CN112946208A

CN112946208A - Filter bag type crude fiber determinator, method and application

Info

Publication number: CN112946208A
Application number: CN202110148624.8A
Authority: CN
Inventors: 王峰; 李冬梅; 李永强; 李健美; 张化涛; 李永亮; 张小超; 冯佰涛
Original assignee: Jinan Alva Instrument Co ltd
Current assignee: Jinan Alva Instrument Co ltd
Priority date: 2021-02-02
Filing date: 2021-02-02
Publication date: 2021-06-11

Abstract

The invention discloses a filter bag type crude fiber determinator, a method and application, comprising a reagent container, a liquid adding system, a constant temperature instant heating device, a reaction container, a filter bag bracket, a filter bag, a driving device, a liquid drainage system and a control system; the reaction vessel is provided with a heating device for heating the reaction vessel; the filter bag support is arranged in the reaction container, and a filter bag is arranged in the filter bag support; the driving device drives the filter bag bracket or the reaction container so as to drive the reagent to flow; the reagent container is connected with a liquid adding system, the liquid adding system is connected with a reagent constant-temperature instant heating device, and the reagent constant-temperature instant heating device is connected with a reagent heating port of the reaction container; the liquid discharge system is connected with the waste liquid container; the control system controls the liquid adding system, the reagent constant-temperature instant heating device, the driving device and the liquid discharging system; the device has small measurement error and high reaction speed, can support not only the traditional acid-base digestion filtration method, but also a paradigm method group, and has very high application value.

Description

Filter bag type crude fiber determinator, method and application

Technical Field

The invention belongs to the field of crude fiber determination, and particularly relates to a filter bag type crude fiber determination instrument and a filter bag type crude fiber determination method, which can be applied to feed crude fiber determination, food crude fiber determination, plant crude fiber determination, grain crude fiber determination, vegetable crude fiber determination, tea crude fiber determination and the like.

Background

The statements herein merely provide background information related to the present disclosure and may not necessarily constitute prior art.

Crude fiber is an important test item parallel to protein and fat in the fields of food and feed, and crude fiber measurement is one of the most important test items of national standard mandatory requirements for detection relating to food safety in the industries of food, medicine, dairy products and the like. Both food and animal feed need to contain a proper amount of crude fiber, so the crude fiber is always used as a detection item for various foods and feeds.

At present, the existing crude fiber measuring apparatus, such as the structures disclosed in patent application No. CN 201120109007.9 and patent application No. CN201921721037.8, mainly has the following problems:

1. the glass structure is a linear structure and mainly comprises a condenser and a glass vessel with a filter device which are combined up and down, and a heating assembly is arranged at the lower end of the glass vessel, so that the sealing is difficult, and the leakage is easy to cause sample testing failure;

2. the existing crude fiber measuring instrument generally adopts a glass sand core as a filtering element, and the actual physical size of the crude fiber is generally larger than 16 meshes, so that the glass sand core is extremely blocked, and the sample measurement fails;

3. after digestion is completed by the crucible suction filtration method, a sample needs to be transferred to a crucible from a glass sand core in a drying link, and because the absolute content of crude fibers of a common test sample is not high, the glass sand core belongs to a porous loose structure, crude fiber residues are easily formed, and a hairbrush is generally adopted in a transfer process, so that sample loss is easily caused, and the sample measurement is low.

Although the crude fiber measuring instrument is simple to implement, due to the above problems, the crude fiber content can be accurately measured in principle, but the crude fiber measuring instrument is practically used. The test fails or the result deviation is too high, so that the original instrument can not be normally used basically.

In prior patent 201710753103.9, a rotary full-automatic feed fiber content measuring device is disclosed, which has the following disadvantages:

1. the device has principle errors, and because the device comprises a condenser, the test result has no credibility and cannot meet the basic test requirement;

2. the device is low in testing speed, the crude fiber is tested by using the acid-base small bamboo raft, the testing time is as long as 9-12 hours, the production rhythm of a normal enterprise cannot be followed, and the practicability is poor.

3. Because the test process involves strong acid, strong base and high temperature, the reliability of the machine is extremely critical, but the device is not designed according to any related protective principle, real full automation is difficult to realize, the test risk is extremely high, and even serious accidents can be caused.

4. The device has high process realization difficulty, and low operability.

Disclosure of Invention

Aiming at the defects in the prior art, the invention aims to provide a novel filter bag type crude fiber tester and a method thereof, and the filter bag type crude fiber tester disclosed by the invention can be used for feeds, foods and the like with the crude fiber content of 0.1% -100%.

In order to achieve the purpose, the invention is realized by the following technical scheme:

in a first aspect, an embodiment of the present invention provides a filter bag type crude fiber determinator, including a reagent container, a liquid adding system, a constant temperature instant heating device, a reaction container, a filter bag support, a filter bag, a driving device, a liquid discharge system, a weighing system, a waste liquid container and a control system;

the reaction vessel is provided with a heating device for heating the reaction vessel;

the weighing system is arranged at the bottom of the reaction container and is used for weighing the reaction container;

the filter bag support is arranged in the reaction container, and the filter bag is placed in the filter bag support;

the driving device drives the filter bag bracket and the reaction container to move relatively, so as to drive the test reagent to flow;

the reagent container is connected with a liquid adding system, the liquid adding system is connected with a constant-temperature instant heating device, and the constant-temperature instant heating device is connected with a reagent heating port of the reaction container;

one end of the liquid discharge system is connected with a liquid discharge port of the reaction container, and the other end of the liquid discharge system is connected with a waste liquid container;

the control system controls the liquid adding system, the constant-temperature instant heating device, the driving device and the liquid discharging system.

