An in-situ headspace sampling device applied to fermented grains detection

Abstract

The application discloses an in-situ headspace sampling device applied to detection of fermented grains, and belongs to the technical field of gas sampling. The device comprises a sampling pipe, a handle, a connecting rod, a headspace sampling head and a sampling head cover. The sampling device is directly inserted into the fermented grains. The sampling head cover can support a sample gas chamber. The fermented grain gas sample around the sampling head cover continuously penetrates into the sample gas chamber. The sample gas is sent into an analysis instrument by using a headspace principle, and in-situ deep sampling of the fermented grains is realized.

Description

TECHNICAL FIELD

[0001] The application belongs to the technical field of gas sampling and relates to an in-situ headspace sampling device applied to the field of fermented grains detection. BACKGROUND

[0002] Due to its unique fermentation process and unique flavor characteristics, Baijiu (liquor) has had a wide impact worldwide. During the production process, the microflora in the environment and the environment dynamically develop and balance during the fermentation of fermented grains, regulate the changes of microorganism species in the pit, and generate and accumulate metabolic products, thereby affecting the quality and style of Luzhou-flavor Baijiu. Taking fermented grains as the object, studying the dynamic change process of the chemical composition of fermented grains over time during the fermentation process can help understand the source and derivation relationship of the complex and diverse components in Baijiu, provide a scientific basis for analyzing the characteristics of microorganisms in the pit, and also coordinate the action of functional bacteria in the pit fermented grains, thereby improving the technical level of Baijiu production.

[0003] In the analysis and research of fermented grains, it is often necessary to determine the chemical composition of fermented grains. Due to the complexity of the components of fermented grains, the presence of many interferents, and the complexity of the environment, the in-situ online detection technology and method of fermented grains has become a major problem. The conventional method for determining fermented grains is to first take a certain amount of fermented grains sample from the cellar, then send it to the laboratory for a series of complex sample pretreatment, and then use headspace or solution extraction methods for sampling, and use chromatography, mass spectrometry, spectroscopy, and their combined equipment for detection.

[0004] Whether it is fermented grains or fermented grains sealed in the pit, as the fermentation process progresses, the physical form of the fermented grains changes from granular to sludge. Fermented grains are fermented in layers, and the fermentation degree of fermented grains at different depths is different, which poses a great challenge to the sampling of fermented grains.

[0005] There are many patents for fermented grains solid samplers, such as a conical sampling head (CN215985309U), a sampling shovel (CN219798748U), a hollow tube with a sampling scraper (CN212059457U), a fermented grains gas detection (CN116256417A), and a gas inlet end of a gas guide structure inserted into the environment to be detected (CN115901661A). SUMMARY

[0006] The main purpose of the present application is to overcome the shortcomings of the prior art, provide a kind of in-situ headspace sampling device for detection of fermented grains.The present application solves the problem of in-situ sampling and deep sampling of fermented grains, realizes in-situ sampling and online analysis of fermented grains.The device is directly inserted into fermented grains, and a sample gas chamber can be formed by the sampling head cover.The gas sample of fermented grains around the sampling head cover continuously penetrates into the sample gas chamber, and the sample gas is sent into the analysis instrument using the headspace principle, realizing in-situ deep sampling of fermented grains, and then analyzed by the analysis instrument.By selecting different lengths of connecting rods, different depth of fermented grains can be sampled, providing a powerful sampling tool support for studying the layered fermentation chemicals of fermented grains.

[0007] The technical scheme of the present application is as follows:

[0008] The present application provides a kind of in-situ headspace sampling device for detection of fermented grains, including sampling tube, handle, connecting rod, headspace sampling head and sampling head cover.

[0009] One end of the sampling tube is connected to an analysis instrument or a sampling bottle, and the other end is sequentially connected to the handle, connecting rod and headspace sampling head; the headspace sampling head is connected to the sampling head cover.

[0010] The headspace sampling head is a hollow cylindrical structure with a protruding platform in the middle, and the end of the headspace sampling head towards the sampling head cover is thickened to form a sampling head gas chamber, and the other end is inserted into the sampling tube.The sampling head gas chamber is connected to a filter core at the end towards the sampling head cover, further preventing fermented grain particles from blocking the sampling channel.Sampling head gas channels are evenly distributed around the headspace sampling head, facilitating the flow of external gas.

