CN109932230A - A kind of nitrate reduction instrument and its application method - Google Patents
A kind of nitrate reduction instrument and its application method Download PDFInfo
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- CN109932230A CN109932230A CN201910251823.4A CN201910251823A CN109932230A CN 109932230 A CN109932230 A CN 109932230A CN 201910251823 A CN201910251823 A CN 201910251823A CN 109932230 A CN109932230 A CN 109932230A
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- Prior art keywords
- pillar
- nitrate reduction
- sample liquid
- cistern
- sample
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- 230000009467 reduction Effects 0.000 title claims abstract description 78
- 229910002651 NO3 Inorganic materials 0.000 title claims abstract description 58
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 title claims abstract description 58
- 238000000034 method Methods 0.000 title claims abstract description 33
- 239000007788 liquid Substances 0.000 claims abstract description 108
- 229910052793 cadmium Inorganic materials 0.000 claims abstract description 25
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 claims abstract description 25
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 30
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 24
- 229910021529 ammonia Inorganic materials 0.000 claims description 15
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 12
- 238000005406 washing Methods 0.000 claims description 7
- 239000002699 waste material Substances 0.000 claims description 7
- 239000011521 glass Substances 0.000 claims description 6
- 238000011017 operating method Methods 0.000 claims description 6
- 238000011084 recovery Methods 0.000 claims description 6
- 238000011069 regeneration method Methods 0.000 claims description 6
- 230000003139 buffering effect Effects 0.000 claims description 5
- 239000003365 glass fiber Substances 0.000 claims description 4
- 238000005554 pickling Methods 0.000 claims description 4
- 238000004140 cleaning Methods 0.000 claims description 3
- 239000003085 diluting agent Substances 0.000 claims description 3
- 238000012544 monitoring process Methods 0.000 claims description 3
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 claims description 3
- 239000000243 solution Substances 0.000 claims 7
- 238000010790 dilution Methods 0.000 claims 1
- 239000012895 dilution Substances 0.000 claims 1
- 239000000203 mixture Substances 0.000 claims 1
- 238000007789 sealing Methods 0.000 claims 1
- 238000007689 inspection Methods 0.000 abstract description 3
- 238000001514 detection method Methods 0.000 description 6
- IOVCWXUNBOPUCH-UHFFFAOYSA-M Nitrite anion Chemical compound [O-]N=O IOVCWXUNBOPUCH-UHFFFAOYSA-M 0.000 description 4
- 238000002798 spectrophotometry method Methods 0.000 description 4
- 238000010586 diagram Methods 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 238000010926 purge Methods 0.000 description 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical class O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 238000003556 assay Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000004587 chromatography analysis Methods 0.000 description 1
- 230000009849 deactivation Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 239000012263 liquid product Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- YBVAXJOZZAJCLA-UHFFFAOYSA-N nitric acid nitrous acid Chemical compound ON=O.O[N+]([O-])=O YBVAXJOZZAJCLA-UHFFFAOYSA-N 0.000 description 1
- 238000005086 pumping Methods 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 238000000870 ultraviolet spectroscopy Methods 0.000 description 1
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- Investigating Or Analysing Materials By Optical Means (AREA)
Abstract
The present invention relates to food inspection equipment technical fields, more particularly to a kind of nitrate reduction instrument and its application method, its structure includes being connected to the vacuum pump module of at least two nitrate reduction modules, cadmium grain is set in pillar in each nitrate reduction module, pillar two-port connects cistern and conduit respectively, conduit is switched equipped with pillar, conduit is plugged into sewer pipe and sample liquid pipe respectively using triple valve, sewer pipe leads to the discard solution receiving pool in hermetically sealed can, sample liquid pipe leads to sample liquid reception tank, hermetically sealed can is connect with vacuum pump module, pressure controller is equipped between hermetically sealed can and vacuum pump module, the side of pillar, which is equipped with, switchs the G1 leve monitor being electrically connected with pillar, the side of sample liquid reception tank is equipped with the G2 leve monitor being electrically connected with pillar switch and triple valve, the volume of the minimum graduation mark of pillar to triple valve is 26~27m The reduction rate of L, the instrument meet national standard, have the advantages that batch sample reduction rate is fast, and its application method is easily operated.
Description
Technical field
The present invention relates to food inspection equipment technical fields, and in particular to a kind of nitrate reduction instrument and its application method.
