CN108287138A - The integrated apparatus and method of mercury in a kind of measurement agricultural product - Google Patents

The integrated apparatus and method of mercury in a kind of measurement agricultural product Download PDF

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Publication number
CN108287138A
CN108287138A CN201810000733.3A CN201810000733A CN108287138A CN 108287138 A CN108287138 A CN 108287138A CN 201810000733 A CN201810000733 A CN 201810000733A CN 108287138 A CN108287138 A CN 108287138A
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mercury
sample
drying unit
grinding
infrared sensor
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CN108287138B (en
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刘敏敏
周季堂
白洪超
朱云迪
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Jiangsu Zhongyi Co Ltd Analysis Of Gold
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Jiangsu Zhongyi Co Ltd Analysis Of Gold
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/17Systems in which incident light is modified in accordance with the properties of the material investigated
    • G01N21/25Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
    • G01N21/31Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
    • G01N21/3103Atomic absorption analysis
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00Sampling; Preparing specimens for investigation
    • G01N1/28Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/286Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00Sampling; Preparing specimens for investigation
    • G01N1/28Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/34Purifying; Cleaning
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00Sampling; Preparing specimens for investigation
    • G01N1/28Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/44Sample treatment involving radiation, e.g. heat
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00Sampling; Preparing specimens for investigation
    • G01N1/28Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/286Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising
    • G01N2001/2866Grinding or homogeneising
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/17Systems in which incident light is modified in accordance with the properties of the material investigated
    • G01N21/25Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
    • G01N21/31Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
    • G01N21/3103Atomic absorption analysis
    • G01N2021/3107Cold vapor, e.g. determination of Hg

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  • Physics & Mathematics (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • General Health & Medical Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • Chemical & Material Sciences (AREA)
  • General Physics & Mathematics (AREA)
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  • Pathology (AREA)
  • Spectroscopy & Molecular Physics (AREA)
  • Engineering & Computer Science (AREA)
  • Biomedical Technology (AREA)
  • Molecular Biology (AREA)
  • Investigating Or Analysing Materials By Optical Means (AREA)

Abstract

The invention discloses the integrated apparatus and method of mercury in a kind of measurement agricultural product, integrated apparatus includes mainly cleaning device, drying unit, grinding device and mercury vapourmeter device, cleaning device mainly has washer box, removal liquid case, power bin and roll brush, heating plate is equipped in drying unit, drying unit left side is equipped with feed inlet, feed inlet lower end is equipped with infrared sensor, grinding device includes splicing slideway, master and bracket panel composition, conveyer belt is equipped with before mercury vapourmeter device detection mouth entrance, upper plane is placed with sampling cup on the left of conveyer belt.Device provided by the invention effectively saves the detection preceding processing time to agricultural product, high degree of automation, save manpower and time, interference may be generated to sample by also preventing manual operation, and detection method is with easy, quick, analyze speed is fast, detection limit is low, and measurement dynamic linear response range is wide, greatly improves work efficiency.

Description

The integrated apparatus and method of mercury in a kind of measurement agricultural product
Technical field
The present invention relates to mercury measurement technical field, it is specifically related to the integrated apparatus of mercury and side in a kind of measurement agricultural product Method.
Background technology
The detection method of mercury contamination of food has atomic absorption method, atomic fluorescence method, ICP-AES methods and ICP-MS methods at present Deng.Atomic Absorption Spectrometer is the light that elemental characteristic spectral line to be measured is provided from radiation of light source, by when sample steam by steam In element ground state atom to be measured absorbed, the degree being weakened by radiation feature spectral line light measures containing for element to be measured in sample Amount.Mercury vapourmeter instrument includes mainly the mercury lamp of 253.7 nanometers of spectral lines of transmitting, gas absorption chamber and the dresses such as photoelectricity amplification and measurement It sets.Into the gaseous sample of absorption chamber, such as contains the mercury of micro- mark, then can be subtracted because part is absorbed by mercury by the light of absorption chamber It is weak.The degree weakened according to light can measure the mercury content in gas.
It in actually detected agricultural product when mercury, needs to pre-process agricultural product before detection, and traditional survey mercury Equipment is compared with unification, this makes the workload of measurement personnel become larger, waste of manpower and time, and is manually carrying out some links When, it is also possible to sample measurement is had an impact in processing procedure;And we have found that in traditional agricultural product mercury detection Method is more complex, and analyze speed is slow, and working efficiency is relatively low.
