oil - Google Patents
The detection device and detection method of hydrogen sulfide in a kind of fluid oil Download PDFInfo
- Publication number
- CN108318550A CN108318550A CN201711440086.XA CN201711440086A CN108318550A CN 108318550 A CN108318550 A CN 108318550A CN 201711440086 A CN201711440086 A CN 201711440086A CN 108318550 A CN108318550 A CN 108318550A
- Authority
- CN
- China
- Prior art keywords
- gas
- sample
- processing tube
- sample processing
- hydrogen sulfide
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/26—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/34—Purifying; Cleaning
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/42—Low-temperature sample treatment, e.g. cryofixation
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/44—Sample treatment involving radiation, e.g. heat
Landscapes
- Life Sciences & Earth Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Pathology (AREA)
- General Physics & Mathematics (AREA)
- Physics & Mathematics (AREA)
- Immunology (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- Molecular Biology (AREA)
- Biomedical Technology (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
- Separation Using Semi-Permeable Membranes (AREA)
- Sampling And Sample Adjustment (AREA)
Abstract
The invention discloses a kind of detection devices of hydrogen sulfide in fluid oil, including are sequentially connected gas purification supply unit, sample treatment unit, sample purification unit and the electrochemical detector of setting；Gas purification supply unit includes adjustable gas flowmeter, silica dehydrator pipe and the oil-free diaphragm vacuum pump being sequentially communicated by the road；Sample treatment unit includes sample processing tube and first gas surge flask, and sample processing tube is placed in a heating mantle, and the both ends of sample processing tube are connected in parallel to standby gas branch；Sample purification unit includes liquid elution vial, second gas surge flask, solid elution vial and the second filter membrane group, and liquid elution vial, second gas surge flask and solid elution vial are placed in a cryostat bottle, and electrochemical detector is electrochemical detector.The present invention meets the detection needs of hydrogen sulfide in fluid oil, and can effectively remove influence of other sulphur-containing substances to testing result, and detection work can be rapidly completed and improve the precision of testing result.
Description
Technical field
The invention belongs to technical field of chemical detection, the detection device of hydrogen sulfide and detection in specifically a kind of fluid oil
Method.
Background technology
Hydrogen sulfide be sulphur hydride in simplest one kind.H when room temperature2S is a kind of colourless play for having rotten egg smell
Poisonous gas should be used in ventilation and must take safeguard procedures.It belongs to sucking health hazard, is strong Nervous toxicity
Element has an intense stimulus effect to mucous membrane, and when low content is easily felt by human hair, but baryodmia can be made one in high-content, such as dense
It spends under 150 ppm, smell is lost in 2-5 minutes, is such as withdrawn not in time, it will soon be fatal.Hydrogen sulfide is widely present in original
Oil and oil product among, the hydrogen sulfide in crude oil is that its own contains, the hydrogen sulfide in oil product in addition in raw material from
Further include the hydrogen sulfide generated as by-product in production except body contains.Therefore, for safety and environmental protection, it is necessary to accurate
Ground measures the hydrogen sulfide content in Crude Oil ＆ Petroleum Products, and is effectively removed to it, so that its content is reduced to safety dense
Below degree.
Due to the complexity of production and the diversity of product, the sulphur-containing substance in oil product includes many types, variety classes
Oil product in sulfide type and content it is also variant, generally comprise elemental sulfur, hydrogen sulfide, mercaptan, thioether, polythiaether,
Epithio ether, thiophene etc..The existing method for measuring hydrogen sulfide has：Iodimetric titration, methylene blue laws, lead acetate reaction rate method, gas
Phase chromatography, detection pipe are than regular way etc..Iodimetric titration is the chemical analysis method of classics, and different hydrogen sulfide sampling amounts can be used,
The section of measurement is larger, but the operation of iodimetric titration is complex, needs pure manual operations, and testing result poor repeatability, detection
Precision is not high, is suitable for purer gas.Methylene blue laws smaller scope of application is 0~25 mgm-3, the method is to sulphur
Change the more stable purified natural gas of hydrogen mass concentration to be more suitble to.Although the measurement result of chromatogram column technique is more accurate, color
Spectrometry has higher requirement to detector, Standard Gases and sampling technique, and needs to purchase dedicated gas-chromatography instrument, input
It is higher.Detection pipe also has the problem identical as iodimetric titration than regular way.Most of existing sulfurated hydrogen detection methods are all detection gaseous states
The method of hydrogen sulfide, most methods are not all suitable for the detection of hydrogen sulfide content in liquid, and even modification uses, by hydrogen sulfide
Stripping out detects, and therefore, how simply sulfur-containing impurities gas is also very big to the detection interference of hydrogen sulfide in some complex samples,
It is quickly detected from liquid phase hydrogen sulfide content, various impurity interference is excluded, especially detects the hydrogen sulfide in liquid complex sample
Content is always the direction that detection method is formulated and instrument and equipment is researched and developed.
