Gas absorbs volume detector and detection method
Technical field
The present invention relates to a kind of gas to absorb volume detector, and the detection method using the detector, suitable for accurate
Detect the gaseous absorptivity energy of various gas absorbents, such as the deoxygenation performance of food deoxidant.
Background technology
Deoxidier is also known as oxygen absorbent, oxygen scavenger, deoxidant, belongs to gas absorbent, can at normal temperatures with packing container
Free oxygen and dissolved oxygen occur oxidation reaction formed oxide, the oxygen absorption in sealing container is fallen, prevents food because of oxygen
Change and moldy metamorphism, so as to extend effective period of food quality;Meanwhile oxygen scavenger can keep the original color of food, prevent insect,
The growth of bacterium, the nutritional ingredient of food is maintained, extend fresh keeping time, play the important function to ensure food safety.Deoxidier
It has been widely used in wet bread flour, wet face, wet-milling silk, the wet point heart, tealeaves, meat products, roasted seeds and nuts, dried food and nuts, half-dried fish product etc.
Numerous food.At present, applicable cases of the deoxidier in different food products processing are:Cake sweet food be 45%, livestock products, aquatic products and
Processing of farm products food is 30%, and tealeaves, coffee etc. are 15%, and other food such as healthy food, homely dish are 10%,
Promote the use of food, the dispatching food and the pharmaceuticals of long shelf-life and healthy food etc. of short shelf-life of high moisture content
In product.
Total oxygen absorbed of deoxidier is the leading indicator for judging deoxidier product technology performance, at present product standard SB/
T10514-2008《Food deoxidier》It is middle that deoxidier is detected using trace oxygen analyzer method and water at atmospheric pressure oil displacement method
Total oxygen absorbed.
1. microanalyser method:
The equipment that the experimental method uses is mainly insulating box, trace oxygen analyzer, K nylon plastic(s)s bag, inflation pin
The equipment such as cylinder;Its continuous mode is:Sample is placed in K nylon plastic(s) bags, poured a certain amount of (10 times of nominal oxygen absorbed)
Air, keep the pressure of sack and normal pressure close, Nylon Bag be put into 25 DEG C of insulating box, nylon is measured after certain time
The oxygen concentration (oxygen concentration should be not less than 3%) of air in bag, then determine Nylon Bag volume with drainage.
Problems with is primarily present in the experimental method:
(1) Nylon Bag selects:
Selection on Nylon Bag, it is desirable to it is the sack of 10 times of nominal oxygen absorbed volumes, it is often total in reality testing to inhale
Oxygen amount is 3-10 times of nominal oxygen absorbed, is calculated according to the air of 10 times of oxygen absorbeds, oxygen content only has 2 times, it is necessary to for several times more
Change.
(2) bag pressure is unmanageable
In this method, being filled with air must keep the pressure of sack close with normal pressure, and this regulation is to being filled with air capacity
How many is difficult control because be aerating device, pressure operates by hand completely, relatively difficult so that the accuracy of inspection
It is difficult to control.
(3) oxygen concentration
In this method, oxygen concentration needs >=3% after experiment, but puts into practice and find according to inventor, and the concentration is difficult control, because
When just being added for sample, quickly, the inside only has 2 times of nominal oxygen absorbed to oxygen absorbed, and often 7-8 hour is dense with regard to that can be drawn onto oxygen
Degree basically reaches less than 1%, and uncontrollable oxygen concentration remains >=3% at all, if by often detecting oxygen concentration
Required to ensure compliance with, then in bag taking during air, can constantly cause air escape with detecting the damage of oxygen concentration air
Lose, largely effect on assay correctness.
(4) Nylon Bag volume calculates
In this method, the calculating of volume uses drainage, and the water of discharge is poured into graduated cylinder, calculates the volume of Nylon Bag,
And so not science, because the weight of water is more much larger than air, make Nylon Bag be difficult to keep original shape, cause volume
It is very big to calculate discrepancy.