As a further technical scheme, the liquid adding system comprises a reagent liquid adding pump, a pipeline and a liquid inlet valve; one end of the pipeline is connected with the reagent container, the other end of the pipeline is connected with the reagent constant-temperature instant heating device, and a reagent charging pump and a liquid inlet valve are installed on the pipeline.

As a further technical scheme, the reagent container comprises a plurality of containers, and the pipeline also comprises a plurality of containers; one pipeline is connected with one reagent container, and each pipeline is provided with one reagent charging pump and one liquid inlet valve.

As a further technical scheme, the reagent instant heating device comprises a liquid inlet, a main body structure, a heating device, a temperature detection sensor and a liquid outlet; the reagent rapid heating system and the liquid adding system work in a matching way; one end of the main structure is a liquid inlet, the other end of the main structure is a liquid outlet, a reagent flowing cavity is arranged in the main structure, and the reagent flowing cavity is communicated with the liquid inlet and the liquid outlet; a temperature sensor is inserted into the side wall of the main body structure, and a measuring head of the temperature sensor is positioned in the reagent flowing cavity; and a heating device is also inserted into the side wall of the main body structure and is used for heating the reagent in the reagent flow cavity.

As a further technical scheme, the filter bag support comprises a cage structure and a sealing cover, the interior of the cage structure is divided into a plurality of small spaces, and a plurality of filter bags can be placed in each small space.

As a further technical scheme, the filter bag is a membrane material made of an acid-resistant, alkali-resistant and corrosion-resistant polymer material, a plurality of through holes are uniformly formed in the surface of the filter bag, liquid and small molecules with the diameter meeting the diameter of the through holes can pass through the through holes, and large-diameter coarse fibers cannot pass through the through holes.

In a second aspect, the invention is based on the crude fiber measuring instrument, and further provides a crude fiber measuring method based on an acid-base digestion filtration method, which comprises the following steps:

step 1, putting the primarily treated sample into a filter bag, and sealing the filter bag;

step 2, placing the filter bag filled with the sample into a filter bag bracket in the reaction container;

step 3, starting the instrument, wherein the liquid adding system can automatically extract the acidic reagent from the reagent container containing the acidic reagent, the acidic reagent is changed from a normal-temperature state to a high-temperature state after flowing through the constant-temperature instant heating device and then enters the reaction container, meanwhile, the driving device in the reaction container enables the reagent to form a flowing state to increase the chemical reaction speed of the sample and the reagent in the filter bag, and after the reaction of the sample and the reagent is finished, the liquid discharging system discharges the reagent in the reaction container;

step 4, the liquid adding system automatically extracts a purified water reagent from a reagent container containing purified water again, the purified water reagent is changed from a normal temperature state to a high temperature state after flowing through the constant temperature instant heating device and then enters the reaction container, meanwhile, a driving device in the reaction container enables the reagent to be in a flowing state to thoroughly wash away various impurities generated in the last step of acid digestion, and after washing is completed, the liquid discharging system discharges the reagent in the reaction container;

step 5, the liquid adding system extracts the alkaline reagent from the reagent container containing the alkaline reagent again, the extracted alkaline reagent is changed from a normal temperature state to a high temperature state after flowing through the constant temperature instant heating device, then the extracted alkaline reagent enters the reaction container, meanwhile, the driving device in the reaction container enables the reagent to form a flowing state to increase the chemical reaction speed of the sample and the reagent in the filter bag, and after the reaction of the sample and the reagent is finished, the liquid discharging system discharges the reagent in the reaction container;

step 6, the liquid adding system extracts the purified water reagent from the reagent container containing the purified water reagent again, the extracted purified water reagent is changed from a normal temperature state to a high temperature state after flowing through the constant temperature instant heating device, then the purified water reagent enters the reaction container, meanwhile, the reagent flowing device in the reaction container enables the reagent to form a flowing state to thoroughly wash away various impurities generated in the last step of acid digestion, and after the washing is finished, the liquid discharging system discharges the reagent in the reaction container; and (4) closing the instrument and taking out and drying the filter bag to enter the subsequent step when the whole experiment is finished.

In a third aspect, the invention is based on the crude fiber analyzer mentioned above, and further provides a neutral detergent fiber measuring method based on a paradigm method, comprising the following steps:

step 1: crushing a sample to be detected so that the sample can completely pass through a sieve with a sieve hole of 0.42 mm;

step 2: putting a sample to be detected into a filter bag, and sealing the filter bag;

and step 3: degreasing the filter bag with sealed opening by petroleum ether (or acetone) in advance for the sample with fat content more than 10%, and if the fat content is less than 10%, the step can be omitted;

and 4, step 4: putting the filter bag filled with the sample into a filter bag support in an instrument reaction kettle;

and 5: 50ml of alpha-high temperature amylase is manually poured into the reaction kettle (the dosage of the amylase can be changed according to the actual dosage and the activity of the used enzyme as appropriate, taking the enzyme with the activity of 10kU/g as an example, not less than 0.2 ml/sample). Or the alpha-high temperature amylase can be added into a container containing the reagent in advance, and the reagent is pumped into the reaction kettle together when the reagent is pumped by the machine.

