CN101726482A - Method for detecting content of elements in oil with inductively coupled plasma (ICP) spectrometer - Google Patents
Method for detecting content of elements in oil with inductively coupled plasma (ICP) spectrometer Download PDFInfo
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- CN101726482A CN101726482A CN200910264829A CN200910264829A CN101726482A CN 101726482 A CN101726482 A CN 101726482A CN 200910264829 A CN200910264829 A CN 200910264829A CN 200910264829 A CN200910264829 A CN 200910264829A CN 101726482 A CN101726482 A CN 101726482A
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Abstract
The invention discloses a method for detecting the content of elements in oil with an inductively coupled plasma (ICP) spectrometer. The ICP spectrometer comprises a torque tube, and the torque tube is formed by three layers of concentric quartz tubes. Cooling gas is guided into the quartz tube of the outer layer, oxygen is guided into the quartz tube of the middle layer and gasoloid of the oil which is diluted by organic solution is injected into the quartz tube of the outer layer. The method for detecting the content of elements in oil with the ICP spectrometer makes up the deficiency of the prior art.
Description
Technical field
The present invention relates to a kind of method that detects constituent content in the oil, particularly a kind of method that detects constituent content in the oil with the ICP spectrometer.
Background technology
Lubricating oil is in machine-building, and communications and transportation is used widely in the numerous areas such as petroleum industry.Additive element content is normally represented the important indicator of quality of lubrication oil and usability in the lubricating oil.What the method application of detection lubricating oil was maximum at present is atomic emission spectrometry, atomic absorption spectrography (AAS) and X fluorescent spectrometry, lubricated oil treatment process generally is by the dry ashing method, the wet type resolution method, Microwave Digestion emulsifying technology method becomes aqueous solution with processes such as extraction separation methods with sample preparation, also has a kind of organic faster direct injected method.
The dry ashing method generally is after making the sample charing by muffle furnace high temperature, becomes aqueous solution with acid dissolving ash treatment, and this method is simple to operate, and the method detection limit is low, but the pre-treatment time is long, and energy consumption is bigger, and is not suitable for the analysis of Volatile Elements.Wet method clear up then be acid by strong oxidizing property with the organic principle carbonization in the sample, be processed into aqueous solution with nitric acid dissolve again.Micro-wave digestion is sample to be placed in the high-pressure closed vessel clear up, and this method is less because of its sample weighting amount, is fit to the mensuration of the higher element of content.Above-mentioned this several method program is more loaded down with trivial details, time-consuming longer, and in the sample preparation process, cause bigger pollution to environment, the X fluorescent spectrometry has it quick, harmless advantage, but the fluoroscopic examination principle has limited its application on determination of trace element.
ICP spectrometer (plasma emission spectrometer) is obtaining application widely as a kind of Atomic Emission Spectrometer AES device of precision aspect the species analysis, the ICP spectrometer mainly is made up of radio-frequency generator and induction coil, torch pipe and air supply system, sample drawing-in system three parts.Wherein torch Guan Yousan layer concentric quartz tubes formed.Outer tube leads to cold gas, and purpose is to make plasma leave outer quartz ampoule inwall, burns quartz ampoule to avoid it.Flue is done in middle level quartz ampoule outlet, feeds Ar gas and works to keep plasma.Carrier gas carrier band sample gasoloid is by in the interior pipe injected plasma, and the sample gasoloid is produced by pneumatic nebulizer or ultrasonic atomizer.
But there are following technical difficulties when adopting the ICP spectrometer that this oil solvent of lubricating oil is analyzed:
(1) organic ICP significantly changes the reflected impedance of plasma after introducing the ICP light source, thereby has changed the impedance matching state of plasma load and radio-frequency generator.Can cause plasma unstable when serious even extinguish fully.Sometimes also can burn ICP torch pipe.
(2) after oil enters ICP, at high temperature decompose the uncombined carbon that produces, easily form carbon granules and be deposited on the mouth of pipe, influence the stable operation and the spectroscopic assay of plasma.