Background technique
Currently, GB5009.33-2016 " measurement of national food safety standard nitrite in food and nitrate " is nitre
The main stream approach of hydrochlorate detection comprising the first method chromatography of ions, the second method spectrophotometry and third ultraviolet spectrometry light
Degree method, and the second method spectrophotometry is more traditional and public practical operation of being more convenient for, and is most common side in three kinds of detection methods
The principle of the method spectrophotometry is by nitrate reduction into nitrite, then by the content of measurement nitrite to count
The content for obtaining Nitrate Content in Food is calculated, therefore, when using spectrophotometry, needs to be first nitrite by nitrate reduction.
Cadmium reduction column be the most effectual way for being reduced into nitrite nitrate.Since traditional cadmium column is difficult to control
It crosses that column flow rate, the operating time is too long, reduction rate is low, releases full-automatic nitrate reduction instrument in this regard, having on the market.However, now
Full-automatic nitrate reduction instrument still have a following defect: one, full-automatic nitrate reduction instrument sampling liquid product and obtained
Reduction sample liquid volume and national standard in require it is different, and its resulting reduction sample liquid need to taken again after colorimetric cylinder constant volume calmly
Sample liquid carries out chromogenic assay after appearance, and the accuracy of subsequent detection and preciseness is caused to be lacking, and is not particularly suitable for method inspection and uses;
Secondly, full-automatic nitrate reduction instrument only every time restore an extracting solution, time-consuming be about 15min, though more traditional cadmium column speed
It is fast, but batch samples are also lacking.
Summary of the invention
For the prior art there are one of above-mentioned technical problem, the present invention provides a kind of can restore multiple sample liquids, energy simultaneously
Automatic monitoring pillar liquid level and energy automatic constant volume receive the nitrate reduction instrument of reduction sample liquid, which has reduction
The advantage that speed is fast, reduction rate is high.
For the prior art there are the two of above-mentioned technical problem, the present invention provides a kind of sample reduction of nitrate reduction instrument
Application method and pillar regenerate application method, and sample reduction application method can quickly restore sample liquid, which makes
Pillar can be rapidly regenerated with method.
One of to achieve the above object, the present invention the following technical schemes are provided:
A kind of nitrate reduction instrument, including vacuum pump module are provided, the vacuum pump module is connected at least two nitric acid
Salt recovery module, each nitrate reduction module includes pillar, filled with reduction cadmium grain, the reduction cadmium in the pillar
Two end faces of grain are equipped with pickling glass fiber, and the Single port of the pillar is connected with cistern, another port connection
There is conduit, pillar is equipped between the pillar and the conduit and is switched, the conduit, which is plugged into, sewer pipe and sample liquid pipe, described to lead
Pipe is plugged into respectively with the sewer pipe and the sample liquid pipe using triple valve, the delivery outlet of the sewer pipe and the sample liquid pipe
Delivery outlet is plugged in a hermetically sealed can, and discard solution receiving pool and sample liquid reception tank, the waste liquid are equipped with inside the hermetically sealed can
The delivery outlet of pipe leads to the discard solution receiving pool, and the delivery outlet of the sample liquid pipe leads to the sample liquid reception tank, the hermetically sealed can
It is connect with the vacuum pump module, pressure controller is equipped between the hermetically sealed can and the vacuum pump module, the pillar is equipped with
Minimum graduation mark, the volume of the minimum graduation mark to the triple valve are 26~27mL;
The side of the pillar is equipped with G1 leve monitor, and the G1 leve monitor is electrically connected with pillar switch,
The G1 leve monitor controls the connection situation of the pillar switch, the side of the sample liquid reception tank according to pillar liquid level
Face is equipped with G2 leve monitor, and the G2 leve monitor is electrically connected with pillar switch and the triple valve respectively, described
G2 leve monitor receives pit level according to sample liquid to control the pillar switch closing and make described in the triple valve steering
Discard solution receiving pool.
Wherein, the pillar, which is erect, places, and the cistern is set to the upper port of the pillar, and pillar and cistern are one
A entirety, the lower port of the pillar are connected to a connector, which is Cylindrical joint, and the lower port of the pillar is plugged on institute
The upper bottom surface of Cylindrical joint is stated, the conduit is by being connected to the side of the Cylindrical joint to the lower port with the pillar
It connects.
