Phthalic acid ester compound sampling tube

Abstract

The utility model discloses a phthalate compound sampling tube, which belongs to the technical field of detection and comprises a glass tube and glass wool filled in the glass tube, a first magnesium silicate section and a second magnesium silicate section are filled on the glass wool, and two ends of the glass tube are sealed by sealing covers after sampling. The sampling tube disclosed by the utility model can be used for effectively collecting phthalic acid ester compounds in air, is simple in subsequent pretreatment method, convenient to carry and suitable for various on-site air sampling, and is used for carrying out gas collection and GCMS (Gas Chromatography Mass Spectrometry) analysis after ultrasonic extraction when the sampling tube disclosed by the utility model is used for carrying out gas collection. The adding standard recovery rate of the adsorption tube is 90.6%-107.2%, and the adsorption tube can meet the test requirements and has wide application prospects.

Description

Technical Field

[0001] The utility model relates to the technical field of detection, in particular to a sampling tube for phthalate compounds. Background Art

[0002] Indoor air pollution in vehicles has become one of the major issues that automotive companies and consumers are jointly concerned about. In fact, volatile organic compounds (VOCs) and semi-volatile organic compounds (SVOCs) emitted from automotive interior parts and materials are the main reasons affecting the air quality in vehicles and are extremely harmful to the human body. Among them, phthalate acid esters (PAEs) have attracted wide attention due to their carcinogenic, teratogenic, and mutagenic characteristics.

[0003] Phthalate acid esters (PAEs) are a kind of synthetic chemicals and are used as plasticizers in various industries, especially in plastic products. However, the binding force between PAEs and plastic products is weak. When the ambient temperature rises or they come into contact with oil-based organic solvents, they will be released into the surrounding environment, causing indoor air pollution in vehicles and posing a health hazard to humans, mainly manifested as endocrine disruption, reproductive toxicity, and carcinogenic, teratogenic, and mutagenic characteristics. At present, many countries and environmental protection organizations around the world, including China, have listed PAEs (especially DNOP, DEHP, BBP, DBP, DEP, and DMP) as "priority control pollutants" and have carried out a large number of studies on the detection and analysis of PAEs in the indoor environment.

[0004] At present, the sampling methods for phthalic acid in the air include solvent direct absorption method, filter membrane sampling method, activated carbon tube sampling method, polystyrene (PS) solid-phase column sampling, etc. However, the solvent direct absorption method has low sampling efficiency, and the filter membrane and activated carbon tube sampling methods are prone to loss of target compounds, and the samples are not easy to preserve. The polystyrene (PS) solid-phase column will introduce new pollutants during the determination process, causing pollution of the sampling tube. The activated carbon sampling method is simple, but the target compounds are easily lost during the sampling process and the pretreatment process. When using the filter membrane sampling method to collect phthalate esters, a large-flow sampling pump can be used, with a large sampling rate and a short sampling time. However, due to environmental influence, the phthalate esters on the filter membrane are easily volatilized during the sampling process, resulting in loss of target compounds, and the samples are not easy to preserve.

[0005] In view of this, this application is proposed. Content of the Utility Model

[0006] The purpose of the present utility model is to overcome the deficiencies of the prior art and provide a sampling tube for phthalate compounds. The sampling tube can effectively collect phthalate compounds in the air, has a simple subsequent pretreatment method, is convenient to carry, is suitable for various on-site air samplings, uses the sampling tube of the present utility model for gas collection, and is analyzed by GCMS after ultrasonic extraction. The spiked recovery rate of the adsorption tube is 90.6% - 107.2%, which can meet the test requirements and has a wide application prospect.

[0007] To achieve the above purpose, the technical solution adopted by the present utility model is as follows:

[0008] A sampling tube for phthalate compounds, comprising a glass tube and glass wool filled inside the glass tube. The glass wool is filled with a first magnesium silicate section and a second magnesium silicate section. After sampling, both ends of the glass tube are sealed by sealing caps.

[0009] Preferably, the distance between the first magnesium silicate section and the second magnesium silicate section is 4 - 10 mm.

[0010] Preferably, the mass ratio of the first magnesium silicate section to the second magnesium silicate section is 50:(50 - 200).

[0011] Preferably, the glass tube includes a glass tube body, an air inlet port and an air outlet port provided at both ends of the glass tube.

[0012] Preferably, a first cut is provided at the connection between the glass tube body and the air inlet port.

[0013] Preferably, a second cut is provided at the connection between the glass tube body and the air outlet port.

[0014] Preferably, the shape of the glass tube body is cylindrical.

[0015] Preferably, the diameter of the glass tube body is 2 - 7 mm and the length is 80 - 150 mm.

[0016] Preferably, the cross-sections of the air inlet port and the air outlet port are arc-shaped or triangular.

[0017] Preferably, the sealing cap is adapted to the shape of the sampling tube.

