CN105974042A - Reversed phase high performance liquid chromatography method for determining content of dibenzyl disulfide in insulating oil - Google Patents
Reversed phase high performance liquid chromatography method for determining content of dibenzyl disulfide in insulating oil Download PDFInfo
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Abstract
The invention provides a reversed phase high performance liquid chromatography method for determining the content of dibenzyl disulfide in insulating oil. The invention relates to a method for determining the content of dibenzyl disulfide in the insulating oil, aiming at solving the problems that an existing gas chromatography-mass spectrometry method for determining the content of the DBDS in the insulating oil that the cost is high and application is limited. The method comprises the following steps: 1, preparing a stock solution; 2, preparing a calibration solution; 3, preparing a solid-phase extraction and adsorption column; 4, preparing a sample solution; 5, analyzing a sample; 6, formulating a calibration curve; and 7, determining the content of the dibenzyl disulfide in the insulating oil to be detected. According to the method provided by the invention, the determination of the content of the dibenzyl disulfide in the insulating oil is realized by utilizing a liquid chromatograph with a relatively cheap price; and the method is simple to operate, high in repeatability and accuracy, relatively low in instrument and equipment price and easy to realize.
Description
Technical field
The present invention relates to a kind of measure the method for benzyl disulfide ether content in insulating oil.
Background technology
In recent years, the transformer fault caused because of active sulfur in insulating oil both at home and abroad frequently occurs, and brings to the safety of electrical network
High risks, and cause bigger economic loss and social influence.In insulating oil, active sulfur has higher corrosion to metal
Activity, directly can react generation metal sulfide with metal under certain condition, cause the corruption of high voltage electric equipment material
Deteriorate bad, including elemental sulfur, hydrogen sulfide, mercaptan, thioether, and some organic molecule sulfide.Result of the test
Showing, in insulating oil, benzyldithio toluene (DBDS) is to cause Transformer to produce Cu2S also causes solid insulation
The reason punctured, currently forms Cu2The transformer oil of S all contains DBDS.International Electrotechnical Commission issued in 2012
New insulating oil standard IEC 60296, with addition of the mensuration to DBDS content, it is desirable to it is content in product oil
Less than 5mg/kg.Therefore detection DBDS is very important for controlling the sulfur corrosion of insulating oil.
At present, the method for DBDS content in insulating oil that measures is mainly gas chromatography-mass spectrography.The method is held high due to needs
Expensive gas chromatograph-mass spectrometer, relatively costly, therefore have a strong impact on the actual application of the method.
Summary of the invention
The present invention seeks to solve the gas chromatography-mass spectrography cost height of DBDS content in existing mensuration insulating oil, application is subject to
The problem of limit, and provide a kind of and measure the reverse efficient liquid-phase chromatography method of benzyl disulfide ether content in insulating oil.
The present invention a kind of measures in insulating oil the reverse efficient liquid-phase chromatography method of benzyl disulfide ether content according to the following steps
Carry out:
One, the preparation of storing solution: weigh 0.100g benzyldithio toluene and 99.900g blank oil, after mixing in temperature be
Stir under conditions of 45～55 DEG C and all dissolve to benzyldithio toluene, then go in brown port grinding bottle, be 3～5 DEG C in temperature
Under conditions of preserve, standby；
In the case of storing solution preserves under conditions of temperature is 3～5 DEG C, effective time is 3 months；
Two, calibrate the preparation of solution: take the storing solution of five parts of step one preparations, be added thereto to blank oil mix homogeneously respectively,
It is configured to concentration and is followed successively by the calibration solution of 5mg/kg, 50mg/kg, 100mg/kg, 300mg/kg and 500mg/kg；
The effective time of calibration solution was less than 3 days；
Three, the preparation of Solid-Phase Extraction adsorption column: put into a piece of sieve plate in 1mL glass syringe, will with syringe fuse
