CN107014918B - The detection method of polymethoxy dibutyl ethers content - Google Patents
The detection method of polymethoxy dibutyl ethers content Download PDFInfo
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Abstract
The invention discloses a kind of detection methods of polymethoxy dibutyl ethers content.Method includes the following steps: the moisture content in (1) Karl_Fischer method measurement polymethoxy dibutyl ethers mixture；(2) acid base titration measurement polymethoxy dibutyl mixes the content of formaldehyde in etherate；(3) centrifugal dehydration；(4) gas chromatographic detection condition is set；(5) it tests and analyzes.The method of the present invention can effectively promote the accuracy of detection, extend gas-chromatography service life.
Description
Technical field
The invention belongs to technical field of analytical chemistry, and in particular to a kind of detection side of polymethoxy dibutyl ethers content
Method.
Background technique
Polymethoxy dibutyl ethers are a kind of higher boiling yellow liquids, and average Cetane number (CN) is high (70 or more), oxygen-containing
Measure high (> 20%), aromatic-free, hardly sulfur-bearing.Its physical property is close with diesel oil, as diesel quality modifier, when use not
It needs to make any change to the engine of In-Use Motor Vehicles.Diesel cetane-number also can be improved, promote oil product oxygen content, significantly
CO pollutant in tail gas, THC, smoke intensity, particulate matter (PM2.5, PM5, PM10) discharge are reduced, it can be largely to the diesel oil tailstock
Positive effect is played in the environmental purification emission reduction of gas, is environment-friendly type diesel quality recognized in the world so as to improve environmental quality
Modifier, therefore, need to establish it is a kind of can the accurate, method that quickly detects polymethoxy dibutyl ethers purity.
Summary of the invention
For above-mentioned deficiency in the prior art, the present invention provides a kind of detection side of polymethoxy dibutyl ethers content
Method can accurately and rapidly detect out polymethoxy dibutyl ethers purity.
A kind of detection method of polymethoxy dibutyl ethers content, comprising the following steps:
(1) moisture content in polymethoxy dibutyl ethers mixture is measured；
(2) content of formaldehyde in polymethoxy dibutyl ethers mixture is measured；
(3) polymethoxy dibutyl ethers mixture is centrifuged, takes supernatant, then desiccant dehydration is added into supernatant,
Obtain sample to be tested；
(4) chromatographic condition is selected: the gas chromatograph with fid detector；Chromatographic column: HP-5 capillary column；Vaporizing chamber
Temperature: 180~280 DEG C；Column temperature: 30~50 DEG C；Detection room temperature: 150~260 DEG C；Temperature programming: with 2~6 DEG C/min rate
45 DEG C are risen to, then rises to 245 DEG C with 50~80 DEG C/min rate, keeps 8~10min；Carrier gas: nitrogen；
(5) gas chromatograph parameters are set by step (4) described chromatographic condition, after baseline walk it is steady after, with sample injector draw to
Sample rinse 3~5 times repeatedly, then detect sample to be tested, then remove moisture obtained in step (1) and (2) and
Content of formaldehyde, the content and purity of polymethoxy dibutyl ethers in you can get it sample.
Further, the method for moisture content is that karr is taken in measurement polymethoxy dibutyl ethers mixture in step (1)
Not method.
Further, measurement polymethoxy dibutyl mixes the method for content of formaldehyde in etherate as soda acid drop in step (2)
Determine method；Wherein, the acid is sulfuric acid, and indicator is Thymol phthalein indicator.
Further, desiccant is molecular sieve, calcium sulfate or calcium chloride in step (3).
Further, chromatographic condition in step (4) are as follows: 35 DEG C of column temperature；Temperature of vaporization chamber: 280 DEG C；Fid detector: 280
℃；Temperature programming: 45 DEG C are risen to 2 DEG C/min rate, then rises to 245 DEG C with 50 DEG C/min rate, keeps 10min；Nitrogen stream
Speed is 150mL/min；Hydrogen flow rate: 40mL/min；Air velocity: 400mL/min.
Further, input mode described in step (5) is split sampling, and sample volume is 0.2~0.4 μ L, and split ratio is
100:1。
The invention has the benefit that
1, by after the mixture high speed centrifugation of polymethoxy dibutyl ethers, the formaldehyde contained in sample can be effectively removed
Grain, avoids the blocking of chromatographic column.
2, after sample to be tested adsorption dewatering, influence of the moisture to chromatographic column can be reduced, the service life of chromatography is improved.
3, using the gas chromatography of temperature programming, each component of sample to be tested can be efficiently separated, improves inspection
The accuracy of survey.