2. water at atmospheric pressure oil displacement method
As shown in figure 1, this method using ear washing bulb 1, silicone gum rubber woven hose 2, support 4,500 or 100mL graduated cylinder 5,
Water or oil is housed, deoxidier sample 3 is placed under the support of support 4 in graduated cylinder 5 during detection in beaker 6, beaker 6 and graduated cylinder 5.
Application number 200610122574.1, publication number CN1995966A, title《A kind of detection method of oxygen absorption capacity of deoxidizer》China
Application for a patent for invention uses substantially similar detection method.
Problems with is primarily present in this method:
(1) operation, which has some setbacks, causes error:Sample need to expose in atmosphere in 24 hours scavenging periods are inhaled every time, can inhale
Oxygen in receiving portions air, and each general rate of ventilation of sample causes oxygen uptake result and legitimate reading to deposit more than 5 times
In error.
(2) error caused by reading uncertainty:Generally use 500mL, the 1000mL graduated cylinder in checkout procedure, minimum are carved
Degree is respectively 5mL, 10mL, and estimation algorithm reading is used on two minimum scales in measurement process, and sample rate of ventilation is more, most
Cause error in reading very big eventually.
Product standard SB/T10514-2008《Food deoxidier》It also specify index:Nominal oxygen time.It is nominal to inhale
The oxygen time is to determine that food selects the foundation of deoxidier specification according to preservativity, and easy short time endomorphosed food needs to select
Nominal deaeration time is short and the bulky deoxidier of nominal oxygen absorbed ratio sample packaging, otherwise only grows one from nominal oxygen time
A little and nominal oxygen absorbed is less than or equal to the deoxidier of packaging volume.The index is to determine the important of product specification and deoxidizing capacity
Foundation, detected in product standard using microanalyser method, and the method is equally existed existing for foregoing microanalyser
Problem (1), (2), (4).
For the measure of the gaseous absorptivity energy of other gas absorbents, more or less there is also same as described above or similar
The problem of.
Need badly can accurately detection gas absorbent gaseous absorptivity can technological means.
The content of the invention
The technical problem to be solved in the present invention:The problem of existing for prior art, propose that a kind of gas absorbs volume inspection
Survey instrument, the gaseous absorptivity energy of the accurate detection gas absorbent of energy;The detection method using the detector is also proposed simultaneously.
The present invention solve above-mentioned technical problem technical scheme be:
A kind of gas absorbs volume detector, including frame and control unit, it is characterized in that, it is solid that the frame is provided with auxiliary
Determine device, the measurement container of vertical placement and both ends open, the top of the measurement container are mounted with the auxiliary fixing device
End is fixedly connected with closure, and the frame is provided with the seal groove to match with measurement container bottom, and one is provided with the seal groove
Group is accommodating the sample box of gas absorbent sample;
The sample box is made up of base and lid, and the base is connected with sealing trench bottom, with hanging on the outside of the lid
Line is connected, and the gas absorbent sample is hung on the inside of lid;
The closure has the wire fixing device being connected with suspension wire, the bleeding point connected through extraction valve with air extractor, warp
The air inlet that intake valve connects with gas source bottle with pressure;The measurement container bottom end side wall has what is connected through liquid feed valve with liquid tank
Inlet;The gas absorbed in the gas source bottle with pressure equipped with supplied gas absorbent sample;
Described control unit is included with the PLC of timer, the liquid level sensor in seal groove, display screen and defeated
Enter equipment;The signal output part of the liquid level sensor and PLC signal input part connect, the display output end of the PLC with
Display screen is connected, and the input of the PLC is connected with input equipment;The extraction valve, intake valve, the controlled end difference of liquid feed valve
It is connected with PLC corresponding controling end.
Further perfect technical scheme is as follows by the present invention:
Preferably, there is the sample box base to be tightly connected with lid, make what gas absorbent sample was isolated from the outside
Air-tight state, and pull lower casing in suspension wire and drive gas absorbent sample and the open mode of base disengaging.