Sieve plate is pushed into the bottom of syringe, then adds alumina adsorbant in syringe at 0.6mL graduation mark, adds
A piece of sieve plate, and press second sieve plate extremely by adsorbent layer compacting with syringe fuse, obtain Solid-Phase Extraction adsorption column, standby
With；
Four, the preparation of sample liquid: 1., the calibration solution that 1.00g concentration is 5mg/kg is added in volumetric flask, then add
Entering 2.0mL chromatographically pure normal hexane, concussion volumetric flask, to fully mixing, obtains mixed liquor, then pours mixed liquor into step
In the Solid-Phase Extraction adsorption column that three obtain, the most naturally flow through adsorbent layer, purer own by 2.0mL chromatograph
Alkane the most naturally flows through adsorbent layer and carries out drip washing, then natural under gravity with 2.0mL chromatograph purified petroleum benzin
Flowing through adsorbent layer to extract, collect extract, add Chromatographic Pure Methanol and be settled to 5mL in extract, concussion is mixed
Sample liquid 1 is obtained after even；2., utilize concentration for 50mg/kg, 100mg/kg, 300mg/kg and 500mg/kg successively
The calibration solution that calibration solution replaces step 4 1. middle concentration to be 5mg/kg, repeats step 4 and 1. operates, obtain sample successively
Liquid 2, sample liquid 3, sample liquid 4 and sample liquid 5；
Owing to benzene is poisonous, therefore aforesaid operations should complete in ventilated chamber；
Five, sample analysis: the formulation of calibration curve: aspiration step four obtains the most respectively with microsyringe sample liquid 1,
Sample liquid 2, sample liquid 3 sample liquid 4 and each 0.025mL of sample liquid 5, and utilize chromatograph of liquid to carry out detection point successively
Analysis, the absworption peak area A of benzyldithio toluene in record sample liquid 1DBDS1, the suction of benzyldithio toluene in sample liquid 2
Receive peak area ADBDS2, the absworption peak area A of benzyldithio toluene in sample liquid 3DBDS3, dibenzyl two in sample liquid 4
The absworption peak area A of thioetherDBDS4With the absworption peak area A of benzyldithio toluene in sample liquid 5DBDS5；
Described chromatograph of liquid detection analysis condition: wavelength is 215nm, flowing is the mixture of water and methanol mutually, wherein
The volume ratio of water and methanol is 1:4, and flow velocity is 1.0mL/min；
Six, the formulation of calibration curve: the absworption peak area A of benzyldithio toluene in the sample liquid 1 obtained by step 5DBDS1、
The absworption peak area A of benzyldithio toluene in sample liquid 2DBDS2, the absworption peak area of benzyldithio toluene in sample liquid 3
ADBDS3, the absworption peak area A of benzyldithio toluene in sample liquid 4DBDS4With the absorption of benzyldithio toluene in sample liquid 5
Peak area ADBDS5Fitting to calibration curve, wherein calibration curve vertical coordinate is absworption peak area ADBDS, abscissa is calibration
Solution concentration CDBDS；
The Calibration equation that wherein calibration curve is corresponding is: y=0.719x, R2=0.999；
Seven, the mensuration of benzyl disulfide ether content in insulating oil to be measured: in utilizing insulating oil to be measured to replace step 4 1., concentration is
The calibration solution of 5mg/kg, repeats step 4 and 1. operates, obtain oil samples liquid to be measured, draw oil to be measured with microsyringe
Sample liquid 0.025mL, and utilize chromatograph of liquid to carry out detection analysis, record benzyldithio toluene in oil samples liquid to be measured
Absworption peak area ADBDS is to be measured, the calibration curve then obtained according to step 6 is calculated benzyl disulfide in insulating oil to be measured
The content of ether.
Beneficial effects of the present invention:
Invention is a kind of measures the reverse efficient liquid-phase chromatography method of benzyl disulfide ether content, exploitation value in insulating oil
The relatively inexpensive chromatograph of liquid of lattice realizes the mensuration of benzyl disulfide ether content in insulating oil, and the method is simple to operate, repeats
Property and accuracy high, instrument and equipment price is relatively low, easily realizes.
Accompanying drawing explanation
The calibration curve that Fig. 1 is fitted to by the absworption peak area recorded by variable concentrations calibration solution in the present invention.