Invention content
The technical problem to be solved by the present invention is to：In view of the deficiencies of the prior art, it provides and vulcanizes in a kind of fluid oil
The detection device and detection method of hydrogen, meet the detection needs of hydrogen sulfide in fluid oil, and can effectively remove other sulfur-bearing objects
The influence of confrontation testing result can be rapidly completed detection work and improve the precision of testing result.
Technical solution is used by the present invention solves above-mentioned technical problem：The detection dress of hydrogen sulfide in a kind of fluid oil
It sets, including is sequentially connected gas purification supply unit, sample treatment unit, sample purification unit and the Electrochemical Detection of setting
Device；The gas purification supply unit includes adjustable gas flowmeter, silica dehydrator pipe and the oil-free being sequentially communicated by the road
The arrival end of vacuum diaphragm pump, the adjustable gas flowmeter is equipped with pneumatic filter, the oil-free diaphragm vacuum pump
Outlet end the first filter membrane group is installed；The sample treatment unit includes sample processing tube and first gas surge flask, institute
Filled with no sulphur higher boiling diluent in the sample processing tube stated, three hole of polytetrafluoroethylene (PTFE) is plugged in the sample processing tube
Plug, the sample processing tube are placed in a heating mantle, and the first filter membrane group is arranged in the oil-free diaphragm vacuum pump
Outlet end and the entrance of the sample processing tube between, the outlet of the sample processing tube and the first gas are slow
The entrance for rushing bottle communicates, and the both ends of the sample processing tube are connected in parallel to standby gas branch, the standby gas branch
The both ends on road are communicated with the entrance and exit of the sample processing tube respectively, and the both ends of the standby gas branch are pacified respectively
Equipped with solenoid valve；The sample purification unit include filled with the liquid elution vial of liquid eluent, second gas surge flask,
Solid elution vial filled with solid-state eluent and the second filter membrane group, the entrance of the liquid elution vial and first gas
The outlet of body surge flask communicates, and the outlet of the liquid elution vial is communicated with the entrance of the second gas surge flask, institute
The outlet for the second gas surge flask stated is communicated with the entrance of the solid elution vial, the liquid elution vial, the second gas
Body surge flask and solid elution vial are placed in a cryostat bottle, outlet and the electrochemical detector of the solid elution vial
Air inlet communicate, the second filter membrane group is mounted on the outlet of the solid elution vial and the electrochemical detector
Air inlet between, the electrochemical detector be electrochemical detector.
The structure of the detecting device of hydrogen sulfide is simple in fluid oil of the present invention, at low cost, and detection efficiency is high, operability
By force.The detection device purges device by gas purification supply unit, and to enter device carrier gas be dusted and
Dehumidifying.The effect of dedusting is to prevent dust from entering device with carrier gas, avoids dust that oil-free diaphragm vacuum pump and electrochemistry is caused to be examined
Device failure is surveyed, testing result deviation is caused；The effect of dehumidifying is to ensure carrier gas drying, is avoided because of moisture and hydrogen sulfide dissolving adherency
Testing result caused by the gas circuit of device is relatively low and parallel misalignment.The effect of sample treatment unit is to liquid sample
It is handled, so that hydrogen sulfide is detached with other most of sulphur-containing substances and organic matter, the hydrogen sulfide in liquid sample is quickly blown
It takes off, stripping gas carries out separating-purifying again by sample purification unit again, rejects remaining unvulcanised hydrogen substance, avoids sulfur-bearing
Influence of the substance to testing result improves accuracy and repdocutbility to sulfurated hydrogen detection in fluid oil.