Specific embodiment
A specific embodiment of the invention is described below, in order to facilitate understanding by those skilled in the art this hair
It is bright, it should be apparent that the present invention is not limited to the ranges of specific embodiment, for those skilled in the art,
As long as various change is in the spirit and scope of the present invention that the attached claims limit and determine, these variations are aobvious and easy
See, all are using the innovation and creation of present inventive concept in the column of protection.
Embodiment 1
A kind of detection method of polymethoxy dibutyl ethers content, comprising the following steps:
(1) 2g polymethoxy dibutyl ethers mixture is weighed, it is mixed using Karl_Fischer method measurement polymethoxy dibutyl ethers
It closes the moisture content in object to be injected into sample in karl Fischer moisture teller with syringe, automatically determines out moisture and contain
Amount.
Karl_Fischer method principle: the card of moisture (free water or the crystallization water) and known titer of any state in sample
Your C.Fischer (iodine, sulfur dioxide, pyridine and methanol composition solution) carry out quantitative reaction, with current potential directing terminal, according to
Consumable liquid volume finds out moisture content, and reaction equation is as follows:
H2O+I2+SO2+3C5H5N→2C5H5N·HI+C5H5N·SO3
C5H5N·SO3+CH3OH→C5H5NH·OSO2OCH3
(2) measurement polymethoxy dibutyl mixes the content of formaldehyde in etherate
Content of formaldehyde in etherate is mixed using determination of acid-basetitration polymethoxy dibutyl, weighs 2g polymethoxy two
Butyl ether mixture is placed in 250mL conical flask, and the dissolution of 50mL sodium sulfite solution is added, then 2~3 drops hundred are added dropwise thereto
In fragrant phenolphthalein indicator, then titrated with the sulfuric acid solution of 1mol/L, until testing sample solution is become colorless by blue, recorded
The volume of the sulfuric acid of consumption, passes through formula:
Wherein, VH2SO4Titrate the volume mL of the sulfuric acid solution of consumption；
C H2SO4Titrate the concentration mol/L of the sulfuric acid solution of consumption；
M- sample to be tested quality g；
You can get it, and polymethoxy dibutyl mixes the content of formaldehyde in etherate.
Measuring principle: it is reacted using formaldehyde with excessive sodium sulfite and generates sodium hydroxide, with the sulfuric acid standard of 1mol/L
The sodium hydroxide that solution titration generates, the amount of formaldehyde are equivalent to the amount for the sodium hydroxide that reaction generates.
Reaction equation is as follows:
HCHO+Na2SO3+H2O=NaOH+CH2(NaSO3)OH
2NaOH+H2SO4=Na2SO4+H2O
Blank control: drawing 50mL sodium sulfite solution and be placed in the conical flask of 250mL, and 2~3 drop thymolphthaleins is added to refer to
Show agent, then become colorless with the sulfuric acid standard solution of 1mol/L titration blue, records the volume of sulfuric acid, this experiment is tried as blank
It tests.
(3) polymethoxy dibutyl ethers mixture is centrifuged, takes supernatant, then calcium sulfate dehydration is added into supernatant,
Obtain sample to be tested.
(4) polymethoxy dibutyl ethers are produced using Beijing DongXi Analytical Instrument Co., Ltd GC-4000A gas chromatograph
Product are analyzed, and gas chromatograph has fid detector, chromatographic column: HP-5 capillary column (30m × 0.32mm × 0.25 μm),
Nitrogen is opened, nitrogen flow is adjusted, makes its flow velocity 150mL/min, will test room temperature and be set as 200 DEG C, temperature of vaporization chamber
180 DEG C are set as, column temperature is set as 35 DEG C, then set being warming up to 50 DEG C with the speed of 5 DEG C/min for temperature programming again, then
260 DEG C are warming up to the speed of 40 DEG C/min, and keeps 8min, operation key is pressed and starts to warm up；Air, hydrogen valve are opened again,
Its flow is adjusted, makes hydrogen flow rate 40mL/min, air velocity 400mL/min, after the completion of heating, start to light a fire, to base
Line can sample introduction after walking surely.
(5) after baseline is walked surely, sample to be tested rinse 4 times repeatedly to be measured are drawn with sample injector, then use split sampling
Method sample to be tested is detected, split ratio 100:1, sample volume be 0.2 μ L, chromatogram is obtained, using area normalization
Method analyzes chromatogram, and calculates the content of each component in sample to be tested, then remove moisture and first obtained in step (1) and (2)
Aldehyde, the content and purity of polymethoxy dibutyl ethers in you can get it sample, the result is shown in tables 1.
