A device for determining carbonyl iron in coal-based methyl acetate

Abstract

The utility model discloses a kind of determination device of carbonyl iron in coal-based methyl acetate, including ultraviolet light source controller, the ultraviolet light source controller is connected to multiple ultraviolet lamp light sources by signal line, ultraviolet light source controller can simultaneously adjust control wattage, wavelength and luminous flux of multiple ultraviolet lamp light sources;Ultraviolet lamp light source is used to irradiate high-transmittance analysis dish, and special coating mirror surface passes reaction image in high-transmittance analysis dish to high-speed camera, and high-speed camera is connected with computer image analysis system.The utility model can realize multiple sample parallel detection, with the characteristics of small error, accurate control.

Description

Technical Field

[0001] This invention belongs to the field of rapid detection devices for ultraviolet photocatalytic colorimetric reactions, specifically relating to a device for determining carbonyl iron in coal-based methyl acetate. Background Technology

[0002] In the industrial production of methyl acetate, coal-based methyl acetate has become one of the important sources of methyl acetate products due to its significant competitive advantages in both output and price.

[0003] However, current coal-based methyl acetate production facilities often fail to meet color standards, mainly manifested as a pale yellow color in the product. The color change process is as follows: after sampling the methyl acetate product in a high borosilicate glass container and exposing it to light, the product will gradually turn pale yellow. After continued exposure to light for a period of time, a small amount of uneven pale yellow flocculent matter will appear.

[0004] Regarding the issue of the pale yellow component in coal-based methyl acetate products, there is currently no corresponding standard detection method. Furthermore, aside from the color change phenomenon under light conditions, it is difficult to determine whether coal-based methyl acetate products contain carbonyl iron. Existing analytical methods suffer from drawbacks such as complex operation, high cost, and strict requirements on sample purity. Based on the research on the determination of carbonyl nickel and carbonyl iron in coal-derived syngas (Liu Yang, et al., Liaoning Chemical Industry, May 2014, Vol. 43, No. 5), a method for detecting the content of carbonyl nickel and carbonyl iron in syngas has been developed. This method is based on graphite furnace atomic absorption spectrometry (Graphite Furnace Atomic Absorption Spectrometry) and mainly includes the following steps: 1. Sample pretreatment: The sample is pretreated with iodine chloride methanol solution absorption. 2. Instrumental analysis: The pretreated sample is analyzed using a graphite furnace atomic absorption spectrometer. 3. Data processing: The presence and content of carbonyl iron are determined through software calculation.

[0005] Comparative experiments showed that GC-MS single-sample detection takes 55 minutes and costs about 80 yuan per sample, which cannot meet the urgent need for rapid, simple and accurate determination of carbonyl iron in actual production. Utility Model Content

[0006] In order to overcome the shortcomings of the existing technology, the purpose of this utility model is to provide a device for determining carbonyl iron in coal-based methyl acetate. This device can realize the parallel detection of multiple samples and has the characteristics of small error and precise control.

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

[0008] An apparatus for determining carbonyl iron in coal-based methyl acetate includes an ultraviolet light source controller 1, which is connected to multiple ultraviolet lamp sources 3 via a signal line 2. The ultraviolet light source controller 1 is used to simultaneously adjust and control the wattage, wavelength and luminous flux of the multiple ultraviolet lamp sources 3.

[0009] The ultraviolet lamp source 3 is used to irradiate the high-transmittance analytical dish 4. The special coated reflective mirror 5 reflects the image in the high-transmittance analytical dish 4 to the high-speed camera 6. The high-speed camera 6 is connected to the computer image analysis system 11 via a line.

[0010] The ultraviolet light source controller 1, the ultraviolet light source 3, the high transmittance analysis dish 4, and the special coating reflective mirror 5 are placed on the same horizontal plane.

[0011] The ultraviolet light source controller 1 is equipped with a current regulation module.

[0012] The high-transmittance analytical dish 4 is equipped with an analytical dish sealing cap 8 on top. The high-transmittance analytical dish 4 is used to hold coal-based methyl acetate sample 10 and potassium thiocyanate (KSCN) particles 9. It has the characteristic of high light transmittance, which helps to fully irradiate the sample with ultraviolet light and ensures that the detection reaction proceeds smoothly.

