CN210097000U - Solid phase extraction separation device - Google Patents
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- CN210097000U CN210097000U CN201920741710.8U CN201920741710U CN210097000U CN 210097000 U CN210097000 U CN 210097000U CN 201920741710 U CN201920741710 U CN 201920741710U CN 210097000 U CN210097000 U CN 210097000U
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- 238000002414 normal-phase solid-phase extraction Methods 0.000 title claims abstract description 145
- 238000000926 separation method Methods 0.000 title claims abstract description 60
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- 239000003153 chemical reaction reagent Substances 0.000 claims abstract description 26
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- 239000000284 extract Substances 0.000 claims description 25
- 150000004945 aromatic hydrocarbons Chemical class 0.000 claims description 24
- 229930195734 saturated hydrocarbon Natural products 0.000 claims description 23
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- 239000000084 colloidal system Substances 0.000 claims description 11
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- 238000004458 analytical method Methods 0.000 abstract description 18
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- OFBQJSOFQDEBGM-UHFFFAOYSA-N Pentane Chemical compound CCCCC OFBQJSOFQDEBGM-UHFFFAOYSA-N 0.000 description 8
- 238000002347 injection Methods 0.000 description 6
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- 238000004821 distillation Methods 0.000 description 4
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Abstract
The utility model provides a solid phase extraction separator. The solid phase extraction separation device comprises: the device comprises at least one extraction reagent storage device, at least one sample storage device to be tested, at least one solid phase extraction column storage device, a sampling device and an automatic control system, wherein at least one extraction reagent supply device is arranged in the extraction reagent storage device; at least one sample supply device to be tested is placed in the sample storage device to be tested; at least one solid-phase extraction column is arranged in the solid-phase extraction column storage device; the sampling device comprises at least one sampling pipeline and sampling needles which are in one-to-one correspondence with the sampling pipeline; and the automatic control system is used for controlling the sampling device to sample. The automatic control system is adopted to control the sampling and sample introduction of the sampling device and the elution of the solid-phase extraction column, so that the time for solid-phase extraction and separation of the sample is effectively reduced, the influence of the experimental data on operators and the environment is small, and the obtained analysis data has the advantages of good parallelism and high accuracy.
Description
Technical Field
The utility model relates to a coal chemical industry field particularly, relates to a solid-phase extraction separator.
Background
The direct coal liquefaction is taken as an efficient clean coal technology which can partially relieve the contradiction between supply and demand of petroleum resources in China, and the processing technology level of the direct coal liquefaction oil is an important factor influencing the application range of the direct coal liquefaction oil. The technical level of the direct coal liquefaction process can be improved only by deeply knowing the chemical composition of the direct coal liquefaction oil. Therefore, a set of efficient and accurate analysis method for the direct coal liquefaction oil is needed, but the direct coal liquefaction oil is complex in composition, and an ideal separation analysis effect is difficult to achieve by directly adopting an instrument for analysis.
The commonly used composition analysis method for petroleum products is to separate the oil sample to be detected into saturated hydrocarbon and aromatic hydrocarbon (or saturated hydrocarbon, aromatic hydrocarbon and colloid) components through a Solid Phase Extraction (SPE) column, and then to separate the oil sample into saturated hydrocarbon such as paraffin and cyclane and aromatic hydrocarbon such as monocyclic aromatic hydrocarbon, bicyclic aromatic hydrocarbon and tricyclic aromatic hydrocarbon through a mass spectrometry means. The standard method for analyzing the middle distillate oil is ASTM D2425, which corresponds to the standard method in China to SH/T0606, and the solid phase extraction adopts a method for separating aromatic hydrocarbon and saturated hydrocarbon in appendix A in SH/T0606, and the method is suitable for petroleum fractions with the distillation range of 204-365 ℃ (5-95V% recovery temperature). The standard adopted for separating the heavy oil fraction is ASTM D2786 and ASTM D3239, China corresponds to SH/T0659, and the method separates the measured oil sample into saturated hydrocarbon, aromatic hydrocarbon and colloid through solid phase extraction and is suitable for petroleum fractions with the distillation range of 205-540 ℃ (5-95V% recovery temperature).