Wherein, the hermetically sealed can is located at the lower section of the pillar, and the receiving port of the discard solution receiving pool is towards the waste liquid
The underface of pipe delivery outlet, the receiving port of the sample liquid reception tank is towards the underface of the sample liquid pipe delivery outlet.
Wherein, the G1 leve monitor and the G2 leve monitor are infrared ray leve monitor.
Wherein, there are six nitrate reduction module, six nitrate reduction modules are equal for the vacuum pump module connection
It is distributed in the side of the vacuum pump module.
Wherein, the top of the shell of the nitrate reduction instrument is installed with the strut of setting, and the strut is set from top to bottom
There are two lassos, and the central axis of the lasso is parallel with the strut, and the cistern is placed through the lasso of top and clamping
On the lasso, the pillar is placed through the lasso of lower section and is connected on the lasso.
Wherein, the volume of the cistern is 50mL.
Wherein, the pillar is glass tube, and the length of the glass tube is 200mm, internal diameter 12mm.
Wherein, the pressure controller is connected with pressure gauge, and the hermetically sealed can is equipped with relief valve.
To achieve the above object two, the present invention the following technical schemes are provided:
A kind of application method of nitrate reduction instrument is provided,
Including sample restoring method and cadmium column regeneration method,
The sample restoring method the following steps are included:
Vacuum pump module is opened, enables multiple nitrate reduction modules, the operating procedure of each nitrate reduction module is such as
Under:
(1) it rinses cadmium column: using pH for 9.6~9.7 ammonia buffer, be 10 times of ammonia buffer volume to its addition
Water, obtain ammonia buffer diluent, the G1 leve monitor and the G2 leve monitor opened simultaneously, the pillar is opened
Pass is in close state, and the triple valve is turned to and is connected to the sewer pipe, and it is dilute that the resulting ammonia buffering of 25mL is added to cistern
Liquid is released to rinse cadmium column, pillar switch is opened manually, adjusts the pressure controller coutroi velocity in 3~5mL/min;
(2) sample restores: taking sample liquid 20mL to be restored using container dress, it is molten that the ammonia buffering that 5mLpH is 9.6~9.7 is added
Liquid mixes, obtains sample mixed liquor, sample mixed liquor is added in cistern, then with 15mL pure water rinsing container, to reservoir
Sample mixed liquor in cup nearly to minimum graduation mark when above-mentioned washing water is added, complete once washing, repeat above-mentioned purge step
It is rapid primary, when all cleaning solutions flow to nearly minimum graduation mark, pure water is filled to cistern, pillar is flowed through with maximum flow rate,
G2 leve monitor monitors the liquid level in sample liquid pond, when G2 leve monitor issues acoustic warning, controls the pillar switch and closes
It closes and controls the triple valve and lead to discard solution receiving pool, can be taken off sample liquid reception tank, the sample in the sample liquid reception tank at this time
Product liquid can be directly measured according to the second method colour developing of GB5009.33;
(3) instrument after use, adds pure water more than half to cistern, then covers cistern rim of a cup;
In aforesaid operations step, if liquid level drops to the minimum graduation mark in pillar, G1 liquid level detector can be sounded an alarm
And it controls pillar switch and closes;
The cadmium column regeneration method the following steps are included:
Triple valve is first turned to connection waste liquid pool, pillar switch is then opened, is flow to the water in cistern and nearly arrive quarter
When spending line, the hydrochloric acid solution that 25mL concentration is 0.1mol/L is drawn rapidly and is washed, coutroi velocity is in 4~5mL/min;To cistern
In hydrochloric acid solution flow to when nearly arriving graduation mark, the pure water of a 25mL is first added to cistern, and adjust the pressure controller
So that with the flow velocity of 10mL/min to the pure water for adding 25mL when nearly arriving minimum graduation mark, and extremely with the flow velocity of 10mL/min
G1 rings alarm, completes the regenerated operation of pillar.
Liquor capacity involved in above-mentioned application method can be modified according to actual use demand.