Step 6: starting a control system, extracting a neutral washing reagent from a reagent container containing the neutral washing reagent by a liquid adding system, enabling the extracted reagent to flow through a constant-temperature reagent instant heating device and then to be in a high-temperature state, then enabling the reagent to enter a reaction kettle, driving the reaction kettle or a filter bag support to rotate by a driving device, enabling the reagent to be in a flowing state, increasing the chemical reaction speed of a sample and the reagent in the filter bag, and enabling the sample and the reagent to react after the reaction is finished;

and 7: the control system controls the liquid discharge system to be started to discharge the reagent in the reaction kettle;

and 8: the liquid adding system extracts a purified water reagent from a container filled with the purified water reagent, the extracted reagent flows through the constant-temperature reagent instant heating device to be in a high-temperature state and then enters the reaction kettle, the driving device drives the reaction kettle or the filter bag support to rotate, the reagent is in a flowing state, the cleaning effect is improved, and after cleaning is finished;

and step 9: the control system controls the liquid discharge system to be started to discharge the reagent in the reaction kettle; and (5) closing the control system when the whole experiment is finished, and taking out and drying the filter bag.

In a fourth aspect, the method for measuring acid washing fiber by using the filter bag type crude fiber measuring instrument based on the paradigm method comprises the following steps:

step 1: crushing a sample to be detected so that the sample can completely pass through a sieve with 1mm sieve pores;

and 5: starting a control system, extracting an acidic washing reagent from a reagent container containing the acidic washing reagent by a liquid adding system, enabling the extracted reagent to flow through a constant-temperature reagent instant heating device and then to be in a high-temperature state, then enabling the reagent to enter a reaction kettle, driving the reaction kettle or a filter bag support to rotate by a driving device, enabling the reagent to be in a flowing state, increasing the chemical reaction speed of a sample and the reagent in the filter bag, and enabling the sample and the reagent to react after the reaction is finished;

step 6: the control system controls the liquid discharge system to be started to discharge the reagent in the reaction kettle;

and 7: the liquid adding system extracts a purified water reagent from a container filled with the purified water reagent, the extracted reagent flows through the constant-temperature reagent instant heating device to be in a high-temperature state and then enters the reaction kettle, the driving device drives the reaction kettle or the filter bag support to rotate, the reagent is in a flowing state, the cleaning effect is improved, and after cleaning is finished;

and 8: the control system controls the liquid discharge system to be started to discharge the reagent in the reaction kettle; and (5) closing the control system when the whole experiment is finished, and taking out and drying the filter bag.

In a fifth aspect, the method for measuring acid washing lignin by using the filter bag type crude fiber measuring instrument based on the paradigm method comprises the following steps:

and step 3: putting the filter bag filled with the sample into a filter bag support in an instrument reaction kettle;

and 4, step 4: starting a control system, extracting an acidic washing reagent from a reagent container containing the acidic washing reagent by a liquid adding system, enabling the extracted reagent to flow through a constant-temperature reagent instant heating device and then to be in a high-temperature state, then enabling the reagent to enter a reaction kettle, driving the reaction kettle or a filter bag support to rotate by a driving device, enabling the reagent to be in a flowing state, increasing the chemical reaction speed of a sample and the reagent in the filter bag, and enabling the sample and the reagent to react after the reaction is finished;

and 5: the control system controls the liquid discharge system to be started to discharge the reagent in the reaction kettle;

step 6: the liquid adding system extracts a purified water reagent from a container filled with the purified water reagent, the extracted reagent flows through the constant-temperature reagent instant heating device to be in a high-temperature state and then enters the reaction kettle, the driving device drives the reaction kettle or the filter bag support to rotate, the reagent is in a flowing state, the cleaning effect is improved, and after cleaning is finished;

and 7: the control system controls the liquid discharge system to be started to discharge the reagent in the reaction kettle; and (5) closing the control system when the whole experiment is finished, and taking out and drying the filter bag.

In a sixth aspect, the present invention also provides an application of the filter bag type crude fiber analyzer or the measuring method in the measurement of crude fiber of food, feed, plant or tea.

The beneficial effects of the above-mentioned embodiment of the present invention are as follows:

1. on the whole, the test speed of the method is high, one-time measurement can be completed only about 60 minutes generally, and the traditional method needs 3-6 hours; mainly lie in this application increased constant temperature instant heating device in the liquid feeding system, the inside cavity for supplying reagent flow of constant temperature instant heating device, and the cavity solvent is less, still be equipped with high-power heating pipe, because the cavity is little, the reagent volume that flows through in the cavity will be less than the reagent volume of conventional heating mode far away, so the power of heating pipe need not do very big just can realize instantaneous heating, normal atmospheric temperature reagent flows through the device and just can be in the twinkling of an eye the reagent heating that will flow through the device to the state of boiling a little, the heating directly gets into in the reaction vessel of crude fiber apparatus behind the reagent outflow the device of the state of boiling a little. The heating mode realizes the function of adding the reagent and heating at the same time, saves more than half of time than the mode of adding the reagent and heating, and greatly improves the speed of the experiment compared with the prior device.

2. The device has large sample measurement quantity, and the device can simultaneously measure 24 samples/batch at least at one time and can measure 60 samples/batch at most; the original device is limited in that the size is generally increased to 6 at a time, and the size of the instrument is greatly reduced.

3. The filter bag is used, the filter bag is only required to be taken out and dried after the chemical reaction is finished, the sample is known to be sealed in the filter bag, so that the sample loss does not exist in the transfer process, meanwhile, compared with the original crude fiber instrument, the system can accurately control the reaction temperature and the fluidity of the reagent, and multiple factors are superposed, so that the accuracy of sample measurement is greatly improved, and the parallel error is really realized to be less than 1%; the existing feed industry already puts forward pricing by the content of crude fiber, the existing measuring method is low in measuring accuracy, the measured content deviation of the crude fiber is caused, great loss is caused to enterprises, and the loss of the enterprises can be reduced by adopting the device along with the fact that the crude fiber is gradually used as one of the pricing factors of the feed.