Embodiment 2
A kind of detection method of polymethoxy dibutyl ethers content, comprising the following steps:
(1) 2g polymethoxy dibutyl ethers mixture is weighed, it is mixed using Karl_Fischer method measurement polymethoxy dibutyl ethers
It closes the moisture content in object to be injected into sample in karl Fischer moisture teller with syringe, automatically determines out moisture and contain
Amount.
Karl_Fischer method principle: the card of moisture (free water or the crystallization water) and known titer of any state in sample
Your C.Fischer (iodine, sulfur dioxide, pyridine and methanol composition solution) carry out quantitative reaction, with current potential directing terminal, according to
Consumable liquid volume finds out moisture content, and reaction equation is as follows:
H2O+I2+SO2+3C5H5N→2C5H5N·HI+C5H5N·SO3
C5H5N·SO3+CH3OH→C5H5NH·OSO2OCH3
(2) measurement polymethoxy dibutyl mixes the content of formaldehyde in etherate
Content of formaldehyde in etherate is mixed using determination of acid-basetitration polymethoxy dibutyl, weighs 2g polymethoxy two
Butyl ether mixture is placed in 250mL conical flask, and the dissolution of 50mL sodium sulfite solution is added, then 2~3 drops hundred are added dropwise thereto
In fragrant phenolphthalein indicator, then titrated with the sulfuric acid solution of 1mol/L, until testing sample solution is become colorless by blue, recorded
The volume of the sulfuric acid of consumption, passes through formula:
Wherein, VH2SO4Titrate the volume mL of the sulfuric acid solution of consumption；
CH2SO4Titrate the concentration mol/L of the sulfuric acid solution of consumption；
M- sample to be tested quality g；
You can get it, and polymethoxy dibutyl mixes the content of formaldehyde in etherate.
Measuring principle: it is reacted using formaldehyde with excessive sodium sulfite and generates sodium hydroxide, with the sulfuric acid standard of 1mol/L
The sodium hydroxide that solution titration generates, the amount of formaldehyde are equivalent to the amount for the sodium hydroxide that reaction generates.
Reaction equation is as follows:
HCHO+Na2SO3+H2O=NaOH+CH2(NaSO3)OH
2NaOH+H2SO4=Na2SO4+H2O
Blank control: drawing 50mL sodium sulfite solution and be placed in the conical flask of 250mL, and 2~3 drop thymolphthaleins is added to refer to
Show agent, then become colorless with the sulfuric acid standard solution of 1mol/L titration blue, records the volume of sulfuric acid, this experiment is tried as blank
It tests.
(3) polymethoxy dibutyl ethers mixture is centrifuged, takes supernatant, then calcium chloride dehydration is added into supernatant,
Obtain sample to be tested.
(4) polymethoxy dibutyl ethers are produced using Beijing DongXi Analytical Instrument Co., Ltd GC-4000A gas chromatograph
Product are analyzed, and gas chromatograph has fid detector, chromatographic column: HP-5 capillary column (30m × 0.32mm × 0.25 μm),
Nitrogen is opened, nitrogen flow is adjusted, makes its flow velocity 150mL/min, will test room temperature and be set as 260 DEG C, temperature of vaporization chamber
280 DEG C are set as, column temperature is set as 50 DEG C, keeps initial temperature 2min, then again sets temperature programming to 50 DEG C/min
Speed be warming up to 260 DEG C, and keep 9min, press operation key and start to warm up；Air, hydrogen valve are opened again, adjust its flow,
Make hydrogen flow rate 40mL/min, air velocity 400mL/min, after the completion of heating, start to light a fire, after baseline is walked surely
Sample introduction.
(5) after baseline is walked surely, sample to be tested rinse 3 times repeatedly to be measured are drawn with sample injector, then use split sampling
Method sample to be tested is detected, split ratio 100:1, sample volume be 0.2 μ L, chromatogram is obtained, using area normalization
Method analyzes chromatogram, and calculates the content of each component in sample to be tested, then remove moisture and first obtained in step (1) and (2)
Aldehyde, the content and purity of polymethoxy dibutyl ethers in you can get it sample, the result is shown in tables 1.
Embodiment 3
A kind of detection method of polymethoxy dibutyl ethers content, comprising the following steps:
(1) 2g polymethoxy dibutyl ethers mixture is weighed, it is mixed using Karl_Fischer method measurement polymethoxy dibutyl ethers
It closes the moisture content in object to be injected into sample in karl Fischer moisture teller with syringe, automatically determines out moisture and contain
Amount.