Detailed description of the invention
Detailed description of the invention one: a kind of of present embodiment measures the most efficiently liquid phase of benzyl disulfide ether content in insulating oil
Chromatographic process sequentially includes the following steps:
One, the preparation of storing solution: weigh 0.100g benzyldithio toluene and 99.900g blank oil, after mixing in temperature be
Stir under conditions of 45～55 DEG C and all dissolve to benzyldithio toluene, then go in brown port grinding bottle, be 3～5 DEG C in temperature
Under conditions of preserve, standby；
In the case of storing solution preserves under conditions of temperature is 3～5 DEG C, effective time is 3 months；
Two, calibrate the preparation of solution: take the storing solution of five parts of step one preparations, be added thereto to blank oil mix homogeneously respectively,
It is configured to concentration and is followed successively by the calibration solution of 5mg/kg, 50mg/kg, 100mg/kg, 300mg/kg and 500mg/kg；
The effective time of calibration solution was less than 3 days；
Three, the preparation of Solid-Phase Extraction adsorption column: put into a piece of sieve plate in 1mL glass syringe, will with syringe fuse
Sieve plate is pushed into the bottom of syringe, then adds alumina adsorbant in syringe at 0.6mL graduation mark, adds
A piece of sieve plate, and press second sieve plate extremely by adsorbent layer compacting with syringe fuse, obtain Solid-Phase Extraction adsorption column, standby
With；
Four, the preparation of sample liquid: 1., the calibration solution that 1.00g concentration is 5mg/kg is added in volumetric flask, then add
Entering 2.0mL chromatographically pure normal hexane, concussion volumetric flask, to fully mixing, obtains mixed liquor, then pours mixed liquor into step
In the Solid-Phase Extraction adsorption column that three obtain, the most naturally flow through adsorbent layer, purer own by 2.0mL chromatograph
Alkane the most naturally flows through adsorbent layer and carries out drip washing, then natural under gravity with 2.0mL chromatograph purified petroleum benzin
Flowing through adsorbent layer to extract, collect extract, add Chromatographic Pure Methanol and be settled to 5mL in extract, concussion is mixed
Sample liquid 1 is obtained after even；2., utilize concentration for 50mg/kg, 100mg/kg, 300mg/kg and 500mg/kg successively
The calibration solution that calibration solution replaces step 4 1. middle concentration to be 5mg/kg, repeats step 4 and 1. operates, obtain sample successively
Liquid 2, sample liquid 3, sample liquid 4 and sample liquid 5；
Owing to benzene is poisonous, therefore aforesaid operations should complete in ventilated chamber；
Five, sample analysis: the formulation of calibration curve: aspiration step four obtains the most respectively with microsyringe sample liquid 1,
Sample liquid 2, sample liquid 3 sample liquid 4 and each 0.025mL of sample liquid 5, and utilize chromatograph of liquid to carry out detection point successively
Analysis, the absworption peak area A of benzyldithio toluene in record sample liquid 1DBDS1, the suction of benzyldithio toluene in sample liquid 2
Receive peak area ADBDS2, the absworption peak area A of benzyldithio toluene in sample liquid 3DBDS3, dibenzyl two in sample liquid 4
The absworption peak area A of thioetherDBDS4With the absworption peak area A of benzyldithio toluene in sample liquid 5DBDS5；
Described chromatograph of liquid detection analysis condition: wavelength is 215nm, flowing is the mixture of water and methanol mutually, wherein
The volume ratio of water and methanol is 1:4, and flow velocity is 1.0mL/min；
Six, the formulation of calibration curve: the absworption peak area A of benzyldithio toluene in the sample liquid 1 obtained by step 5DBDS1、
The absworption peak area A of benzyldithio toluene in sample liquid 2DBDS2, the absworption peak area of benzyldithio toluene in sample liquid 3
ADBDS3, the absworption peak area A of benzyldithio toluene in sample liquid 4DBDS4With the absorption of benzyldithio toluene in sample liquid 5
Peak area ADBDS5Fitting to calibration curve, wherein calibration curve vertical coordinate is absworption peak area ADBDS, abscissa is calibration
Solution concentration CDBDS；
The Calibration equation that wherein calibration curve is corresponding is: y=0.719x, R2=0.999；
Seven, the mensuration of benzyl disulfide ether content in insulating oil to be measured: in utilizing insulating oil to be measured to replace step 4 1., concentration is
The calibration solution of 5mg/kg, repeats step 4 and 1. operates, obtain oil samples liquid to be measured, draw oil to be measured with microsyringe
Sample liquid 0.025mL, and utilize chromatograph of liquid to carry out detection analysis, record benzyldithio toluene in oil samples liquid to be measured
Absworption peak area ADBDS is to be measured, the calibration curve then obtained according to step 6 is calculated benzyl disulfide in insulating oil to be measured
The content of ether.
