CN109612816A - A kind of pre-treating method of higher boiling aromatic compound trace metal ion test - Google Patents
A kind of pre-treating method of higher boiling aromatic compound trace metal ion test Download PDFInfo
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- CN109612816A CN109612816A CN201811291970.6A CN201811291970A CN109612816A CN 109612816 A CN109612816 A CN 109612816A CN 201811291970 A CN201811291970 A CN 201811291970A CN 109612816 A CN109612816 A CN 109612816A
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- aromatic compound
- higher boiling
- boiling aromatic
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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
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/40—Concentrating samples
- G01N1/4044—Concentrating samples by chemical techniques; Digestion; Chemical decomposition
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Abstract
The invention discloses a kind of pre-treating methods of higher boiling aromatic compound trace metal ion test, higher boiling aromatic compound is placed in platinum crucible, gradient increased temperature is heated to higher boiling aromatic compound and is evaporated, and is proportionally added into after cooling to be measured after dilute nitric acid solution.Pre-treating method provided by the invention realizes the resolution of higher boiling aromatic compound completely, and elapsed time is short, shortens detection time, so that it is guaranteed that the detection reproducibility of sample, improves the accuracy of testing result.
Description
Technical field
The present invention relates to the pre-treatment of trace metal ion test more particularly to a kind of higher boiling aromatic compound are micro
The pre-treating method of metal ion test.
Background technique
Lithium-ion battery electrolytes oxidationreduction electricity has become lithium ion battery to additive and overcharges protection limiting voltage additives
Chief component.This kind of compounds mainly include aromatic compound, Metallocenic compound, polypyridine complex, lithium
Halide, thianthrene, anisole etc..Wherein aromatic compound includes biphenyl (BP), cyclohexyl benzene (CHB), toluene class chemical combination
Object, aromatic radical adamantane, naphthalene derivatives and poly benzene etc. will not generally be generated cycle performance to battery and storage life
It is apparent to influence, it is the limiting voltage additives of lithium ion battery most application value and prospect.
It is extremely stringent in view of control requirement of the lithium-ion battery electrolytes to foreign metal ion, therefore to additive therefor
Foreign metal ion is even more stringent control to ppm grades.Currently, the detection of metal ion generally uses inductively coupled plasma atom
Emission spectrometer (ICP) is detected, and in the detection process, instrument sampling system requires the content of organics of sample to the instrument
It cannot be too high.Because organic matter has very high phosphorus content, and ICP is " electrical fire flame ", and organic matter can not in argon atmospher
Full combustion, will form carbon distribution, will lead to flame-out when serious, and the organic matter of high volatile can change the thermodynamic behaviour of ICP,
So that spectrum behavior becomes unstable, thus for the sample of ICP test need to carry out pre-treatment resolution remove it is organic in sample
Object.There are three types of modes for conventional test pre-treatment digestion procedure: wet digestion, dry method resolution, micro-wave digestion, and dry method resolution needs
Carbonization ashing is carried out to sample, time-consuming, and easily entrains pollution, wherein common wet digestion general operation process is to weigh
Sample is placed in polytetrafluoroethylene beaker, and HNO is added3Heating resolution is done to close, cooling, then is diluted to one with lower concentration nitric acid
It is quantitative, while doing blank.It is found when testing the aromatic compounds such as similar biphenyl, the result of Duplicate Samples is found in test process
Difference increases, and collimation is poor, and result precision is not high, and torch pipe carbon distribution is serious, plasma unstable, and preliminary judgement should
It is that polytetrafluoroethylene beaker can not carry out High-temperature Digestion, causes the resolution of the aromatic compounds such as similar biphenyl incomplete, sample introduction
Caused by determinand contains certain organic matter in the process, and HNO is added in digestion process3, evolution is sour in a heated condition
Property gas, influences the health of operator, also polluted atmospheric environment.
In consideration of it, when carrying out the detection of aromatic metal compound foreign ion, it is necessary to which providing a kind of can make in sample
Aromatic compound can clear up completely, improve detection accuracy and environment amenable pre-treating method.
Summary of the invention
The present invention provides a kind of using inductively coupled plasma atomic emission spectrometry instrument test higher boiling aromatic compound
The pre-treating method of middle minor metallic element, resolution is time-consuming short, shortens detection time, guarantees that aromatic compound disappears completely
Solution, it is ensured that the detection reproducibility of sample improves accuracy in detection, and no acidic gas overflowing when resolution, reduces to operator
The influence of health reduces the pollution of atmospheric environment.