At present, the solid-phase extraction and separation of coal-liquefied oil products in laboratories is referred to as the separation method of the petroleum products, and the operation mode is a manual SPE method. The method comprises the following specific operation steps: firstly, sucking a certain amount of activating reagent by using an injector A and dripping the activating reagent into the SPE small column; then, a certain amount of the oil sample to be detected is sucked by an injector B and is dripped into the activated SPE small column; then sucking the alkane leaching liquid drops by using a syringe C to extract saturated hydrocarbon on the sample of the SPE small column; and then, a polar solvent leacheate is absorbed by an injector D and dripped into the SPE small column to extract the aromatic hydrocarbon, a solvent leacheate with stronger polarity is absorbed by an injector E and dripped into the SPE small column to extract the colloid (if the step is not carried out in the middle distillate oil separation), and finally, the hydrocarbon composition analysis is carried out on the extraction liquid of the saturated hydrocarbon, the aromatic hydrocarbon and the colloid by adopting a gas chromatography-mass spectrometry technology. The method adopts manual operation in the whole process, takes long time, has great influence on operators and environment, and has poor data parallelism because the precision is difficult to control when samples and extraction liquid are manually sucked.
At present, a solid phase extraction separation device in an analytical chemistry laboratory is mainly used for analyzing trace substances such as food, medicines, blood, pollutants in water and the like. The method has large sample injection volume, the sample with large volume is generally more than 200mL, the sample with small volume is 0-50mL, and the extracted sample is not analyzed any more. The volume of the sample loaded in the solid-phase extraction and separation of the coal liquefied oil is about 0.1mL generally, the precision requirement of a sample injection system is high, the extraction is separated into three parts (the middle fraction oil is separated into two parts) according to the standard, the extraction separation is a main sample to be detected, and extracts of each section cannot be mixed. In view of the above problems, there is a need to develop a new solid phase extraction separation device suitable for coal liquefaction oil separation.
SUMMERY OF THE UTILITY MODEL
The utility model discloses a main aim at provides a solid phase extraction separator to there is the relatively poor problem of data precision uncontrollable and analysis data parallelism in the test procedure in the manual SPE method of solving current oil analysis and adopting.
In order to achieve the above object, according to the present invention, there is provided a solid phase extraction separation device, comprising: the device comprises at least one extraction reagent storage device, at least one sample storage device to be tested, at least one solid phase extraction column storage device, a sampling device and an automatic control system, wherein at least one extraction reagent supply device is arranged in the extraction reagent storage device; at least one sample supply device to be tested is placed in the sample storage device to be tested; at least one solid-phase extraction column is arranged in the solid-phase extraction column storage device; the sampling device comprises at least one sampling pipeline and sampling needles which are in one-to-one correspondence with the sampling pipeline; and the automatic control system is used for controlling the sampling device to sample.
Further, the solid phase extraction separation device further comprises: at least one activating reagent storage device, wherein the activating reagent storage device is provided with an activating reagent storage and supply device.
Further, the solid phase extraction separation device also comprises at least one waste liquid storage device, at least one waste liquid recovery device is placed in the waste liquid storage device, and the waste liquid recovery device is in one-to-one correspondence with the solid phase extraction columns.
Further, the solid phase extraction separation device also comprises at least one injection pump, and the injection pump is arranged on the sampling pipeline.
Furthermore, the solid phase extraction separation device also comprises at least one air-blowing switch, and the air-blowing switches are in one-to-one correspondence with the sampling pipelines and are used for controlling the pressure in the sampling pipelines.
Furthermore, a plurality of solid phase extraction columns are arranged in the solid phase extraction column storage device, and the solid phase extraction columns comprise a middle distillate oil solid phase extraction column and a heavy oil fraction solid phase extraction column.
Further, the solid phase extraction column comprises 5 middle distillate solid phase extraction columns and 5 heavy oil fraction solid phase extraction columns.
Furthermore, the upper end of the solid phase extraction column is provided with a snap-in type blank cap.