[0018] The beneficial effects of the present utility model are as follows: (1) The sampling tube of the present utility model can effectively collect phthalate compounds in the air. The subsequent pretreatment method is simple, it is convenient to carry, and it is suitable for various on-site air samplings. Using the sampling tube of the present utility model for gas collection, after ultrasonic extraction, it is analyzed by GCMS. The spike recovery rate of this adsorption tube is 90.6% - 107.2%, which can meet the test requirements and has broad application prospects. (2) The present utility model adopts a first magnesium silicate section and a second magnesium silicate section. The magnesium silicate (Florisil) is an adsorbent synthesized from diatomaceous earth and magnesium chloride. It is an amorphous magnesium silicate with high porosity and specific surface chemical properties. Due to the strong polarity of Florisil, it can effectively adsorb polar compounds. Phthalate gas in the air is easily adsorbed when passing through the magnesium silicate (Florisil). Description of the Drawings

[0019] Figure 1 It is a schematic structural diagram of the present utility model.

[0020] Reference numerals in the figure: 1, glass tube body; 2, glass wool; 3, first magnesium silicate section; 4, second magnesium silicate section; 5, intake port; 6, outlet port; 7, first cut; 8, second cut; 9, sealing cover. Detailed Embodiments

[0021] To make the objectives, technical solutions, and advantages of the embodiments of the present application clearer, the technical solutions in the embodiments of the present application will be clearly and completely described below. Obviously, the described embodiments are some, but not all, of the embodiments of the present application. All other embodiments obtained by those of ordinary skill in the art based on the embodiments of the present application without creative efforts shall fall within the scope of protection of the present application.

[0022] In the present application, regarding numerical ranges, unless otherwise specified, the above numerical ranges are considered continuous and include the minimum and maximum values of the range, as well as each value between such minimum and maximum values. Further, when the range refers to integers, it includes each integer between the minimum and maximum values of the range. In addition, when multiple ranges are provided to describe features or characteristics, the ranges can be combined. In other words, unless otherwise specified, all ranges disclosed herein should be understood to include any and all sub-ranges subsumed therein.

[0023] Unless otherwise specified, the component raw materials used in each embodiment and comparative example of the present utility model are all commercially available raw materials, and the component raw materials used in each parallel experiment are the same kind.

[0024] In addition, the terms "first" and "second" are for descriptive purposes only and should not be construed as indicating or implying relative importance or implicitly specifying the quantity of the indicated technical features. Thus, features defined with "first" and "second" may explicitly or implicitly include at least one such feature. In the description of the present utility model, "a plurality of" means at least two, such as two, three, etc., unless otherwise specifically defined.

[0025] Please refer to Figure 1 , the present utility model provides a sampling tube for phthalate compounds, which includes a glass tube and glass wool 2 filled inside the glass tube. A first magnesium silicate section 3 and a second magnesium silicate section 4 are filled on the glass wool. After sampling, both ends of the glass tube are sealed by sealing caps 9.

[0026] The sampling tube of the present utility model can effectively collect phthalate compounds in the air. The subsequent pretreatment method is simple, and it is convenient to carry. It is suitable for various on-site air sampling applications. The gas is collected using the sampling tube of the present utility model and analyzed by GCMS after ultrasonic extraction. The spike recovery rate of this adsorption tube is 90.6% - 107.2%, which can meet the test requirements and has broad application prospects.

[0027] The present utility model uses a first magnesium silicate section and a second magnesium silicate section. The magnesium silicate (Florisil) is an adsorbent synthesized from diatomaceous earth and magnesium chloride. It is an amorphous magnesium silicate with high porosity and specific surface chemical properties. Due to the strong polarity of Florisil, it can effectively adsorb polar compounds. Phthalate gas in the air is easily adsorbed when passing through magnesium silicate (Florisil).

[0028] In one embodiment, the distance between the first magnesium silicate section and the second magnesium silicate section is 4 - 10 mm.

[0029] In one embodiment, the mass ratio of the first magnesium silicate section to the second magnesium silicate section is 50:(50 - 200).

[0030] In one embodiment, the glass tube includes a glass tube body 1, an air inlet port 5 and an air outlet port 6 provided at both ends of the glass tube.

[0031] In one embodiment, a first cut 7 is provided at the connection between the glass tube body and the air inlet port.

[0032] In one embodiment, a second cut 8 is provided at the connection between the glass tube body and the air outlet port.

[0033] In one embodiment, the shape of the glass tube body is cylindrical.

[0034] In one embodiment, the diameter of the glass tube body is 2-7 mm, and the length is 80-150 mm.

[0035] In one embodiment, the cross-sections of the air inlet port and the air outlet port are arc-shaped or triangular.

[0036] In one embodiment, the shape of the sealing cap is adapted to that of the sampling tube.

[0037] In one embodiment, the preparation method of the phthalate compound sampling tube is as follows: put magnesium silicate into a conical flask, dry it at 100 °C, weigh magnesium silicate according to the mass ratio of the magnesium silicate section and the second magnesium silicate section, fill a certain mass of magnesium silicate and glass wool into the glass tube in sequence, dissolve the two ends of the glass at high temperature and seal it for storage to make the sampling tube.

