KR101168199B1 - Procedures and device for the rapid on-site analysis of scheduled chemicals - Google Patents

Abstract

PURPOSE: A method and an apparatus for rapid on-site analyzing specific chemicals are provided to minimize damages from chemical weapons by rapidly verifying the existence of the chemical weapons and preparing countermeasures. CONSTITUTION: A method for rapid on-site analyzing specific chemicals in a movable laboratory includes the following: specimens containing volatile materials are sorted from various specimens by using an electronic nose; the sorted specimens are pre-treated; the pre-treated specimens are analyzed by using a gas chromatography mass spectrometer(GC/MS) with a rapid analysis condition; and precision analysis is implemented using a general GC/MS. In the rapid analysis, the initial oven temperature of the GC/MS is in a range between 40 and 80 degrees Celsius, and the lamp temperature of the oven is 30 to 80 degrees Celsius per minute.

Description

Method for rapid on-site verification of a specific chemical and its device {Procedures and Device for the Rapid On-site Analysis of Scheduled Chemicals}

The present invention relates to a method for rapid on-site verification and analysis of specific chemicals.

Chemical agent verification technology is essential for obtaining chemical agent evidence in situations such as chemical warfare and chemical weapon terrorism. There are two verification techniques, off-site verification and on-site verification. Out-of-site verification is a technique to verify specific chemicals by transferring to a laboratory when conducting a sample from a contaminated area and conducting an analysis for verification. “Specific chemicals” are substances that can be used in the manufacture of chemical weapons, which are one, two, or three chemicals, and sometimes referred to as including a single organic chemical (prohibition of chemical and biological weapons and certain chemical substances). Act on the Regulations on the Manufacturing and Import and Export of Biological Agents, etc. [Enforcement 2011. 4. 14] [Law No. 10592, April 14, 2011, Partial Amendment]).

The off-site verification procedure is carried out by the "Recommended operating procedures for sampling and analysis in the verification of chemical disarmament (ROP)" provided by the Verification Institute for the Chemical Weapons Convention in Finland (FIG. 1). When the collected sample arrives at the laboratory, the sample is pretreated by an appropriate method according to the shape. Samples prepared for pretreatment are screened using GC and appropriately selected detectors (GC-FID / DFPD). Forensic analysis not only obtains mass spectrometric information once more accurately for chemical agents or chemical weapons convention (CWC) -related substances obtained from screening analyzes, but also obtains retention index (RI) information. This is the final step in the analysis to accurately determine the presence or absence of chemical agents or related substances.

However, in the off-site verification, there was a time penalty to move the samples taken from the contaminated area to an off-site analysis lab for chemical agent verification. . Due to these problems, the necessity of on-site verification mobile laboratory apparatus capable of performing verification tasks in the context of chemical warfare, chemical weapon terrorism, WMD elimination operations and high-level international events has emerged.

The present inventors are able to perform rapid verification of on-site verification mobile laboratories and specific chemicals that can perform verification missions in situations such as chemical warfare, chemical weapon terrorism, anti-lethal weapons operations, and international events (high-end). Efforts have been made to develop a rapid verification procedure system to ensure that this is possible. As a result, unlike the existing verification method that undergoes pretreatment process for all the collected samples, the volatile sample is first selected by using the electronic nose to prioritize the sample analysis, and the selected samples are quickly set up for GC / MS. In the case of analysis using the present invention, it was found that the verification of a specific chemical substance can be performed within a significantly shorter time than the existing verification method, thereby completing the present invention.

Therefore, the purpose of the present invention is to find the volatile substances using the electronic nose in the screening analysis, which is the first analysis step for identifying unknown substances in the research of chemical agent verification technology, and to determine the priority of analysis on the sample collected and analyze the next step. The present invention provides a method for rapid on-site verification of chemicals that enables faster chemical agent verification.

Another object of the present invention is to develop the GC / MS verification procedure conditions for on-site verification in the rapid analysis step using GC / MS to verify chemical decomposition products within 15 minutes to analyze the existing chemical agents. It provides a rapid on-site verification method for chemicals that can be quickly validated by reducing analysis time by more than half of the analysis time.

It is still another object of the present invention to provide a mobile device or mobile laboratory for on-site verification that employs a breakthrough screening and rapid analysis method that reduces analysis time by more than half of the conventional chemical agent analysis method.