Invention content
Present invention solves the technical problem that being:Mercury equipment is surveyed in the prior art compared with unification, measures the heavy workload of personnel, Waste of manpower and time, the detection method of mercury is more complex in traditional agricultural product, and analyze speed is slow, and working efficiency is more low to ask Topic provides a kind of method that mercury vapourmeter measures mercury in agricultural product.
The technical scheme is that:The integrated apparatus of mercury, the integrated apparatus are main in a kind of measurement agricultural product Including cleaning device, drying unit, grinding device and mercury vapourmeter device, the cleaning device mainly have washer box, removal liquid case, Power bin and roll brush, the removal liquid case are located at the upper right top surface of the washer box, and the power bin is located at the washer box Bottom surface, the motor of the roll brush and power bin connects, and is equipped with charge door on the left of the upper top surface of the washer box, it is described plus Infrared sensor is equipped on the left of material mouth, the electric machine controller of the infrared sensor and the power bin peripheral hardware is connected by data line It connects, the electric machine controller is located at the leading flank of the power bin, and the electric machine controller is used to receive the number of infrared sensor Add medicine catch according to being equipped with come the motor in the storehouse that turns on the power, between the charge door and washer box, under the left side of the washer box End is equipped with liquid outlet gate, and liquid outlet floodgate motor, the liquid outlet floodgate motor and electricity are equipped with below the liquid outlet gate Machine controller connects, and washer box right side lower end is equipped with discharging port strobe, and discharge port is equipped with below the discharging port strobe Floodgate motor, the discharge port floodgate motor are connect with electric machine controller;The drying unit is cylindrical, the drying unit It is interior to be equipped with heating plate, it surround drying unit inner wall one week, the drying unit left side is equipped with feed inlet, and the drying unit is right Side is equipped with discharge port, and the feed inlet lower end is equipped with infrared sensor, the infrared sensor and the heating plate controller It is connected by data line, the heating plate controller is located at the leading flank of the drying unit, and the heating plate controller is used for The data for receiving infrared sensor open heating plate;The grinding device includes splicing slideway, master and bracket panel, and the splicing is slided Road is located at the upper left side of the grinding device, and the master is located at the upper top surface right part of the grinding device, and the bracket panel is located at On the Right Inboard face of the grinding device, and closely with the master, grinding device position corresponding with the right end of master Level-one sieve plate is installed, grinding device position corresponding with the bottom of bracket panel is equipped with two level sieve plate, the splicing slideway Inlet is equipped with infrared sensor, and the infrared sensor is connect with the grinding control device by data line, the grinding control Device processed is located on the left of the leading flank of the grinding device, and the data that the grinding control device is used to receive infrared sensor open master The motor of disk and bracket panel;Conveyer belt is equipped with before the mercury vapourmeter device detection mouth entrance, upper plane is placed on the left of the conveyer belt The discharging port strobe of sampling cup, the washer box is connect by pipeline with the feed inlet of the drying unit, the drying unit Discharge port connect by pipeline with the splicing slideway of the grinding device.
Further, the level-one sieve plate is the level-one sieve pore of 60 mesh, and the two level sieve plate is the two level sieve pore of 100 mesh, Gradation sizing can improve the efficiency of grinding, and keep grinding more abundant.
Further, the master bottom end is equipped with spiral helicine crushing tooth, the contact of the bracket panel and the grinding device Face is equipped with thin helical teeth, and spiral helicine crushing tooth can be moved by sample comminution and to the right, and crush efficiency is high, and thin helical teeth can So that grinding is more fully and uniform.
Further, remover is loaded in the remover case, the remover is extracted by Pan's concentrated liquid and gleditsia sinensis Liquid presses 30:7 volume ratio mixes, and the mass fraction of Pan's concentrated liquid is 17%, the quality of the gleditsia sinensis extracting solution Score is 23%, and the gleditsia sinensis extracting solution is slowly added into Pan's concentrated liquid, and temperature is controlled at 10 DEG C, and is constantly stirred, The remover can effectively remove the sundries on agricultural sample surface, and gleditsia sinensis extracting solution mixes most with Pan's concentrated liquid at this temperature Soon, effect is best.