Preferably, the pneumatic filter is fabric filter, if the first filter membrane group is filtered by dried layer nylon
Film forms, if the second filter membrane group is made of dried layer glass fiber filter, the heating mantle is asbestos heating mantle.
Further, the aperture of the nylon leaching film described in every layer is 5 μm or less.
Preferably, the arrival end of the pneumatic filter is connected with the elution vial equipped with acetic acid lead solution by the road,
It is the hydrogen sulfide gas and gas sulfur substance removed in carrier gas that it, which is acted on, further increases sulfurated hydrogen detection knot in fluid oil
The precision of fruit.
Preferably, the no sulphur higher boiling diluent is no sulphur atoleine, the liquid eluent is through nothing
The normal octane of water calcium chloride dehydration, the solid-state eluent are the clinoptilolite powder of 300 mesh handled by high-temperature activation.
A kind of detection method detecting hydrogen sulfide in fluid oil by above-mentioned detection device, includes the following steps：
（1）It is switched on, gas in emptier, then cryostat bottle is cooled to -22~-18 DEG C, heating mantle is warming up to 58~65
DEG C, oil-free diaphragm vacuum pump work, the flow of adjusting adjustable gas flowmeter is to 380~420 mL/min, after steady air current,
Device is purged by gas purification supply unit, and the carrier gas for entering device is dusted and is dehumidified, ensures carrier gas
It is clean, dry；
（2）After the detection voltage stabilization of electrochemical detector, and after cryostat bottle and jacket temperature stabilization, open standby gas
The solenoid valve at branch both ends, standby gas branch are opened, and gas does not circulate in sample processing tube, is loaded in advance in sample processing tube
There are 20 mL without sulphur higher boiling diluent, the sample of 5 mL fluid oils is measured by Subtraction method, by sample through polytetrafluoroethylene (PTFE) three
In the injection port injection sample processing tube of hole beyond the Great Wall, injection port is stoppered immediately, waits for 3~5 minutes, waits for the temperature of sample processing tube
After stabilization, sample data is inputted into electrochemical detector, the solenoid valve at turning off standby gas branch both ends, standby gas branch closes
It closes, gas circuit switches to sample cell branch, and gas circulates in sample processing tube, opens the detection switch of electrochemical detector, electrification
Detector is learned to start to work；
（3）Be heated while electrochemical detector works, in sample processing tube and the hydrogen sulfide after air stripping and other contain
Sulfur material and low-boiling organic matter are blown out together with carrier gas, and liquid elution vial is entered after first gas surge flask ,-
At a temperature of 22~-18 DEG C of cryostat, most of organic matter from sample processing tube is condensed and stays in liquid elution vial,
Other most of sulphur-containing substances are cooled and dissolved by the liquid eluent in liquid elution vial, hydrogen sulfide and minimal amount of organic
Object and minimal amount of sulphur-containing substance enter solid elution vial with carrier gas through second gas surge flask, in solid elution vial, mixing
Gas is cleaned again, and solid-state eluent adsorbs unvulcanised hydrogen substance, and hereafter, mixed gas is solid through the filtering removal of the second filter membrane group
After entering electrochemical detector after body particle, detected to obtain hydrogen sulfide content by electrochemical detector.
Compared with the prior art, the advantages of the present invention are as follows：The detection dress of hydrogen sulfide in fluid oil disclosed by the invention
Simple in structure, at low cost, detection efficiency height is set, operability is strong.The detection device is by gas purification supply unit to device
It is purged, and the carrier gas for entering device is dusted and is dehumidified, the effect of sample treatment unit is carried out to liquid sample
Processing makes hydrogen sulfide be detached with other most of sulphur-containing substances and organic matter, the quick stripping of hydrogen sulfide in liquid sample is gone out
Come, stripping gas carries out separating-purifying again by sample purification unit again, rejects remaining unvulcanised hydrogen substance, avoids sulphur-containing substance
Influence to testing result improves accuracy and repdocutbility to sulfurated hydrogen detection in fluid oil.Liquid disclosed by the invention
The detection device and detection method of hydrogen sulfide in oil product meet the detection needs of hydrogen sulfide in fluid oil, and can effectively remove it
His influence of the sulphur-containing substance to testing result, can be rapidly completed detection work and improve the precision of testing result.
