CN106198108B - The method for quantitatively determining and dedicated unit of active sulfur in a kind of insulating oil - Google Patents
The method for quantitatively determining and dedicated unit of active sulfur in a kind of insulating oil Download PDFInfo
- Publication number
- CN106198108B CN106198108B CN201610571742.9A CN201610571742A CN106198108B CN 106198108 B CN106198108 B CN 106198108B CN 201610571742 A CN201610571742 A CN 201610571742A CN 106198108 B CN106198108 B CN 106198108B
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- oil
- sampler
- silver
- sample
- oily suspension
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Classifications
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/02—Devices for withdrawing samples
- G01N1/10—Devices for withdrawing samples in the liquid or fluent state
- G01N1/14—Suction devices, e.g. pumps; Ejector devices
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
- G01N21/64—Fluorescence; Phosphorescence
Abstract
The invention discloses the method for quantitatively determining and dedicated unit of active sulfur in a kind of insulating oil.Method for quantitatively determining is using silver --- after oily suspension and insulating oil constant temperature, timing, oscillating reactions, with ultraviolet fluorescence method quantitative assay.Dedicated unit includes sampler, silver --- oily suspension preparation and save set, constant temperature oscillation reactor.Sampler realizes sample collector and reactor integration, without shifting insulation oil samples, sampling and detection process is isolated with outside air, guarantees the accuracy of testing result.Sampler is provided with multichannel sealed valve, and there is sole operation long handle to be directed toward sealed end, simple and convenient.Oily suspension, air-isolation save and quantify output silver --- oily suspension preparation and save set can facilitate preparation silver ---.
Description
Technical field:
The present invention relates to the method for quantitatively determining and dress of active sulfur in a kind of measuring method more particularly to a kind of insulating oil
It sets.
Background technique:
Insulating oil is the important dielectric of oil-filled electric equipment, and the active sulfur in oil can be golden with transformer winding etc.
Category material, which reacts, generates Cu2S deposition, influences the partial discharge performance of insulation, and the electrical equipments service life such as transformer is caused to contract
It is short, seriously affect the safe operation of equipment.
Currently, active sulfur mostly uses greatly the qualitative checking methods such as copper sheet or gas chromatography to measure oil in detection insulating oil
In benzyl disulfide ingredient, accuracy is not high, while oily sample is contacted with air in detection process, and substance to be detected can be with sky
Ingredient reaction in gas, it is accurately fixed to influence testing result.
Summary of the invention:
One kind is provided and can be realized insulating oil sampling, inspection it is an object of the invention to overcome the shortcomings of above-mentioned prior art
Survey the quantitative survey that overall process completely cuts off active sulfur in the insulating oil that air impact, testing result are accurate, detection is simple and convenient
Determine method.
The purpose of the present invention can be reached by following measure: the quantitative determination side of active sulfur in a kind of insulating oil
Method comprising following steps:
One, sample acquires:
Using active sulfur samplers sample operation insulation oil samples in special isolation oil, specific sample collection method is such as
Under:
1. the oil discharge outlet for running dissolved gases in insulating oil analytical sampling device, thief hatch are clamped by hose coupling respectively
Hose, the hose for connecting oil discharge outlet connect catch of used oil, and the hose for connecting thief hatch connects insulating oil Sampler valves；
2. unique long handle of control multichannel sealed valve is threaded at sample introduction fast interface, sample introduction fast interface is isolated,
Insulating oil Sampler valves are opened, by thief hatch, oil discharge outlet draining provisions dead angle and the dead oil of fuel outlet valve is to catch of used oil
In；
3. unique long handle of control multichannel sealed valve is threaded at oil discharge outlet, oil discharge outlet is isolated, by transformer
The natural pressure of oil makes oil inject sampler ontology by sample introduction fast interface, with insulation oil flushing sampler ontology to be measured；
4. at the unique long handle thief hatch for controlling multichannel sealed valve, thief hatch is isolated, push sampler piston logical
It crosses flushing oil in oil discharge outlet discharge sampler ontology and adjusts sampler ontology tilt angle, it is ensured that all into catch of used oil