[0013] The surface coating of the special coating mirror 5 is a nano silver / zinc oxide composite coating with a silver content of ≥60wt% and a coating thickness of 50-100nm.

[0014] The high-speed camera 6 records the entire color change process of coal-based methyl acetate 10.

[0015] The computer image analysis system 11 receives image signals from the high-speed camera 6.

[0016] The computer image analysis system 11 is model NVIDIA Jetson Nano Developer Kit B01.

[0017] The bottom of the special coated reflector surface 5 is equipped with a reflector tilt adjustment mechanism 12 for adjusting the reflection angle. The angle β adjustment range of the reflector tilt adjustment mechanism 12 is 30°-60°. The reflector tilt adjustment mechanism 12 is composed of a graduated rotating bracket.

[0018] The beneficial effects of this utility model are:

[0019] In actual production testing, this invention was used to test multiple batches of coal-based methyl acetate samples. The average testing time was only 10 minutes, with an accuracy rate exceeding 98%. Compared to traditional methods, efficiency was improved by 80%, effectively solving the problem of rapid detection of iron carbonyl in enterprise production. It is simple to operate, fast, and highly accurate, accelerating sample reaction and effectively improving testing efficiency. Multiple sample holders allow simultaneous testing of similar samples with varying iron carbonyl contents, making the reaction process more comparative and effectively mitigating errors caused by visual observation and the delayed color change effect. Furthermore, the device has a relatively low cost, making it highly suitable for widespread application. Attached Figure Description

[0020] Figure 1 This is a schematic diagram of the structure of this utility model.

[0021] Figure 2 This is a top view of the present invention.

[0022] Figure label:

[0023] 1-UV light source controller; 2-Signal line; 3-UV lamp light source; 4-High transmittance analytical dish; 5-Special coated reflector; 6-High-speed camera; 12-Reflector tilt adjustment mechanism; 8-Analytical dish sealing cap; 9-Potassium thiocyanate (KSCN) particles; 10-Methyl acetate sample; 11-Computer image analysis system. Detailed Implementation

[0024] The present invention will now be described in further detail with reference to the accompanying drawings.

[0025] This invention provides a device for determining carbonyl iron in coal-based methyl acetate. Multiple ultraviolet lamps 3 are connected to an ultraviolet light source controller 1, enabling precise control of power (10-40W), wavelength (350-500nm), and luminous flux (300-450lm). A high-transmittance analytical dish 4 and a specially coated reflective mirror 5 accelerate the colorimetric reaction to 10 minutes, while quantitative dosing (5mL sample + 0.1g reagent) ensures stability. A high-speed camera 6 (1000fps) captures the colorimetric dynamics, and the RGB colors are analyzed using an NVIDIA Jetson Nano system (R>180 indicates a positive result). This achieves industrial-grade detection targets with parallel multi-sample detection, an error of <±2%, and a false positive rate of 2%.

[0026] The ultraviolet light source controller 1, through its built-in current adjustment module and user interface, simultaneously regulates the wattage (power), wavelength, and luminous flux of multiple ultraviolet lamp sources 3. Specifically, by inputting target parameter values, the controller automatically adjusts the current to change the power, fine-tunes the voltage or frequency to change the wavelength, and adjusts the luminous flux by changing the power or the position of optical elements. The controller also features real-time monitoring to ensure that the light source always operates within the set range, thereby achieving precise control.

[0027] The functions of the ultraviolet light source controller 1 include: power management (providing stable power output); parameter setting (setting the wattage, wavelength, and luminous flux of the light source through a user interface or preset program); real-time monitoring (monitoring the operating status of the light source to ensure operation within the set range); the ultraviolet light source controller 1 is an Omron UV-LED irradiator controller (model: ZUV-C30H). Example

[0028] Take 5 mL of coal-based methyl acetate sample (known water content 0.01%, acetic acid content 0.0339%) into a covered high-transmittance analytical dish. Accurately weigh 0.1 g (0.08-0.12 g) of potassium thiocyanate granules and add them to the test tube. Directly irradiate the high-transmittance analytical dish containing the coal-based methyl acetate sample with an ultraviolet lamp (power 20W (±5% rated power), wavelength 365 nm, luminous flux 350 lm). After 10 min, the solution gradually turns blood red, indicating the presence of carbonyl iron in the sample.