Present embodiments provide for a kind of measuring the reverse efficient liquid-phase chromatography method of benzyl disulfide ether content in insulating oil, profit
Realizing the mensuration of benzyl disulfide ether content in insulating oil with the chromatograph of liquid that price is relatively inexpensive, the method is simple to operate,
Repeatability and accuracy are high, and instrument and equipment price is relatively low, easily realizes.
Detailed description of the invention two: present embodiment is unlike detailed description of the invention one: in step one after mixing in temperature be
Stir under conditions of 48～53 DEG C to benzyldithio toluene and all dissolve.Other steps and parameter and detailed description of the invention one phase
With.
Detailed description of the invention three: present embodiment is unlike detailed description of the invention one or two: in temperature after mixing in step one
Degree stirs under conditions of being 50 DEG C to benzyldithio toluene and all dissolves.Other steps and parameter and detailed description of the invention one or
Two is identical.
Detailed description of the invention four: present embodiment is unlike one of detailed description of the invention one to three: in temperature in step one
Preserve under conditions of being 4 DEG C, standby.Other steps and parameter are identical with one of detailed description of the invention one to three.
Detailed description of the invention five: present embodiment is unlike one of detailed description of the invention one to four: described in step 5
Chromatograph of liquid detection analysis condition: wavelength is 215nm, flowing is the mixture of water and methanol mutually, wherein water and methanol
Volume ratio be 1:4, flow velocity is 1.0mL/min.Other steps and parameter are identical with one of detailed description of the invention one to four.
By following verification experimental verification beneficial effects of the present invention:
Test one: this test a kind of measure in insulating oil the reverse efficient liquid-phase chromatography method of benzyl disulfide ether content by with
Lower step is carried out:
For No. 1 main transformer dispatched from the factory by Ukraine's production in 1997 being applied to 500kV transformer station.Transformator is specified
Capacity is 640MVA, and oil-filled weight is 145t, and oil sources is Ukraine's transformers imported oil.
Utilize the method for the invention that the content of benzyldithio toluene in the transformer oil in this transformator carries out detection concrete
Step is as follows:
One, the preparation of storing solution: weigh 0.100g benzyldithio toluene and 99.900g blank oil, after mixing in temperature be
Stir under conditions of 50 DEG C and all dissolve to benzyldithio toluene, then go in brown port grinding bottle, at the bar that temperature is 4 DEG C
Preserve under part, standby；
In the case of storing solution preserves under conditions of temperature is 3～5 DEG C, effective time is 3 months；
Two, calibrate the preparation of solution: take the storing solution of five parts of step one preparations, be added thereto to blank oil mix homogeneously respectively,
It is configured to concentration and is followed successively by the calibration solution of 5mg/kg, 50mg/kg, 100mg/kg, 300mg/kg and 500mg/kg；
The effective time of calibration solution was less than 3 days；
Three, the preparation of Solid-Phase Extraction adsorption column: put into a piece of sieve plate in 1mL glass syringe, will with syringe fuse
Sieve plate is pushed into the bottom of syringe, then adds alumina adsorbant in syringe at 0.6mL graduation mark, adds
A piece of sieve plate, and press second sieve plate extremely by adsorbent layer compacting with syringe fuse, obtain Solid-Phase Extraction adsorption column, standby
With；
Four, the preparation of sample liquid: 1., the calibration solution that 1.00g concentration is 5mg/kg is added in volumetric flask, then add
Entering 2.0mL chromatographically pure normal hexane, concussion volumetric flask, to fully mixing, obtains mixed liquor, then pours mixed liquor into step
In the Solid-Phase Extraction adsorption column that three obtain, the most naturally flow through adsorbent layer, purer own by 2.0mL chromatograph
Alkane the most naturally flows through adsorbent layer and carries out drip washing, then natural under gravity with 2.0mL chromatograph purified petroleum benzin
Flowing through adsorbent layer to extract, collect extract, add Chromatographic Pure Methanol and be settled to 5mL in extract, concussion is mixed