Bubble and flushing oil are expelled in catch of used oil；
5. unique long handle of control multichannel sealed valve is threaded at oil discharge outlet, oil discharge outlet is isolated, by transformer
The natural pressure of oil makes oil inject sampler ontology by sample introduction fast interface, acquires 100mL oil sample；Control multichannel sealing valve
Unique long handle of door is threaded at sample introduction fast interface, and sampler is isolated, and is closed insulating oil Sampler valves, is removed each connection hose
And hose coupling, sample information label is filled in, is affixed on sampler, then sampler is put into the sales kit (SK) being protected from light, is prepared
Silver is added in next step --- oily suspension；
Two, silver-colored --- the preparation and storage of oily suspension:
1. using silver --- oily suspension preparation facilities prepares silver powder, and the silver powder of equivalent volumes is mixed with insulating oil,
It is fitted into silver --- in oily suspension memory；
2. connecting the sampling of silver-colored --- silver of oily suspension memory --- oily suspension inlet and outlet and sampler with hose
Mouthful, open multichannel sealed valve and silver --- oily suspension takes out valve, pushes memory piston, by 1mL silver --- oil is outstanding
Turbid is injected in the intrinsic 100mL insulating oil oil sample of sampler of above-mentioned sampler, and multichannel sealed valve is closed；
Three, constant temperature oscillation reacts:
To be added silver-colored --- the sampler of oily suspension is put into constant temperature oscillation reactor, and sampler strip is embedded in and is shaken
In the sampler fixed card slot of disk, concussion disk buckle is buckled well, power supply is opened, sets 98 DEG C~102 DEG C of constant temperature controller, constant temperature
For 24 hours, 275 ± 3 beats/min of sequence device vibration frequency of setting oscillation step, oscillation amplitude: 35mm, oscillation mode: (oscillation 10min+ is stood
50min)/h starts isothermal vibration reaction；
Four, it detects:
It is #1 oil sample, #2 oil sample 1. the sample collection method according to above-mentioned " one " acquires two 100mL oil samples, #1 is not done
Silver is added by above-mentioned processing method in any processing, #2 oil sample --- and oily suspension, heating, constant temperature oscillation reaction are for 24 hours；
2. install sintered glass filter core additional between the multichannel sealed valve and sample introduction fast interface of the sampler of #2 oil sample,
Sampler piston is pushed, filtering oil sample is used for following detection；
3. sulphur standard curve: opening UV suLfur anaLyzer, adjust suitable apparatus measures parameter, vapourizing temperature setting
It is 900 DEG C, ignition temperature is 1000 DEG C, and cracking oxygen is set as 430m L/min, and import oxygen is 60m L/min, argon gas 160m
L/min, negative high voltage 485V, micro current amplifier are set as high, taken after instrument stabilizer concentration be 2.5mg/L, 5mg/L,
The sulphur standard sample of 7.5mg/L, 10.0mg/L take 20.0 μ L with micro syringe, record test result, it is ensured that curvilinear correlation
Coefficient is higher than 99.99%, calculates and generates sulphur standard curve；
4. sample detection: UV suLfur anaLyzer being adjusted to experiment condition identical with sulphur standard curve, with micro note
Emitter takes 20.0 μ L, detects original sulfur content C in #1 sample oil respectively1With add silver --- the #2 sample sulphur after the reaction of oily suspension
Content C2, sample oil in active sulfur content C=C1-C2。
The method for quantitatively determining of active sulfur active sulfur sampler, feature in special isolation oil in a kind of insulating oil
It is that it includes sampler ontology, sampler ontology can be pushed away using cylinder and hemisphere integrated structure, interior be equipped with of sampler ontology
The sampler piston of drawing；The hemisphere top of sampler ontology is equipped with sample introduction fast interface, and sample introduction fast interface passes through multichannel
Sealed valve is separately connected oil discharge outlet, thief hatch；Sampler body tip is equipped with the fastening strip for protruding from body plane, fastening
The cross section of strip is that notch is round.
Method for quantitatively determining silver --- the oily suspension preparation facilities of active sulfur in a kind of insulating oil, it is characterised in that
It includes container casing, is equipped with silver bullion in container casing, and silver bullion connects under spring thrust with abrasive wheel, there is grinding on abrasive wheel
Face, the middle part of abrasive wheel connect shaft, insulating oil are equipped in container casing, shaft drives abrasive wheel rotation, made by silver bullion
Standby silver powder is mixed with insulating oil.