Still other objects and advantages of the present invention will become apparent from the following detailed description, claims and drawings.

In the field of chemical agent verification technology development research, there has been a need to develop a verification database and mobile laboratory device operation technology for rapid on-site verification and identification of chemical agents. Started production of prototypes. The inventors used AMDIS software to build a database for chemical agent verification for chemical agent identification through chemical agent synthesis and analysis in the Agency for Chemical Analysis. You can also take advantage of OCAD provided by the Organization for the Prohibition of Chemical Weapons (OPCW).

One aspect of the present invention relates to a method comprising the steps of (i) pretreatment of a sample and (ii) analyzing the pretreated sample using a gas chromatography mass spectrometer (GC / MS) with rapid analysis conditions and (iii) general It provides a rapid on-site verification method for chemicals that includes precise analysis using GC / MS.

In the present invention, the step (i) pretreatment of the sample refers to a process of extracting the active ingredient to remove the interference in the analysis and to adjust the sample concentration suitable for detection. In general, pretreatment of the sample enables analysis results of high sensitivity, selectivity and precision, and also protects the analytical column.

In the present invention, the step of pretreating the sample may be performed by, for example, centrifugation, filtration, liquid-liquid extraction (solvent extraction), solid phase extraction (solid phase extraction), derivatization, but is not necessarily limited thereto. In consideration of the type and amount of the component, the matrix containing the component, etc., it may be appropriately selected from among the known pretreatment methods.

The rapid on-site verification method for a specific chemical substance of the present invention comprises (i) analyzing the sample after the pretreatment step, and (ii) analyzing the pretreated sample using a gas chromatography mass spectrometer (GC / MS) in which rapid analysis conditions are set. Characterized by going through the steps.

The present inventors have made intensive research and efforts to find analytical conditions that can drastically shorten the analysis time required to identify the type of chemical agent, and have thus established GC / MS rapid analytical conditions. That is, in the present invention, in order to improve that the analysis time was long in the precise analysis procedure for identification of the agent type, rapid analysis was not possible. In the gas chromatography mass spectrometer (GC / MS), the lamp temperature of the oven was changed. The sample was analyzed by changing the initial oven temperature after setting constant, or by analyzing the sample while changing the lamp temperature of the oven after setting the initial oven temperature constant.

As used herein, the term “fast analysis” refers to advanced analytical techniques that allow for the rapid identification of chemical agent types compared to conventional precision analytical methods.

In the method of the present invention, the rapid analysis condition means that the temperature of the initial oven of GC / MS is set to 40 to 80 ℃ or the ramp temperature of the oven is set to 30 to 80 ℃ per minute.

If the initial oven temperature is set too low, it will not be suitable for rapid analysis because it will delay the time to complete the analysis and lower the oven temperature to the initial temperature.If the initial temperature is too high, the peak splitting on the TIC will occur. ) Can greatly reduce the resolution. Therefore, in the present invention, the temperature of the initial oven for achieving rapid analysis may preferably be 40 to 80 ° C, more preferably 50 ° C (1 min).

In addition, if the lamp temperature of the oven is set too low, the temperature rise rate is slow, and the analysis time is longer. If the lamp temperature is set too high, the time is faster, but the resolution may be difficult to interpret the result. Therefore, the lamp temperature of the oven for achieving rapid analysis in the present invention may preferably be 30 ° C to 80 ° C / min, more preferably 50 ° C / min.

In a preferred embodiment, rapid assay conditions mean that the temperature of the initial oven of GC / MS is set to 40 to 80 ° C., and at the same time the ramp temperature of the oven is set to 30 to 80 ° C. per minute.

In another preferred embodiment, the rapid analysis condition means that the GC / MS is set at an inlet temperature of 200 to 300 ° C, an initial oven temperature of 40 to 80 ° C, and an oven lamp temperature of 30 to 80 ° C per minute. do.

In another preferred embodiment, the rapid analysis conditions GC / MS is an inlet temperature of 200 to 300 ℃, splitless time (splitless time) of 0.1 to 1.5 minutes, the temperature of the initial oven 40 to 80 ℃, lamp of the oven (Ramp) means that the temperature is set to 30 to 80 ° C per minute.