Preferably, the measurement container has:It is close upwardly and out that container is measured under auxiliary fixing device drive
Sealing groove, the first state for loading or unloading gas absorbent sample, measurement container bottom are tightly connected and are evacuated with seal groove
Valve, intake valve, liquid feed valve Close All make sample box be contained in measurement container and make to form confined space in measurement container
Second state, extraction valve and liquid feed valve, unlatching air extractor are opened on the basis of the second state makes liquid enter survey from liquid tank
Amount container, still there is liquid continuous with liquid holding in measurement container in liquid tank and in now when measuring hydraulically full in container
The third state of extraction valve and air extractor is closed, intake valve is opened on the basis of the third state makes gas in gas source bottle enter survey
Liquid in measurement container is simultaneously pushed back liquid tank, closes air inlet when liquid level drops to predeterminated position in measurement container by amount container
4th state of valve, the sample box lid for hanging gas absorbent sample is lifted by wire fixing device on the basis of the 4th state
To preset height and start the gaseous absorptivity energy of detection gas absorbent sample until the 5th state of detection end;It is described
Predeterminated position is less than the top edge of sample box base.
Preferably, described control unit has:
The first state of extraction valve, intake valve, liquid feed valve is opened or closed respectively by the instruction of input equipment, is set by input
Standby instruction monitors the second state that liquid volume changes in measurement container by liquid level sensor, leads to by the instruction of input equipment
Cross third state during timer.
Preferably, the measurement container head and bottom have notch, the measurement container head notch and sealing respectively
Sealing ring is respectively provided between lid, between measurement container bottom end slot mouth and seal groove;The wire fixing device be with sealing gasket and
It is compacted the silking tubing string of nut;The liquid feed valve is in the connecting tube of connection measurement container inlet and liquid tank, the company
End of the adapter in liquid tank is less than liquid level in liquid tank.
It is highly preferred that the material of the closure is stainless steel material;The material of the seal groove is plastic material.
Preferably, the auxiliary fixing device includes the vertical support bar being fixed in frame, the vertical support bar week
To circle folder is arranged with, the circle fixture has the chuck of clamping measurement container.
Preferably, the air extractor include the exhaust tube that is connected with bleeding point, the safety bottle that top connects with exhaust tube,
And the aspiration pump connected by the road with safety bottle top.
The present invention also provides:
The detection method of volume detector is absorbed using These gases, it is characterized in that, comprise the following steps:
The first step, by auxiliary fixing device by measure container be promoted to predetermined altitude, the lid of sample box is opened, in gas
Punched on the sample sack of body absorbent sample, and gas absorbent sample is suspended on lid, afterwards by gas absorbent sample
Product are erect and are placed in sample box, and covering lid makes sample box closed;
Second step, fallen container is measured by auxiliary fixing device, and measurement container bottom and seal groove sealing is connected
Connect;Extraction valve, intake valve, liquid feed valve Close All are kept simultaneously, sample box is contained in measurement container and makes measurement container
Interior formation confined space;
3rd step, the liquid for injecting into liquid tank predetermined, open extraction valve and liquid feed valve by control unit, open
Opening air extractor makes liquid enter from liquid tank in measurement container;When measuring hydraulically full in container, still there is liquid in liquid tank
Body keeps continuous with liquid in measurement container, while closes extraction valve and air extractor by control unit;
4th step, intake valve is opened by control unit gas is entered measurement container, and container will be measured
Interior liquid pushes back liquid tank, and intake valve is closed by control unit when liquid level drops to predeterminated position in measurement container;It is described
Predeterminated position is less than the top edge of sample box base;
5th step, by wire fixing device by hang gas absorbent sample sample box lid be promoted to preset height after,
Control unit monitors liquid volume in measurement container by liquid level sensor and changed to calculate the total air-breathing of gas absorbent sample
Amount, while timing, and make total air-breathing amount-time graph;When monitoring is reached home, control unit stops monitoring, and opens
Intake valve, the residual liquid measured in container is discharged into liquid tank;Measurement airtight lid for container is opened afterwards, is taken out gas and is absorbed
Agent sample;Detection terminates.