Karl_Fischer method principle: the card of moisture (free water or the crystallization water) and known titer of any state in sample
Your C.Fischer (iodine, sulfur dioxide, pyridine and methanol composition solution) carry out quantitative reaction, with current potential directing terminal, according to
Consumable liquid volume finds out moisture content, and reaction equation is as follows:
H2O+I2+SO2+3C5H5N→2C5H5N·HI+C5H5N·SO3
C5H5N·SO3+CH3OH→C5H5NH·OSO2OCH3
(2) measurement polymethoxy dibutyl mixes the content of formaldehyde in etherate
Content of formaldehyde in etherate is mixed using determination of acid-basetitration polymethoxy dibutyl, weighs 2g polymethoxy two
Butyl ether mixture is placed in 250mL conical flask, and the dissolution of 50mL sodium sulfite solution is added, then 2~3 drops hundred are added dropwise thereto
In fragrant phenolphthalein indicator, then titrated with the sulfuric acid solution of 1mol/L, until testing sample solution is become colorless by blue, recorded
The volume of the sulfuric acid of consumption, passes through formula:
Wherein, VH2SO4Titrate the volume mL of the sulfuric acid solution of consumption；
CH2SO4Titrate the concentration mol/L of the sulfuric acid solution of consumption；
M- sample to be tested quality g；
You can get it, and polymethoxy dibutyl mixes the content of formaldehyde in etherate.
Measuring principle: it is reacted using formaldehyde with excessive sodium sulfite and generates sodium hydroxide, with the sulfuric acid standard of 1mol/L
The sodium hydroxide that solution titration generates, the amount of formaldehyde are equivalent to the amount for the sodium hydroxide that reaction generates
Reaction equation is as follows:
HCHO+Na2SO3+H2O=NaOH+CH2(NaSO3)OH
2NaOH+H2SO4=Na2SO4+H2O
Blank control: drawing 50mL sodium sulfite solution and be placed in the conical flask of 250mL, and 2~3 drop thymolphthaleins is added to refer to
Show agent, then become colorless with the sulfuric acid standard solution of 1mol/L titration blue, records the volume of sulfuric acid, this experiment is tried as blank
It tests.
(3) polymethoxy dibutyl ethers mixture is centrifuged, takes supernatant, then calcium sulfate dehydration is added into supernatant,
Obtain sample to be tested.
(4) polymethoxy dibutyl ethers are produced using Beijing DongXi Analytical Instrument Co., Ltd GC-4000A gas chromatograph
Product are analyzed, and gas chromatograph has fid detector, chromatographic column: HP-5 capillary column (30m × 0.32mm × 0.25 μm),
Nitrogen is opened, nitrogen flow is adjusted, makes its flow velocity 150mL/min, will test room temperature and be set as 220 DEG C, temperature of vaporization chamber
240 DEG C are set as, column temperature is set as 40 DEG C, then set being warming up to 50 DEG C with the speed of 5 DEG C/min for temperature programming again, then
260 DEG C are warming up to the speed of 40 DEG C/min, and keeps 8min, operation key is pressed and starts to warm up；Air, hydrogen valve are opened again,
Its flow is adjusted, makes hydrogen flow rate 40mL/min, air velocity 400mL/min, after the completion of heating, start to light a fire, to base
Line can sample introduction after walking surely.
(5) after baseline is walked surely, sample to be tested rinse 5 times repeatedly to be measured are drawn with sample injector, then use split sampling
Method sample to be tested is detected, split ratio 100:1, sample volume be 0.2 μ L, chromatogram is obtained, using area normalization
Method analyzes chromatogram, and calculates the content of each component in sample to be tested, then remove moisture and first obtained in step (1) and (2)
Aldehyde, the content and purity of polymethoxy dibutyl ethers in you can get it sample, the result is shown in tables 1.
Each component content in 1 sample to be tested of table
Claims (5)
1. a kind of detection method of polymethoxy dibutyl ethers content, which comprises the following steps:
(1) moisture content in polymethoxy dibutyl ethers mixture is measured；
(2) content of formaldehyde in polymethoxy dibutyl ethers mixture is measured；
(3) polymethoxy dibutyl mixture is centrifuged, takes supernatant, then desiccant dehydration is added into supernatant, obtains to be measured
Sample；
(4) chromatographic condition is selected: the gas chromatograph with fid detector；Chromatographic column: HP-5 capillary column；Chromatographic condition are as follows:
35 DEG C of column temperature；Temperature of vaporization chamber: 280 DEG C；Fid detector: 280 DEG C；Temperature programming: rising to 45 DEG C with 2 DEG C/min rate, then with
50 DEG C/min rate rises to 245 DEG C, keeps 10min；Nitrogen flow rate is 150mL/min；Hydrogen flow rate: 40mL/min；Air stream
Speed: 400mL/min；
(5) gas chromatograph parameters are set by step (4) described chromatographic condition, after baseline is walked surely, is drawn with sample injector to test sample
Product rinse 3~5 times repeatedly, then detect sample to be tested, then remove moisture and formaldehyde obtained in step (1) and (2)
Content, the content and purity of polymethoxy dibutyl ethers in you can get it sample.