In the rapid analysis (GC / MS) procedure step using the GC / MS in which the rapid analysis condition is set, the analysis time for analyzing one aliquot may be less than 15 minutes. Rapid analytical procedures have the advantage of verifying the degradation products of specific chemicals that are not detected in the screening assays, thereby increasing the accuracy of the analysis.

The rapid on-site verification method of the chemical substance of the present invention is characterized in that (ii) after the rapid analysis step using the GC / MS analysis conditions, and (iii) performing a precise analysis using the general GC / MS analysis conditions. .

Analysis results processed using GC / MS with fast analysis conditions are interpreted using AMDIS software, and GC / MSD (Gas Chromatography / Mass Selective) is the first priority for samples that show positive (check AMDIS results) in rapid analysis. Detector) By enabling precise analysis, the overall analysis time can be shortened.

The precise analysis means an analysis method using analytical conditions generally used in the field to which gas chromatography mass spectrometry belongs. For example, an inlet temperature of 250 ° C., an initial oven temperature of 40 ° C., and an oven lamp ) The sample may be analyzed using a general GC / MS with the temperature set at 10 ° C. per minute.

In embodiments, the precise analysis conditions are the inlet temperature of the GC / MS 200 to 300 ℃, splitless time (splitless time) 0.1 to 1.5 minutes, the temperature of the initial oven 40 to 50 ℃, ramp of the oven (Ramp) The temperature may be set to 10 to 20 ℃ per minute.

According to a preferred embodiment of the present invention, the rapid on-site verification method of the chemical of the present invention, prior to performing the step (i) pre-treatment of the sample, using the electronic nose (volatile) in a plurality of samples using an electronic nose It characterized in that it further comprises the step of selecting a sample comprising a.

In conventional off-site verification, GC / FID / DFPD technology is used for screening analysis after sample pretreatment, and the chemical sample must be precisely analyzed without linearity regardless of the type and number of samples. The presence or absence of and the verification could be terminated. On the other hand, in the on-site verification technology of the present invention, the sample is directly screened using an electronic nose, for example, zNose, before sample preparation. In the case of electronic screening analysis, volatile specific chemicals (eg, agents, etc.) are directly analyzed without any pretreatment, and volatile substances can be detected within 2 minutes.

In the method of the present invention, a sample pretreatment is first performed on a sample in which a positive (relevant peak) result is shown after an electronic nose analysis prior to pretreatment of various samples. In this way, the next step analysis is performed in a state where the sample analysis is prioritized, so that the sample containing the chemical agent can be analyzed more precisely in advance.

An electronic nose (e-nose) used in the method of the present invention is a device having a pattern detection function such as a chemical detector and an neural network, such as an electronic sensor, which distinguishes odors and analyzes chemical components. Just as the nose smells and delivers to the brain, chemicals are detected and processed by electronic sensors. In the present invention, the electronic nose is used to screen a plurality of samples to give priority to the analyte. The electronic nose used in the present invention is preferably zNose.

Another aspect of the invention is to (i) screening a sample comprising volatiles from a plurality of samples using an electronic nose (ii) pretreating the selected sample and (iii) the pretreated It provides a method for rapid on-site verification of a chemical comprising analyzing a sample to verify the contained volatiles.

The present inventors, in contrast to the conventional off-site verification procedure, in which the rapid on-site verification of the chemical material is performed after all samples have been pretreated without prioritization, analyzes by first selecting a sample to be pretreated using an electronic nose. In the case of doing so, the present invention has been completed in view of the fact that the analysis time for checking the presence of a chemical agent can be drastically reduced. That is, a significant shortening of the analysis time can be achieved by simply inserting a step of first selecting a sample to be pretreated using an electronic nose separately from the rapid analysis procedure of GS / MS described above.

In an embodiment, step (iii) of selecting a sample to be analyzed first by the electronic nose and then analyzing the pretreated sample to verify the volatile substances included therein is commonly used to analyze and detect a specific chemical. It can be carried out by the method. For example, nuclear magnetic resonance, infrared spectroscopy, Raman spectroscopy, X-ray spectroscopy, ultraviolet, visible light spectroscopy, near infrared spectroscopy, Auger electron spectroscopy, X-ray photoelectron spectroscopy, elemental spectroscopy, induced plasma spectroscopy, spectroscopy microscopy, Raman spectroscopy Microscopy, Infrared Spectroscopy, Electron Collision Ionization, Chemical Ionization, Electrospray Ionization, MALDI, Secondary Ionization, Inductive Plasma Ionization, Mass Spectrometry, Gas Chromatography, Gas Solid Chromatography ), Gas-Liquid Chromatography, Liquid Chromatography, Normal Chromatography, Reversed Phase Chromatography, Gel Permeation Chromatography, Supercritical Fluid Chromatography, Plate Chromatography, Electrophoresis, Crystallographic Analysis, etc. But is not necessarily limited to, chemical analysis And if the method is commonly used to detect it can be appropriately selected and used according to the nature of the material to be detected.