Description of the drawings
Fig. 1 is the structure connection diagram of detection device in embodiment.
Specific implementation mode
Below in conjunction with attached drawing embodiment, present invention is further described in detail.
The detection device of hydrogen sulfide in the fluid oil of embodiment, as shown in Figure 1, net including the gas for being sequentially connected setting
Change supply unit 1, sample treatment unit 2, sample purification unit 3 and electrochemical detector 4；Gas purification supply unit 1 includes
Adjustable gas flowmeter 11, silica dehydrator pipe 12 and the oil-free diaphragm vacuum pump 13 being sequentially communicated by the road, adjustable gas flow
The arrival end of meter 11 is equipped with pneumatic filter 14, and the outlet end of oil-free diaphragm vacuum pump 13 is equipped with the first filter membrane group 15；Sample
Product processing unit 2 includes sample processing tube 21 and first gas surge flask 22, and sample processing tube 21 is interior filled with no sulphur higher boiling
Diluent is plugged with three stopple 23 of polytetrafluoroethylene (PTFE) in sample processing tube 21, and sample processing tube 21 is placed in a heating mantle 24, and first
Filter membrane group 15 is arranged between the outlet end of oil-free diaphragm vacuum pump 13 and the entrance of sample processing tube 21, sample processing tube 21
Outlet is communicated with the entrance of first gas surge flask 22, and the both ends of sample processing tube 21 are connected in parallel to standby gas branch 5, wait for
The both ends of machine gas branch 5 are communicated with the entrance and exit of sample processing tube 21 respectively, and the both ends of standby gas branch 5 are pacified respectively
Equipped with solenoid valve 51；Sample purification unit 3 includes the liquid elution vial 31 for being filled with liquid eluent, second gas surge flask
32, the solid elution vial 33 filled with solid-state eluent and the second filter membrane group 34, the entrance and first gas of liquid elution vial 31
The outlet of surge flask 22 communicates, and the outlet of liquid elution vial 31 is communicated with the entrance of second gas surge flask 32, and second gas is slow
The outlet for rushing bottle 32 is communicated with the entrance of solid elution vial 33, liquid elution vial 31, second gas surge flask 32 and solid elution
Bottle 33 is placed in a cryostat bottle 35, and the outlet of solid elution vial 33 is communicated with the air inlet of electrochemical detector 4, the second filter membrane group
34 are mounted between the outlet and the air inlet of electrochemical detector 4 of solid elution vial 33, and electrochemical detector 4 is examined for electrochemistry
Survey device 4.
No sulphur higher boiling diluent can accelerate stripping and the precipitation of hydrogen sulfide, in the present embodiment, no sulphur higher boiling diluent
For no sulphur atoleine；Liquid eluent is the normal octane being dehydrated through anhydrous calcium chloride；Solid-state eluent is 300 mesh through excessively high
The clinoptilolite powder of warm activation process；Pneumatic filter 14 is cocoanut active charcoal crude fibre filter；First filter membrane group 15 is by two
Layer nylon leaching film 16 forms, and the aperture of every layer of nylon leaching film 16 is 5 μm or less；Second filter membrane group 34 is filtered by layer glass fiber
Film 36 forms；Heating mantle 24 is asbestos heating mantle.
Since the detection of hydrogen sulfide is affected by other sulfur-containing impurities gases, while again due to the physics and chemistry of hydrogen sulfide spy
Different property should all pass through processing for the transfer pipeline of detection equipment and hydrogen sulfide, avoid humidity and being passivated be handled, in order to avoid
Hydrogen sulfide remains, and influences testing result.Therefore it is all have hydrogen sulfide by pipeline all use polytetrafluoroethylene (PTFE) material, container is also all
For glass container.