[0011] The sampling head cover is a cylindrical structure with a hollow center and a triangular arrow shape at the front end, and multiple long strip-shaped recessed areas are evenly distributed on the cylindrical structure of the sampling head cover, and a filter screen is covered outside the area.The rear end of the sampling head cover is connected to the headspace sampling head, and the end of the headspace sampling head with the filter core is inserted into the center of the sampling head cover, forming a sample gas chamber between the front end of the filter core and the inside of the sampling head cover, and the fermented grain sample gas continuously penetrates into the sample gas chamber through the filter screen.

[0012] The connecting rod is a hollow cylinder with a thick end and a thin end, and the thin end is connected to a hollow cylindrical handle, and the thick end is connected to the headspace sampling head, forming a connecting rod gas chamber between the sampling heads.

[0013] The gap between the sampling tube and the handle and the connecting rod forms a connecting rod gas channel.

[0014] The connecting rod gas channel, connecting rod gas chamber, sampling head gas channel, sample gas chamber, sampling head gas chamber and sampling tube are sequentially connected.

[0015] Further, in the technical scheme, the length of the connecting rod can be adjusted according to sampling needs, and a plurality of connecting rods are connected in series to extend the sampling distance.

[0016] Further, in the technical scheme, the length of the connecting rod is 0.2-3m.

[0017] Further, in the technical scheme, the sampling tube outer wall is provided with a heating device. The sampling tube outer wall can be heated to reduce sample residue.

[0018] Further, in the technical scheme, the filter screen mesh number is 100-1000, and the filter screen mesh number is determined by the nature of the fermented grains, and each sample is replaced once. When the fermented grains are in a granular form, the mesh number is 100-500; when the fermented grains are in a sludge form, the mesh number is 500-1000,

[0019] Further, in the technical scheme, a filter screen fixing rib is sleeved at both ends of the filter screen to firmly fix the filter screen on the sampling head cover, facilitating replacement.

[0020] After the headspace sampling device is inserted into the fermented grains, when sampling, the sampling pump of the analysis instrument draws air in the sampling tube, and the environmental gas enters the sample gas chamber along the connecting rod air channel, the connecting rod air chamber and the sampling head air channel. The gas components of the fermented grain sample are continuously volatilized into the sample gas chamber, and the sample gas is driven by the airflow, passes through the filter core, enters the analysis instrument through the sampling head air chamber and the sampling tube, and realizes in-situ deep sampling.

[0021] Advantages of the application

[0022] The application provides an in-situ headspace sampling device applied to fermented grain detection, is designed based on a headspace principle, can collect chemical components volatilized from fermented grains in-situ and on-line, can realize sampling at different depths by adjusting the length of the connecting rod, solves the problem of supplementing headspace gas inserted into a depth of 1-2m or more through unique air channel design, facilitates insertion of the sampling device into fermented grains through arrow design, effectively prevents the air channel from being blocked by fermented grains through two filter screens, and facilitates replacement of the filter screens after sampling. The sampling tube can be heated to reduce sample residue. The headspace gas of the fermented grains collected by using the patent can realize in-situ deep sampling of the fermented grains, reduces sample waste, and realizes rapid detection and analysis of the fermented grains without pretreatment of the gas analysis. BRIEF DESCRIPTION OF DRAWINGS

[0023] Figure 1 FIG. 1 is a structural schematic view of an in-situ headspace sampling device applied to fermented grains;

[0024] Figure 2 FIG. 5 is a detection spectrum diagram of the sampling head inserted into fermented grains at different depths in ion mobility spectrometry detection in Embodiment 2;

[0025] Figure 3This is a comparison of ion mobility spectra obtained from the same sample mash surface and ion mobility spectra inserted 20 cm into the mash in Example 3.

[0026] In the diagram, 1-sampling tube; 2-handle; 3-connecting rod airway; 4-connecting rod; 5-connecting rod air chamber; 6-headspace sampling head; 7-sampling head airway; 8-sampling head air chamber; 9-filter fixing rib; 10-filter screen; 11-filter element; 12-sample air chamber; 13-sampling head cover. Detailed Implementation

[0027] The embodiments of the present invention will be described in detail below. It should be emphasized that the following description is merely exemplary and not intended to limit the scope and application of the present invention.

[0028] Example 1

[0029] like Figure 1 As shown, an in-situ headspace sampling device for detecting fermented mash includes a sampling tube 1, a handle 2, a connecting rod 4, a headspace sampling head 6, and a sampling head cover 13.