(3) during the ICP spectral analysis of organic sample, light emitted goes out multiple molecule bands of a spectrum, disturb determination of trace elements, particularly cyanogen band spectrum is particularly serious to the interference of determination of trace element, the generation of its cyanogen band spectrum comes from carbon and the reaction of N on every side that the sample gasoloid decomposites in plasma flame, form stable cyanogen compound.
(4) various organic solvents and its viscosity of oils sample and physical property are widely different, increase workload to sample preparation.
(5) standard model preparation difficulty generally will be prepared standard specimen solution with corresponding organometallics.And organometallics can not prepare and obtain easily.Commercially available organic standard sample type rareness and price are more expensive.
Summary of the invention
At above-mentioned the deficiencies in the prior art, the technical problem to be solved in the present invention provides a kind of method with constituent content in the ICP spectrometer detection oil, overcomes the difficulty that prior art exists.
For solving the problems of the technologies described above, the present invention adopts following technical scheme:
A kind of method that detects constituent content in the oil with the ICP spectrometer, described ICP spectrometer comprises a torch pipe, described torch Guan Yousan layer concentric quartz tubes formed, this ICP spectrometer is when analyzing oil, in the outer quartz ampoule of described torch pipe, feed cold gas, aerating oxygen in the quartz ampoule of the middle level of described torch pipe injects the gasoloid by the oil after the described oil solution dilution in the internal layer quartz ampoule of described torch pipe.
Preferably, the flow of described cold gas is 18L/ minute.
Preferably, the flow of described oxygen is 0.3L/ minute.
Preferably, the organic solution of diluting described oil is light diesel fuel or dimethylbenzene or MIBK.
Preferably, the oil of being analyzed is lubricating oil.
Technique scheme has following beneficial effect: in this scheme, by in the outer quartz ampoule of torch pipe, feeding cold gas, around making plasma air and plasma are separated, stop nitrogen to enter plasma, reduce the formation of cyanogen band spectrum, avoid its interference determination of trace element.Aerating oxygen in the quartz ampoule of the middle level of torch pipe can be avoided the oxidation of coal that produces in the oily sample testing process to form carbon distribution at the torch pipe mouth of pipe on the one hand, can suppress the generation of cyanogen band spectrum on the other hand.If oil viscosity is bigger, can adopt organic solution that oil is diluted, can make oil enter atomizing more easily behind the ICP spectrometer.
Embodiment
Below the preferred embodiments of the present invention are described in detail.
Below by using the ICP spectrometer that the embodiment that constituent content in the lubricating oil carries out check and analysis is come the present invention is described in detail.At first lubricating oil is diluted with organic solution, organic solution can be selected light diesel fuel or dimethylbenzene or MIBK for use, and these three kinds of organic solvents all can dissolve lubricating oil, and better bin stability is arranged, but from the security consideration of thinning agent, we select light diesel fuel as thinning agent.Lubricating oil after will diluting after lubricating oil dilution is finished injects in the internal layer quartz ampoule of ICP spectrometer torch pipe, meanwhile in the outer quartz ampoule of this torch pipe, lead to cold gas, the flow of cold gas is 18L/ minute, logical oxygen in the quartz ampoule of the middle level of this torch pipe, and the flow of oxygen is 0.3L/ minute.
Adopt such scheme by in the outer quartz ampoule of torch pipe, feeding cold gas, plasma is separated air and plasma on every side, stop nitrogen to enter plasma, reduce the formation of cyanogen band spectrum, avoid its interference determination of trace element.Aerating oxygen in the quartz ampoule of the middle level of torch pipe can be avoided the oxidation of coal that produces in organic sample testing process to form carbon distribution at the torch pipe mouth of pipe on the one hand, can suppress the generation of cyanogen band spectrum on the other hand.Because lubricating oil viscosity is bigger, adopt organic solution that lubricating oil is diluted, can make lubricating oil enter atomizing more easily behind the ICP spectrometer.
Following table is carried out 7 test findings of replicate determination for adopting this method to same lubricating oil standard specimen.