In a preferred embodiment, the analysis of the pretreated sample is characterized in that it is carried out using a gas chromatography mass spectrometer (GC / MS).

In another preferred embodiment, the analysis of the pre-treated sample is characterized by consisting of a method for performing a rapid analysis using a general GC / MS, after performing a rapid analysis using a GC / MS set the rapid analysis conditions In this case, the rapid analysis condition means that the temperature of the initial oven is set to 40 to 80 ° C. or the ramp temperature of the oven is set to 30 to 80 ° C. per minute.

Thus, prior to the pretreatment of the sample, the step of first selecting the sample target to be pretreated by using the electronic nose and the step of performing the rapid analysis using the GC / MS in which the rapid analysis conditions are set, the reduction in analysis time Synergies can be created, further reducing the analysis time required to identify the type of chemical agent.

Another aspect of the present invention is to provide an apparatus for on-site verification and analysis of chemical substances, including gas chromatography mass spectrometers (GC / MS), in which rapid analysis conditions are set.

In a preferred embodiment, the field verification and analysis device of a specific chemical of the present invention is characterized in that the mobile device to a mobile laboratory, more preferably characterized in that the vehicle equipped with GC / MS set the fast analysis conditions . For faster on-site verification, the vehicle can be further equipped with an electronic nose.

The mobile device for the on-site verification of the present invention or the mobile laboratory can immediately determine the presence or absence of chemical weapons through the real-time verification by immediately dispatching to the site where the chemical warfare, chemical weapon terrorism, or chemical weapon spraying is suspected. Due to the convenience of terrorism, it is possible to quickly obtain evidence of terrorism, so that it can quickly cope with the damage caused by the spread of chemical weapons.

In order to perform chemical agent verification in the existing off-site verification, there is a time disadvantage that the sample collected in the contaminated area must be transferred to an off-site analysis laboratory, so that prompt verification cannot be performed to deal with the risk situation immediately. Could not. The inventors have developed an on-site verification device to solve this problem.

The field verification apparatus of the present invention is a mobile device or a mobile laboratory that can move to a contaminated area in case of an emergency such as chemical warfare or chemical weapon terrorism, and establishes a system for quickly and accurately analyzing chemical agents and related degradation materials in the field. Doing.

Mobile device for on-site verification of the present invention can immediately determine the presence or absence of chemical weapons through real-time verification by immediately dispatched to the site suspected of chemical warfare, chemical weapons terrorism, or chemical weapons spraying and convenience of movement As a result, it is possible to secure evidence of terrorism quickly, and thus to cope with the damage caused by the spread of chemical weapons.

Rapid verification and analysis is important to minimize damage in situations such as chemical warfare, chemical weapon terrorism, weapons of mass destruction, and international events. According to the present invention, a mobile laboratory apparatus for on-site verification capable of performing a verification mission for securing evidence of chemical weapons terrorism is disposed on a site so that a chemical agent verification analysis can be quickly performed in a field during a dangerous situation, and chemical weapons can be shortened by an analysis time. It will be able to quickly determine the existence and to prepare a countermeasure quickly, thereby laying the foundation for minimizing damage to chemical weapons. That is, the biggest advantage of the field verification method of the present invention is that due to the narrowness of the mobile laboratory apparatus, even when the mass spectrometer is operated in Taiwan, the chemical agent can be quickly verified by reducing the time compared to the off-site verification procedure.

1 is a flowchart of an off-site verification method.
2 is a flowchart of a field verification method.
3 is a GC / MS TIC according to the initial temperature change of the oven after setting the ramp temperature 50oC.
4 is a GC / MS TIC according to the ramp temperature change after setting the initial temperature of the oven 50oC.
5 shows a flowchart of the field verification method of the present invention.
6 is a flowchart illustrating a sample pretreatment method.