Sample liquid 1 is obtained after even；2., utilize concentration for 50mg/kg, 100mg/kg, 300mg/kg and 500mg/kg successively
The calibration solution that calibration solution replaces step 4 1. middle concentration to be 5mg/kg, repeats step 4 and 1. operates, obtain sample successively
Liquid 2, sample liquid 3, sample liquid 4 and sample liquid 5；
Owing to benzene is poisonous, therefore aforesaid operations should complete in ventilated chamber；
Five, sample analysis: the formulation of calibration curve: aspiration step four obtains the most respectively with microsyringe sample liquid 1,
Sample liquid 2, sample liquid 3 sample liquid 4 and each 0.025mL of sample liquid 5, and utilize chromatograph of liquid to carry out detection point successively
Analysis, the absworption peak area A of benzyldithio toluene in record sample liquid 1DBDS1, the suction of benzyldithio toluene in sample liquid 2
Receive peak area ADBDS2, the absworption peak area A of benzyldithio toluene in sample liquid 3DBDS3, dibenzyl two in sample liquid 4
The absworption peak area A of thioetherDBDS4With the absworption peak area A of benzyldithio toluene in sample liquid 5DBDS5；
Described chromatograph of liquid detection analysis condition: wavelength is 215nm, flowing is the mixture of water and methanol mutually, wherein
The volume ratio of water and methanol is 1:4, and flow velocity is 1.0mL/min；
Six, the formulation of calibration curve: the absworption peak area A of benzyldithio toluene in the sample liquid 1 obtained by step 5DBDS1、
The absworption peak area A of benzyldithio toluene in sample liquid 2DBDS2, the absworption peak area of benzyldithio toluene in sample liquid 3
ADBDS3, the absworption peak area A of benzyldithio toluene in sample liquid 4DBDS4With the absorption of benzyldithio toluene in sample liquid 5
Peak area ADBDS5Fitting to calibration curve, wherein calibration curve vertical coordinate is absworption peak area ADBDS, abscissa is calibration
Solution concentration CDBDS；
The Calibration equation that wherein calibration curve is corresponding is: y=0.719x, R2=0.999；
Seven, the mensuration of benzyl disulfide ether content in insulating oil to be measured: in utilizing insulating oil to be measured to replace step 4 1., concentration is
The calibration solution of 5mg/kg, repeats step 4 and 1. operates, obtain oil samples liquid to be measured, draw oil to be measured with microsyringe
Sample liquid 0.025mL, and utilize chromatograph of liquid to carry out detection analysis, record benzyldithio toluene in oil samples liquid to be measured
Absworption peak area ADBDS is to be measured, the calibration curve then obtained according to step 6 is calculated benzyl disulfide in insulating oil to be measured
The content of ether.
Result: in the transformer oil in Calibration equation described in step 6 is calculated this transformator, benzyldithio toluene contains
Amount is 97.5mg/kg.
Under 95% confidence level, the repeatability of this method is that the difference of two results measured is less than the 10% of meansigma methods, this
The repeatability of method is that the difference of two results measured is less than the 25% of meansigma methods.
Claims (5)
1. one kind measures the reverse efficient liquid-phase chromatography method of benzyl disulfide ether content in insulating oil, it is characterised in that the method
Sequentially include the following steps:
One, the preparation of storing solution: weigh 0.100g benzyldithio toluene and 99.900g blank oil, after mixing in temperature be
Stir under conditions of 45～55 DEG C and all dissolve to benzyldithio toluene, then go in brown port grinding bottle, be 3～5 DEG C in temperature
Under conditions of preserve, standby；
Two, calibrate the preparation of solution: take the storing solution of five parts of step one preparations, be added thereto to blank oil mix homogeneously respectively,
It is configured to concentration and is followed successively by the calibration solution of 5mg/kg, 50mg/kg, 100mg/kg, 300mg/kg and 500mg/kg；
Three, the preparation of Solid-Phase Extraction adsorption column: put into a piece of sieve plate in 1mL glass syringe, will sieve with syringe fuse
Plate is pushed into the bottom of syringe, then adds alumina adsorbant in syringe at 0.6mL graduation mark, adds a piece of
Sieve plate, and press second sieve plate extremely by adsorbent layer compacting with syringe fuse, obtain Solid-Phase Extraction adsorption column, standby；
Four, the preparation of sample liquid: 1., the calibration solution that 1.00g concentration is 5mg/kg is added in volumetric flask, be subsequently adding