Beneficial effects of the present invention:
(1) vacuum pump module of the invention connects multiple recovery modules, and reduction instrument is enabled to restore multiple samples simultaneously,
Reduction rate, and vacuum pump module energy pumping liquid are improved, liquid is improved and crosses column speed, further improves reduction speed
Degree, meanwhile, nitrate reduction instrument of the invention still keeps higher nitrate reduction rate;G1 leve monitor monitors pillar in time
Liquid level, when liquid level graduation mark minimum lower than pillar, G1 leve monitor sounds an alarm and automatically controls catheter switch closing and leads
Pipe, can not only remind user's adding liquid in time in this way, moreover it is possible to effectively prevent pillar liquid level is too low so that restoring cadmium in pillar
The problem of grain oxidation deactivation, avoids because resulting in the need for the problem of replacement is every grain every grain oxidation, is conducive to simplify operating procedure;G2 liquid
Position monitor can monitor the liquid level of sample liquid reception tank in time, when the received liquid volume of reception tank institute reaches up to spectrophotometer institute
When the detection volume needed, G2 leve monitor is sounded an alarm and automatic control tee valve turns to discard solution receiving pool, so that sample liquid connects
The operation of subsequent constant volume sample liquid is not only omitted in receives pond energy automatic constant volume in this way, it is thus also avoided that because of the detection error caused by constant volume,
Convenient for improving the accuracy rate of detection.
(2) sample of nitrate reduction instrument of the present invention restores application method, and the application method operating procedure is simple, can be quickly
It restores single sample liquid sample to be restored and multiple sample liquid samples to be restored can be restored simultaneously, substantially increase reduction rate;And
G1 leve monitor and G2 leve monitor can accurately and timely level monitoring, monitor liquid level without the artificial moment, people can be saved
Power.
(3) pillar of nitrate reduction instrument of the present invention regenerates application method, and the application method operating procedure is simple, and can be fast
Pillar is regenerated fastly, so that the reduction rate of pillar is maintained within the scope of national standard.
(4) nitrate reduction instrument structure of the present invention is simple, easily operated, is suitable for large-scale production and application.
Detailed description of the invention
Fig. 1 is a kind of structural schematic diagram of the single recovery module of nitrate reduction instrument of the present invention;
Fig. 2 is a kind of overlooking structure diagram of nitrate reduction instrument of the present invention.
Appended drawing reference:
Vacuum pump module 1;Nitrate reduction module 2;Pillar 3;Restore cadmium grain 4;Pickling glass fiber 5;Cistern 6;It leads
Pipe 7;Pillar switch 8;Sewer pipe 9;Sample liquid pipe 10;Triple valve 11;Hermetically sealed can 12;Discard solution receiving pool 13;Sample liquid reception tank 14;Control
Depressor 15;G1 leve monitor 16;G2 leve monitor 17;Lasso 18;Shell 19;Connector 20;Bracket 21;Minimum graduation mark
22;Relief valve 23.
Specific embodiment
Below in conjunction with specific embodiments and drawings, the present invention is described in detail.
Embodiment 1
One of the present embodiment nitrate reduction instrument, shown in Fig. 2, including vacuum pump module 1, vacuum pump module 1 connect
Six recovery modules 2, and each nitrate reduction module 2 is connect with vacuum pump module 1, so that multiple nitrate reduction modules
2 carry out restoring operation simultaneously, and each nitrate reduction module 2 is connect with vacuum pump module 1 by pressure controller 15, controlled with this
The flow velocity of liquid had both guaranteed that liquid restored the residence time, and also can spend the column time by accelerating liquid as much as possible.
Shown in Fig. 1, each nitrate reduction module 2 includes pillar 3, and reduction cadmium grain 4 is filled in pillar 3, restores cadmium grain 4
Two end faces be equipped with pickling glass fiber 5, so as to formed reduction cadmium column.The Single port integrally connected of pillar 3 is connected to reservoir
Cup 6, another port is connected with conduit 7, pillar switch 8 is equipped between pillar 3 and conduit 7, conduit 7, which is plugged into, sewer pipe 9 and sample
Liquid pipe 10, conduit 7 are plugged into sewer pipe 9 and sample liquid pipe 10 respectively using triple valve 11, the delivery outlet and sample liquid pipe 10 of sewer pipe 9
Delivery outlet be plugged in a hermetically sealed can 12, inside hermetically sealed can 12 be equipped with discard solution receiving pool 13 and sample liquid reception tank 14, give up
The delivery outlet of liquid pipe 9 leads to discard solution receiving pool 13, and the delivery outlet of sample liquid pipe 10 leads to sample liquid reception tank 14, hermetically sealed can 12 and vacuum
Pump module 1 connects, and pressure controller 15 is equipped between hermetically sealed can 12 and vacuum pump module 1, and vacuum pump module 1 to produce in hermetically sealed can 12
Raw negative pressure, so that liquid be made to cross column.Pillar 3 is equipped with minimum graduation mark 22, the volume of the minimum graduation mark 22 to triple valve 11
For 26~27mL, to guarantee that last received sample liquid can reach 26~27mL.