[0030] The sampling tube is connected to the analysis instrument at one end and passes through the handle and connecting rod in sequence at the other end, and is connected to the headspace sampling head; the headspace sampling head is connected to the head cover.

[0031] The headspace sampling head 6 is a hollow cylindrical structure with a protrusion in the middle. The headspace sampling head widens at one end facing the sampling head cover, forming a sampling head air chamber 8, and the sampling tube 1 can be inserted into the other end. A filter element 11 is connected to the end of the sampling head air chamber 8 facing the sampling head cover to further prevent mash particles from clogging the sampling channel. Sampling head air passages 7 are evenly distributed around the headspace sampling head to facilitate the inflow of external gas.

[0032] The sampling head cover 13 is a cylindrical structure with a centrally hollowed-out center and a triangular arrowhead-shaped front end. Multiple elongated hollowed-out recessed areas are evenly distributed on the cylindrical structure of the sampling head cover. A filter screen 10 is covered on the outside of each area, and a filter screen fixing rib 9 is fitted at each end of the filter screen 10 to firmly fix the filter screen 10 to the sampling head cover 13 for easy replacement. The rear end of the sampling head cover is connected to a headspace sampling head 6. One end of a filter core 11 in the headspace sampling head 6 is inserted into the center of the sampling head cover 13, forming a sample gas chamber 12 at the front end of the filter core 11 and inside the sampling head cover. The sample gas from the fermented mash continuously permeates into the sample gas chamber 12 through the filter screen 10.

[0033] The connecting rod 4 is a hollow cylinder with one thick end and a hollow cylindrical handle connected to the thinner end. The thicker end is connected to the headspace sampling head 6, and a connecting rod air chamber 5 is formed between the sampling heads.

[0034] The sampling tube 1 is connected with an analysis instrument at one end, sequentially passes through the handle 2, the connecting rod 4, and is connected with the headspace sampling head 6. The gap between the sampling tube 1 and the handle 2, the connecting rod 4 forms the connecting rod air channel 3.

[0035] The connecting rod air channel, the connecting rod air chamber, the sampling head air channel, the sample air chamber, the sampling head air chamber, and the sampling tube are sequentially communicated.

[0036] The connecting rod 4 can be adjusted in length according to the sampling needs, or a plurality of connecting rods 4 are connected in series to prolong the sampling distance.

[0037] The sampling tube 1 can be heated on the outer wall to reduce sample residue.

[0038] The filter screen 10 is determined by the nature of the fermented grains, and each sample is replaced once.

[0039] After the headspace sampling device is inserted into the fermented grains, when sampling, the sampling pump of the analysis instrument in the sampling tube 1 draws air, and the environmental gas enters the sample air chamber 12 along the connecting rod air channel 3, the connecting rod air chamber 5, the sampling head air channel 7, the gas components of the fermented grain sample are continuously volatilized into the sample air chamber 12, and the sample gas is driven by the airflow to pass through the filter core 11, and then enters the analysis instrument along the sampling head air chamber 8 and the sampling tube 1 to realize in-situ deep sampling.

[0040] Example 2

[0041] The analysis instrument is an ion mobility spectrum, and the ion mobility spectrum detects the alcohol content in the fermented grains by inserting the headspace sampling device of example 1 into three same fermented grains 3# sample, 5# sample, and 7# sample. As the insertion depth changes, the alcohol content in the fermented grains continuously increases, and the content of other substances decreases. Further, it is proved that the stacked fermented grains have the characteristics of layered fermentation.

[0042] Example 3

[0043] The analysis instrument is an ion mobility spectrum, and the ion mobility spectrum detects 3# sample, and the headspace sampling device of example 1 is away from the surface of the stacked fermented grains and inserted into the fermented grain stack. The collected other clean air is diluted by 20 times for detection. The comparison of the detection spectrum shows that the direct insertion of the sampling head into the fermented grains can detect a large number of substances with high content.

[0044] The above is a further detailed description of the present application in combination with specific / preferred embodiments, and cannot be regarded as a limitation of the specific implementation of the present application. For ordinary skilled persons in the technical field to which the present application belongs, without departing from the concept of the present application, they can make a number of substitutions or modifications to the described embodiments, and these substitutions or modifications shall be regarded as belonging to the protection scope of the present application.

