CN101532993B - Method for analyzing and detecting organic trace impurity in high-purity phenol - Google Patents
Method for analyzing and detecting organic trace impurity in high-purity phenol Download PDFInfo
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- CN101532993B CN101532993B CN2009100668163A CN200910066816A CN101532993B CN 101532993 B CN101532993 B CN 101532993B CN 2009100668163 A CN2009100668163 A CN 2009100668163A CN 200910066816 A CN200910066816 A CN 200910066816A CN 101532993 B CN101532993 B CN 101532993B
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Abstract
The invention discloses a method used for analyzing and detecting organic trace impurity in high-purity phenol. The invention is characterized in that a sample experiences solid phase micro-extraction and high-temperature desorption before entering into a gas chromatograph; a dimethyl siloxane fibre extraction head is arranged; the coating thickness is 30-100mum; the extraction is carried out under the temperature of 25 DEG C to 80 DEG C for 5 to 40 minutes; and the desorption is carried out under the temperature of 200 DEG C to 250 DEG C for 30 to 120 seconds. The invention has the advantages that the dosage of phenol sample is few; the method does not require any organic solvent; the method can save the sample and the organic solve with low cost and is also good for environmental protection; the invention can analyze trace components which can not be analyzed by the normal method; the invention is based on an adsorption equilibrium theory, so that the invention is easy for calculating and controlling the extraction process; a structure of an extraction device is designed according to a sample inlet of the gas chromatograph, so that the extraction device is convenient for operating; and the invention can carry out both the qualitative analysis and the quantitative analysis on the trace component with exact and reliable results.
Description
Technical field
The present invention relates to a kind of Trace Organic Compounds analysis, in particular, relate to the preceding treatment technology of sample analysis.
Background technology
In the constituent analysis of technical benzene phenolic product and detecting, gas chromatography analysis method is adopted in the analysis of trace organic impurities and detection basically, and these methods are most of to be adopted after the phenol sample dissolution, utilizes the direct injected mode to analyze.The method is feasible for the higher impurity analysis of content in the phenol, yet the analyzing and testing for trace organic impurities in the high-purity phenol does not reach certain sensitivity usually, is difficult to realize accurate quantitative test.In addition, the direct injected mode, the sample size and the organic solvent amount that need are bigger, and capillary chromatographic column is had very big shortcoming, and solvent peak constitutes interference to composition to be detected, and the serviceable life that can reduce capillary chromatographic column.The accuracy of organic impurities analytical approach is low in the conventional phenol, also is unfavorable for environmental protection.
In recent years, the demand of engineering plastics and functional plastics is increased sharply, most materials requires high-purity phenol as raw material, and high-purity phenol has strict restriction to the content of organic impurities.Strict monitoring and raising all need be done to product quality by the manufacturer of each phenol product, and therefore, the real time sample of phenol product is parsed into and is one of long-term routine work task of manufacturer.
Summary of the invention
The objective of the invention is to set up a rational route, sample is carried out extraction process before analysis, accurately analyze foundation efficiently for raising phenol product quality provides for the analytical approach of organic impurities in the phenol.
The present invention uses gas chromatography or gas chromatograph-mass spectrometer (GCMS) in detection, it is characterized in that, is provided with solid-phase micro-extracting device, and the concrete steps of this analytical approach are:
1, choose the solid phase micro-extraction extraction head that analyte is had high selectivity, like dimethyl silicone polymer (PDMS) fibre abstraction head, its coating thickness is selected according to effect of extracting, commonly 30～100 μ m.
2, get the phenol sample and place the SPME sample bottle, with a spot of ultrapure water dissolving, sealed sample is positioned over sample bottle on the magnetic agitation well heater.
3, extracting head is aging at the injection port of gas chromatography, 180 ℃～240 ℃ of aging temperatures, 0.5～2 minute time.
4, pierce through the sample bottle silicagel pad, promote the push rod of solid-phase micro-extracting device, make on extracting head exposure and the fluid sample liquid level, carry out head space (headspace) extraction.
5, be 25 ℃～80 ℃ in temperature, under the stirring condition, the time is 5～40 minutes, and organic impurities extracts among the Pyrogentisinic Acid, optimizes 30 ℃～60 ℃ of temperature, and the time is 20～35 minutes.
6, after the extraction, extraction equipment is placed the gas chromatography injection port, pierce through liner; In vaporizer, carry out the high temperature desorb, temperature is controlled at 200 ℃～250 ℃, and desorption time is 30～120 seconds; 210 ℃～240 ℃ of preferred temperature; Time is 80～100 seconds, and then organic impurities obtains separating in gas chromatographic column.