Method for quantitatively determining silver --- the oily suspension memory of active sulfur in a kind of insulating oil, it is characterised in that its
Including memory ontology, the memory piston that can be pushed and pulled is equipped in memory ontology；The front end of memory ontology is equipped with fast quick access
Mouthful, fast interface passes through silver --- oily suspension takes out valve connection silver --- oily suspension inlet and outlet.
The method for quantitatively determining constant temperature oscillation reactor of active sulfur in a kind of insulating oil, it is characterised in that it includes outer
Shell, shell is interior to be equipped with concussion disk, constant temperature controller, insulating layer, power switch, oscillation sequential control device, the fastening with sampler
Power switch, constant temperature controller and oscillation step is arranged in sampler fixed card slot that strip matches, concussion disk buckle, outer side of shell
Sequence controller, shell inside is equipped with insulating layer, concussion disk is equipped in shell, and after turning on the power switch, concussion disk is in thermostatic control
Reciprocating vibration is done under device and oscillation sequential control device control, fixed card slot is groove, is located on concussion disk, with sampler fixing card
Item matches, and concussion disk buckle is located on concussion disk, is used for the fixed earthquake disk of sampler.
The present invention can produce following good effect compared with the prior art:
1. reactant is using silver --- oily suspension, making reaction, testing result is more acurrate more rapidly, completely.
--- oily suspension preparation facilities can facilitate preparation silver --- the oily suspension 2. devising silver.
--- oily suspension storage device facilitates preservation silver --- the oily suspension 3. devising silver, equipped with fast interface, energy
Enough and sampling apparatus rapid abutting joint realizes sampling and reaction overall process and air insulated, completely cuts off air impact, guarantees sample detection
Accuracy；
4. constant temperature oscillation reactor is equipped with accurate constant temperature controller and oscillation sequential control device, reaction can be accurately controlled
Temperature and amplitude of oscillation, frequency promote reaction completely.
5. dedicated quantitative sampler is sealed on hemisphere top equipped with multichannel using cylinder and hemisphere integrated structure
Valve, can flexible conversion channel, under conditions of air-isolation, realize be not involved in circulation dead volume oil accumulation discharge, sampler
It rinses and oil sample acquires.Further, sampler sets accurate quantification volume mark, can be in sampling simultaneous quantitative, without secondary
Volume adjusts or transfer, avoids secondary pollution；
6. the handle of multichannel sealed valve be equipped with unique long handle, and mark off mark, can 360 rotation, be directed toward end be
Sealed end, it is easy to operate.
7. sampler, each interface of multichannel sealed valve, silver powder filter and silver --- oily suspension reservoir goes out
The total interfaces such as mouth, hose connection are spiral Universal-purpose quick interface, can quickly install additional, remove, dock, and it is convenient to operate.
Detailed description of the invention:
Fig. 1 is the structural schematic diagram of special sampler of the invention (operation dissolved gases in insulating oil analytical sampling device)；
Fig. 2 is silver of the invention --- the structural schematic diagram of oily suspension preparation facilities；
Fig. 3 is silver of the invention --- the structural schematic diagram of oily suspension reservoir；
Fig. 4 is the structural schematic diagram of constant temperature oscillation reactor of the invention.
Specific embodiment:
Specific embodiments of the present invention will be described in detail with reference to the accompanying drawing:
Embodiment: a kind of method for quantitatively determining of active sulfur in insulating oil comprising following steps:
One, sample acquires:
Using active sulfur sampler (abbreviation sampler) acquisition operation insulation oil samples in special isolation oil；
The operation dissolved gases in insulating oil analytical sampling device (referring to Fig. 1) includes sampler ontology 1-2, sampler
For ontology 1-2 using cylinder and hemisphere integrated structure, sampler ontology 1-2 is interior to be equipped with the sampler piston 1-1 that can be pushed and pulled；Sampling
The hemisphere top of device ontology 1-2 is equipped with sample introduction fast interface 1-3, and sample introduction fast interface 1-3 passes through multichannel sealed valve 1-5
It is separately connected oil discharge outlet 1-4, thief hatch 1-6.Sampler body tip is equipped with the fastening strip 1-7 for protruding from body plane, tightly
Gu the cross section of strip 1-7 is that notch is round, when placement, is downward by notch plane, contacts with desktop, it is ensured that sampler is placed
Steadily.