First gas surge flask 22 works as a buffer, and no sulphur higher boiling diluent is avoided to be blown in liquid elution vial 31；Liquid
Body elution vial 31 rejects other most of sulphur-containing substances and organic matter to elute the gas after purification sample stripping；Second gas
Body surge flask 32 is to buffer, in case liquid eluent is blown to solid elution vial 33 and influences elution effect；Second filter membrane group 34 is used
To filter the impurity such as dust and solid elution vial molecule in gas circuit again, avoids it from entering electrochemical detector 4, influence to examine
It surveys.
Electrochemical detector 4 uses the prior art, should be calibrated before the use using standard hydrogen sulfide gas, surveys
It is scheduled on detector voltage value under unloaded and certain concentration of hydrogen sulfide, and then obtains concentration and the linear relationship of voltage, in practical inspection
When survey, according to voltage versus time curve under fixed flow velocity, integrating meter calculates after hydrogen sulfide total amount divided by sample quality
Obtain the content of hydrogen sulfide.
In practical applications, washing equipped with acetic acid lead solution can also be connected by the road in the arrival end of pneumatic filter 14
Carry bottle（It is not shown in figure）, effect is the hydrogen sulfide gas and gas sulfur substance removed in carrier gas, further increases liquid
The precision of hydrogen sulfide in oil product testing result.
The detection method that hydrogen sulfide in fluid oil is detected by the detection device of above-described embodiment, includes the following steps：
（1）It is switched on, gas in emptier, then cryostat bottle 35 is cooled to -20 DEG C, heating mantle 24 is warming up to 60 DEG C, nothing
Oily vacuum diaphragm pump 13 works, and adjusts the flow of adjustable gas flowmeter 11 to 400 mL/min, after steady air current, passes through gas
Body purification supply unit 1 purges device, and the carrier gas for entering device is dusted and is dehumidified, guarantee carrier gas cleaning,
It is dry；
（2）After the detection voltage stabilization of electrochemical detector 4 is within 10 mV, and cryostat bottle 35 and 24 temperature of heating mantle are steady
After fixed, the solenoid valve 51 at standby 5 both ends of gas branch is opened, standby gas branch 5 is opened, and gas does not flow in sample processing tube 21
It is logical, 20 mL are filled in sample processing tube 21 in advance without sulphur higher boiling diluent, 5 mL are measured by Subtraction method（About 4 g, essence
Really to 0.01 g）Sample is injected sample processing tube by the sample of fluid oil through the injection port on three stopple 23 of polytetrafluoroethylene (PTFE)
In 21, injection port is stoppered immediately, since the temperature of sample processing tube 21 after injection sample can decline, is waited for 3~5 minutes,
After the temperature of sample processing tube 21 is stablized, sample data is inputted into electrochemical detector 4,5 both ends of turning off standby gas branch
Solenoid valve 51, standby gas branch 5 closes, and gas circuit switches to sample cell branch, and gas circulation in sample processing tube 21 is opened
The detection switch of electrochemical detector 4, electrochemical detector 4 are started to work；
（3）While electrochemical detector 4 works, the temperature of sample processing tube 21 is maintained at 60 DEG C, at such a temperature, liquid
The gaseous matter of the sulfur-bearings such as hydrogen sulfide, methyl mercaptan, ethyl mercaptan, methyl sulfide in oil product volatilizees and overflows, in sample processing tube 21
The heated and hydrogen sulfide after air stripping and other sulphur-containing substances and low-boiling organic matter are blown out together with carrier gas, are passed through
Enter liquid elution vial 31 after first gas surge flask 22, at a temperature of -20 DEG C of cryostat, outside vulcanisation hydrogen, at sample
Most of organic matter of reason pipe 21 is condensed and stays in liquid elution vial 31, other most of sulphur-containing substances are cooled and by liquid
Liquid eluent dissolving in body elution vial 31, hydrogen sulfide and minimal amount of organic matter and minimal amount of sulphur-containing substance are passed through with carrier gas
Second gas surge flask 32 enters solid elution vial 33, and in solid elution vial 33, mixed gas is cleaned again, solid-state elution
Unvulcanised hydrogen substance is adsorbed in agent, and hereafter, mixed gas enters electrochemistry after the second filter membrane group 34 filters removal solid particle and examines
After surveying device 4, hydrogen sulfide content is obtained by the detection of electrochemical detector 4.