Furthermore, the solid phase extraction separation device comprises at least one extraction liquid receiving unit, wherein the extraction liquid receiving unit is internally provided with at least one extraction liquid receiving device, and the extraction liquid receiving devices correspond to extraction liquids obtained by separation from the solid phase extraction column one by one.
Further, the extraction liquid receiving device comprises a saturated hydrocarbon extraction liquid receiving device and an aromatic hydrocarbon extraction liquid receiving device corresponding to the middle distillate, and a saturated hydrocarbon extraction liquid receiving device, an aromatic hydrocarbon extraction liquid receiving device and a colloid extraction liquid receiving device corresponding to the heavy oil fraction.
Furthermore, the sampling device comprises five sampling pipelines and five sampling needles corresponding to the sampling pipelines.
Use the technical scheme of the utility model, this method provides in the solid phase extraction separator, its sample that adopts automatic control system control sampling device, advances kind and the work of the elution of solid phase extraction post to effectively reduced the time of sample solid phase extraction separation, improved experimental efficiency. Meanwhile, in the step of extracting and separating the direct coal liquefaction oil by adopting the solid phase extraction and separation device, the experimental data is less influenced by operators and the environment, so that the obtained analysis data has the advantages of good parallelism and high accuracy.
Drawings
The accompanying drawings, which form a part of the present application, are included to provide a further understanding of the invention, and are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the description serve to explain the invention and not to limit the invention. In the drawings:
fig. 1 is a schematic structural view of a solid phase extraction separation apparatus according to a preferred embodiment of the present invention; and
FIG. 2-1 shows a schematic diagram of an arrangement used in a middle distillate solid phase extraction liquid receiving apparatus in a preferred embodiment of the present application;
fig. 2-2 shows a schematic diagram of an arrangement for a solid phase extraction liquid receiving device for heavy oil fraction according to a preferred embodiment of the present application.
Wherein the figures include the following reference numerals:
10. an extraction reagent storage device; 20. a sample storage device to be tested; 30. a solid phase extraction column storage device; 40. a sampling device; 50. an automatic control system; 60. an activation reagent storage device; 70. a waste liquid storage device; 80. an extract receiving unit.
Detailed Description
It should be noted that the embodiments and features of the embodiments in the present application may be combined with each other without conflict. The present invention will be described in detail with reference to examples.
As described in the background art, the manual SPE method adopted by the existing oil separation has the problems that the data precision is difficult to control and the data analysis parallelism is poor in the test process. In order to solve the above technical problem, the present application provides a solid-phase extraction separation apparatus, including: the device comprises at least one extraction reagent storage device 10, at least one sample storage device 20 to be tested, at least one solid phase extraction column storage device 30, a sampling device 40 and an automatic control system 50, wherein at least one extraction reagent supply device is placed in the extraction reagent storage device 10; at least one sample supply device to be tested is placed in the sample storage device 20 to be tested; at least one solid-phase extraction column is placed in the solid-phase extraction column storage device 30; the sampling device 40 comprises at least one sampling pipeline and sampling needles corresponding to the sampling pipeline one by one; and an automatic control system 50 for controlling the sampling device 40 to perform sampling.
The method provides a solid phase extraction separation device, which adopts an automatic control system 50 to control the sampling and sample introduction of a sampling device 40 and the elution of a solid phase extraction column, thereby effectively reducing the time of solid phase extraction separation of a sample and improving the experimental efficiency. Meanwhile, in the step of extracting and separating the direct coal liquefaction oil by adopting the solid phase extraction and separation device, the experimental data is less influenced by operators and the environment, so that the obtained analysis data has the advantages of good parallelism and high accuracy. Particularly, for the test process with less sample amount, the superiority of the detection result is more obvious when the method is adopted for detection.
Preferably, the sampling range of the sampling system in the solid phase extraction separation device is 0-1 mL, the sampling precision is ± 1%, and 30 samples to be detected are placed in the sample storage device 20 to be detected and are arranged in six rows, and five samples are arranged in each row.