2. the detection method of polymethoxy dibutyl ethers content according to claim 1, which is characterized in that in step (1)
The method for measuring moisture content in polymethoxy dibutyl ethers mixture is Karl_Fischer method.
3. the detection method of polymethoxy dibutyl ethers content according to claim 1, which is characterized in that in step (2)
Measuring the method that polymethoxy dibutyl mixes content of formaldehyde in etherate is acid-base titration；Wherein, the acid is sulfuric acid, instruction
Agent is Thymol phthalein indicator.
4. the detection method of polymethoxy dibutyl ethers content according to claim 1, which is characterized in that in step (3)
The desiccant is molecular sieve, calcium sulfate or calcium chloride.
5. the detection method of polymethoxy dibutyl ethers content according to claim 1, which is characterized in that in step (5)
The input mode is split sampling, and sample volume is 0.2~0.4 μ L, split ratio 100:1.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2011012339A1 (en) * | 2009-07-31 | 2011-02-03 | Man Nutzfahrzeuge Aktiengesellschaft | Use of polyoxymethylene (alkyl polyglycol) ethers as an additive to diesel fuels for lowering the soot emission in spontaneous combustion engines |
| CN105753666A (en) * | 2016-05-10 | 2016-07-13 | 中国人民解放军总后勤部油料研究所 | Method for preparing polyoxymethylene dimethyl ether |
-
2017
- 2017-03-31 CN CN201710207436.1A patent/CN107014918B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2011012339A1 (en) * | 2009-07-31 | 2011-02-03 | Man Nutzfahrzeuge Aktiengesellschaft | Use of polyoxymethylene (alkyl polyglycol) ethers as an additive to diesel fuels for lowering the soot emission in spontaneous combustion engines |
| CN105753666A (en) * | 2016-05-10 | 2016-07-13 | 中国人民解放军总后勤部油料研究所 | Method for preparing polyoxymethylene dimethyl ether |
Non-Patent Citations (2)
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| 新型柴油添加剂聚缩醛二甲醚的分离研究;胡国庆 等;《石油与天然气化工》;20151231;第44卷(第5期);第52-59页 |
| 无标样聚甲氧基二甲醚校正因子的测定;郑妍妍 等;《高效化学工程学报》;20150630;第29卷(第3期);第506页 |
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Address after: Dazhou City, Sichuan Province, 635066 River Road District No. 25 Patentee after: Sichuan Daxing Energy Co., Ltd Patentee after: Institute of Military New Energy Technology, Institute of Systems Engineering, Academy of Military Sciences Address before: Dazhou City, Sichuan Province, 635066 River Road District No. 25 Patentee before: SICHUAN DAXING ENERGY Co.,Ltd. Patentee before: INSTITUTE OF OIL PLANT, LOGISTIC SUPPORT DEPARTMENT OF THE CENTRAL MILITARY COMMISSION |
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Effective date of registration: 20211027 Address after: Dazhou City, Sichuan Province, 635000 River Road District No. 25 Patentee after: Sichuan Daxing Energy Co., Ltd Patentee after: Institute of military new energy technology, Academy of systems engineering, Academy of Military Sciences Patentee after: Beijing Dongfang Hongsheng New Energy Application Technology Research Institute Co.,Ltd. Address before: No.25 Xihe Road, Tongchuan District, Dazhou City, Sichuan Province Patentee before: Sichuan Daxing Energy Co., Ltd Patentee before: Institute of Military New Energy Technology, Institute of Systems Engineering, Academy of Military Sciences |
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Correction item: Patentee|Address|Patentee Correct: Sichuan Daxing Energy Co., Ltd|Dazhou City, Sichuan Province, 635000 River Road District No. 25|Institute of military new energy technology, Institute of systems engineering, Academy of Military Sciences|Beijing Dongfang Hongsheng New Energy Application Technology Research Institute Co., Ltd False: Sichuan Daxing Energy Co., Ltd|Dazhou City, Sichuan Province, 635000 River Road District No. 25|Institute of military new energy technology, Academy of systems engineering, Academy of Military Sciences|Beijing Dongfang Hongsheng New Energy Application Technology Research Institute Co., Ltd Number: 46-01 Volume: 37 |