4. In the application, the surface of the filter bag is provided with a large number of through holes with certain apertures, and the apertures are uniform, so that the filter bag can play a role in filtering and can completely replace a glass sand core; and the size of the through hole is determined through a large number of tests according to the size of the sample, so that the filter bag does not have the problem of being blocked by the sample.

5. The device can support not only the traditional acid-base digestion filtration method, but also a paradigm method group, such as NDF/ADF, the problem that the traditional acid-base digestion filtration method measurement method is lower in principle has been greatly carried out in enterprises in many industries, upstream and downstream enterprises are more and more approved to the paradigm method, and the national standards committee and the like have started to promote the standardization work of the paradigm method, so the device is also greatly innovated compared with the original crude fiber measurement device principle by being compatible with the paradigm method and the acid-base digestion filtration method.

6. The application has also added a weighing system which has the following effects:

firstly, judging the liquid adding amount of the instrument. The liquid adding amount in the reaction kettle can be detected, namely when the liquid adding system adds a reagent into the reaction kettle, the weighing system can detect the amount of the liquid adding amount in real time in a weight detection mode; the reagent added by a normal instrument is specified by the liquid adding amount (less liquid adding amount causes inaccurate experiment, more liquid adding amount causes reagent waste).

And secondly, judging whether the reaction kettle leaks. In the experimentation, theoretically say, because reation kettle itself need carry out the cooperation with mixing system, liquid feeding system, flowing back system, have the connection of a lot of pipelines etc. and be possible to have the leakage problem of unexpected condition such as pipeline damage, so weighing system can judge whether there is the leakage condition through real-time detection weight in the experimentation, because in case the leakage weight will detect, the instrument can produce audible and visual alarm and remind operating personnel.

And thirdly, judging whether the experimenter has operation errors. The reation kettle is covered, and laboratory operating personnel need cover the reation kettle lid (put into the filter bag and can cover after the support), and some laboratory personnel probably neglect to have forgotten the lid, and the reation kettle lid has certain weight, and weighing system can judge whether the laboratory personnel is correct to cover the reation kettle lid through weight.

And fourthly, judging whether the reagent in the reaction kettle is discharged completely. The instrument has the flow of discharging the reagent in the reation kettle in the course of working, and the instrument is that whether the reagent of reation kettle inside discharges totally is judged through weighing system check weighing.

Drawings

The accompanying drawings, which are incorporated in and constitute a part of this specification, are included to provide a further understanding of the invention, and are incorporated in and constitute a part of this specification, illustrate exemplary embodiments of the invention and together with the description serve to explain the invention and not to limit the invention.

FIG. 1 is a schematic diagram of the present invention;

FIG. 2 is a schematic structural diagram of one embodiment of the present invention;

FIG. 3 is a schematic structural diagram of one embodiment of the present invention;

FIG. 4 is a schematic structural diagram of a rapid reagent heating device disclosed in the present invention;

FIG. 5 is a schematic structural view of a filter bag holder disclosed in the present invention;

FIG. 6 is a schematic structural view of a sealing cover of a filter bag holder disclosed in the present invention;

in the figure: the spacing or dimensions between each other are exaggerated to show the location of the various parts, and the illustration is for illustrative purposes only.

The device comprises a liquid inlet valve 1, a liquid adding pump 2, a reagent rapid heating device 3, a filter bag support 4, a reaction vessel heating device 5, a motor 6, a coupler 7, a transmission shaft 8, a reaction vessel 9, a liquid discharge valve 10, a support 11, a weighing device 12 and a connecting frame 13;

3-1 liquid inlet, 3-2 temperature sensor, 3-3 device main structure, 3-4 heating pipe, 3-5 liquid outlet, 3-6 reagent flow cavity and 3-7 reagent flow velocity sensor;

4-1 partition wall, 4-2 side wall, 4-3 through hole, 4-4 bottom, 4-5 through hole, 4-6 central part and 4-7 sealing cover.

Detailed Description

It is to be understood that the following detailed description is exemplary and is intended to provide further explanation of the invention as claimed. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs.

It is noted that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of exemplary embodiments according to the invention. As used herein, the singular forms "a", "an", and/or "the" are intended to include the plural forms as well, unless the invention expressly state otherwise, and it should be understood that when the terms "comprises" and/or "comprising" are used in this specification, they specify the presence of stated features, steps, operations, devices, components, and/or combinations thereof;

for convenience of description, the words "up", "down", "left" and "right" in the present invention, if any, merely indicate correspondence with the directions of up, down, left and right of the drawings themselves, and do not limit the structure, but merely facilitate the description of the invention and simplify the description, rather than indicate or imply that the device or element referred to must have a particular orientation, be constructed and operated in a particular orientation, and therefore should not be construed as limiting the invention.