In order to improve the accuracy of the analysis data, preferably, the solid phase extraction separation apparatus further includes: at least one activated reagent storage device 60, and an activated reagent storage supply device is disposed in the activated reagent storage device 60. Meanwhile, the activation reagent storage device 60 provided with the activation reagent supply device can absorb the activation reagent by using the sampling device 40, and the activation reagent is dripped into the solid-phase extraction column to complete activation, so that the automation degree of the solid-phase extraction process is improved, and the separation time is further shortened. Preferably, the solid phase extraction separation device comprises five activating reagent storage devices 60. In a preferred embodiment, the solid-phase extraction separation device further includes at least one waste liquid storage device 70, and at least one waste liquid recovery device is disposed in the waste liquid storage device 70, and the waste liquid recovery devices correspond to the solid-phase extraction columns one to one. The waste liquid storage device 70 is used for receiving the needle washing waste liquid of the sampling needle and the pipeline bubble discharge waste liquid, which is beneficial to improving the environmental protection of the solid phase extraction separation device and reducing the environmental pollution.
In a preferred embodiment, the solid phase extraction separation device further comprises at least one syringe pump, and the syringe pump is arranged on the sampling pipeline. The provision of a syringe pump can facilitate control of the flow rate of the sample in the sampling line. In order to further control the pressure in the sampling pipeline, more preferably, the solid phase extraction separation device further comprises at least one air-blowing switch, and the air-blowing switches are in one-to-one correspondence with the sampling pipelines.
The coal liquefaction oil has more complex components, so that the accuracy of analysis data is further improved. In a preferred embodiment, a plurality of solid phase extraction columns are disposed in the solid phase extraction column storage device 30, and the solid phase extraction columns include a middle distillate solid phase extraction column and a heavy oil fraction solid phase extraction column. The coal liquefaction oil is divided into two parts of saturated hydrocarbon and aromatic hydrocarbon (middle distillate oil) or three parts of saturated hydrocarbon, aromatic hydrocarbon and colloid (heavy oil fraction) through instrument operation, and the solid phase extraction separation device is more targeted, so that the obtained analysis data is more accurate. More preferably, the solid phase extraction column comprises 5 middle distillate solid phase extraction columns and 5 heavy oil fraction solid phase extraction columns.
In a preferred embodiment, the solid phase extraction separation device comprises four solid phase extraction column storage devices 30, wherein two of the solid phase extraction column storage devices 30 are provided with middle distillate solid phase extraction columns, and the other two solid phase extraction column storage devices 30 are provided with heavy oil fraction solid phase extraction columns. More preferably, three rows of solid phase extraction column sliders are disposed in each solid phase extraction column storage device 30, and five middle distillate solid phase extraction columns or heavy oil fraction solid phase extraction columns are disposed in each solid phase extraction column slider. As shown in FIG. 2-1, an extract receiving bottle for saturated hydrocarbon is arranged below S, and an extract receiving bottle for aromatic hydrocarbon is arranged below A; as shown in FIG. 2-2, a saturated hydrocarbon extract receiving bottle is placed under S, an aromatic hydrocarbon extract receiving bottle is placed under A, and a colloidal extract receiving bottle is placed under R.
In a preferred embodiment, the upper end of the solid phase extraction column is provided with a snap-in closure. The snap-in type blank cap plays a role in sealing when the sampling needle is inserted into the solid phase extraction column, so that air bubbles in a sampling pipeline can be reduced, and the accuracy of an analysis result can be improved.
In order to further improve the accuracy of the analysis result, it is preferable that the solid phase extraction separation device further includes a pressurizing device for pressurizing the solid phase extraction column to press the reagent remaining in the solid phase extraction column into the extraction liquid receiving device.