Claims (6)
1. the detection device of hydrogen sulfide in a kind of fluid oil, it is characterised in that：Gas purification including being sequentially connected setting is defeated
Send unit, sample treatment unit, sample purification unit and electrochemical detector；The gas purification supply unit includes through pipe
Adjustable gas flowmeter, silica dehydrator pipe and the oil-free diaphragm vacuum pump that road is sequentially communicated, the adjustable gas flowmeter
Arrival end is equipped with pneumatic filter, and the outlet end of the oil-free diaphragm vacuum pump is equipped with the first filter membrane group；The sample
Product processing unit includes sample processing tube and first gas surge flask, and the sample processing tube is interior dilute filled with no sulphur higher boiling
Agent is released, three stopple of polytetrafluoroethylene (PTFE) is plugged in the sample processing tube, the sample processing tube is placed in a heating mantle, institute
The the first filter membrane group stated is arranged between the outlet end of the oil-free diaphragm vacuum pump and the entrance of the sample processing tube,
The outlet of the sample processing tube is communicated with the entrance of the first gas surge flask, the both ends of the sample processing tube
Be connected in parallel to standby gas branch, the both ends of the standby gas branch respectively with the entrance of the sample processing tube and
Outlet communicates, and the both ends of the standby gas branch are separately installed with solenoid valve；The sample purification unit includes filling
There are the liquid elution vial of liquid eluent, second gas surge flask, filtered filled with the solid elution vial of solid-state eluent and second
Film group, the entrance of the liquid elution vial are communicated with the outlet of the first gas surge flask, the liquid elution vial
Outlet communicated with the entrance of the second gas surge flask, outlet and the solid of the second gas surge flask
The entrance of elution vial communicates, and the liquid elution vial, second gas surge flask and solid elution vial are placed in a cryostat bottle, institute
The outlet for the solid elution vial stated is communicated with the air inlet of the electrochemical detector, and the second filter membrane group is mounted on institute
Between the outlet for the solid elution vial stated and the air inlet of the electrochemical detector, the electrochemical detector is electrification
Learn detector.
2. the detection device of hydrogen sulfide in a kind of fluid oil according to claim 1, it is characterised in that：The gas
Filter is fabric filter, if the first filter membrane group is made of dried layer nylon leaching film, if the second filter membrane group by
Dried layer glass fiber filter forms, and the heating mantle is asbestos heating mantle.
3. the detection device of hydrogen sulfide in a kind of fluid oil according to claim 2, it is characterised in that：Described in every layer
The aperture of nylon leaching film is 5 μm or less.
4. the detection device of hydrogen sulfide in a kind of fluid oil according to claim 1, it is characterised in that：The gas
The arrival end of filter is connected with the elution vial equipped with acetic acid lead solution by the road.
5. the detection device of hydrogen sulfide in a kind of fluid oil according to claim 1, it is characterised in that：It is described without sulphur
Higher boiling diluent is no sulphur atoleine, and the liquid eluent is the normal octane being dehydrated through anhydrous calcium chloride, described
Solid-state eluent is the clinoptilolite powder of 300 mesh handled by high-temperature activation.