Hereinafter, the present invention will be described in more detail with reference to Examples. It is to be understood that both the foregoing general description and the following detailed description are exemplary and explanatory only and are not to be construed as limiting the scope of the present invention. It will be self-evident.

Example

<Comparison of Sample Analysis Time for Off-Site Verification and On-Site Verification>

In the existing off-site verification analysis method, the pretreatment was performed without prior zNose analysis and the GC / FID / DFPD screening analysis was performed. Therefore, the pretreatment process and screening analysis was performed even for one sample containing no chemical agent. It took about 18 minutes of unnecessary analysis time.

However, the field verification analysis method of the present invention could be excluded from priorities in the pretreatment process for the sample showing the negative result through the zNose analysis and analyzed by performing the rapid analysis (GC / MS) without GC / FID / DFPD screening analysis. A significant shortening of time has been achieved. Specifically, the pretreated sample was prepared using Inlet temperature: 250 ° C., Aux. Temperature: 280 ° C, oven initial temperature 50 ° C (1 minute), lamp temperature: 50 ° C / min, final: 280 ° C (5.4 minutes), GC / MS with rapid analysis conditions in Splitless mode (0.75 minutes) (Agilent 5973N Mass selective detector equipped with Agilent 6890 plus gas chromatograph) was used, and the analytical data was analyzed using AMDIS software. Samples that are positive in the rapid analysis (checking the AMDIS results) can reduce the overall analysis time by ensuring that GC / MSD precision analysis is performed first.

The experimental results are shown in Table 1 by comparing the on-site and off-site verification methods.

<Establishment of Rapid Analysis Conditions>

The system performance test solution was analyzed by changing the initial temperature to 40 ℃ ~ 80 ℃ after setting the ramp temperature to 50 ℃ / min. As a result, the most suitable initial temperature for the on-site verification technology was 50 ° C., and the resolution was the best when the rapid analysis was performed (FIG. 3). When the initial temperature was set lower than 40 ° C., the analysis time was delayed due to the delay in lowering the oven temperature to the initial temperature after completing the analysis, which was not suitable for rapid analysis. If the initial temperature is too high, the resolution of the peaks of system performance test solutions split on TIC during analysis.

In addition, after the initial temperature was set to 50 ° C (1 minute), the specific chemicals were analyzed while changing the lamp temperature to 20 ° C ~ 80 ° C / min. When the lamp temperature was set at 20 ° C./min and the analysis was carried out, the temperature rise rate was slowed and the analysis time was longer. On the other hand, if the analysis proceeds by setting the lamp temperature to 80 ℃ / min or more, the analysis time is faster but the resolution is difficult to interpret the data (Fig. 4).

Based on the results, a rapid analysis condition suitable for the field verification technology was constructed as shown in [Table 2] below.

<On-site verification method evaluation>

Six samples (three soil samples and three aqueous samples) were subjected to a field verification method. Among the six samples, only one of the chemicals was present, and if volatiles were detected with zNose (Example 1) and volatiles were not detected with zNose, specific chemicals were identified from the last sample through rapid analysis. Case (Example 2) was tested.

Example  One: zNose Field verification when volatile substances are detected in one type of sample

After sample reception, six samples were screened (zNose). In this process, one sample showing a positive peak of volatile material was selected and analyzed in advance in the next analysis step, pretreatment. Three fractional analysis samples were prepared by pretreatment as shown in FIG. 6. After the pretreatment, one fraction of the sample was immediately analyzed and the second sample was pretreated. In the rapid analysis (GC / MS), the analysis was performed on one blank and one fraction, assuming that a specific chemical was verified in the first fraction. Rapid analysis was able to read the types of chemical agents and degradation products not detected in zNose. Finally, one fraction and one control sample were analyzed for precision. Table 3 shows the total analysis time from sample receipt to all unknowns.

Comparative Example 1: Very lucky off-site validation analysis time when a specific chemical was identified in the first selected analytical sample

Six samples were received and pretreated as shown in FIG. The fraction obtained after the pretreatment of one sample was immediately subjected to screening analysis (GC / FID / DFPD) and to the unknown analysis using other analysis equipment (GC / MS) to identify the unknown substances and the results are shown in the following table. 4 is shown.