Shown in Fig. 1, the side of pillar 3 is equipped with G1 leve monitor 16, and G1 leve monitor 16 is electrically connected with the switch of pillar 3
It connects, G1 leve monitor 16 controls the connection situation of pillar switch 8, the side of sample liquid reception tank 14 according to 3 liquid level of pillar
Equipped with G2 leve monitor 17, G2 leve monitor 17 is electrically connected with pillar switch 8 and triple valve 11 respectively, G2 leve monitor
17 receive pit level according to sample liquid to control the closing of pillar switch 8 and triple valve 11 is made to turn to discard solution receiving pool 13.
In the present embodiment, pillar 3, which is erect, to be placed, and cistern 6 is set to the upper port of pillar 3, and the lower port of pillar 3 is connected to one
A connector 20, the connector 20 are Cylindrical joint 20, and the lower port of pillar 3 is plugged on the upper bottom surface of Cylindrical joint 20, and conduit 7 passes through
The side of Cylindrical joint 20 is connected to connect with the lower port of pillar 3, hermetically sealed can 12 is located at the lower section of pillar 3, and waste liquid connects
The receiving port of receives pond 13 is exported towards the underface of 9 delivery outlet of sewer pipe, the receiving port of sample liquid reception tank 14 towards sample liquid pipe 10
The underface of mouth, so that entire apparatus structure is compact, and convenient for going out liquid or connecing sample.
In the present embodiment, G1 leve monitor 16 and G2 leve monitor 17 are infrared ray leve monitor.
In the present embodiment, it is preferable that there are six nitrate reduction module 2, six nitrate reductions for the connection of vacuum pump module 1
Module 2 is distributed in the side of vacuum pump module 1.
In the present embodiment, the top of the shell 19 of nitrate reduction instrument is installed with the strut 21 of setting, strut 21 on toward
Lasso 18 there are two dividing into, the central axis of lasso 18 is parallel with strut 21, and cistern 6 is placed through the lasso 18 of top and is clamped
On the lasso 18, pillar 3 is placed through the lasso 18 of lower section and is connected on the lasso 18.
In the present embodiment, the volume of cistern 6 is 50mL, and pillar 3 is glass tube, and the length of the glass tube is 200mm, interior
Diameter is 12mm, so that required constant volume volume is adapted.
In the present embodiment, pressure controller 15 is connected with pressure gauge, consequently facilitating observation pressure, hermetically sealed can 12 are equipped with relief valve
23, consequently facilitating adjusting the pressure in hermetically sealed can 12.