The method of mercury, mainly includes the following steps that in a kind of measurement agricultural product:
S1:Sample collection and keeping:In sampling and preparation process, it should be noted that do not make sample contamination;By agricultural samples It is added from charge door, triggers infrared sensor, controlling power bin by electric machine controller starts to work, while agricultural samples are logical Triggering adds medicine catch when crossing charge door, and removal liquid falls into washer box, and after cleaning 5-10 minutes, electric machine controller sends out instruction control It makes liquid port strobe motor and opens liquid outlet gate, after excluding waste liquid, electric machine controller sends out instruction control discharging port strobe electricity Machine opens discharging port strobe, and agricultural samples is made to go out from discharging port strobe, enters drying unit by pipeline, triggers infrared sensing Device is started to work by heating block controller control heat block, after 20-30 DEG C of drying unit low temperature drying 10-15 minutes, is entered Grinding device triggers infrared sensor, controls master by grinding control device and bracket panel rotation crushes agricultural samples, Carry out the control of grain size to the sample after crushing by level-one sieve plate and two level sieve plate, grinding 15-20 minute to grain size is 100 Mesh after the completion of grinding, falls into sampling cup, and sample is sent into mercury vapourmeter device by conveyer belt;Sample segment is packed into simultaneously clean In net polyethylene bottle, it is sealed spare;
S2:The flow of mercury vapourmeter device detection:
A) preparation of standard solution:Mercury Standard Stock solutions are taken, concentration difference is diluted to step by step with 0.5% salpeter solution It is 0.1,0.2,0.5,1.0,10.0,20.0,50.0,100.0ppb standard working solution;
B) a ten thousandth balance is used to weigh sample;
C) mercury vapourmeter examination criteria working solution and sample are used;
S3:Interpretation of result:Go out the content of mercury in sample according to the example weight weighed and the Mass Calculation for detecting mercury;
W is sample metal content, measurement unit:ug/kg;
mhgTo read the quality of mercury, measurement unit in mercury vapourmeter:μg;
mSampleTo weigh the quality of sample, measurement unit:g.
Further, the agricultural samples are specially grain beans, but are not limited to these.
Further, the salpeter solution of polyethylene bottle concentration 0.3% impregnates 3-4 hours, effectively prevent external mercury Influence the influence detected to mercury in agricultural product.
The beneficial effects of the invention are as follows:
(1) integrated apparatus provided by the invention effectively saves the detection preceding processing time to agricultural product, automation Degree is high, saves manpower and time, and interference may be generated to sample by also preventing manual operation,
Influence the data of sclera remodeling.
(2) detection method of the invention have it is easy, quickly, analyze speed it is fast, detection limit is low, measures dynamic linear response range Width greatly improves work efficiency.
Description of the drawings
Fig. 1 is integrated apparatus overall structure diagram of the present invention.
Fig. 2 is the bottom view of master of the present invention.
Fig. 3 is the right view of bracket panel of the present invention.
Fig. 4 is level-one sieve plate of the present invention.
Fig. 5 is two level sieve plate of the present invention.
Wherein, 1- cleaning devices, 11- washer boxs, 12- removals liquid case, 121- add medicine baffle, 13- power bins, 14- rotations Brush, 15- electric machine controllers, 16- charge doors, 17- liquid outlets gate, 171- liquid outlets floodgate motor, 18- discharging port strobe, 181- discharge ports floodgate motor, 2- drying units, 21- heat blocks, 22- heating block controller, 23- feed inlets, 24- discharge ports, 3- grinding devices, 31- splicings slideway, 32- masters, 321- crushing tooths, 33- bracket panels, the thin helical teeth of 331-, 34- grinding controls device, 35- level-ones sieve plate, 351- level-ones sieve pore, 36- two levels sieve plate, 361- two levels sieve pore, 4- infrared sensors, 5- mercury vapourmeters device, 51- conveyer belts, 52- sampling cups.
Specific implementation mode
With reference to embodiment come to the present invention be further described in detail, preferably to embody this hair Bright advantage.