Specific sample collection method is as follows:
1. the oil discharge outlet 1-4, the thief hatch 1-6 that run dissolved gases in insulating oil analytical sampling device are connect by hose respectively
Head clamping hose, the hose of connection oil discharge outlet 1-4 connect catch of used oil, and the hose of connection thief hatch 1-6 connects insulating oil sampling valve
Door；
2. unique long handle of control multichannel sealed valve 1-5 is threaded at sample introduction fast interface 1-3, isolation sample introduction is quick
Interface 1-3, open insulating oil Sampler valves, by thief hatch 1-6, oil discharge outlet 1-4 draining provisions dead angle and fuel outlet valve it is dead
Oil is into catch of used oil；
3. unique long handle of control multichannel sealed valve 1-5 is threaded at oil discharge outlet 1-4, oil discharge outlet 1-4 is isolated, by
Oily natural pressure makes oil inject sampler ontology 1-2 by sample introduction fast interface 1-3 in transformer, with insulation oil flushing to be measured
Sampler ontology 1-2；
4. at the unique long handle thief hatch 1-6 for controlling multichannel sealed valve 1-5, thief hatch 1-6 is isolated, sampling is pushed
Device piston 1-1 is discharged flushing oil in sampler ontology 1-2 by oil discharge outlet 1-4 and adjusts sampler ontology into catch of used oil
1-2 tilt angle, it is ensured that all bubbles and flushing oil are expelled in catch of used oil；
5. unique long handle of control multichannel sealed valve 1-5 is threaded at oil discharge outlet 1-4, oil discharge outlet 1-4 is isolated, by
Oily natural pressure makes oil inject sampler ontology 1-2 by sample introduction fast interface 1-3 in transformer, acquires 100mL oil sample；Control
Unique long handle of multichannel sealed valve 1-5 processed is threaded at sample introduction fast interface 1-3, and sampler is isolated, and is closed insulating oil and is adopted
Sample valve removes each connection hose and hose coupling, fills in sample information label, be affixed on sampler, then put sampler
Enter in the sales kit (SK) being protected from light, prepare that silver is added in next step --- oily suspension.
Two, silver-colored --- the preparation and storage of oily suspension:
1. using silver --- oily suspension preparation facilities prepares silver powder and mixes with insulating oil, is packed into silver --- oily suspension
In memory；
2. connecting adopting for silver-colored --- silver of oily suspension memory --- oily suspension inlet and outlet 3-5 and sampler with hose
Sample mouth 1-6 opens multichannel sealed valve 1-5 and silver --- and oily suspension takes out valve 3-4, pushes memory piston 3-1, will
1mL silver --- oily suspension injects in the 100mL insulating oil oil sample in the sampler ontology 1-2 of above-mentioned sampler, closes multi-pass
Road sealed valve 1-5.
The silver --- oily suspension preparation facilities (referring to fig. 2) includes container casing 2-5, is set in container casing 2-5
There are silver bullion 2-3, silver bullion 2-3 to connect under spring 2-6 thrust with abrasive wheel 2-2, there is abradant surface, abrasive wheel 2-2 on abrasive wheel 2-2
Middle part connect shaft 2-1, insulating oil 2-4 is equipped in container casing 2-5.Shaft 2-1 drives abrasive wheel 2-2 rotation, passes through silver
Silver powder prepared by block 2-3 is mixed with insulating oil 2-4.Silver powder preparation carries out in insulating oil 2-4, and insulating oil 2-4 plays isolation
Air prevents silver powder oxidation, the effect of lubrication and heat dissipation, has abradant surface on abrasive wheel 2-2, rotates, grinds under shaft 2-1 drive
Silver bullion 2-3 is ground, silver bullion is worn into silver powder in insulating oil, the silver powder of equivalent volumes is mixed with insulating oil and is stored in silver --- oil
In suspension reservoir.
The silver --- oily suspension memory (referring to Fig. 3) includes memory ontology 3-2, in memory ontology 3-2
Equipped with the memory piston 3-1 that can be pushed and pulled；The front end of memory ontology 3-2 is equipped with fast interface 3-3, and fast interface 3-3 passes through
Oily suspension imports and exports 3-5 to silver --- oily suspension takes out valve 3-4 connection silver ---.It will by pull memory piston 3-1
Silver-colored --- silver powder of the equivalent volumes in oily suspension preparation facilities is mixed with insulating oil passes through silver --- oily suspension inlet and outlet
3-5, fast interface 3-3 are stored in memory ontology 3-2.