The present invention and existing conventional compared with techniques have lot of advantages, and solid phase micro-extraction technique is a kind of novel solvent-free abstraction technique, in the process for preparation of phenol sample, need not use any organic solvent, as long as make water make solvent.On the use amount of sample, only used the sample of very small amount, do not need a large amount of samplings.This techniques save a large amount of organic solvent and the use amount of sample, be a kind of green abstraction technique, help environmental protection.On extracting power, can realize that most of organic impurities extracts among the Pyrogentisinic Acid, the non-detectable trace constituent of some conventional methods can enough this laws be analyzed.In addition, because present technique is based on the adsorption equilibrium principle, the accuracy of easy for calculation and control extraction.The structure of used extraction equipment designs according to the injection port of gas chromatography, does not need extra step, directly carries out desorb, separation and detection after the extraction.
Description of drawings
Fig. 1 forms synoptic diagram for solid-phase micro-extracting device among the present invention.
Fig. 2 constitutes synoptic diagram for analyzing and testing of the present invention system.
Fig. 3 is one group of sample analysis chromatogram.
Push rod 1, extracting head 2, sample 3, magnetic agitation and well heater 4, solid-phase micro-extracting device 5, gas chromatograph vaporizer 6, gas chromatograph 7 are arranged among the figure.
Embodiment
Below in conjunction with accompanying drawing and instantiation the utility model is made detailed description further.
The phenol product quality analysis adopts gas chromatography or gas chromatography and mass spectrophotometry method for combined use to carry out, and essence of the present invention is the treatment technology to the sample of being analyzed, and the technology of the sample preparation before a kind of analytical instrument detects promptly is provided.
As shown in Figure 1, push rod 1 is arranged in the solid-phase micro-extracting device 5, the dimethyl silicone polymer fiber is an extracting head 2, its coating thickness is 100 μ m; Sample thief 0.1～0.3 gram is put into solid phase micro collection bottle, need not any organic solvent, with ultrapure water dissolving, sealed sample 3; And place on magnetic agitation and the well heater 4, this well heater has intensification and control temperature function, pierces through sample bottle and uses silicagel pad, promotes push rod 1; Extracting head 2 is exposed on the sample liquid level, carries out headspace extraction, its temperature is 25 ℃～80 ℃ and has under the stirring condition; Time is 5～40 minutes, and to different organic impurities, parameters such as extraction temperature, extraction time can be carried out further optimized choice, after the extraction; Extraction equipment 5 is placed the injection port of gas chromatography, pierce through liner, in vaporizer 6, carry out the high temperature desorb; Temperature is controlled at 200 ℃～250 ℃, and the time is 30～120 seconds, and the present invention adopts U.S. 30m * 0.32mm i.d. * 0.25 μ m RTX-5 chromatographic column; The column temperature condition is 50 ℃, behind the maintenance 1min, is warmed up to 80 ℃ with 10 ℃/min again, is warmed up to 180 ℃ with 10 ℃/min, and then is warmed up to 250 ℃ with 20 ℃/min, keeps 5min; Adopt the split sampling mode to carry out stratographic analysis.
For the composition of a large amount of difficult discriminatings, can adopt the gas chromatography-mass spectrography method to carry out qualitative analysis and quantitative test.
Fig. 3 provides the chromatogram of a sample, adopts dimethyl silicone polymer fibre abstraction head 2, and its coating thickness is 100 μ m, 200 ℃ of aging temperatures, and 1 minute time, 230 ℃ of desorption temperatures, the time is 80 seconds, corresponding impurity title and analysis data such as table 1.
Table 1.
| Sequence number | The organic impurities title | ppm(W％) |
| 1 | Acetophenone | 3 |
| 2 | 2-methyl coumarone | 10 |
| 3 | 2-methyl isophthalic acid-propenylbenzene | 5 |
| 4 | 1-methyl dihydroindene-2-ketone | 15 |
| 5 | 1,1 '-(1,1,2,2-tetramethyl-1,2-ethylidene) hexichol | 28 |
| 6 | 2,4-diphenyl-4-methyl-1-pentene | 26 |
Can find out according to this instance, use in this law Pyrogentisinic Acid sample the trace organic impurities and analyze, highly sensitive, can realize influencing the analyzing and testing of the impurity of phenol quality.And then, can be according to the kind and the characteristic of impurity, the process conditions of Pyrogentisinic Acid's device are improved and are optimized, thereby improve product quality, improve added value of product, strengthen the competitive power on market.