Technical solution provided by the present invention is as follows:
A kind of pre-treating method of higher boiling aromatic compound trace metal ion test, by higher boiling aromatic compound
Object is placed in platinum crucible, and higher boiling aromatic compound is placed in platinum crucible, and gradient increased temperature is heated to higher boiling fragrance
Compounds of group is evaporated, and is proportionally added into after cooling to be measured after dilute nitric acid solution.
The present invention is using the digestion container that platinum crucible is as higher boiling aromatic compound, and platinum crucible fusing point is
It 1775.5 DEG C, can tolerate high-temperature heating, and heating condition controlled by gradient increased temperature, heating condition is avoided acutely to lead to higher boiling
Aromatic compound rapid expanding is overflowed, and is caused sample loss, is influenced testing result accuracy, by higher boiling aromatic compound
It is evaporated and is carbonized completely, dilute nitric acid solution is added after cooling and sufficiently dissolves sample, reduces analytical error, realizes elapsed time
It is short, shorten detection time, and higher boiling aromatic compound is cleared up completely, reduces interference of the aromatic compound to inspection,
Ensure the detection reproducibility of sample, and processing method provided by the present invention is not necessarily to that dust technology is added in heating digestion process,
It avoids thering is sour gas evolution stimulation applications personnel respiratory mucosa to cause discomfort in heating process, while also reducing sour gas
It is discharged into atmospheric environment, reduces atmosphere pollution.
Further, the platinum crucible outer wall height is 5cm or more.The height of platinum crucible outer wall then adds lower than 5cm
Higher boiling aromatic compound is easily overflowed by thermal evaporation expansion capacity in thermal evaporation process, is caused object to be detected to lose, is influenced to detect
Result precision.
Further, it is 80 DEG C~100 DEG C that the gradient increased temperature heating condition, which is initial temperature, with 2 DEG C~5 DEG C/min
Constant temperature 0.5~2.0 hour after heating rate is warming up to 220 DEG C~500 DEG C.Initial temperature controls within the scope of 80 DEG C~100 DEG C
After so that low-boiling compound is volatilized, constant temperature 0.5 after being to slowly warm up to 220 DEG C~500 DEG C with 2 DEG C~5 DEG C/min heating rates~
2.0 hours, avoiding the too fast higher boiling aromatic compound expansion of heating rate from overflowing led to sample loss, influenced testing result
Accuracy, constant temperature 0.5~2.0 hour certifiable higher boiling aromatic compound is cleared up completely after being warming up to maximum temperature.
Further, the additive amount of the higher boiling aromatic compound is 0.1~1.0g.Additive amount is then measured lower than 0.1g
It is very few, lower than equipment detection limit, influence the confidence level of testing result；Additive amount is higher than 1.0g, and then additive amount is excessive, heating resolution
Container is overflowed in Shi Rongyi expansion, leads to sample loss, influences the accuracy of testing result.
Further, the higher boiling aromatic compound is biphenyl, cyclohexyl benzene, methylbenzenes.It is high boiling to reveal
Closing object is lithium-ion battery electrolytes oxidationreduction point to the main constituents in additive, further include aromatic radical adamantane,
Naphthalene derivatives and poly benzene etc..
Further, the ratio of the higher boiling aromatic compound and dilute nitric acid solution is 1: 20~1: 30.Dust technology
Solution additive amount is excessively few then can not sufficiently to dissolve sample, influence the reproducibility of inspection result, additive amount excessively then leads to sample
Concentration is too low, influences the accuracy of inspection result.
Further, the mass fraction of the dilute nitric acid solution is 0.1~1.0%.Dust technology in this concentration range
Solution is oxidable to decompose most of organic matters, and it is optimal resolution object that the metal of most dissolving with hydrochloric acid can also be dissolved with nitric acid
Dissolution solvent.