[0038] When the phthalate compound sampling tube is sampling, it is opened at the first cutting port and the second cutting port, and the gas flow direction is from the air inlet port to the air outlet port. After sampling, the two ends of the sampling tube are covered with sealing caps and stored.

[0039] Example 1

[0040] This example provides a phthalate compound sampling tube, which includes a glass tube and glass wool filled inside the glass tube. The glass wool is filled with a first magnesium silicate section and a second magnesium silicate section. The filling mass of the first magnesium silicate section is 100 g, the filling mass of the second magnesium silicate section is 50 g, and the distance between the first magnesium silicate section and the second magnesium silicate section is 8 mm.

[0041] Among them, the glass tube body, the air inlet port and the air outlet port provided at both ends of the glass tube, a first cutting port is provided at the connection between the glass tube body and the air inlet port, and a second cutting port is provided at the connection between the glass tube body and the air outlet port.

[0042] Among them, the shape of the glass tube body is cylindrical, the diameter of the glass tube is 7 mm, and the length is 150 mm.

[0043] Among them, the cross-sections of the air inlet port and the air outlet port are arc-shaped.

[0044] After sampling, the two ends of the glass tube are sealed by sealing caps, and the shape of the sealing cap is adapted to that of the sampling tube.

[0045] Test Example

[0046] Usage method: Open it at the first cutting port and the second cutting port, the gas flow direction is from the air inlet port to the air outlet port. After sampling, the two ends of the sampling tube are covered with sealing caps and stored.

[0047] Sampling was carried out by connecting the intake port and the sampling pump with a silica gel tube. Air entered the sampling tube through the intake port at a sampling speed of 2 L / min for 60 min. 5 ml of toluene was added and ultrasonically treated at room temperature for 15 min. After filtration with a 0.45-μm filter membrane, it was analyzed by GCMS to calculate the concentration of phthalates.

[0048] Sampling flow rate: The sampling flow rate range of the sampling tube is 50 ml / min to 2000 ml / min, which can meet the sampling of low, medium, and high flow rates.

[0049] Experiments show that magnesium silicate has strong polarity and can effectively adsorb polar compounds. Phthalates in the air are easily adsorbed by magnesium silicate when passing through.

[0050] A mixed standard solution containing 0.3 μg of phthalates (specifically shown in Table 1, phthalates include but are not limited to the following types) was quantitatively added to the sampling tube, and high-purity nitrogen at 1000 mL / min was passed through to simulate the air sampling process. The recovery rate of various phthalates ≥ 90%.

[0051] Table 1 Mixed standard solution of phthalates

[0052]

[0053] It can be seen from Table 1 that the sampling tube described in the present invention can effectively collect phthalate compounds in the air. The subsequent pretreatment method is simple and it is convenient to carry, suitable for various on-site air sampling. Gas collection is carried out with the sampling tube of the present invention and analyzed by GCMS after ultrasonic extraction. The spiked recovery rate of this adsorption tube is 90.6% - 107.2%, which can meet the test requirements and has a wide application prospect.

[0054] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of the present invention rather than to limit the protection scope of the present invention. Although the present invention has been described in detail with reference to the preferred embodiments, those of ordinary skill in the art should understand that the technical solutions of the present invention can be modified or equivalently replaced without departing from the essence and scope of the technical solutions of the present invention.

Claims

1. A phthalate compound sampling tube, characterized in that: The method comprises a glass tube and glass wool filled in the glass tube, wherein the glass wool is filled with a first magnesium silicate segment and a second magnesium silicate segment, and after sampling, both ends of the glass tube are sealed by a sealing cover.

2. The phthalate compound sampling tube according to claim 1, characterized in that: The distance between the first magnesium silicate segment and the second magnesium silicate segment is 4-10 mm.

3. The phthalate compound sampling tube according to claim 1, characterized in that: The mass ratio of the first magnesium silicate segment to the second magnesium silicate segment is 50:(50-200).

4. The phthalate compound sampling tube according to claim 1, characterized in that: The glass tube comprises a glass tube body, and an air inlet port and an air outlet port arranged at two ends of the glass tube.

5. The phthalate sampling tube according to claim 4, characterized in that: A first cutting opening is provided at the connection between the glass tube body and the air inlet port.

6. The phthalate compound sampling tube according to claim 4, characterized in that: A second cutting opening is provided at the connection between the glass tube body and the gas outlet port.

7. The phthalate compound sampling tube according to claim 4, characterized in that: The shape of the glass tube body is cylindrical.

8. The phthalate compound sampling tube according to claim 4, characterized in that: The glass tube body has a diameter of 2 to 7 mm and a length of 80 to 150 mm.

9. The phthalate compound sampling tube according to claim 4, characterized in that: The cross sections of the air inlet port and the air outlet port are arc-shaped or triangular-shaped.

10. The phthalate compound sampling tube according to claim 1, characterized in that: The sealing cover is adapted to the shape of the sampling tube.

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