2.0mL chromatographically pure normal hexane, concussion volumetric flask, to fully mixing, obtains mixed liquor, then pours mixed liquor into step 3 and obtain
To Solid-Phase Extraction adsorption column in, the most naturally flow through adsorbent layer, then with 2.0mL chromatographically pure normal hexane at weight
Naturally flow through adsorbent layer under power effect and carry out drip washing, then the most naturally flow through absorption with 2.0mL chromatograph purified petroleum benzin
Oxidant layer extracts, and collects extract, adds Chromatographic Pure Methanol and is settled to 5mL, obtain sample after concussion mixing in extract
Product liquid 1；2., the calibration solution that concentration is 50mg/kg, 100mg/kg, 300mg/kg and 500mg/kg is utilized to replace successively
Step 4 1. in concentration be the calibration solution of 5mg/kg, repeat step 4 and 1. operate, obtain successively sample liquid 2, sample liquid 3,
Sample liquid 4 and sample liquid 5；
Five, sample analysis: the formulation of calibration curve: aspiration step four obtains the most respectively with microsyringe sample liquid 1,
Sample liquid 2, sample liquid 3 sample liquid 4 and each 0.025mL of sample liquid 5, and utilize chromatograph of liquid to carry out detection analysis successively,
The absworption peak area A of benzyldithio toluene in record sample liquid 1DBDS1, the absworption peak face of benzyldithio toluene in sample liquid 2
Long-pending ADBDS2, the absworption peak area A of benzyldithio toluene in sample liquid 3DBDS3, the suction of benzyldithio toluene in sample liquid 4
Receive peak area ADBDS4With the absworption peak area A of benzyldithio toluene in sample liquid 5DBDS5；
Six, the formulation of calibration curve: the absworption peak area A of benzyldithio toluene in the sample liquid 1 obtained by step 5DBDS1、
The absworption peak area A of benzyldithio toluene in sample liquid 2DBDS2, the absworption peak area of benzyldithio toluene in sample liquid 3
ADBDS3, the absworption peak area A of benzyldithio toluene in sample liquid 4DBDS4With the absorption of benzyldithio toluene in sample liquid 5
Peak area ADBDS5Fitting to calibration curve, wherein calibration curve vertical coordinate is absworption peak area ADBDS, abscissa is calibration
Solution concentration CDBDS；
Seven, the mensuration of benzyl disulfide ether content in insulating oil to be measured: in utilizing insulating oil to be measured to replace step 4 1., concentration is
The calibration solution of 5mg/kg, repeats step 4 and 1. operates, obtain oil samples liquid to be measured, draw oil sample to be measured with microsyringe
Product liquid 0.025mL, and utilize chromatograph of liquid to carry out detection analysis, record the suction of benzyldithio toluene in oil samples liquid to be measured
Receive peak area ADBDS is to be measured, the calibration curve then obtained according to step 6 is calculated benzyldithio toluene in insulating oil to be measured
Content.
The most according to claim 1 a kind of measure the reverse high performance liquid chromatography side of benzyl disulfide ether content in insulating oil
Method, it is characterised in that stir under conditions of temperature is 48～53 DEG C to benzyldithio toluene after mixing in step one and all dissolve.
The most according to claim 1 a kind of measure the reverse high performance liquid chromatography side of benzyl disulfide ether content in insulating oil
Method, it is characterised in that stir under conditions of temperature is 50 DEG C to benzyldithio toluene after mixing in step one and all dissolve.
The most according to claim 1 a kind of measure the reverse high performance liquid chromatography side of benzyl disulfide ether content in insulating oil
Method, it is characterised in that preserve under conditions of temperature is 4 DEG C in step one, standby.
The most according to claim 1 a kind of measure the reverse high performance liquid chromatography side of benzyl disulfide ether content in insulating oil
Method, it is characterised in that the chromatograph of liquid detection analysis condition described in step 5: wavelength is 215nm, flowing be water mutually with
The mixture of methanol, wherein the volume ratio of water and methanol is 1:4, and flow velocity is 1.0mL/min.
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| CN109164181A (en) * | 2018-09-10 | 2019-01-08 | 南方电网调峰调频发电有限公司检修试验分公司 | The chemical analysis method of benzyldithio toluene in insulating oil |
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