Further perfect technical scheme is the present invention:
Preferably, in the 5th step, in monitoring process, when the total air-breathing amount of gas absorbent sample reaches its nominal air-breathing
During amount, timing time now as the nominal inspiratory duration of the sample and is shown in display screen by control unit;The sample exists
After air-breathing 24 hours, when in preset time, measurement container in liquid volume change be no more than 10ml when, then monitor up to end
Point, control unit is using timing time now as the total air-breathing time of the sample and using total air-breathing amount now as the sample
The total air-breathing amount of product, and it is shown in display screen.
Compared with prior art, beneficial effects of the present invention are as follows:
(1) can thoroughly overcome existing detection method because operation etc. factor cause measurement error very big the problem of, volume can essence
Really to 1 milliliter, timing can be accurate to 1 second, effectively ensure that the accuracy of detection data.
(2) in detection process, Automated condtrol can be achieved, without manually operated, avoid bringing interference from human factor inspection into
Survey result.
(3) blank that the domestic field lacks full-automatic detection device is filled up.
(4) it is applied widely, the detection of deoxidier deoxygenation performance is can be used not only for, also can detect other gas absorbents
Gaseous absorptivity can (such as CO, CO2、NO、NO2、SO2Deng), the multiple fields such as chemical industry, medicine, biological products can be widely used in.
Brief description of the drawings
Fig. 1 is the installation drawing that background technology refers to water at atmospheric pressure oil displacement method.
Fig. 2 is the structural representation of the embodiment of the present invention.
Fig. 3 is the electrical diagram of the embodiment of the present invention.
Embodiment
Illustrate the specific steps of the present invention by the following examples, but be not limited by the example.
Used term in the present invention, unless otherwise indicated, typically there are those of ordinary skill in the art generally to manage
The implication of solution.
The present invention is described in further detail with reference to specific embodiment and with reference to data.It should be understood that the embodiment is
In order to demonstrate the invention, rather than the scope that limit the invention in any way.
In the examples below, the various processes and method not being described in detail are conventional methods as known in the art.Under
The present invention is further described in conjunction with specific embodiments in face.
Embodiment
Illustrated by taking food deoxidant detector as an example.
As shown in Figure 2 and Figure 3, it is food deoxidant detector that the present embodiment gas, which absorbs volume detector, including frame 11
With control unit 12, frame 11 is provided with auxiliary fixing device, and vertical place and both ends open is mounted with auxiliary fixing device
Container 13 is measured, the top of measurement container 13 is fixedly connected with closure 14, and frame 11 is provided with to match with measurement container 13 bottom
Seal groove 15, one group is provided with seal groove 15 to accommodate the sample box 17 of food deoxidant sample 16;Sample box 17 is the bottom of by
Seat and lid are formed, and base is connected with the bottom of seal groove 15, are connected on the outside of lid with suspension wire, food deoxidant sample 16 is hung on
On the inside of lid;Closure 14 has the wire fixing device being connected with suspension wire, the bleeding point connected through extraction valve 18 with air extractor, warp
The air inlet that intake valve 19 connects with gas source bottle 20 with pressure;Measuring the bottom side wall of container 13 has through liquid feed valve 21 and liquid tank 22
The inlet of connection.The oxygen absorbed for food deoxidant sample 16 is housed in gas source bottle 20 with pressure;
Control unit 12 is included with the PLC of timer, the liquid level sensor in seal groove 15, display screen and defeated
Enter equipment;The signal output part of liquid level sensor and PLC signal input part connect, and PLC display output end and display screen connect
Connect, PLC input is connected with input equipment;Extraction valve 18, intake valve 19, the controlled end phase with PLC respectively of liquid feed valve 21
Control terminal is answered to connect.