Three, constant temperature oscillation reacts
To be added silver-colored --- the sampler of oily suspension was put into constant temperature oscillation reactor (referring to fig. 4), by sampler card
In the sampler fixed card slot 4-4 of item insertion concussion disk, concussion disk buckle is buckled well, power supply is opened, sets 98 DEG C of constant temperature controller
~102 DEG C, for 24 hours, setting oscillation 275 ± 3 beats/min of sequence device vibration frequency of step, oscillation amplitude: oscillation mode: 35mm's constant temperature (shakes
Swing 10min+ and stand 50min)/h, start isothermal vibration reaction.
Concussion disk 4-3, constant temperature are equipped in the constant temperature oscillation reactor (referring to fig. 4), including shell 4-1, shell 4-1
Controller 4-8, it insulating layer 4-2, power supply 4-7, oscillation sequential control device 4-9, adopts with what the fastening strip 1-7 of sampler matched
Sample device fixed card slot 4-4, concussion disk buckle 4-5.Setting power switch 4-7, constant temperature controller 4-8 and oscillation on the outside of shell 4-1
It is equipped with insulating layer 4-2 on the inside of sequential control device 4-9, shell 4-1, concussion disk 4-3 is equipped in shell 4-1, turns on the power switch 4-7
Afterwards, concussion disk 4-3 does reciprocating vibration at constant temperature controller 4-8 and oscillation sequential control device 4-9 control, and fixed card slot 4-4 is
Groove is located on concussion disk 4-3, matches with sampler fixing strip 1-7, and concussion disk buckle 4-5 is located on concussion disk 4-3,
For sampler to be fixed earthquake disk 4-3.
Four, it detects:
It is #1 oil sample, #2 oil sample 1. the sample collection method according to above-mentioned " one " acquires two 100mL oil samples, #1 is not done
Silver is added by above-mentioned processing method in any processing, #2 oil sample --- and oily suspension, heating, constant temperature oscillation reaction are for 24 hours；
2. installing sintering glass additional between the multichannel sealed valve 1-5 and sample introduction fast interface 1-3 of the sampler of #2 oil sample
Glass filter core, pushes sampler piston 1-1, and filtering oil sample is used for following detection；
3. sulphur standard curve: opening UV suLfur anaLyzer, adjust suitable apparatus measures parameter, vapourizing temperature setting
It is 900 DEG C, ignition temperature is 1000 DEG C, and cracking oxygen is set as 430m L/min, and import oxygen is 60m L/min, argon gas 160m
L/min, negative high voltage 485V, micro current amplifier are set as high, taken after instrument stabilizer concentration be 2.5mg/L, 5mg/L,
The sulphur standard sample of 7.5mg/L, 10.0mg/L take 20.0 μ L with micro syringe, record test result, it is ensured that curvilinear correlation
Coefficient is higher than 99.99%, calculates and generates sulphur standard curve；
4. sample detection: UV suLfur anaLyzer being adjusted to experiment condition identical with sulphur standard curve, with micro note
Emitter takes 20.0 μ L, detects original sulfur content C in #1 sample oil respectively1With add silver --- the #2 sample sulphur after the reaction of oily suspension
Content C2, sample oil in active sulfur content C=C1-C2。
Above embodiment is only that preferred embodiments of the present invention will be described, and other preferred embodiments are herein
Do not tire out one by one and state, and is not intended to limit the scope of the present invention, without departing from the spirit of the design of the present invention, this field
The various changes and improvements that ordinary engineering and technical personnel makes technical solution of the present invention should all fall within right of the invention and want
In the protection scope for asking book to determine.