In a preferred embodiment, the solid phase extraction separation device comprises at least one extraction liquid receiving unit 80, at least one extraction liquid receiving device is disposed in the extraction liquid receiving unit 80, and the extraction liquid receiving device corresponds to extraction liquid separated from the solid phase extraction column one by one. Preferably, the solid phase extraction separation device comprises two middle distillate extraction liquid receiving units, wherein five extraction liquid receiving devices are arranged in each row of each middle distillate extraction liquid receiving unit, six rows are provided, 30 extraction liquid receiving devices can be arranged in each row, 60 extraction liquid receiving devices, 30 extraction liquid receiving devices of saturated hydrocarbon (S) extraction liquid and 30 extraction liquid receiving devices of aromatic hydrocarbon (A) extraction liquid are arranged in each two middle distillate extraction liquid receiving units; the solid phase extraction separation device comprises two heavy oil fraction extract receiving units, wherein five extract receiving devices are arranged in each row of the heavy oil fraction extract receiving units, six rows are provided, 30 extract receiving devices can be arranged in total, 60 extract receiving devices are arranged in total in the two heavy oil fraction extract receiving units, 20 extract receiving devices for saturated hydrocarbon (S) extract, 20 extract receiving devices for aromatic hydrocarbon (A) extract and 20 extract receiving devices for colloid (R) extract.
Because the solid phase extraction methods of the middle distillate oil and the heavy oil fraction are different, the setting of the extraction liquid receiving device is different for different oil samples to be tested. In a preferred embodiment, the extraction liquid receiving device comprises a saturated hydrocarbon extraction liquid receiving device and an aromatic hydrocarbon extraction liquid receiving device corresponding to the middle distillate solid phase extraction column, and a saturated hydrocarbon extraction liquid receiving device, an aromatic hydrocarbon extraction liquid receiving device and a colloid extraction liquid receiving device corresponding to the heavy oil fraction solid phase extraction column.
In a preferred embodiment, the sampling device 40 includes five sampling lines and five sampling needles corresponding to the sampling lines.
The present application is described in further detail below with reference to specific examples, which should not be construed as limiting the scope of the invention as claimed.
Example 1
The solid phase extraction separation was performed by using the apparatus shown in FIG. 1.
Taking coal to directly liquefy oil A, wherein the distillation range is 220-260 ℃, putting the coal into five to-be-tested sample supply devices (sample bottles) on a to-be-tested sample storage device 20 (a sample frame), putting five 3mL SPE small columns on a sliding block on a solid phase extraction separation device (a middle distillate SPE frame), and activating by taking 0.5mL of n-pentane; 0.1mL of oil sample is sucked and dropped into a solid phase extraction column of middle distillate oil; 2mL of n-pentane is adopted to extract saturated hydrocarbon, and the extraction rate is 1.5 mL/min; aromatic hydrocarbons were extracted with 2mL of methylene chloride at an extraction rate of 1.0 mL/min. Then, internal standards are respectively added into the extraction liquid, the results after sample injection analysis by gas chromatography-mass spectrometry are shown in the following table 1, an extraction liquid receiving bottle of saturated hydrocarbon is placed below S, and an extraction liquid receiving bottle of aromatic hydrocarbon is placed below A.
TABLE 1
Example 2
The solid phase extraction separation was performed by using the apparatus shown in FIG. 1.
Taking coal to directly liquefy oil B, wherein the distillation range is 200-420 ℃, putting the coal into five to-be-detected sample supply devices (sample bottles) on a to-be-detected sample storage device 20 (a sample frame), putting five 6mL SPE small columns on a sliding block on a solid phase extraction separation device (a heavy oil fraction SPE frame), and taking 2mL of n-pentane for activation; sucking 0.1mL of oil sample and dropping the oil sample into a heavy oil solid phase extraction column; extracting saturated hydrocarbon by adopting 3mL of n-pentane, wherein the extraction rate is 1.5 mL/min; extracting aromatic hydrocarbon by 4mL of dichloromethane, wherein the extraction rate is 1.0 mL/min; the colloid was extracted with 3mL of a mixed solution of dichloromethane and ethanol (volume ratio 1: 1) at an extraction rate of 1.0 mL/min. Then, internal standards are respectively added into the extraction liquid, the results after sample injection analysis by gas chromatography-mass spectrometry are shown in the following table 2, an extraction liquid receiving bottle of saturated hydrocarbon is placed below S, an extraction liquid receiving bottle of aromatic hydrocarbon is placed below A, and an extraction liquid receiving bottle of colloid is placed below R.