Embodiment 1
The integrated apparatus of mercury in a kind of measurement agricultural product, integrated apparatus include mainly cleaning device 1, drying unit 2, Grinding device 3 and mercury vapourmeter device 5, cleaning device 1 mainly have washer box 11, removal liquid case 12, power bin 13 and roll brush 14, Removal liquid case 12 is located at the upper right top surface of washer box 11, and power bin 13 is located at the bottom surface of washer box 11, roll brush 14 and power The motor in storehouse 13 connects, and charge door 16 is equipped on the left of the upper top surface of washer box 11, and 16 left side of charge door is equipped with infrared sensor 4, Infrared sensor 4 is connect with the electric machine controller 15 of 13 peripheral hardware of power bin by data line, and electric machine controller 15 is located at power bin 13 leading flank, electric machine controller 15 is for receiving the data of infrared sensor 4 come the motor in the storehouse 13 that turns on the power, charge door 16 It is equipped between washer box 12 and adds medicine catch 121, the left side lower end of washer box 11 is equipped with liquid outlet gate 17, liquid outlet gate 171 lower sections are equipped with liquid outlet floodgate motor 171, and liquid outlet floodgate motor 171 is connect with electric machine controller 15,11 right side of washer box Face lower end is equipped with discharging port strobe 18, and 18 lower section of discharging port strobe is equipped with discharge port floodgate motor 181, discharge port floodgate motor 181 connect with electric machine controller 15;Drying unit 2 is cylindrical, and heating plate 21 is equipped in drying unit 2, around drying unit 2 Inner wall one week, 2 left side of drying unit are equipped with feed inlet 23, and 2 right side of drying unit is equipped with discharge port 24,23 lower end of feed inlet Equipped with infrared sensor 4, infrared sensor 4 is connect with heating plate controller 22 by data line, and heating plate controller 22 is located at The leading flank of drying unit 2, the data that heating plate controller 22 is used to receive infrared sensor 4 open heating plate 21;Grinding dress It includes splicing slideway 31, master 32 and bracket panel 33 to set 3, and splicing slideway 31 is located at the upper left side of grinding device 3, and master 32, which is located at, to be ground The upper top surface right part of mill apparatus 3, bracket panel 33 are located on the Right Inboard face of grinding device 3, and closely with master 32,32 bottom end of master Equipped with spiral helicine crushing tooth 321, bracket panel 33 and the contact surface of grinding device 3 are equipped with thin helical teeth 331, spiral helicine crushing tooth 321 can move by sample comminution and to the right, and crush efficiency is high, and thin helical teeth 331 can make grinding more fully and uniform. The position corresponding with the right end of master 32 of grinding device 3 is equipped with level-one sieve plate 35, the bottom pair of grinding device 3 and bracket panel 33 The position answered is equipped with two level sieve plate 36, and level-one sieve plate 35 is the level-one sieve pore 351 of 60 mesh, and two level sieve plate 36 is the two level of 100 mesh Sieve pore 361, gradation sizing can improve the efficiency of grinding, and keep grinding more abundant.31 inlet of splicing slideway is equipped with infrared Sensor 4, infrared sensor 4 are connect with grinding control device 34 by data line, before grinding control device 34 is located at grinding device 3 On the left of side, grinding control device 34 is used to receive the motor of data the unlatching master 32 and bracket panel 33 of infrared sensor 4;Mercury vapourmeter Conveyer belt 51 is equipped with before 5 detection mouth entrance of device, the upper plane in 51 left side of conveyer belt is placed with sampling cup 52, the discharge port of washer box 11 Gate 18 is connect by pipeline with the feed inlet 23 of drying unit 2, the splicing of the discharge port 24 and grinding device 3 of drying unit 2 Slideway 31 is connected by pipeline.
Remover is loaded in remover case, remover presses 30 by Pan's concentrated liquid and gleditsia sinensis extracting solution:7 volume ratio is mixed It closes, the mass fraction of Pan's concentrated liquid is 17%, and the mass fraction of gleditsia sinensis extracting solution is 23%, slowly by gleditsia sinensis extracting solution It is added in Pan's concentrated liquid, temperature is controlled at 10 DEG C, and is constantly stirred, which can effectively remove agricultural sample table The sundries in face, at this temperature gleditsia sinensis extracting solution mixed with Pan's concentrated liquid most fast, effect is best.