Analysis time comparison = (on site analysis time / off site analysis time) x 100 = 132 minutes / 160 x 100 = 83%

When only one of six samples contained specific chemicals and the specific chemicals were volatile and detected with zNose, the on-site verification process reduced the analysis time by 17% compared to off-site verification procedures.

Example  2: zNose Field-tested analysis time when no volatiles were detected and rapid detection of specific chemicals in the last analyte

Agonist degradation products and nonvolatile agents were not detected in zNose, and the experiment was performed on the worst case that the chemical agent was identified in the last of six samples, and the analysis time obtained is shown in Table 5. . Precision analysis has increased the accuracy of the analysis.

Comparative Example 2: Off-site verification analysis time when a specific chemical was identified in the last analysis sample

The analysis time is shown when the chemical agent is verified in the last sample. The fractions obtained after the pretreatment of one sample were immediately subjected to screening analysis (GC / FID / DFPD) and to the unknown analysis using other analysis equipment (GC / MS) to identify unknown materials and the resulting analysis time. Is shown in Table 6. Screening assays (GC / FID / DFPD) were able to detect phosphorous and sulfur but did not provide accurate information to verify the type of agent. Accurate analysis of the agent types required precise analysis of all fractions.

Analysis time comparison = (on site analysis time / off site analysis time) x 100 = 642 minutes / 1,350 x 100 = 48%

When zNose was unable to detect a particular chemical because the specific chemical was nonvolatile, the on-site verification process took 48% of the analysis time compared to the off-site verification process. In other words, the on-site verification process reduced the analysis time by 52% compared to the existing analysis time.

Example  3: zNose On-site verification when volatile substances are detected in one type of sample

As in Example 1, volatile substances were detected by zNose in one of six samples received, and the samples were analyzed by giving an analysis priority. An analysis time of 12 minutes for screening analysis (zNose), 20 minutes for pretreatment, 30 minutes for rapid analysis and 70 minutes for precise analysis was taken as in Example 1. Total analysis time was 132 minutes (Table 3).

Comparative example  3: When a specific chemical is identified in the last analytical sample Off-site  Validation Analysis Time

As shown in Comparative Example 2, the analysis time was compared with the field verification method when the specific chemicals were detected in the last sample when analyzing the six received samples (Table 6). Total analysis time was 1,350 minutes.

 Analysis time comparison = (on site analysis time / off site analysis time) x 100 = 132 minutes / 1,350 x 100 = 10%

When zNose detected a specific chemical because the specific chemical was volatile, the on-site validation procedure took only 10% of the analysis time compared to the off-site validation procedure that identified the specific chemical in the last analytical sample. In other words, the on-site verification process reduced the analysis time by as much as 90% compared to the existing analysis time.

Many types of chemical agents are volatiles and are likely to be detected in the nose. It is highly likely to preferentially screen samples containing agents from a large number of samples by detecting volatiles using electronic noses. Therefore, the field verification technology developed in the present invention compared to the off-site verification technology greatly improved the possibility of identifying a specific chemical in the first sample. In the off-site verification technique, there is no way to prioritize the possibility of agent presence in the sample, so it is very rare to identify the presence of chemical agent in the first sample and give priority to the analysis.

In the above embodiment, the case of a very extreme situation has been compared and analyzed. However, even in this case, it was confirmed that the analysis time was shortened by the field verification procedure.

Claims (6)

(i) screening a sample comprising volatiles from the plurality of samples using an electronic nose; Then
(ii) pretreating the selected sample; Then
(iii) analyzing the pretreated sample using a gas chromatography mass spectrometer (GC / MS) with fast analysis conditions; Then
(iv) a rapid on-site verification method for the validation of scheduled chemicals performed in mobile laboratories, including the step of performing precise analysis using general GC / MS;
Herein, the rapid analysis condition means that the temperature of the initial oven of the GC / MS is set to 40 to 80 ° C. and the ramp temperature of the oven is set to 30 to 80 ° C. per minute. delete  The method of claim 1, wherein the rapid analysis condition is further set such that an inlet temperature of the GC / MS is 200 to 300 ° C. and a splitless time is 0.1 to 1.5 minutes. According to claim 1, the precision analysis conditions GC / MS, the inlet temperature is 200 to 300 ℃, the splitless time (splitless time) 0.1 to 1.5 minutes, the temperature of the initial oven 40 to 50 ℃, the lamp of the oven (Ramp ) The temperature is set to 10-20 ° C. per minute. delete delete

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