Liquid-liquid extraction pretreatment device for phthalate compounds

Abstract

The utility model relates to a liquid-liquid extraction pretreatment device for phthalate compounds, which comprises a device shell, a rotatable rotating shaft is arranged in the device shell, an extraction box is arranged on the rotating shaft, the extraction box is composed of two fixed sponges, a sample bottle is clamped in one of the fixed sponges, and the other of the fixed sponges is connected with the extraction box. And the other fixed sponge covers the sample bottle. The device disclosed by the utility model has the advantages that 1) the sample injection bottle is directly used for extraction, the operation is convenient, and extra pollution is not introduced; 2) the extraction process can be closed and kept away from light, and target decomposition in the extraction process is prevented; 3) the problem of inaccurate results caused by high background values of phthalic acid esters in air, water and experimental vessels in a laboratory is solved, an additional separation step is avoided, and the reliability and accuracy of the experiment are improved; and 4) by using the method, the time required by pretreatment can be saved, the concentration is not needed, the extraction can be directly carried out on a machine after the extraction is completed, and the phthalic acid ester pollution introduced after the solvent concentration is reduced.

Description

Technical Field

[0001] The utility model relates to the technical field of pre-treatment devices, in particular to a liquid-liquid extraction pre-treatment device for phthalate compounds. Background Art

[0002] At present, the known laboratory pretreatment methods for extracting phthalate compounds include liquid-liquid extraction, liquid microextraction, ultrasonic assisted extraction, microwave assisted extraction, solid phase extraction, solid phase microextraction, etc. Among them, the liquid-liquid extraction method is the most widely used, also known as solvent extraction, adding an immiscible solvent to the liquid sample, and using the different distribution coefficients of the target in different solvents to separate and extract the target analyte from the liquid sample matrix. The liquid-liquid extraction method has a wide range of applications, mature technology, strong repeatability, and can process large quantities of samples. However, the operation is complicated and requires multiple extractions, which is easy to introduce pollution and reduce the recovery rate of the target.

[0003] However, since phthalate compounds are widely used in plastic products and are not chemically bonded to plastics, they are easily released into the external environment and cause pollution. Phthalates not only exist in the air and tap water, affecting the experimental results, but also exist in solvents. Concentrating large extraction volume solvents will increase the detection of such compounds, thereby causing false positive results for samples. Therefore, the current detection method cannot avoid the above problems and is likely to have an adverse effect on the accuracy of the experiment. Summary of the invention

[0004] The purpose of the utility model is to provide a liquid-liquid extraction pretreatment device for phthalate compounds based on the above-mentioned deficiencies in the prior art, which adopts the sample bottle originally used for sampling to perform rotary extraction without introducing additional pollution, thereby achieving effective liquid-liquid extraction of phthalate compounds and improving experimental accuracy.

[0005] The purpose of this utility model is achieved by the following technical solutions:

[0006] A liquid-liquid extraction pretreatment device for phthalate compounds, characterized in that it includes a device shell, a rotatable rotating shaft is installed in the device shell, an extraction box is arranged on the rotating shaft, and the extraction box is composed of two fixed sponges, one of which has a sample bottle stuck in it, and the other fixed sponge covers the top of the sample bottle.

[0007] Rotary bearings are respectively installed at both ends of the rotating shaft, and the rotating bearings are connected to the inner wall of the device housing.

[0008] The rotating shaft is connected and controlled by a control panel, and the control panel is arranged outside the device housing.

[0009] A plurality of rotating shafts are arranged inside the device housing and are evenly spaced apart along the height direction.

[0010] A plurality of sample bottles are arranged in the fixed sponge; the plurality of sample bottles are evenly spaced along the axial direction of the rotating shaft.

[0011] The advantages of the utility model are:

[0012] 1) Directly use the injection bottle for extraction, which is easy to operate and does not introduce additional pollution;

[0013] 2) The extraction process can be sealed and protected from light to prevent the target from decomposing during the extraction process;

[0014] 3) It solves the problem of inaccurate results caused by high background values ​​of phthalates in laboratory air, water, and experimental utensils, avoids additional separation steps, and increases the reliability and accuracy of the experiment;

[0015] 4) This method can save the time required for pre-treatment. There is no need for concentration. After the extraction is completed, it can be directly put into the machine, reducing the phthalate pollution introduced after the solvent is concentrated. BRIEF DESCRIPTION OF THE DRAWINGS

[0016] Figure 1 It is a schematic diagram of the structure of the utility model;

[0017] Figure 2 It is a schematic diagram of the control panel in the utility model. DETAILED DESCRIPTION

[0018] The following is a further detailed description of the features of the present invention and other related features through embodiments in conjunction with the accompanying drawings to facilitate understanding by technicians in the same industry:

[0019] like Figure 1-2 As shown, the marks 1-6 in the figure respectively represent: control panel 1, device housing 2, fixed sponge 3, fixed sponge 4, sample bottle 5, and rotating bearing 6.

[0020] Example: Figure 1 As shown, the liquid-liquid extraction pretreatment device for phthalate compounds in this embodiment can realize the rotary extraction of phthalate compounds.