As introduced by the background art, the present invention provides a coarse fiber measuring apparatus and method of filter bag type, in order to solve the above technical problems, as shown in fig. 1, the coarse fiber measuring apparatus of filter bag type includes a reagent container, a liquid adding system, a constant temperature instant heating device, a reaction container heating device, a filter bag support, a filter bag, a driving device, a liquid discharging system, a waste liquid container, a weighing system and a control system; the reaction vessel is provided with a reaction vessel heating device for heating the reaction vessel; the bottom of the reaction kettle is provided with a weighing device, a filter bag support is arranged in the reaction container, and a plurality of filter bags are fixed on the filter bag support; the driving device drives the filter bag bracket or the reaction container to move; the reagent container is connected with a liquid adding system, the liquid adding system is connected with a reagent constant-temperature instant heating device, and the reagent constant-temperature instant heating device is connected with a reagent heating port of the reaction container; one end of the liquid discharge system is connected with a liquid discharge port of the reaction container, and the other end of the liquid discharge system is connected with a waste liquid container.

It should be further noted that there are many ways for the driving device to drive the filter bag holder or the reaction container to move in this embodiment, for example, the way shown in fig. 2 is that the driving device is connected to the filter bag holder to drive the filter bag holder 4 to rotate, so as to drive the reagent to flow, so that the reagent can fully react with the sample in the filter bag; the method can also be the mode as shown in figure 3, and the whole reaction container is driven to rotate by the driving device, so as to drive the reagent to flow, and the reagent can fully react with the sample in the filter bag; it is understood that the present invention is not limited to the above-described embodiments, and any other motion may be used as long as the reaction vessel is driven by the driving device to oscillate or vibrate, and the motion can sufficiently react the reagent with the sample in the filter bag.

Further, the reaction container may be provided with a heating means at the bottom thereof for heating the reagent in the reaction container, and the heating means may be a heating block made of aluminum, an infrared radiation tube, or the like, and is not limited to a specific heating means as long as the reagent in the reaction container can be heated.

Furthermore, the top of the reaction container is matched with a sealing cover of the reaction container, the sealing cover of the reaction container is similar to a pot cover, and the sealing cover is mainly used for covering the reaction container to form a closed space inside the reaction container, so that steam generated in the heating process of the reagent in the experiment process is prevented from leaking into the air, and the reagent is prevented from being sputtered out of the reaction container in the stirring process. The filter bag support is placed in the reaction container, and the filter bag filled with the sample in the support and the reagent generate various chemical reactions in the reaction container; it should be further noted that the reaction vessel itself in this embodiment is required to satisfy the requirements of acid resistance, alkali resistance and corrosion resistance.

Furthermore, a temperature sensor is also arranged in the reaction container, and the temperature sensor is arranged in the reaction container and used for detecting the temperature of a reagent in the reaction container in real time; the temperature sensor is not limited to its type, and may be a platinum resistor, a K-type thermocouple, or the like.

Further, the reaction vessel waste liquid discharge system comprises a pipeline and a liquid discharge valve; the reaction vessel is connected to the liquid inlet of the liquid discharge valve through a pipeline, the liquid outlet of the liquid discharge valve is connected with a pipeline, and the pipeline is directly communicated to the outside of the machine shell and is mainly used for discharging waste liquid after an experiment is finished inside the reaction vessel.

Further, the liquid adding system comprises a reagent liquid adding pump 2, a pipeline and a liquid inlet valve 1; one end of the pipeline is connected with a reagent container, the other end of the pipeline is connected with a reagent constant-temperature instant heating device 3, and a reagent charging pump 2 and a liquid inlet valve 1 are installed on the pipeline.

The reagent container includes a plurality of containers, and the pipeline includes a plurality of containers; one pipeline is connected with one reagent container, and each pipeline is provided with one reagent charging pump and one liquid inlet valve; a solvent for reacting with a product to be tested is placed in the test container, the reagent charging pump and the liquid inlet valve can be opened as required, and if only one reagent needs to be added, the other reagent charging pumps and the liquid inlet valve can be closed; alternatively, when several reagents are required to be added simultaneously, a plurality of reagents may be added simultaneously.

As a further technical scheme, as shown in fig. 4, the reagent constant-temperature instant heating device 3 comprises a liquid inlet 3-1, a main body structure 3-3, a heating device 3-4, a temperature detection sensor 3-2, and a liquid outlet 3-5; the reagent constant-temperature instant heating device is matched with the liquid adding system to work; one end (corresponding to the left end of the attached drawing) of the main body structure is a liquid inlet 3-1, the other end (corresponding to the right end of the attached drawing) of the main body structure is a liquid outlet 3-5, a reagent flowing cavity 3-6 is arranged inside the main body structure, and the reagent flowing cavity 3-6 is communicated with the liquid inlet 3-1 and the liquid outlet 3-5; a temperature sensor 3-2 is inserted in the side wall of the main body structure, and a measuring head of the temperature sensor is positioned in the reagent flowing cavity; it should be further noted that the temperature sensor in this embodiment is disposed near the liquid inlet, and is inserted along a direction perpendicular to the axial direction of the main body structure.

Furthermore, a heating pipe 3-4 is inserted into the side wall of the main body structure, the heating pipe 3-4 is used for heating the reagent in the reagent flow cavity, the heating device is horizontally inserted into the main body structure, and an electric wire of the heating device is connected from the liquid outlet side.

Furthermore, a reagent flow velocity sensor is also inserted in the reagent constant-temperature instant heating device 3, and the reagent flow velocity sensor can detect the flow velocity of the reagent in real time, thereby effectively preventing the alpha-high temperature amylase from losing efficacy due to high temperature. The alpha-high temperature amylase is an additive which must be used for detecting crude fibers and has the function of decomposing starch in a sample; the reagent has the defects that the temperature environment capable of keeping activity is within 100 ℃ (including 100 ℃), when the additive flows in the rapid heating device, although the boiling temperature of the liquid reagent is not more than 100 ℃ (consistent with the boiling temperature of water), the additive can inevitably touch a main body structure with higher temperature when flowing in the cavity of the rapid heating device, so that the flow rate sensor can detect the mobility of the reagent in real time in order to ensure the activity of the additive, the reagent is ensured to have a certain flow rate, and the problem that the additive is ineffective due to the fact that the flow rate is too slow and the additive contacts with high temperature in the cavity for a long time is avoided.