TABLE 2
Comparative example 1
The differences from example 1 are: and adopting a manual SPE method.
The S, A values tested are as follows:
TABLE 3
From the above description, it can be seen that the above-mentioned embodiments of the present invention achieve the following technical effects: the automatic control system is adopted to control the sampling and sample introduction of the sampling device and the elution of the solid-phase extraction column, so that the time for solid-phase extraction and separation of the sample is effectively shortened, and the experimental efficiency is improved. Meanwhile, in the step of extracting and separating the direct coal liquefaction oil by adopting the solid phase extraction and separation device, the experimental data is less influenced by operators and the environment, so that the obtained analysis data has the advantages of good parallelism and high accuracy.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (11)
1. A solid phase extraction separation apparatus, comprising:
at least one extraction reagent storage device (10), at least one extraction reagent supply device being placed in the extraction reagent storage device (10);
at least one sample storage device (20) to be tested, wherein at least one sample supply device to be tested is placed in the sample storage device (20) to be tested;
at least one solid phase extraction column storage device (30), wherein at least one solid phase extraction column is placed in the solid phase extraction column storage device (30);
the sampling device (40), the said sampling device (40) includes at least one sampling pipeline and the said sampling pipeline one-to-one sampling needle; and
an automatic control system (50), the automatic control system (50) is used for controlling the sampling device (40) to perform sampling.
2. The solid phase extraction separation device of claim 1, further comprising: at least one activating reagent storage device (60), wherein an activating reagent storage and supply device is arranged in the activating reagent storage device (60).
3. The solid-phase extraction separation device according to claim 1 or 2, further comprising at least one waste liquid storage device (70), wherein at least one waste liquid recovery device is disposed in the waste liquid storage device (70), and the waste liquid recovery devices correspond to the solid-phase extraction columns one to one.
4. The solid phase extraction separation device of claim 3, further comprising at least one syringe pump disposed on the sampling line.
5. The solid phase extraction separation device of claim 4, further comprising at least one air-blowing switch, wherein the air-blowing switch is in one-to-one correspondence with the sampling pipeline and is used for controlling the pressure in the sampling pipeline.
6. The solid phase extraction separation device according to claim 5, wherein the solid phase extraction column storage device (30) is configured to store a plurality of solid phase extraction columns, and the solid phase extraction columns include a middle distillate solid phase extraction column and a heavy oil fraction solid phase extraction column.
7. The solid-phase extraction separation device of claim 6, wherein the solid-phase extraction column comprises 5 middle distillate solid-phase extraction columns and 5 heavy oil fraction solid-phase extraction columns.
8. The solid phase extraction separation device of claim 6, wherein the upper end of the solid phase extraction column is provided with a snap-in cover.
9. The solid phase extraction separation device according to claim 5, wherein the solid phase extraction separation device comprises at least one extraction liquid receiving unit (80), at least one extraction liquid receiving device is arranged in the extraction liquid receiving unit (80), and the extraction liquid receiving devices correspond to extraction liquids separated from the solid phase extraction column one by one.
10. The solid phase extraction separation device of claim 9, wherein the extract receiving device comprises a saturated hydrocarbon extract receiving device and an aromatic hydrocarbon extract receiving device corresponding to the middle distillate, and a saturated hydrocarbon extract receiving device, an aromatic hydrocarbon extract receiving device and a colloid extract receiving device corresponding to the heavy oil fraction.
11. The solid phase extraction separation device of claim 1, wherein the sampling device (40) comprises five sampling pipes and five sampling needles corresponding to the sampling pipes.
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| CN113952760A (en) * | 2021-09-24 | 2022-01-21 | 国网山东省电力公司电力科学研究院 | Automatic extraction device for furfural solid phase in transformer oil |
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| CN113952760A (en) * | 2021-09-24 | 2022-01-21 | 国网山东省电力公司电力科学研究院 | Automatic extraction device for furfural solid phase in transformer oil |
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