Sample box 17 has:The sealed shape that base is tightly connected with lid, makes food deoxidant sample 16 be isolated from the outside
State, and pull lower casing in suspension wire and drive food deoxidant sample 16 and the open mode of base disengaging.
Measurement container 13 has:Auxiliary fixing device drive under measure container 13 upwardly and out seal groove 15,
First state for loading or unloading food deoxidant sample 16, the measurement bottom of container 13 are tightly connected and are evacuated with seal groove 15
Valve 18, intake valve 19, the Close All of liquid feed valve 21 make sample box 17 be contained in measurement container 13 and make shape in measurement container 13
Into the second state of confined space, extraction valve 18 and liquid feed valve 21, unlatching air extractor are opened on the basis of the second state makes liquid
Body enters measurement container 13 from liquid tank 22, still has liquid to hold with measurement in liquid tank 22 when measuring hydraulically full in container 13
Liquid keeps, continuously and in the third state for now closing extraction valve 18 and air extractor, beating on the basis of the third state in device 13
Drive into air valve 19 make in gas source bottle 20 gas enter measurement container 13 and will in measurement container 13 liquid push back liquid tank 22, when
The 4th state of intake valve 19 is closed when liquid level drops to predeterminated position in measurement container 13, by solid on the basis of the 4th state
The lid of sample box 17 for hanging food deoxidant sample 16 is promoted to preset height and starts to detect food deoxidant by line apparatus
The deoxygenation performance of sample 16 is until the 5th state that detection terminates;Predeterminated position is less than the top edge of the base of sample box 17.
Control unit 12 has:Extraction valve 18, intake valve 19, liquid feed valve are opened or closed respectively by the instruction of input equipment
21 first state, second of liquid volume change in measurement container 13 is monitored by liquid level sensor by the instruction of input equipment
State, pass through third state during timer by the instruction of input equipment.
In addition, the measurement top of container 13 and bottom have a notch respectively, measure the top notch of container 13 and closure 14 it
Between, measurement the bottom notch of container 13 and seal groove 15 between be respectively provided with sealing ring;Wire fixing device is with sealing gasket and compacting
The silking tubing string of nut;Liquid feed valve 21 is in the connecting tube 23 of the connection measurement inlet of container 13 and liquid tank 22, connecting tube
23 end in liquid tank 22 is less than liquid level in liquid tank 22.The material of closure 14 is stainless steel material;Seal groove 15
Material be plastic material.Auxiliary fixing device includes the vertical support bar 24 being fixed in frame 11, vertical support bar 24 weeks
To circle folder 25 is arranged with, circle folder 25 has the chuck of clamping measurement container 13.Air extractor includes the pumping connected with bleeding point
Safety bottle 27 (such as vial) that pipe 26, top connect with exhaust tube 26 and by the road connected with the top of safety bottle 27
Aspiration pump 28.