[0021] Specifically, the device in this embodiment includes a device housing 2, the interior of which is empty as a cavity. Three horizontally arranged rotating shafts are arranged inside the device housing 2, and the three rotating shafts are evenly spaced along the height direction of the device housing 2 to avoid mutual position interference during rotation. Rotating bearings 6 are respectively arranged at both ends of each rotating shaft, so that the rotating shaft can rotate smoothly inside the device housing 2; the rotating bearings 6 are connected to the inner wall of the device housing 2.

[0022] In this embodiment, in order to rotate the rotating shaft, a power device, such as a motor, is also provided in the device housing 2, and the motor is connected to the rotating shaft so that the rotating shaft can rotate; when there are multiple rotating shafts, a motor can be configured for each rotating shaft, or a transmission mechanism can be designed to allow one motor to drive multiple rotating shafts to rotate. In order to further control the rotation time and rotation speed of the rotating shaft, a control panel 1 is also provided outside the device housing 2. The control panel 1 can be connected to the power device signal that drives the rotating shaft to rotate by wire or wireless means, so that the operator can control the working state of the rotating shaft through the control panel 1 outside the device housing 2 to meet the extraction requirements.

[0023] An extraction box consisting of a fixed sponge 3 and a fixed sponge 4 is arranged on each rotating shaft, and a sample bottle 5 containing phthalate compounds can be inserted into the fixed sponge 3. Specifically, Figure 1 As shown, in this embodiment, a plurality of slots matching the sample bottle 5 are arranged at intervals on the fixed sponge 3, and the slots are generally slightly smaller than the size of the sample bottle 5, so that the sample bottle 5 can be firmly inserted into the slots by utilizing the elasticity of the sponge, and then firmly placed in the extraction box. The fixed sponge 4 can cover the top of the fixed sponge 3 to cover and limit the sample bottle 5.

[0024] When using this embodiment, the following usage process is included:

[0025] Rinse the beaker with n-hexane several times to make the content of phthalate compounds in the beaker less than the detection limit, then accurately pour out 10 ml of water from the 250 ml sample bottle 5 to make the water volume in the sample bottle 5 240 ml, then use a pipette to transfer 4 ml of n-hexane to the sample bottle 5, add 40 μL of 10 mg / L deuterated diethylhexyl phthalate-D4 (internal standard), put it into the fixed sponge 4 of the extraction box, cover the fixed sponge 3 to make the sample bottle 5 firmly placed in the extraction box, lock the extraction box, set the extraction time and the rotation speed of the rotating axis in the control panel 1, turn over the extraction for 5 minutes, and put it in the fume hood after the extraction is completed, let it stand for 5 minutes, the density of n-hexane is smaller than that of water, and it floats on the upper bottle mouth, directly use a Pasteur pipette to transfer about 1 ml and put it into the injection vial for on-machine detection.

[0026] After the gas chromatography-mass spectrometry was used, the detection limit of di(2-ethyl)hexyl phthalate was 0.32μg / L, and the recovery rate was 93.5-102% when the concentration of six spikes was 100μg / L. The recovery rate was good and met the needs of actual detection. At the same time, the entire experimental process avoided contact with plastic products to prevent contamination by phthalate compounds.

[0027] In the specific implementation of this embodiment: in addition to phthalate compounds, this embodiment can also be applied to other organic pollutant indicators extracted using solvents, such as polychlorinated biphenyls, polycyclic aromatic hydrocarbons, organic chlorine compounds and the like.

[0028] Sample bottle 5 uses a brown threaded open glass bottle for light-proof and airtight extraction. The pressure in the glass bottle can be adjusted by slightly loosening the threaded cap at one end, so that the entire extraction process can be smooth and leak-free. It is equipped with a polytetrafluoroethylene threaded cap for sealing.

[0029] Although the above embodiments have described the concepts and embodiments of the purpose of the utility model in detail with reference to the accompanying drawings, ordinary technicians in this field can recognize that various improvements and modifications can still be made to the utility model without departing from the scope of the claims, so they are not described one by one here.

Claims

1. A liquid-liquid extraction pretreatment device for phthalate compounds, characterized in that: The device comprises a device shell, a rotatable rotating shaft is installed in the device shell, an extraction box is arranged on the rotating shaft, and the extraction box is composed of two fixed sponges, one of which has a sample bottle stuck in it, and the other fixed sponge covers the top of the sample bottle.

2. The liquid-liquid extraction pretreatment device for phthalate ester compounds according to claim 1, characterized in that: Rotary bearings are respectively installed at both ends of the rotating shaft, and the rotating bearings are connected to the inner wall of the device housing.

3. The liquid-liquid extraction pretreatment device for phthalate ester compounds according to claim 1, characterized in that: The rotating shaft is connected and controlled by a control panel, and the control panel is arranged outside the device housing.

4. The liquid-liquid extraction pretreatment device for phthalate ester compounds according to claim 1, characterized in that: A plurality of rotating shafts are arranged inside the device housing and are evenly spaced apart along the height direction.

5. The liquid-liquid extraction pretreatment device for phthalate ester compounds according to claim 1, characterized in that: A plurality of sample bottles are arranged in the fixed sponge; the plurality of sample bottles are evenly spaced along the axial direction of the rotating shaft.

Images