The cavity that constant temperature instant heating device 3 inside supplies reagent to flow, and the cavity solvent is less, still be equipped with high-power heating device 3-4, because the cavity is little, the reagent amount that flows through in the cavity will be less than the reagent amount of conventional heating mode far away, so the power of heating pipe need not do very big just can realize in good time heating, normal atmospheric temperature reagent flows through the device and just can heat the reagent that flows through the device to the microboiling state in the twinkling of an eye, the reagent that heats to the microboiling state directly gets into in the digestion container of coarse fibre apparatus after flowing out the device. The heating mode realizes the function of adding the reagent and heating at the same time, saves more than half of time than the mode of adding the reagent and heating, and greatly improves the speed of the experiment.

Because reagent flows through this quick heating device and just boils the state a little after getting into the digestion container, so reagent adds and just can begin to disappear and boil the timing, and the digestion time timing is more accurate, improves experiment repeatability precision, has overcome the big problem of experiment result error between the different batches that the timing is inaccurate to disappear.

Because the reagent flows through the quick heating device and enters the digestion container to be in a slightly-boiling state, the process of heating the reagent in the digestion container again does not exist, only a low-power heating device is needed to maintain the slightly-boiling state of the reagent, a slow temperature rise process generated by heating a large amount of reagents is omitted, the reagent heating time is greatly saved, and the test progress is accelerated.

The heating mode that the device adopted is instant heating type, need not heat and keep warm reagent for a long time, can not cause the reagent shelf life to shorten.

The heating mode that the device adopted is instant heating type, and this kind of heating mode is applicable to all reagents, even those can only be in the reagent that can only preserve for a long time under the low temperature condition also are applicable, can not cause reagent scheduling problem such as rotten.

The reagent constant-temperature instant heating device is small in size and small in occupied space, can be integrated into the interior of a case of a filter bag type crude fiber determinator, and the external preheating water container occupies a very large space and is inconvenient to use.

The built-in high accuracy temperature sensor of reagent constant temperature instant heating device can real-time detection reagent's heating temperature, prevents that heating temperature is too high to lead to reagent to become the bumping, influences the experimental effect.

As a further technical solution, as shown in fig. 5 and 6, the filter bag holder 4 includes a sealing cover 4-7, a bottom 4-4, a side wall 4-2, a partition wall 4-1 and a central portion 4-6, the side wall 4-2 is arranged around the bottom 4-4, the central portion 4-6 is located inside the side wall and at the central position of the bottom 4-4, the partition wall 4-1 divides an annular space formed by the central portion and the outer side wall into a plurality of small spaces, each of the small spaces can be used for placing a plurality of filter bags therein, the side wall 4-2 is matched with the sealing cover 4-7, and the whole filter bag holder edge forms a sealed cage structure after the sealing cover 4-7 is covered; the bottom and the side wall are provided with a plurality of through holes, a large number of through holes on the bracket can allow liquid reagents to freely enter and exit, but the filter bag with larger volume is sealed in the bracket.

The filter bag is convenient to place and take out, operation convenience is greatly improved, and efficiency is improved. The support adopts the cage structure, puts into the wall space of support with the filter bag, covers sealed lid and can seal the filter bag in the support the inside, opens sealed lid and can take out the filter bag. The filter bags are not rigidly connected with the filter bag supports, some types of supports on the market are rigidly connected with the filter bag supports, and each filter bag is independently fixed, for example, the filter bags are fixed by screws, namely holes need to be formed in each filter bag, and then the filter bags are fixed on the supports by screws penetrating through the holes in the filter bags. The filter bag placement in this application is not required. The support has no requirement on the placement mode of the filter bag, namely the support can be placed in a positive or reverse mode, and the shape of the filter bag is also not required. The filter bag placing spaces on some supports on the market are designed according to the shapes and the sizes of filter bags, only the filter bags with specific shapes and sizes can be prevented, the placing directions of the filter bags are fixed, the supports cannot adapt to the filter bags with various styles, and the operation convenience is low.

The chemical reaction speed of the sample and the reagent is accelerated. Unique partition formula structure, partition wall above the support main part have the boosting effect to the filter bag, and at support pivoted in-process promptly, the partition wall can push away the filter bag of every partition space the inside and rotate, can accelerate the chemical reaction speed of the sample of filter bag the inside and reagent, and then shortens the experimental time and improves experimental efficiency.

In the experimentation, have a large amount of impurity in the filter bag and see through the filter bag and enter into in the reagent and then adhere to on the filter bag support, a large amount of through-holes still are convenient for wash except can guaranteeing reagent freely pass in and out the support above this support, because the existence of a large amount of through-holes, directly wash the impurity that can adhere above the support with the clear water and wash, even the inside impurity of support also can be washed through a large amount of through-holes.

Furthermore, the filter bag support 4 is connected with a transmission shaft 8, the transmission shaft 8 is connected with a motor 6 through a coupler 7, the motor 6 is positioned in the reaction container, and a reagent is arranged in the reaction container when crude fibers are measured in the reaction container, so that the motor is a waterproof motor or a motor for liquid.