6. a kind of detection device by described in any one of claim 1-5 detects the detection side of hydrogen sulfide in fluid oil
Method, which is characterized in that include the following steps：
（1）It is switched on, gas in emptier, then cryostat bottle is cooled to -22~-18 DEG C, heating mantle is warming up to 58~65
DEG C, oil-free diaphragm vacuum pump work, the flow of adjusting adjustable gas flowmeter is to 380~420 mL/min, after steady air current,
Device is purged by gas purification supply unit, and the carrier gas for entering device is dusted and is dehumidified, ensures carrier gas
It is clean, dry；
（2）After the detection voltage stabilization of electrochemical detector, and after cryostat bottle and jacket temperature stabilization, open standby gas
The solenoid valve at branch both ends, standby gas branch are opened, and gas does not circulate in sample processing tube, is loaded in advance in sample processing tube
There are 20 mL without sulphur higher boiling diluent, the sample of 5 mL fluid oils is measured by Subtraction method, by sample through polytetrafluoroethylene (PTFE) three
In the injection port injection sample processing tube of hole beyond the Great Wall, injection port is stoppered immediately, waits for 3~5 minutes, waits for the temperature of sample processing tube
After stabilization, sample data is inputted into electrochemical detector, the solenoid valve at turning off standby gas branch both ends, standby gas branch closes
It closes, gas circuit switches to sample cell branch, and gas circulates in sample processing tube, opens the detection switch of electrochemical detector, electrification
Detector is learned to start to work；
（3）Be heated while electrochemical detector works, in sample processing tube and the hydrogen sulfide after air stripping and other contain
Sulfur material and low-boiling organic matter are blown out together with carrier gas, and liquid elution vial is entered after first gas surge flask ,-
At a temperature of 22~-18 DEG C of cryostat, most of organic matter from sample processing tube is condensed and stays in liquid elution vial,
Other most of sulphur-containing substances are cooled and dissolved by the liquid eluent in liquid elution vial, hydrogen sulfide and minimal amount of organic
Object and minimal amount of sulphur-containing substance enter solid elution vial with carrier gas through second gas surge flask, in solid elution vial, mixing
Gas is cleaned again, and solid-state eluent adsorbs unvulcanised hydrogen substance, and hereafter, mixed gas is solid through the filtering removal of the second filter membrane group
After entering electrochemical detector after body particle, detected to obtain hydrogen sulfide content by electrochemical detector.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711440086.XA CN108318550B (en) | 2017-12-27 | 2017-12-27 | Detection device and detection method for hydrogen sulfide in liquid oil product |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711440086.XA CN108318550B (en) | 2017-12-27 | 2017-12-27 | Detection device and detection method for hydrogen sulfide in liquid oil product |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN108318550A true CN108318550A (en) | 2018-07-24 |
| CN108318550B CN108318550B (en) | 2020-05-12 |
Family
ID=62892915
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201711440086.XA Expired - Fee Related CN108318550B (en) | 2017-12-27 | 2017-12-27 | Detection device and detection method for hydrogen sulfide in liquid oil product |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN108318550B (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112710812A (en) * | 2020-11-17 | 2021-04-27 | 中国石油天然气股份有限公司 | Integrated process for detecting and treating toxic gas in crude oil produced by oil field |
| CN114509476A (en) * | 2020-11-16 | 2022-05-17 | 中国石油化工股份有限公司 | System and method for sampling mixed-phase produced fluid of heavy oil well and detecting content of hydrogen sulfide |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101718741A (en) * | 2009-11-17 | 2010-06-02 | 中国海洋石油总公司 | Method and device for absorbing dissolved hydrogen sulfide in liquid |
| RU2426985C1 (en) * | 2010-05-07 | 2011-08-20 | Федеральное государственное автономное образовательное учреждение высшего профессионального образования "Сибирский федеральный университет" (ФГАОУ ВПО СФУ) | Procedure for determination of contents of hydrogen sulphide and light mercaptans in oil |
| CN102455294A (en) * | 2010-10-22 | 2012-05-16 | 中国石油化工股份有限公司 | Detection device, and detection method for hydrogen sulfide in oil product |
| CN102455299A (en) * | 2010-10-22 | 2012-05-16 | 中国石油化工股份有限公司 | Detection device and detection method of hydrogen sulfide in oil product |
| RU2608852C1 (en) * | 2015-10-26 | 2017-01-25 | Ильдар Зафирович Денисламов | Method for determining concentration of hydrogen sulphide in pipeline oil under pressure |