It is provided by the invention to have the beneficial effect that:
The first, digestion time is short, shortens detection time；The present invention is using platinum crucible resistant to high temperature as higher boiling aromatic series
The carrier of compound, guaranteeing that heating condition mitigates and can rise to high temperature using gradient increased temperature heating method makes higher boiling aromatic series
It closes object sufficiently to clear up, solves traditional digestion procedure and need to guarantee sample by extending digestion time due to cannot achieve High-temperature Digestion
The problem of product are sufficiently cleared up substantially reduces digestion time, to also shorten entire sample detection time, improves detection effect
Rate；
The second, favorable reproducibility is detected, accuracy in detection is improved；Conventional wet resolution general operation process is that will weigh sample
It is placed in polytetrafluoroethylene beaker, nitration acid heat is added and clears up to close dry, cooling, then is diluted to centainly with lower concentration nitric acid
Amount, while blank is done, but higher boiling aromatic compound can not be cleared up completely when test higher boiling aromatic compound, it lead
Cause Duplicate Samples test result difference big, collimation is poor；The present invention by step high temperature clear up, gradient increased temperature heating condition it is initial
Temperature is 80 DEG C~100 DEG C, constant temperature 0.5~2.0 hour after being warming up to 220 DEG C~500 DEG C with 2 DEG C~5 DEG C/min heating rates
It clears up higher boiling aromatic compound sufficiently, adds dilute nitric acid solution dilution and dissolve up to the sample solution cleared up completely,
Aromatic compound is avoided not clear up completely the difference for leading to replicate test result；
Third, treatment process are mildly pollution-free；The present invention utilizes platinum crucible property resistant to high temperature, directly passes through gradient height
Temperature heating resolution higher boiling aromatic compound makes heated it is not necessary that the acid solutions such as nitric acid are added as auxiliary resolution solvent
Sour gas evolution is not had in journey, avoids operator from sucking sour gas stimulation respiratory mucosa and do not feel good, may be used also
Acid gas emissions are reduced into atmospheric environment, are reduced environmental pollution.
Specific embodiment
In order to which the technical problems, technical solutions and beneficial effects solved by the present invention is more clearly understood, below in conjunction with
Embodiment, the present invention will be described in further detail.It should be appreciated that specific embodiment described herein is only used to explain
The present invention is not intended to limit the present invention.
The invention discloses a kind of pre-treating methods of higher boiling aromatic compound trace metal ion test: will be high boiling
Point aromatic compound is placed in platinum crucible, and gradient increased temperature is heated to higher boiling aromatic compound and is evaporated, it is cooling after by than
It is to be measured after example addition dilute nitric acid solution, while blank sample is done with the nitric acid solution of same concentration.
Wherein, the outer wall height of the platinum crucible is 5cm or more.
Wherein, the initial temperature of the gradient increased temperature heating condition is 80 DEG C~100 DEG C, is heated up with 2 DEG C~5 DEG C/min
Constant temperature 0.5~2.0 hour after rate is warming up to 220 DEG C~500 DEG C.
Wherein, the additive amount of the higher boiling aromatic compound is 0.1~1.0g.
Wherein, the higher boiling aromatic compound is biphenyl, cyclohexyl benzene, methylbenzenes.
Wherein, the ratio of the higher boiling aromatic compound and dilute nitric acid solution is 1: 20~1: 30.
Wherein, the mass fraction of the dilute nitric acid solution is 0.1~1.0%.
Below by way of specific embodiment, the present invention will be described in detail.It should be appreciated that these embodiments be only it is exemplary,
It does not constitute a limitation on the scope of protection of the present invention.
Embodiment 1
It weighs biphenyl (BP) 0.5000g sample to be placed in the platinum crucible of a height of 5cm of wall, in heating on electric hot plate, initially
Temperature is 80 DEG C and is heated to sample dissolution, is warming up to 280 DEG C with 3 DEG C/min of heating rates, is heated to the steaming of crucible bottom sample
It is dry, then sample on sidewall of crucible will be condensate in constant temperature 1 hour after 300 DEG C with 3 DEG C/min of raising temperature and be evaporated, it is dilute to be added 0.2%
Nitric acid solution 15mL, while blank is done with 0.2% dilute nitric acid solution.Data measured is as follows, same sample test result twice
Collimation is good.
Embodiment 2
It weighs cyclohexyl benzene (CHB) 0.5000g sample to be placed in the platinum crucible of a height of 5cm of wall, in heating on electric hot plate
Initial temperature is 100 DEG C and is heated to sample dissolution, is warming up to 260 DEG C with 5 DEG C/min of heating rates, is heated to crucible bottom sample
Product are evaporated, then will be condensate in sample on sidewall of crucible to constant temperature 2 hours after 280 DEG C with 5 DEG C/min of raising temperature and be evaporated, and are added
0.5% dilute nitric acid solution 10mL, while blank is done with 0.5% dilute nitric acid solution.Data measured is as follows, and the same sample is surveyed twice
Test result collimation is good.