Based on the filter bag type crude fiber measuring instrument disclosed in the above embodiment, the method for measuring crude fibers by using the filter bag type crude fiber measuring instrument based on the acid-base digestion filtration method in the embodiment includes the following steps:

The following is a detailed description of the method based on acid-base digestion filtration, taking the determination of the content of crude fiber in the feed as an example:

1. sample pretreatment

And (3) taking a proper amount of air-dried sample (or drying the sample at 45 ℃ by using an oven, and strictly drying the sample at high temperature) and crushing the sample by using a crusher (the crushing fineness is 16 meshes).

2. Pretreatment of equipment

Firstly, numbering filter bags by using an acid and alkali resistant pen, placing the filter bags into a blast drying oven after numbering, drying for 1H at 103 ℃, and then placing the filter bags into a drying dish for later use.

Secondly, numbering the crucibles, cleaning the crucibles, putting the crucibles into an ashing furnace, drying the crucibles for 1H at 500 ℃, and then putting the crucibles into a drying vessel for later use.

3. Weighing a sample

Firstly, taking the pretreated filter bag, weighing, and recording the weight of the filter bag (M1).

② a small amount of the pretreated sample (0.5g-1.2g) is put into a filter bag, weighed to the accuracy of 0.0001g, and the total weight of the filter bag and the sample is recorded (M2).

Taking another pretreated filter bag, weighing, and recording the weight of the filter bag (M3).(Note, this filter bag is used To make blank contrast)

Inserting a power supply of the sealing machine, and adjusting the gear of the sealing machine to 4 gears; putting the filter bag with the weighed sample into a sealing machine, pressing a connecting rod of the sealing machine until the connecting rod shows a negative sign, and continuing to wait for 2S, wherein the sealing position is 5mm away from the opening of the filter bag.

Fourthly, a seam is cut by scissors in the middle between the sealing position of the filter bag and the mouth of the filter bag.

4. Soaking in acetone (or 30-60 deg.C petroleum ether)

Putting all the filter bags with sealed openings into a beaker, pouring an acetone solution (or petroleum ether at 30-60 ℃) into the beaker, and ensuring that all the filter bags are submerged; the beaker was placed in a fume hood, shaken continuously by hand for 10S, and then left to stand for 10 min to ensure sufficient soaking. After 10 min, pouring out the acetone (or petroleum ether at 30-60 ℃), then placing the filter bag on a ceramic tray, placing the ceramic tray in a fume hood for 10 min, and fully volatilizing the acetone (or petroleum ether at 30-60 ℃) in the filter bag and the sample.

5. Instrument preparation

And preparing reagents required by the experiment, respectively loading the reagents into corresponding reagent containers, and correspondingly placing the reagent tubes on the right side of the machine into the reagent containers.

The reaction vessel lid was opened, the treated sample filter bag was placed on top of the filter bag holder, and then the reaction vessel lid was closed.

Starting the instrument, wherein the liquid adding system can automatically extract the acidic reagent from the reagent container containing the acidic reagent, the acidic reagent is changed from a normal-temperature state to a high-temperature state after flowing through the constant-temperature instant heating device and then enters the reaction container, meanwhile, the driving device in the reaction container enables the reagent to form a flowing state to increase the chemical reaction speed of the sample and the reagent in the filter bag, and after the reaction of the sample and the reagent is finished, the liquid discharging system discharges the reagent in the reaction container;

the liquid adding system can automatically extract a purified water reagent from a reagent container containing purified water again, the purified water reagent is changed from a normal temperature state to a high temperature state after flowing through the constant temperature instant heating device and then enters the reaction container, meanwhile, a driving device in the reaction container enables the reagent to form a flowing state to thoroughly wash away various impurities generated in the last step of acid digestion, and after the washing is finished, the liquid discharging system discharges the reagent in the reaction container;

the liquid adding system extracts the alkaline reagent from the reagent container containing the alkaline reagent again, the extracted alkaline reagent is changed into a high-temperature state from a normal-temperature state after flowing through the constant-temperature instant heating device and then enters the reaction container, meanwhile, the driving device in the reaction container enables the reagent to form a flowing state to increase the chemical reaction speed of the sample and the reagent in the filter bag, and after the reaction of the sample and the reagent is finished, the liquid discharging system discharges the reagent in the reaction container;

the liquid adding system extracts the purified water reagent from the reagent container containing the purified water reagent again, the extracted purified water reagent is changed from a normal temperature state to a high temperature state after flowing through the constant temperature instant heating device, then enters the reaction container, meanwhile, the reagent flowing device in the reaction container can enable the reagent to form a flowing state to thoroughly wash away various impurities generated in the last step of acid digestion, and after the washing is finished, the liquid discharging system discharges the reagent in the reaction container; and (4) closing the instrument and taking out and drying the filter bag to enter the subsequent step when the whole experiment is finished.

6. Soaking in acetone (or 30-60 deg.C petroleum ether)

The pot cover is opened (if the pot cover is not easy to open, the knob of the red pressure valve can be shifted to an air release gear to balance the pressure inside the pot and outside the pot), the fixed ring is taken down firstly, then the upper cover of the support is taken down, then the filter bags are taken out, and all the filter bags are overlapped together and lightly pressed by hands to drain moisture.