-
2017
- 2017-12-27 CN CN201711440086.XA patent/CN108318550B/en not_active Expired - Fee Related
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101718741A (en) * | 2009-11-17 | 2010-06-02 | 中国海洋石油总公司 | Method and device for absorbing dissolved hydrogen sulfide in liquid |
| RU2426985C1 (en) * | 2010-05-07 | 2011-08-20 | Федеральное государственное автономное образовательное учреждение высшего профессионального образования "Сибирский федеральный университет" (ФГАОУ ВПО СФУ) | Procedure for determination of contents of hydrogen sulphide and light mercaptans in oil |
| CN102455294A (en) * | 2010-10-22 | 2012-05-16 | 中国石油化工股份有限公司 | Detection device, and detection method for hydrogen sulfide in oil product |
| CN102455299A (en) * | 2010-10-22 | 2012-05-16 | 中国石油化工股份有限公司 | Detection device and detection method of hydrogen sulfide in oil product |
| RU2608852C1 (en) * | 2015-10-26 | 2017-01-25 | Ильдар Зафирович Денисламов | Method for determining concentration of hydrogen sulphide in pipeline oil under pressure |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114509476A (en) * | 2020-11-16 | 2022-05-17 | 中国石油化工股份有限公司 | System and method for sampling mixed-phase produced fluid of heavy oil well and detecting content of hydrogen sulfide |
| CN112710812A (en) * | 2020-11-17 | 2021-04-27 | 中国石油天然气股份有限公司 | Integrated process for detecting and treating toxic gas in crude oil produced by oil field |
| CN112710812B (en) * | 2020-11-17 | 2023-02-24 | 中国石油天然气股份有限公司 | Integrated process for detecting and treating toxic gas in crude oil produced by oil field |
Also Published As
| Publication number | Publication date |
|---|---|
| CN108318550B (en) | 2020-05-12 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN205333581U (en) | Be applicable to continuous detecting system of VOCs in wet flue gas of stationary source | |
| CN104483423B (en) | Sample collection and thermal desorption sampling device and method and trace detection equipment | |
| DE102015226806B4 (en) | Sample feeding device | |
| Taylor et al. | Trace-level automated mercury speciation analysis | |
| CN106461592B (en) | Gas component concentration measuring apparatus and method for measuring gas component concentration | |
| CN205538861U (en) | Volatile organic compounds on -line monitoring system | |
| CN108318550A (en) | The detection device and detection method of hydrogen sulfide in a kind of fluid oil | |
| CN106501431B (en) | A kind of method of Polychlorinated biphenyls in post detection dairy products using silica gel chromatograph | |
| CN202676680U (en) | Device capable of detecting low-concentration freon in seawater | |
| CN102359896A (en) | Sample collection device for polycyclic aromatic hydrocarbon pollutants in individual exposure air and analysis and evaluation method for pollutants | |
| CN107607644B (en) | A kind of chromatographic column of modified high-molecular porous microsphere and preparation method thereof and measurement sulfur hexafluoride decomposition product | |
| CZ181093A3 (en) | Apparatus for taking samples and their treatment | |
| US20230358714A1 (en) | Gas sensor | |
| WO2016052914A1 (en) | Real-time automatic analysis device for organic contaminant in water | |
| CN203745446U (en) | Flue gas detection device | |
| CN108344616A (en) | Coal gas on-line analysis pretreatment system and method | |
| CN208314002U (en) | A kind of positive pressure explosion-proof type VOCs monitoring system | |
| CN207408359U (en) | External renewable formula the drying plant of carrier gas in a kind of gas chromatograph examination | |
| KR20200065439A (en) | sensor-type chromatograph analysis apparatus | |
| KR100830953B1 (en) | Apparatus and method for measuring mercury content of a sample | |
| CN207923575U (en) | A kind of PID gas detectors are used for the gas handling system of VOC detections | |
| CN106770261A (en) | A kind of kit for water sample lead field quick detection | |
| CN206387612U (en) | A kind of device for power plant sulfur dioxide concentration Site Detection | |
| CN110006730A (en) | A kind of coal gas on-line analysis pretreatment unit and its preprocess method | |
| CN203745274U (en) | Solvent desorption device |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| TA01 | Transfer of patent application right |
Effective date of registration: 20200403 Address after: 315000, 9 Ma Yuan Road, Haishu District, Zhejiang, Ningbo Applicant after: Cheng Shigang Address before: 315812 109 Binhai Road, Daxie Development Area, Beilun District, Ningbo, Zhejiang Applicant before: DAXIE ENTRY-EXIT INSPECTION AND QUARANTINE BUREAU OF P.R.C. |
|
| TA01 | Transfer of patent application right | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20200512 Termination date: 20201227 |
|
| CF01 | Termination of patent right due to non-payment of annual fee |