The method of mercury, mainly includes the following steps that in a kind of measurement agricultural product:
S1:Sample collection and keeping:In sampling and preparation process, it should be noted that do not make sample contamination;By agricultural samples It is added from charge door 16, triggers infrared sensor 4, controlling power bin 13 by electric machine controller 15 starts to work, while agricultural production Product sample adds medicine catch 121 by being triggered when charge door 16, and removal liquid falls into washer box 11, and when cleaning after five minutes, motor controls Device 15 sends out instruction control liquid outlet floodgate motor 171 and opens liquid outlet gate 17, and after excluding waste liquid, electric machine controller 15 is sent out Instruction control discharge port floodgate motor 181 opens discharging port strobe 18, so that agricultural samples is gone out from discharging port strobe 181, passes through Pipeline enters drying unit 2, triggers infrared sensor 4, and the start-up operation of heat block 21, drying are controlled by heating block controller 22 2 20 DEG C of low temperature dryings of device after ten minutes, into grinding device 3, trigger infrared sensor 4, are controlled by grinding control device 34 Master 32 and the rotation of bracket panel 33 crush agricultural samples, by level-one sieve plate 35 and two level sieve plate 36 to the sample after crushing Product carry out grain size control, grinding 15 minutes to grain size be 100 mesh, after the completion of grinding, fall into sampling cup 52, pass through conveyer belt 51 Sample is sent into mercury vapourmeter device 5;Sample segment is fitted into clean polyethylene bottle simultaneously, polyethylene bottle concentration 0.3% Salpeter solution impregnates 3 hours, and external mercury is effectively prevent to influence the influence detected to mercury in agricultural product;It is sealed spare;
S2:The flow that mercury vapourmeter device 5 detects:
A) preparation of standard solution:Mercury Standard Stock solutions are taken, concentration difference is diluted to step by step with 0.5% salpeter solution It is 0.1,0.2,0.5,1.0,10.0,20.0,50.0,100.0ppb standard working solution;
B) a ten thousandth balance is used to weigh sample;
C) mercury vapourmeter examination criteria working solution and sample are used;
S3:Interpretation of result:Go out the content of mercury in sample according to the example weight weighed and the Mass Calculation for detecting mercury;
W is sample metal content, measurement unit:ug/kg;
mhgTo read the quality of mercury, measurement unit in mercury vapourmeter:μg;
mSampleTo weigh the quality of sample, measurement unit:g.
Embodiment 2
The integrated apparatus of mercury in a kind of measurement agricultural product, integrated apparatus include mainly cleaning device 1, drying unit 2, Grinding device 3 and mercury vapourmeter device 5, cleaning device 1 mainly have washer box 11, removal liquid case 12, power bin 13 and roll brush 14, Removal liquid case 12 is located at the upper right top surface of washer box 11, and power bin 13 is located at the bottom surface of washer box 11, roll brush 14 and power The motor in storehouse 13 connects, and charge door 16 is equipped on the left of the upper top surface of washer box 11, and 16 left side of charge door is equipped with infrared sensor 4, Infrared sensor 4 is connect with the electric machine controller 15 of 13 peripheral hardware of power bin by data line, and electric machine controller 15 is located at power bin 13 leading flank, electric machine controller 15 is for receiving the data of infrared sensor 4 come the motor in the storehouse 13 that turns on the power, charge door 16 It is equipped between washer box 12 and adds medicine catch 121, the left side lower end of washer box 11 is equipped with liquid outlet gate 17, liquid outlet gate 171 lower sections are equipped with liquid outlet floodgate motor 171, and liquid outlet floodgate motor 171 is connect with electric machine controller 15,11 right side of washer box Face lower end is equipped with discharging port strobe 18, and 18 lower section of discharging port strobe is equipped with discharge port floodgate motor 181, discharge port floodgate motor 181 connect with electric machine controller 15;Drying unit 2 is cylindrical, and heating plate 21 is equipped in drying unit 2, around drying unit 2 Inner wall one week, 2 left side of drying unit are equipped with feed inlet 23, and 2 right side of drying unit is equipped with discharge port 24,23 lower end of feed inlet Equipped with infrared sensor 4, infrared sensor 4 is connect with heating plate controller 22 by data line, and heating plate controller 22 is located at The leading flank of drying unit 2, the data that heating plate controller 22 is used to receive infrared sensor 4 open heating plate 21;Grinding dress It includes splicing slideway 31, master 32 and bracket panel 33 to set 3, and splicing slideway 31 is located at the upper left side of grinding device 3, and master 32, which is located at, to be ground The upper top surface right part of mill apparatus 3, bracket panel 33 are located on the Right Inboard face of grinding device 3, and closely with master 32,32 bottom end of master Equipped with spiral helicine crushing tooth 321, bracket panel 33 and the contact surface of grinding device 3 are equipped with thin helical teeth 331, spiral helicine crushing tooth 321 can move by sample comminution and to the right, and crush efficiency is high, and thin helical teeth 331 can make grinding more fully and uniform. The position corresponding with the right end of master 32 of grinding device 3 is equipped with level-one sieve plate 35, the bottom pair of grinding device 3 and bracket panel 33 The position answered is equipped with two level sieve plate 36, and level-one sieve plate 35 is the level-one sieve pore 351 of 60 mesh, and two level sieve plate 36 is the two level of 100 mesh Sieve pore 361, gradation sizing can improve the efficiency of grinding, and keep grinding more abundant.31 inlet of splicing slideway is equipped with infrared Sensor 4, infrared sensor 4 are connect with grinding control device 34 by data line, before grinding control device 34 is located at grinding device 3 On the left of side, grinding control device 34 is used to receive the motor of data the unlatching master 32 and bracket panel 33 of infrared sensor 4;Mercury vapourmeter Conveyer belt 51 is equipped with before 5 detection mouth entrance of device, the upper plane in 51 left side of conveyer belt is placed with sampling cup 52, the discharge port of washer box 11 Gate 18 is connect by pipeline with the feed inlet 23 of drying unit 2, the splicing of the discharge port 24 and grinding device 3 of drying unit 2 Slideway 31 is connected by pipeline.