Claims (5)
1. the method for quantitatively determining of active sulfur in a kind of insulating oil comprising following steps:
One, sample acquires:
It is as follows using active sulfur samplers sample operation insulation oil samples, specific sample collection method in special isolation oil:
1. by run dissolved gases in insulating oil analytical sampling device oil discharge outlet, thief hatch pass through respectively hose coupling be clamped it is soft
Pipe, the hose for connecting oil discharge outlet connect catch of used oil, and the hose for connecting thief hatch connects insulating oil Sampler valves；
2. unique long handle of control multichannel sealed valve is threaded at sample introduction fast interface, sample introduction fast interface is isolated, opens
Insulating oil Sampler valves, by thief hatch, oil discharge outlet draining provisions dead angle and the dead oil of fuel outlet valve is into catch of used oil；
3. unique long handle of control multichannel sealed valve is threaded at oil discharge outlet, oil discharge outlet is isolated, by oily in transformer
Natural pressure makes oil inject sampler ontology by sample introduction fast interface, with insulation oil flushing sampler ontology to be measured；
4. at the unique long handle thief hatch for controlling multichannel sealed valve, thief hatch is isolated, sampler piston is pushed to pass through row
Hydraulic fluid port is discharged flushing oil in sampler ontology and adjusts sampler ontology tilt angle, it is ensured that all bubbles into catch of used oil
It is expelled in catch of used oil with flushing oil；
5. unique long handle of control multichannel sealed valve is threaded at oil discharge outlet, oil discharge outlet is isolated, by oily in transformer
Natural pressure makes oil inject sampler ontology by sample introduction fast interface, acquires 100mL oil sample；Control multichannel sealed valve
Unique long handle is threaded at sample introduction fast interface, and sampler is isolated, and closes insulating oil Sampler valves, removes each connection hose and soft
Pipe fitting is filled in sample information label, is affixed on sampler, then sampler is put into the sales kit (SK) being protected from light, and prepares next
Silver is added in step --- oily suspension；
Two, silver-colored --- the preparation and storage of oily suspension:
1. using silver --- oily suspension preparation facilities prepares silver powder, and the silver powder of equivalent volumes is mixed with insulating oil, is packed into
Silver --- in oily suspension memory；
2. connecting the thief hatch of silver-colored --- silver of oily suspension memory --- oily suspension inlet and outlet and sampler with hose, beat
Open multichannel sealed valve and silver --- oily suspension takes out valve, pushes memory piston, by 1mL silver --- oily suspension is infused
Enter in the intrinsic 100mL insulating oil oil sample of sampler of above-mentioned sampler, closes multichannel sealed valve；
Three, constant temperature oscillation reacts:
To be added silver-colored --- the sampler of oily suspension is put into constant temperature oscillation reactor, and sampler strip is embedded in concussion disk
In sampler fixed card slot, buckle well concussion disk buckle, open power supply, set 98 DEG C~102 DEG C of constant temperature controller, constant temperature for 24 hours, if
Fixed 275 ± 3 beats/min of sequence device vibration frequency of oscillation step, oscillation amplitude: 35mm, oscillation mode: (oscillation 10min+ stands 50min)/
H starts isothermal vibration reaction；
Four, it detects:
It is #1 oil sample, #2 oil sample, #1 does not do any 1. the sample collection method according to above-mentioned " one " acquires two 100mL oil samples
Silver is added by above-mentioned processing method in processing, #2 oil sample --- and oily suspension, heating, constant temperature oscillation reaction are for 24 hours；
2. installing sintered glass filter core additional between the multichannel sealed valve and sample introduction fast interface of the sampler of #2 oil sample, push
Sampler piston, filtering oil sample are used for following detection；
3. sulphur standard curve: opening UV suLfur anaLyzer, adjust suitable apparatus measures parameter, vapourizing temperature is set as 900
DEG C, ignition temperature is 1000 DEG C, and cracking oxygen is set as 430m L/min, and import oxygen is 60m L/min, and argon gas is 160m L/
Min, negative high voltage 485V, micro current amplifier are set as high, and it is 2.5mg/L, 5mg/L, 7.5mg/ that concentration is taken after instrument stabilizer
L, the sulphur standard sample of 10.0mg/L takes 20.0 μ L with micro syringe, records test result, it is ensured that curve correlation coefficient is high
In 99.99%, calculates and generate sulphur standard curve；
4. sample detection: UV suLfur anaLyzer being adjusted to experiment condition identical with sulphur standard curve, uses micro syringe
20.0 μ L are taken, detect original sulfur content C in #1 sample oil respectively1With add silver --- the #2 sample sulfur content after the reaction of oily suspension
C2, sample oil in active sulfur content C=C1-C2。
2. the method for quantitatively determining of active sulfur active sulfur in special isolation oil in a kind of insulating oil described in claim 1
Sampler, it is characterised in that it includes sampler ontology (1-2), and sampler ontology (1-2) is tied in conjunction with hemisphere using cylinder
Structure, sampler ontology (1-2) is interior to be equipped with the sampler piston (1-1) that can be pushed and pulled；The hemisphere top of sampler ontology (1-2) is set
Have sample introduction fast interface (1-3), sample introduction fast interface (1-3) is separately connected oil discharge outlet (1- by multichannel sealed valve (1-5)
4), thief hatch (1-6)；Sampler body tip is equipped with the fastening strip (1-7) for protruding from body plane, fastens strip (1-7)
Cross section be that notch is round.