Embodiment 2
A kind of application method of nitrate reduction instrument of the present embodiment, including sample restoring method and cadmium column regeneration method,
The sample restoring method the following steps are included:
Vacuum pump module is opened, enables multiple nitrate reduction modules, the operating procedure of each nitrate reduction module is such as
Under:
(1) it rinses cadmium column: using pH for 9.6~9.7 ammonia buffer, be 10 times of ammonia buffer volume to its addition
Water, obtain ammonia buffer diluent, the G1 leve monitor and the G2 leve monitor opened simultaneously, the pillar is opened
Pass is in close state, and the triple valve is turned to and is connected to the sewer pipe, and it is dilute that the resulting ammonia buffering of 25mL is added to cistern
Liquid is released to rinse cadmium column, pillar switch is opened manually, adjusts the pressure controller coutroi velocity in 3~5mL/min;
(2) sample restores: taking sample liquid 20mL to be restored using container dress, it is molten that the ammonia buffering that 5mLpH is 9.6~9.7 is added
Liquid mixes, obtains sample mixed liquor, sample mixed liquor is added in cistern, then with 15mL pure water rinsing container, to reservoir
Sample mixed liquor in cup nearly to minimum graduation mark when above-mentioned washing water is added, complete once washing, repeat above-mentioned purge step
It is rapid primary, when all cleaning solutions flow to nearly minimum graduation mark, pure water is filled to cistern, pillar is flowed through with maximum flow rate,
G2 leve monitor monitors the liquid level in sample liquid pond, when G2 leve monitor issues acoustic warning, controls the pillar switch and closes
It closes and controls the triple valve and lead to discard solution receiving pool, can be taken off sample liquid reception tank, the sample in the sample liquid reception tank at this time
Product liquid can be directly measured according to the second method colour developing of GB5009.33;
(3) instrument after use, adds pure water more than half to cistern, then covers cistern rim of a cup;
In aforesaid operations step, if liquid level drops to the minimum graduation mark in pillar, G1 liquid level detector can be sounded an alarm
And it controls pillar switch and closes;
The cadmium column regeneration method the following steps are included:
Triple valve is first turned to connection waste liquid pool, pillar switch is then opened, is flow to the water in cistern and nearly arrive quarter
When spending line, the hydrochloric acid solution that 25mL concentration is 0.1mol/L is drawn rapidly and is washed, coutroi velocity is in 4~5mL/min;To cistern
In hydrochloric acid solution flow to when nearly arriving graduation mark, the pure water of a 25mL is first added to cistern, and adjust the pressure controller
It alarms so as to be rung with the flow velocity of 10mL/min to G1, then adds the pure water of another secondary 25mL, and again with the stream of 10mL/min
Speed is rung to G1 alarms, and completes the regenerated operation of pillar.
Finally it should be noted that the above embodiments are merely illustrative of the technical solutions of the present invention, rather than the present invention is protected
The limitation of range is protected, although explaining in detail referring to preferred embodiment to the present invention, those skilled in the art are answered
Work as understanding, it can be with modification or equivalent replacement of the technical solution of the present invention are made, without departing from the reality of technical solution of the present invention
Matter and range.
Claims (10)
1. a kind of nitrate reduction instrument, it is characterized in that: including vacuum pump module, the vacuum pump module is connected at least two nitre
Hydrochlorate recovery module, each nitrate reduction module includes pillar, filled with reduction cadmium grain, the reduction in the pillar
Two end faces of cadmium grain are equipped with pickling glass fiber, and the Single port of the pillar is connected with cistern, and another port connects
It is connected to conduit, pillar is equipped between the pillar and the conduit and is switched, the conduit, which is plugged into, sewer pipe and sample liquid pipe, described
Conduit is plugged into the sewer pipe and the sample liquid pipe respectively using triple valve, the delivery outlet of the sewer pipe and the sample liquid pipe
Delivery outlet be plugged in a hermetically sealed can, discard solution receiving pool and sample liquid reception tank are equipped with inside the hermetically sealed can, it is described useless
The delivery outlet of liquid pipe leads to the discard solution receiving pool, and the delivery outlet of the sample liquid pipe leads to the sample liquid reception tank, the sealing
Tank is connect with the vacuum pump module, and pressure controller is equipped between the hermetically sealed can and the vacuum pump module, is set on the pillar
There is minimum graduation mark, the volume of the minimum graduation mark to the triple valve is 26~27mL;
The side of the pillar is equipped with G1 leve monitor, and the G1 leve monitor is electrically connected with pillar switch, described
G1 leve monitor controls the connection situation of the pillar switch according to pillar liquid level, and the side of the sample liquid reception tank is set
There is G2 leve monitor, the G2 leve monitor is electrically connected with pillar switch and the triple valve respectively, the G2 liquid
Position monitor receives pit level according to sample liquid to control the pillar switch closing and the triple valve is made to turn to the waste liquid
Reception tank.
2. a kind of nitrate reduction instrument according to claim 1 is placed, the reservoir it is characterized in that: the pillar is erect
Cup is set to the upper port of the pillar, and the lower port of the pillar is connected to a connector, which is Cylindrical joint, the pillar
Lower port be plugged on the upper bottom surface of the Cylindrical joint, the conduit by be connected to the side of the Cylindrical joint to
The lower port of the pillar is connected.
3. a kind of nitrate reduction instrument according to claim 1, it is characterized in that: the hermetically sealed can is located under the pillar
Side, the receiving port of the discard solution receiving pool is towards the underface of the sewer pipe delivery outlet, the receiving port of the sample liquid reception tank
Towards the underface of the sample liquid pipe delivery outlet.