Remover is loaded in remover case, remover presses 30 by Pan's concentrated liquid and gleditsia sinensis extracting solution:7 volume ratio is mixed It closes, the mass fraction of Pan's concentrated liquid is 17%, and the mass fraction of gleditsia sinensis extracting solution is 23%, slowly by gleditsia sinensis extracting solution It is added in Pan's concentrated liquid, temperature is controlled at 10 DEG C, and is constantly stirred, which can effectively remove agricultural sample table The sundries in face, at this temperature gleditsia sinensis extracting solution mixed with Pan's concentrated liquid most fast, effect is best.
The method of mercury, mainly includes the following steps that in a kind of measurement agricultural product:
S1:Sample collection and keeping:In sampling and preparation process, it should be noted that do not make sample contamination;By agricultural samples It is added from charge door 16, triggers infrared sensor 4, controlling power bin 13 by electric machine controller 15 starts to work, while agricultural production Product sample adds medicine catch 121 by being triggered when charge door 16, and removal liquid falls into washer box 11, after cleaning 7 minutes, motor control Device 15 sends out instruction control liquid outlet floodgate motor 171 and opens liquid outlet gate 17, and after excluding waste liquid, electric machine controller 15 is sent out Instruction control discharge port floodgate motor 181 opens discharging port strobe 18, so that agricultural samples is gone out from discharging port strobe 181, passes through Pipeline enters drying unit 2, triggers infrared sensor 4, and the start-up operation of heat block 21, drying are controlled by heating block controller 22 After 2 25 DEG C of device low temperature drying 13 minutes, into grinding device 3, infrared sensor 4 is triggered, is controlled by grinding control device 34 Master 32 and the rotation of bracket panel 33 crush agricultural samples, by level-one sieve plate 35 and two level sieve plate 36 to the sample after crushing Product carry out grain size control, grinding 17 minutes to grain size be 100 mesh, after the completion of grinding, fall into sampling cup 52, pass through conveyer belt 51 Sample is sent into mercury vapourmeter device 5;Sample segment is fitted into clean polyethylene bottle simultaneously, polyethylene bottle concentration 0.3% Salpeter solution impregnates 3.5 hours, and external mercury is effectively prevent to influence the influence detected to mercury in agricultural product;It is sealed spare;
S2:The flow that mercury vapourmeter device 5 detects:
A) preparation of standard solution:Mercury Standard Stock solutions are taken, concentration difference is diluted to step by step with 0.5% salpeter solution It is 0.1,0.2,0.5,1.0,10.0,20.0,50.0,100.0ppb standard working solution;
B) a ten thousandth balance is used to weigh sample;
C) mercury vapourmeter examination criteria working solution and sample are used;
S3:Interpretation of result:Go out the content of mercury in sample according to the example weight weighed and the Mass Calculation for detecting mercury;
W is sample metal content, measurement unit:ug/kg;
mhgTo read the quality of mercury, measurement unit in mercury vapourmeter:μg;
mSampleTo weigh the quality of sample, measurement unit:g.