Claims (3)
1. method that is used for high-purity phenol trace organic impurities analyzing and testing; Be included in and use gas chromatograph or gas chromatograph-mass spectrometer (GCMS) in the analyzing and testing, it is characterized in that, be provided with solid-phase micro-extracting device (5); Be provided with dimethyl silicone polymer fibre abstraction head (2); Its coating thickness is 30～100 μ m, is provided with desorption process, the concrete operations step:
A, get phenol sample (3) and place the SPME sample bottle, with the ultrapure water dissolving, sealed sample (3) is positioned over sample bottle on the magnetic agitation well heater (4);
B, extracting head (2) wear out at the injection port of gas chromatography, 180 ℃～240 ℃ of aging temperatures, 0.5～2 minute time;
C, pierce through the sample bottle silicagel pad, promote the push rod (1) of solid-phase micro-extracting device, extracting head (2) is exposed on fluid sample (3) liquid level, carry out headspace extraction;
D, having under the stirring condition, extraction temperature is controlled at 25 ℃～80 ℃, and the time is 5～40 minutes, and organic impurities extracts among the Pyrogentisinic Acid;
After E, the extraction, extraction equipment is placed gas chromatograph (7) injection port, pierce through liner, in vaporizer (6), carry out the high temperature desorb, temperature is controlled at 200 ℃～250 ℃, and desorption time is 30～120 seconds; Adopt the RTX-5 chromatographic column, in gas chromatographic column, separate organic impurities, concrete chromatographic condition is: temperature programme: the column temperature condition is 50 ℃, keeps 1min, rises to 180 ℃ with 10 ℃/min speed, rises to 250 ℃ with 20 ℃/min speed again, keeps 5min.
2. according to the said a kind of method that is used for high-purity phenol trace organic impurities analyzing and testing of claim 1, it is characterized in that having under the stirring condition, extraction temperature is controlled at 30 ℃～60 ℃, and the time is 20～40 minutes.
3. according to the said a kind of method that is used for high-purity phenol trace organic impurities analyzing and testing of claim 1, it is characterized in that, the high temperature desorb, temperature is controlled at 210 ℃～240 ℃, and desorption time was controlled at 80～100 seconds.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101912769B (en) * | 2010-07-09 | 2013-02-27 | 中山大学 | Extraction head detachable type solid phase micro extraction probe and preparation method thereof |
| CN101992062B (en) * | 2010-09-02 | 2012-09-05 | 天津春发生物科技集团有限公司 | Method for preparing metal carrier stirring extraction rod |
| CN101992075B (en) * | 2010-09-02 | 2012-09-05 | 天津春发生物科技集团有限公司 | Preparation method of solid phase micro extraction fiber of metal carrier Tenax coating |
| CN102565236A (en) * | 2011-12-31 | 2012-07-11 | 聚光科技(杭州)股份有限公司 | Substance testing method |
| US9134208B2 (en) * | 2012-07-31 | 2015-09-15 | Smiths Detection Montreal Inc. | Solid phase micro extraction (SPME) vacuum inlet |
| CN103630627A (en) * | 2013-07-19 | 2014-03-12 | 吉林化工学院 | Co-detection method for trace organic impurities in complex water sample |
| CN103472161A (en) * | 2013-10-10 | 2013-12-25 | 华东理工大学 | Preprocessing device, preprocessing method and method for detecting organic impurities in high-purity reagent |
| CN109342614A (en) * | 2018-09-30 | 2019-02-15 | 力合科技（湖南）股份有限公司 | Water sample processing system |
| CN110514774B (en) * | 2019-08-30 | 2021-07-20 | 哈尔滨工业大学 | Method for analyzing phenolic compounds in water |
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| CN1299692A (en) * | 2000-12-18 | 2001-06-20 | 武汉大学 | Extracting head for solid phase micro extraction of hydrocarbon crown ether and its preparation |
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| CN1299692A (en) * | 2000-12-18 | 2001-06-20 | 武汉大学 | Extracting head for solid phase micro extraction of hydrocarbon crown ether and its preparation |
Non-Patent Citations (2)
| Title |
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| 姬志强 等.普通铁线蕨挥发油的HS-SPME-GC-MS分析.《中国药房》.2008,第19卷(第30期),2359-2361. * |
| 李英 等.顶空固相微萃取-气相色谱质谱法测定蜂蜜中的苯酚残留量.《分析试验室》.2008,第27卷(第2期), * |
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