4. a kind of nitrate reduction instrument according to claim 1, it is characterized in that: the G1 leve monitor and the G2 liquid
Position monitor is infrared ray leve monitor.
5. a kind of nitrate reduction instrument according to claim 1, it is characterized in that: there are six nitre for vacuum pump module connection
Hydrochlorate recovery module, six nitrate reduction modules are distributed in the side of the vacuum pump module.
6. a kind of nitrate reduction instrument according to claim 1, it is characterized in that: the top of the shell of the nitrate reduction instrument
End is installed with the strut of setting, and the strut is set from top to bottom there are two lasso, and the central axis of the lasso and the strut are flat
Row, the cistern are placed through the lasso of top and are connected on the lasso, and the pillar is placed through the lasso of lower section simultaneously
It is connected on the lasso.
7. a kind of nitrate reduction instrument according to claim 1, it is characterized in that: the volume of the cistern is 50mL.
8. a kind of nitrate reduction instrument according to claim 1, it is characterized in that: the pillar is glass tube, the glass tube
Length be 200mm, internal diameter 12mm.
9. a kind of nitrate reduction instrument according to claim 1, it is characterized in that: the pressure controller is connected with pressure gauge, institute
It states hermetically sealed can and relief valve is installed.
10. a kind of application method of nitrate reduction instrument according to any one of claims 1 to 9, it is characterized in that:
Including sample restoring method and cadmium column regeneration method,
The sample restoring method the following steps are included:
Vacuum pump module is opened, enables multiple nitrate reduction modules, the operating procedure of each nitrate reduction module is as follows:
(1) it rinses cadmium column: using pH for 9.6~9.7 ammonia buffer, be 10 times of ammonia buffer volume to its addition
Water obtains ammonia buffer diluent, and the G1 leve monitor and the G2 leve monitor are opened simultaneously, the pillar switch
It is in close state, the triple valve is turned to and is connected to the sewer pipe, the resulting ammonia buffering dilution of 25mL is added to cistern
Liquid rinses cadmium column, opens pillar switch manually, adjusts the pressure controller coutroi velocity in 3~5mL/min;
(2) sample restores: taking sample liquid 20mL to be restored using container dress, the ammonia buffer that 5mLpH is 9.6~9.7 is added, mix
It is even, sample mixed liquor is obtained, sample mixed liquor is added in cistern, then with 15mL pure water rinsing container, in cistern
Sample mixed liquor nearly to minimum graduation mark when above-mentioned washing water is added, complete once washing, repeat above-mentioned washing step one
It is secondary, when all cleaning solutions flow to nearly minimum graduation mark, pure water is filled to cistern, pillar, G2 liquid are flowed through with maximum flow rate
The liquid level in position monitor monitoring sample liquid pond, when G2 leve monitor issues acoustic warning, control pillar switch close with
And the control triple valve leads to discard solution receiving pool, can be taken off sample liquid reception tank, the sample liquid in the sample liquid reception tank at this time
It can be directly measured according to the second method colour developing of GB5009.33;
(3) instrument after use, adds pure water more than half to cistern, then covers cistern rim of a cup;
In aforesaid operations step, if liquid level drops to the minimum graduation mark in pillar, G1 liquid level detector can be sounded an alarm and be controlled
Pillar switch processed is closed;
The cadmium column regeneration method the following steps are included:
Triple valve is first turned to connection waste liquid pool, pillar switch is then opened, is flow to the water in cistern and nearly arrive graduation mark
When, the hydrochloric acid solution that 25mL concentration is 0.1mol/L is drawn rapidly and is washed, and coutroi velocity is in 4~5mL/min;To in cistern
Hydrochloric acid solution is flow to when nearly arriving graduation mark, and the pure water of a 25mL is first added to cistern, and adjust the pressure controller so that
With the flow velocity of 10mL/min to the pure water for adding 25mL when nearly arriving minimum graduation mark, and rung with the flow velocity of 10mL/min to G1
The regenerated operation of pillar is completed in alarm.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
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CN201910251823.4A CN109932230A (en) | 2019-03-29 | 2019-03-29 | A kind of nitrate reduction instrument and its application method |
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