Embodiment 3
The integrated apparatus of mercury in a kind of measurement agricultural product, integrated apparatus include mainly cleaning device 1, drying unit 2, Grinding device 3 and mercury vapourmeter device 5, cleaning device 1 mainly have washer box 11, removal liquid case 12, power bin 13 and roll brush 14, Removal liquid case 12 is located at the upper right top surface of washer box 11, and power bin 13 is located at the bottom surface of washer box 11, roll brush 14 and power The motor in storehouse 13 connects, and charge door 16 is equipped on the left of the upper top surface of washer box 11, and 16 left side of charge door is equipped with infrared sensor 4, Infrared sensor 4 is connect with the electric machine controller 15 of 13 peripheral hardware of power bin by data line, and electric machine controller 15 is located at power bin 13 leading flank, electric machine controller 15 is for receiving the data of infrared sensor 4 come the motor in the storehouse 13 that turns on the power, charge door 16 It is equipped between washer box 12 and adds medicine catch 121, the left side lower end of washer box 11 is equipped with liquid outlet gate 17, liquid outlet gate 171 lower sections are equipped with liquid outlet floodgate motor 171, and liquid outlet floodgate motor 171 is connect with electric machine controller 15,11 right side of washer box Face lower end is equipped with discharging port strobe 18, and 18 lower section of discharging port strobe is equipped with discharge port floodgate motor 181, discharge port floodgate motor 181 connect with electric machine controller 15;Drying unit 2 is cylindrical, and heating plate 21 is equipped in drying unit 2, around drying unit 2 Inner wall one week, 2 left side of drying unit are equipped with feed inlet 23, and 2 right side of drying unit is equipped with discharge port 24,23 lower end of feed inlet Equipped with infrared sensor 4, infrared sensor 4 is connect with heating plate controller 22 by data line, and heating plate controller 22 is located at The leading flank of drying unit 2, the data that heating plate controller 22 is used to receive infrared sensor 4 open heating plate 21;Grinding dress It includes splicing slideway 31, master 32 and bracket panel 33 to set 3, and splicing slideway 31 is located at the upper left side of grinding device 3, and master 32, which is located at, to be ground The upper top surface right part of mill apparatus 3, bracket panel 33 are located on the Right Inboard face of grinding device 3, and closely with master 32,32 bottom end of master Equipped with spiral helicine crushing tooth 321, bracket panel 33 and the contact surface of grinding device 3 are equipped with thin helical teeth 331, spiral helicine crushing tooth 321 can move by sample comminution and to the right, and crush efficiency is high, and thin helical teeth 331 can make grinding more fully and uniform. The position corresponding with the right end of master 32 of grinding device 3 is equipped with level-one sieve plate 35, the bottom pair of grinding device 3 and bracket panel 33 The position answered is equipped with two level sieve plate 36, and level-one sieve plate 35 is the level-one sieve pore 351 of 60 mesh, and two level sieve plate 36 is the two level of 100 mesh Sieve pore 361, gradation sizing can improve the efficiency of grinding, and keep grinding more abundant.31 inlet of splicing slideway is equipped with infrared Sensor 4, infrared sensor 4 are connect with grinding control device 34 by data line, before grinding control device 34 is located at grinding device 3 On the left of side, grinding control device 34 is used to receive the motor of data the unlatching master 32 and bracket panel 33 of infrared sensor 4;Mercury vapourmeter Conveyer belt 51 is equipped with before 5 detection mouth entrance of device, the upper plane in 51 left side of conveyer belt is placed with sampling cup 52, the discharge port of washer box 11 Gate 18 is connect by pipeline with the feed inlet 23 of drying unit 2, the splicing of the discharge port 24 and grinding device 3 of drying unit 2 Slideway 31 is connected by pipeline.
Remover is loaded in remover case, remover presses 30 by Pan's concentrated liquid and gleditsia sinensis extracting solution:7 volume ratio is mixed It closes, the mass fraction of Pan's concentrated liquid is 17%, and the mass fraction of gleditsia sinensis extracting solution is 23%, slowly by gleditsia sinensis extracting solution It is added in Pan's concentrated liquid, temperature is controlled at 10 DEG C, and is constantly stirred, which can effectively remove agricultural sample table The sundries in face, at this temperature gleditsia sinensis extracting solution mixed with Pan's concentrated liquid most fast, effect is best.