[0029] Table 1. Results of Methyl Acetate Analysis

[0030]

[0031]

[0032] Verified through 12 sets of comparative experiments:

[0033] When the tilt angle β of the reflector is 60°, the light flux utilization rate reaches 92.7%;

[0034] The colorimetric stability was optimal when the potassium thiocyanate addition was 0.08-0.12 g (relative standard deviation (RSD) = 1.23%).

[0035] The working principle of this utility model is as follows:

[0036] This invention relates to a rapid qualitative analysis device for carbonyl iron in coal-based methyl acetate. First, the parameters of the controlled ultraviolet light source 3 are set via an ultraviolet light source controller 1: power, ultraviolet wavelength, and luminous flux. 5 mL of coal-based methyl acetate sample 10 is placed in a high-transmittance analytical dish 4 with a sealed analytical dish cap 8, and 0.08-0.12 g of potassium thiocyanate (KSCN) granules 9 are added. Ultraviolet light is turned on to induce a reaction between the two. The tilt adjustment mechanism 12 of the specially coated reflective mirror 5 is adjusted to clearly transmit the image of the chemical reaction to a high-speed camera 6. A computer image analysis system 11 is connected to the high-speed camera 6, which captures the process of whether a thiocyanate-iron complex is formed in real time. The computer image analysis system 11 receives and analyzes the captured images. The signal line 2 uses the RS485 bus protocol with a transmission rate of 115200 bps and a connection distance ≤50 m. The device utilizes ultraviolet light to selectively decompose carbonyl iron compounds, and potassium thiocyanate reacts with Fe3+. + With a specific colorimetric reaction, it eliminates interference from other ions. Through the detailed steps and judgment criteria described above, the presence of carbonyl iron in the sample can be clearly determined, providing a reliable detection basis for actual production.

[0037] Fe(CO)5→Fe 3+ +5CO (UV light irradiation);

[0038] Colorimetric reaction formula: Fe 3+ +3SCN - →Fe(SCN)3.

Claims

1. An apparatus for determining carbonyl iron in coal-based methyl acetate, characterized in that, It includes an ultraviolet light source controller (1), which is connected to multiple ultraviolet light sources (3) via a signal line (2). The ultraviolet light source controller (1) is used to simultaneously adjust and control the wattage, wavelength and luminous flux of the multiple ultraviolet light sources (3). An ultraviolet lamp light source (3) is used to irradiate a high-transmittance analytical dish (4). A special coated reflective mirror (5) reflects the image in the high-transmittance analytical dish (4) to a high-speed camera (6). The high-speed camera (6) is connected to a computer image analysis system (11) via a line.

2. The apparatus for determining carbonyl iron in coal-based methyl acetate according to claim 1, characterized in that, The ultraviolet light source controller (1), ultraviolet light source (3), high transmittance analytical dish (4), and special coated reflective surface (5) are placed on the same horizontal plane.

3. The apparatus for determining carbonyl iron in coal-based methyl acetate according to claim 1, characterized in that, The ultraviolet light source controller (1) is equipped with a current regulation module.

4. The apparatus for determining carbonyl iron in coal-based methyl acetate according to claim 1, characterized in that, The high transmittance analytical dish (4) is equipped with an analytical dish sealing cap (8) on top. The high transmittance analytical dish (4) is used to hold coal-based methyl acetate sample (10) and potassium thiocyanate (KSCN) particles (9).

5. The apparatus for determining carbonyl iron in coal-based methyl acetate according to claim 1, characterized in that, The surface coating material of the special coating mirror (5) is "nano silver / zinc oxide composite coating, with a coating thickness of 50-100nm".

6. The apparatus for determining carbonyl iron in coal-based methyl acetate according to claim 1, characterized in that, The computer image analysis system (11) receives image signals from the high-speed camera (6); The computer image analysis system (11) is model NVIDIA Jetson Nano Developer Kit B01.

7. The apparatus for determining carbonyl iron in coal-based methyl acetate according to claim 1, characterized in that, The bottom of the special coating reflector surface (5) is equipped with a reflector tilt adjustment mechanism (12) for adjusting the reflection angle. The angle between the reflector tilt adjustment mechanism (12) and the horizontal plane is β, and the adjustment range of β is 30°-60°. The reflector tilt adjustment mechanism (12) is composed of a scaled rotating bracket.

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