By the analysis to above table, the relative deviation (PSD) of each constituent content of lubricating oil is all less than 5% in these 7 times experiments, and visible the method has good repeatability.
Mark-on reclaims experiment:
Take by weighing 2.0,8.0 respectively, 20.0g lubricating oil standard solution with light diesel fuel dilution and constant volume, then obtains concentration and is respectively 2.0,8.0 in the 100ml volumetric flask, and the sample solution of 20.0mg/L20 kind detects with ICP, and the recovery sees the following form.
By analysis, adopt this kind method that lubricating oil is analyzed as can be known and have the higher recovery simultaneously above table.
More than a kind of method that detects constituent content in the oil with the ICP spectrometer was described in detail to the embodiment of the invention provides; for one of ordinary skill in the art; thought according to the embodiment of the invention; part in specific embodiments and applications all can change; in sum; this description should not be construed as limitation of the present invention, and all any changes of making according to design philosophy of the present invention are all within protection scope of the present invention.
Claims (5)
1. method that detects constituent content in the oil with the ICP spectrometer, described ICP spectrometer comprises a torch pipe, described torch Guan Yousan layer concentric quartz tubes formed, it is characterized in that: this ICP spectrometer is when analyzing oil, in the outer quartz ampoule of described torch pipe, feed cold gas, aerating oxygen in the quartz ampoule of the middle level of described torch pipe injects the gasoloid by the oil after the described oil solution dilution in the internal layer quartz ampoule of described torch pipe.
2. the method with constituent content in the ICP spectrometer detection oil according to claim 1, it is characterized in that: the flow of described cold gas is 18L/ minute.
3. the method with constituent content in the ICP spectrometer detection oil according to claim 1, it is characterized in that: the flow of described oxygen is 0.3L/ minute.
4. the method with constituent content in the ICP spectrometer detection oil according to claim 1, it is characterized in that: the organic solution of diluting described oil is light diesel fuel or dimethylbenzene or MIBK.
5. the method with constituent content in the ICP spectrometer detection oil according to claim 1, it is characterized in that: the oil of being analyzed is lubricating oil.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102692407A (en) * | 2011-03-24 | 2012-09-26 | 张家港市国泰华荣化工新材料有限公司 | Method for analysis of metal impurity ions of organic solvent |
| CN103604940A (en) * | 2013-11-26 | 2014-02-26 | 福州大学 | Inductively coupled plasma-atomic emission spectrometry/mass spectrometry (ICP-AES/ MS) switching-free type organic sampling device |
| CN108444983A (en) * | 2018-03-22 | 2018-08-24 | 山东出入境检验检疫局检验检疫技术中心 | A kind of torch pipe for measuring volatile materials |
| CN111721753A (en) * | 2020-05-15 | 2020-09-29 | 上海应用技术大学 | Device and method for directly feeding samples into oil product |
| CN112858263A (en) * | 2021-01-15 | 2021-05-28 | 中国神华煤制油化工有限公司 | Method for measuring content of metal elements in organic solution |
-
2009
- 2009-12-24 CN CN200910264829A patent/CN101726482A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102692407A (en) * | 2011-03-24 | 2012-09-26 | 张家港市国泰华荣化工新材料有限公司 | Method for analysis of metal impurity ions of organic solvent |
| CN103604940A (en) * | 2013-11-26 | 2014-02-26 | 福州大学 | Inductively coupled plasma-atomic emission spectrometry/mass spectrometry (ICP-AES/ MS) switching-free type organic sampling device |
| CN108444983A (en) * | 2018-03-22 | 2018-08-24 | 山东出入境检验检疫局检验检疫技术中心 | A kind of torch pipe for measuring volatile materials |
| CN111721753A (en) * | 2020-05-15 | 2020-09-29 | 上海应用技术大学 | Device and method for directly feeding samples into oil product |
| CN111721753B (en) * | 2020-05-15 | 2023-06-30 | 上海应用技术大学 | Device and method for directly sampling oil |
| CN112858263A (en) * | 2021-01-15 | 2021-05-28 | 中国神华煤制油化工有限公司 | Method for measuring content of metal elements in organic solution |
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