The present embodiment uses the detection method of foregoing food deoxidant detector, comprises the following steps:
The first step, predetermined altitude is promoted to by container 13 is measured by auxiliary fixing device, opens the lid of sample box 17,
Punched on the sample sack of food deoxidant sample 16, and food deoxidant sample 16 is suspended on lid, afterwards by food
Deoxidier sample 16 is erect and is placed in sample box 17, and covering lid makes sample box 17 closed;
Second step, fallen container 13 is measured by auxiliary fixing device, and will the measurement bottom of container 13 and seal groove 15
It is tightly connected;Extraction valve 18, intake valve 19, the Close All of liquid feed valve 21 are kept simultaneously, sample box 17 is contained in measurement container
In 13 and make to form confined space in measurement container 13;
3rd step, into liquid tank 22 inject predetermined liquid (such as pure water), opened by control unit 12
Extraction valve 18 and liquid feed valve 21, opening air extractor makes liquid enter from liquid tank 22 in measurement container 13;When measurement container 13
Still there is liquid to keep continuous with liquid in measurement container 13 when interior hydraulically full, in liquid tank 22, while pass through control unit 12
Close extraction valve 18 and air extractor;
4th step, make gas entrance measurement container 13 in gas source bottle 20, and general by the opening intake valve 19 of control unit 12
Liquid pushes back liquid tank 22 in measurement container 13, when liquid level drops to predeterminated position in measurement container 13 by control unit 12
Close intake valve 19;Predeterminated position is less than the top edge of the base of sample box 17;
5th step, by wire fixing device by hang food deoxidant sample 16 the lid of sample box 17 be promoted to preset height
Afterwards, control unit 12 monitors liquid volume in measurement container 13 by liquid level sensor and changed to calculate food deoxidant sample 16
Total oxygen absorbed, while timing, and make total oxygen absorbed-time graph;When monitoring is reached home, control unit 12 stops
Monitoring, and intake valve 19 is opened, the residual liquid measured in container 13 is discharged into liquid tank 22;Measurement container 13 is opened afterwards
Closure 14, take out food deoxidant sample 16;Detection terminates.
In 5th step, in monitoring process, when total oxygen absorbed of food deoxidant sample 16 reaches its nominal oxygen absorbed,
Timing time now as the nominal oxygen time of the sample and is shown in display screen by control unit 12;The sample is being inhaled
After oxygen 24 hours, when in preset time, measurement container 13 in liquid volume change be no more than 10ml when, then monitor up to end
Point, control unit 12 are used as this using timing time now as total oxygen time of the sample and using total oxygen absorbed now
Total oxygen absorbed of sample, and it is shown in display screen.
In addition, in the 5th step, the compacting nut of wire fixing device is turned on, up carries suspension wire, be allowed to open the box of sample box 17
Lid, and after lid and sample are promoted into preset height, pressed to wire fixing device into latex plug, tightening nuts, now, if liquid level is not
In predeterminated position, then supplemental oxygen makes liquid level be attributed to predeterminated position.
Specifically, 2000ml tubulose lucite can be selected in the measurement container 13 of the present embodiment detector,Connecting tube 23 residing for liquid feed valve 21 is straight curved, 5 × 20cm;Four are respectively equipped with each seal groove 15
Sample box 17;Closure 14 is provided with 4 wire fixing devices, 1 vacuum tube with 90 ° of right angles of valve, 1 with valve and pressure gauge
90 ° of oxygen hoses, two pipe diameters are
Auxiliary fixing device can also use following structure:Using quoit,The a length of 10cm circles of handle
Cylinder, the handle other end are welded on the lifting arm being threaded with slide bar in scalariform, the interior slide bar of lifting arm for 2cm × 1cm ×
1.73cm, a diameter of 2cm of threaded rod semicircle shape, screw thread are M27 × 2, and long 50cm, lift-bolt and runner position are in 0.7m
Place, lower end are plastic cement rod, and plastic cement rod is shaft-like, long 1.2m, wide 5cm, the high 5cm of cuboid, built-in metal at plastic cement rod 70cm
Chute, body are the hollow body of litter, and plastic cement rod is fixed in frame 11.
In addition, the particular technique parameter of the present embodiment is:
Voltage is 220V ± 10V;Electric current is 0.2A;Total oxygen absorbed measuring accuracy:±1mL;Total oxygen time measuring accuracy:
±1s;Nominally oxygen time measuring accuracy is:±1s.
The present embodiment fully meets standard requirement in technical requirements, and the equipment can be designed to bilateral test dress in parallel
Put, the public frame 11 of stream oriented device, independent test device and independent control circuit, the requirement of Duplicate Samples detection can be met.
For other gas absorbents detection when, then equipped with accordingly by absorption gas in gas source bottle 20, after detection most
Total air-breathing amount, nominal inspiratory capacity, and total air-breathing time are obtained eventually.