3. the method for quantitatively determining silver of active sulfur in a kind of insulating oil described in claim 1 --- oily suspension preparation dress
It sets, it is characterised in that it includes container casing (2-5), is equipped with silver bullion (2-3) in container casing (2-5), silver bullion (2-3) is in spring
Connect under (2-6) thrust with abrasive wheel (2-2), there is abradant surface on abrasive wheel (2), the middle part of abrasive wheel (2-2) connects shaft (2-
1) it, is equipped with insulating oil (2-4) in container casing (2-5), shaft (2-1) drives abrasive wheel (2-2) rotation, passes through silver bullion (2-3)
Prepared silver powder is mixed with insulating oil (2-4).
4. the method for quantitatively determining silver of active sulfur in a kind of insulating oil described in claim 1 --- oily suspension storage
Device, it is characterised in that it includes memory ontology (3-2), is equipped with the memory piston (3- that can be pushed and pulled in memory ontology (3-2)
1)；The front end of memory ontology (3-2) is equipped with fast interface (3-3), and fast interface (3-3) passes through silver --- and oily suspension takes out
Valve (3-4) connection silver --- oily suspension imports and exports (3-5).
5. the method for quantitatively determining constant temperature oscillation reactor of active sulfur in a kind of insulating oil described in claim 1, special
Sign is that it includes shell (4-1), be equipped in shell (4-1) concussion disk (4-3), constant temperature controller (4-8), insulating layer (4-2),
The sampler fixing card that the fastening strip (1-7) of power switch (4-7), oscillation sequential control device (4-9) and sampler matches
Slot (4-4), concussion disk buckle (4-5), shell (4-1) outside setting power switch (4-7), constant temperature controller (4-8) and oscillation
Sequential control device (4-9), shell (4-1) inside are equipped with insulating layer (4-2), and concussion disk (4-3), opening are equipped in shell (4-1)
After power switch (4-7), concussion disk (4-3) is done reciprocal under constant temperature controller (4-8) and oscillation sequential control device (4-9) control
Oscillation, fixed card slot (4-4) are groove, are located in concussion disk (4-3), match with sampler fixing strip (1-7), shake disk
It buckles (4-5) to be located in concussion disk (4-3), for sampler is fixed earthquake disk (4-3).
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| CN201610571742.9A CN106198108B (en) | 2016-07-20 | 2016-07-20 | The method for quantitatively determining and dedicated unit of active sulfur in a kind of insulating oil |
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| CN108693085B (en) * | 2018-03-29 | 2020-07-28 | 重庆山楂树科技有限公司 | Gas storage device for dust detection |
| CN108731251A (en) * | 2018-05-31 | 2018-11-02 | 江苏雄义环保自动化设备有限公司 | A kind of liquid heater |
| CN112305137B (en) * | 2020-09-28 | 2022-10-11 | 国网浙江省电力有限公司嘉兴供电公司 | Oil transfer auxiliary device for full-automatic gas chromatograph sampling injector |
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| CN102478470A (en) * | 2010-11-26 | 2012-05-30 | 中国石油化工股份有限公司 | Piston type vacuum degasser and its degassing method |
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| CN102478470A (en) * | 2010-11-26 | 2012-05-30 | 中国石油化工股份有限公司 | Piston type vacuum degasser and its degassing method |
| CN102692519A (en) * | 2011-03-24 | 2012-09-26 | 江苏江分电分析仪器有限公司 | Multipath liquid sampler |
| CN103969246A (en) * | 2014-05-21 | 2014-08-06 | 国家电网公司 | Method for quantitatively detecting content of corrosive sulfur in mineral insulating oil |
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