Embodiment 3
It weighs naphthalene 0.5000g sample to be placed in the platinum crucible of a height of 5cm of wall, is in heating initial temperature on electric hot plate
100 DEG C are heated to sample dissolution, are warming up to 220 DEG C with 2 DEG C/min of heating rates, are heated to crucible bottom sample and are evaporated, then with
2 DEG C/min of raising temperature will be condensate in sample on sidewall of crucible to constant temperature 2 hours after 240 DEG C and be evaporated, and it is molten that 1.0% dust technology is added
Liquid 15mL, while blank is done with 1.0% dilute nitric acid solution.Data measured is as follows, same sample test result collimation twice
It is good.
Embodiment 4
It weighs cyclohexyl benzene (CHB) 0.1050g sample to be placed in the platinum crucible of a height of 5cm of wall, in heating on electric hot plate
Initial temperature is 100 DEG C and is heated to sample dissolution, is warming up to 260 DEG C with 5 DEG C/min of heating rates, is heated to crucible bottom sample
Product are evaporated, then will be condensate in sample on sidewall of crucible to constant temperature 1 hour after 280 DEG C with 5 DEG C/min of raising temperature and be evaporated, and are added
0.5% dilute nitric acid solution 10mL, while blank is done with 0.5% dilute nitric acid solution.Data measured is as follows, and the same sample is surveyed twice
Test result collimation is good.
In conclusion the pre-treating method of higher boiling aromatic compound trace metal ion test provided by the invention,
Higher boiling aromatic compound can be cleared up completely, eliminate influence of the aromatic compound to test result collimation, improve knot
Fruit accuracy, and can effectively shorten its digestion process time, greatly improve detection efficiency.
The foregoing is only a preferred embodiment of the present invention, is not intended to limit the present invention in any form；It is all
The those of ordinary skill of the industry can implement the present invention by the above and swimmingly；But all technologies for being familiar with this profession
Personnel without departing from the scope of the present invention, a little change for being made using disclosed above technology contents,
Modification and the equivalent variations developed, are equivalent embodiment of the invention；Meanwhile all substantial technologicals according to the present invention are to above
The variation, modification and evolution etc. of any equivalent variations made by embodiment still fall within the protection model of technical solution of the present invention
Within enclosing.
Claims (6)
1. a kind of pre-treating method of higher boiling aromatic compound trace metal ion test, it is characterised in that: by higher boiling
Aromatic compound is placed in platinum crucible, and gradient increased temperature is heated to higher boiling aromatic compound and is evaporated, after cooling in proportion
It is to be measured after addition dilute nitric acid solution.
2. the pre-treating method of higher boiling aromatic compound trace metal ion test according to claim 1, special
Sign is: the initial temperature of the gradient increased temperature heating condition is 80 DEG C~100 DEG C, with 2 DEG C~5 DEG C/min heating rate liters
Temperature was to constant temperature 0.5~2.0 hour after 220 DEG C~500 DEG C.
3. the pre-treating method of higher boiling aromatic compound trace metal ion test according to claim 1, special
Sign is: the additive amount of the higher boiling aromatic compound is 0.1~1.0g.
4. the pre-treating method of higher boiling aromatic compound trace metal ion test according to claim 3, special
Sign is: the higher boiling aromatic compound is biphenyl, cyclohexyl benzene, methylbenzenes.
5. the pre-treatment of higher boiling aromatic compound trace metal ion test according to any one of claims 1 to 4
Method, it is characterised in that: the ratio of the higher boiling aromatic compound and dilute nitric acid solution is 1: 20~1: 30.
6. the pre-treating method of higher boiling aromatic compound trace metal ion test according to claim 5, special
Sign is: the mass fraction of the dilute nitric acid solution is 0.1~1.0%.
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Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1662446A (en) * | 2002-04-18 | 2005-08-31 | 信大科学－生产有限股份公司 | Method for producing diamond-containing synthetic materials |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1662446A (en) * | 2002-04-18 | 2005-08-31 | 信大科学－生产有限股份公司 | Method for producing diamond-containing synthetic materials |
Non-Patent Citations (2)
| Title |
|---|
| 白凤有: "原油中微量金属元素检测样品处理技术", 《2018油气田勘探与开发国际会议论文集》 * |
| 穆琳: "基于原子光谱技术的润滑油监测与磨损机理研究", 《中国优秀硕士学位论文全文数据库 工程科技I辑》 * |
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Application publication date: 20190412 |