Claims

1. An in-situ headspace sampling device for detecting fermented mash, characterized in that: It comprises a sampling tube, a handle, a connecting rod, a headspace sampling head and a sampling head cover. One end of the sampling tube is connected with an analytical instrument or a sampling bottle, and the other end is connected with the headspace sampling head through the handle and the connecting rod. The headspace sampling head is a hollow cylindrical structure with a protruding platform in the middle. The headspace sampling head is connected with the sampling head cover. The headspace sampling head is a hollow cylindrical structure with a protruding platform in the middle. The headspace sampling head is connected with the sampling head cover. The headspace sampling head is a hollow cylindrical structure with a protruding platform in the middle.

2. The apparatus of claim 1, wherein: The headspace sampling head is connected with the sampling head cover.

3. The apparatus of claim 1, wherein: The headspace sampling head is a hollow cylindrical structure with a protruding platform in the middle.

4. The apparatus of claim 1, wherein: The headspace sampling head is connected with the sampling head cover.

5. The apparatus of claim 1, wherein: The headspace sampling head is a hollow cylindrical structure with a protruding platform in the middle.

6. The apparatus of claim 1, wherein: The headspace sampling head is connected with the sampling head cover. The headspace sampling head is a hollow cylindrical structure with a protruding platform in the middle. The headspace sampling head is connected with the sampling head cover. The headspace sampling head is a hollow cylindrical structure with a protruding platform in the middle. The headspace sampling head is connected with the sampling head cover. The headspace sampling head is a hollow cylindrical structure with a protruding platform in the middle. The headspace sampling head is connected with the sampling head cover. The headspace sampling head is a hollow cylindrical structure with a protruding platform in the middle. The headspace sampling head is connected with the sampling head cover. The headspace sampling head is a hollow cylindrical structure with a protruding platform in the middle. The headspace sampling head is connected with the sampling head cover. The headspace sampling head is a hollow cylindrical structure with a protruding platform in the middle. The headspace sampling head is connected with the sampling head cover. The headspace sampling head is a hollow cylindrical structure with a protruding platform in the middle. The headspace sampling head is connected with the sampling head cover. The headspace sampling head is a hollow cylindrical structure with a protruding platform in the middle. The headspace sampling head is connected with the sampling head cover. The headspace sampling head is a hollow cylindrical structure with a protruding platform in the middle. The headspace sampling head is connected with the sampling head cover. The headspace sampling head is a hollow cylindrical structure with a protruding platform in the middle. The headspace sampling head is connected with the sampling head cover. The headspace sampling head is a hollow cylindrical structure with a protruding platform in the middle. The headspace sampling head is connected with the sampling head cover. The headspace sampling head is a hollow cylindrical structure with a protruding platform in the middle. The headspace sampling head is connected with the sampling head cover. The headspace sampling head is a hollow cylindrical structure with a protruding platform in the middle. The headspace sampling head is connected with the sampling head cover. The headspace sampling head is a hollow cylindrical structure with a protruding platform in the middle. The headspace sampling head is connected with the sampling head cover. The headspace sampling head is a hollow cylindrical structure with a protruding platform in the middle. The headspace sampling head is connected with the sampling head cover. The headspace sampling head is a hollow cylindrical structure with a protruding platform in the middle. The headspace sampling head is connected with the sampling head cover. The headspace sampling head is a hollow cylindrical structure with a protruding platform in the middle. The headspace sampling head is connected with the sampling head cover. The headspace sampling head is a hollow cylindrical structure with a protruding platform in the middle. The headspace sampling head is connected with the sampling head cover. The headspace sampling head is a hollow cylindrical structure with a protruding platform in the middle. The headspace sampling head is connected with the sampling head cover. The headspace sampling head is a hollow cylindrical structure with a protruding platform in the middle. The headspace sampling head is connected with the sampling head cover. The headspace sampling head is a hollow cylindrical structure with a protruding platform in the middle. The headspace sampling head is connected with the sampling head cover. The headspace sampling head is a hollow cylindrical structure with a protruding platform in the middle. The headspace sampling head is connected with the sampling head cover. The headspace sampling head is a hollow cylindrical structure with a protruding platform in the middle. The headspace sampling head is connected with the sampling head cover. The headspace sampling head is a hollow cylindrical structure with a protruding platform in the middle. The headspace sampling head is connected with the sampling head cover. The headspace sampling head is a hollow cylindrical structure with a protruding platform in the middle. The head

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