Putting all filter bags with water drained into a beaker, pouring acetone solution (or petroleum ether at 30-60 ℃) into the beaker, and ensuring that all filter bags are submerged; the beaker was placed in a fume hood, shaken continuously by hand for 10S, and then left to stand for 10 min to ensure sufficient soaking. After 10 min, pouring out the acetone (or petroleum ether at 30-60 ℃), then placing the filter bag on a ceramic tray, placing the ceramic tray in a fume hood for 10 min, and fully volatilizing the acetone (or petroleum ether at 30-60 ℃) in the filter bag and the sample.

7. Drying by baking

And (5) putting the filter bag which is completely volatilized into a blast drying oven to be dried for 4H at the temperature of 105 ℃. And taking out the dried mixture and putting the dried mixture into a drying dish, completely cooling the dried mixture, and weighing the mixture for multiple times until the weight is constant. The weight of the bag containing the sample was (M4), the weight of the empty bag was (M5), and the number weights were recorded once according to the bag number.

8. Ashing

Taking out the dried crucible from the drying dish, weighing, recording the weight (M6), and putting the filter bag filled with the sample after drying and weighing into the crucible; a further crucible was taken, the weight was recorded (M7), and the dried and weighed empty filter belt was placed in the crucible.

Putting the crucible with the filter bag into an ashing furnace, ashing for 2H at 500 ℃, then putting the crucible into a drying dish, and weighing for multiple times after completely cooling until the weight is constant. The weight of the crucible containing the filter bag containing the sample was (M8), and the weight of the crucible containing the empty filter tape was (M9).

9. Computing

The embodiment also provides a neutral washing fiber measuring method based on a paradigm method by using the filter bag type crude fiber measuring instrument, which is characterized by comprising the following steps:

The embodiment also provides a method for measuring acid washing fibers by using the filter bag type crude fiber measuring instrument based on a paradigm method, which comprises the following steps:

The embodiment also provides a method for measuring acid washing lignin by using the filter bag type crude fiber measuring instrument based on a paradigm method, which comprises the following steps:

Finally, it is also noted that relational terms such as first and second, and the like, may be used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions.

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

1. A filter bag type crude fiber tester is characterized by comprising a reagent container, a liquid adding system, a constant-temperature instant heating device, a reaction container, a filter bag bracket, a filter bag, a driving device, a liquid discharging system, a weighing system, a waste liquid container and a control system;

the control system controls the liquid adding system, the reagent constant-temperature instant heating device, the driving device and the liquid discharging system.

2. The filter bag type crude fiber measuring apparatus according to claim 1, wherein the reagent container comprises a plurality of containers and the pipeline comprises a plurality of containers; one pipeline is connected with one reagent container, and each pipeline is provided with one reagent charging pump and one liquid inlet valve.

3. The coarse fiber analyzer in the form of filter bag of claim 1, wherein the liquid feeding system comprises a reagent feeding pump, a pipeline, a liquid feeding valve; one end of the pipeline is connected with the reagent container, the other end of the pipeline is connected with the reagent constant-temperature instant heating device, and a reagent charging pump and a liquid inlet valve are installed on the pipeline.

4. The coarse fiber analyzer of the filter bag type as claimed in claim 1, wherein the constant temperature instant heating device comprises a liquid inlet, a main body structure, a heating device, a temperature detection sensor and a liquid outlet; one end of the main structure is a liquid inlet, the other end of the main structure is a liquid outlet, a reagent flowing cavity is arranged in the main structure, and the reagent flowing cavity is communicated with the liquid inlet and the liquid outlet; a temperature sensor is inserted into the side wall of the main body structure, and a measuring head of the temperature sensor is positioned in the reagent flowing cavity; and a heating device is also inserted into the side wall of the main body structure.

5. The filter bag type crude fiber measuring apparatus according to claim 1, wherein said filter bag holder comprises a cage structure and a sealing cover, said cage structure is divided into a plurality of small spaces, and a plurality of filter bags can be placed in each of said small spaces.

6. The coarse fiber analyzer of filter bag type as claimed in claim 1, wherein the filter bag is made of a membrane material made of a high polymer material with acid, alkali and corrosion resistance, and the surface of the filter bag is uniformly provided with a plurality of through holes, the diameter of the through holes is satisfied, liquid and small molecules can pass through the through holes, and the large diameter coarse fibers cannot pass through the through holes.

7. The apparatus for measuring crude fiber in the form of filter bag according to claim 1, wherein a temperature sensor is also provided in said reaction vessel.

8. A method for measuring crude fiber by using the filter bag type crude fiber measuring instrument according to any one of claims 1 to 7 based on an acid-base digestion filtration method, comprising the steps of:

9. A method for measuring neutral detergent fiber by using the filter bag-type crude fiber measuring apparatus according to any one of claims 1 to 7, based on a normal form method, comprising the steps of:

and 5: pouring 50ml of alpha-high temperature amylase into the reaction kettle manually; or the alpha-high temperature amylase is added into a container containing the reagent in advance, and the reagent is pumped into the reaction kettle together when the reagent is pumped by the machine;

10. A method for measuring acid washing fiber by using the filter bag type crude fiber measuring apparatus according to any one of claims 1 to 7 based on a paradigm method, comprising the steps of:

11. A method for measuring acid washing lignin by using the filter bag type crude fiber measuring instrument according to any one of claims 1 to 7 based on a paradigm method, comprising the steps of:

12. Use of the filter bag type crude fiber measuring instrument according to any one of claims 1 to 7 in a crude fiber measurement of food, feed, plant or tea.

13. Use of the method for measuring crude fiber in a filter bag according to any one of claims 8 to 9 in a crude fiber measurement for food, feed, plant or tea.