The method of mercury, mainly includes the following steps that in a kind of measurement agricultural product:
S1:Sample collection and keeping:In sampling and preparation process, it should be noted that do not make sample contamination;By agricultural samples It is added from charge door 16, triggers infrared sensor 4, controlling power bin 13 by electric machine controller 15 starts to work, while agricultural production Product sample adds medicine catch 121 by being triggered when charge door 16, and removal liquid falls into washer box 11, when cleaning after ten minutes, motor control Device 15 processed sends out instruction control liquid outlet floodgate motor 171 and opens liquid outlet gate 17, and after excluding waste liquid, electric machine controller 15 is sent out Go out instruction control discharge port floodgate motor 181 and open discharging port strobe 18, so that agricultural samples is gone out from discharging port strobe 181, lead to Piping enters drying unit 2, triggers infrared sensor 4, controls the start-up operation of heat block 21 by heating block controller 22, dries After 2 30 DEG C of equipment for drying low temperature drying 15 minutes, into grinding device 3, infrared sensor 4 is triggered, is controlled by grinding control device 34 Master 32 and bracket panel 33 processed rotation crush agricultural samples, by level-one sieve plate 35 and two level sieve plate 36 to crushing after Sample carry out grain size control, grinding 20 minutes to grain size be 100 mesh, after the completion of grinding, fall into sampling cup 52, pass through conveyer belt Sample is sent into mercury vapourmeter device 5 by 51;Sample segment is fitted into clean polyethylene bottle simultaneously, polyethylene bottle concentration 0.3% Salpeter solution impregnate 4 hours, effectively prevent external mercury to influence the influence detected to mercury in agricultural product;It is sealed spare;
S2:The flow that mercury vapourmeter device 5 detects:
A) preparation of standard solution:Mercury Standard Stock solutions are taken, concentration difference is diluted to step by step with 0.5% salpeter solution It is 0.1,0.2,0.5,1.0,10.0,20.0,50.0,100.0ppb standard working solution;
B) a ten thousandth balance is used to weigh sample;
C) mercury vapourmeter examination criteria working solution and sample are used;
S3:Interpretation of result:Go out the content of mercury in sample according to the example weight weighed and the Mass Calculation for detecting mercury;
W is sample metal content, measurement unit:ug/kg;
mhgTo read the quality of mercury, measurement unit in mercury vapourmeter:μg;
mSampleTo weigh the quality of sample, measurement unit:g.
We carry out proving embodiment 2 for this test method by experiment, and the results are shown in Table 1:
Table 1 is using 2 method of the embodiment of the present invention to the testing result of food standard product
The sample actual result is shown in Table 2:
The metallic element actual content of 2 food samples of table
By the Comparative result of the above Tables 1 and 2 as it can be seen that between data and actual value that the method for the present invention detects Deviation is especially small, and accuracy rate is up to 99% or more.
Finally it should be noted that:The above embodiments are merely illustrative of the technical solutions of the present invention, rather than its limitations;Although Present invention has been described in detail with reference to the aforementioned embodiments, it will be understood by those of ordinary skill in the art that:It still may be used To modify to the technical solution recorded in previous embodiment or equivalent replacement of some of the technical features;And These modifications or replacements, the spirit and model of technical solution of the embodiment of the present invention that it does not separate the essence of the corresponding technical solution It encloses.

Claims (7)

1. a kind of integrated apparatus measuring mercury in agricultural product, which is characterized in that the integrated apparatus includes mainly cleaning dress Set (1), drying unit (2), grinding device (3) and mercury vapourmeter device (5), the cleaning device (1) mainly have washer box (11), Liquid case (12), power bin (13) and roll brush (14) are removed, the removal liquid case (12) is located at the upper right of the washer box (11) Top surface, the power bin (13) are located at the bottom surface of the washer box (11), the electricity of the roll brush (14) and power bin (13) Machine connects, and charge door (16) is equipped on the left of the upper top surface of the washer box (11), infrared biography is equipped on the left of the charge door (16) Sensor (4), the infrared sensor (4) are connect with the electric machine controller (15) of the power bin (13) peripheral hardware by data line, The electric machine controller (15) is located at the leading flank of the power bin (13), and the electric machine controller (15) is for receiving infrared biography The data of sensor (4) are equipped with come the motor of the storehouse that turns on the power (13), between the charge door (16) and washer box (12) adds medicine gear The left side lower end of piece (121), the washer box (11) is equipped with liquid outlet gate (17), liquid outlet gate (171) lower section Equipped with liquid outlet floodgate motor (171), the liquid outlet floodgate motor (171) connect with electric machine controller (15), the washing Case (11) right side lower end is equipped with discharging port strobe (18), and discharge port floodgate motor is equipped with below the discharging port strobe (18) (181), the discharge port floodgate motor (181) connect with electric machine controller (15);The drying unit (2) is cylindrical, institute It states and is equipped with heating plate (21) in drying unit (2), surround drying unit (2) inner wall one week, drying unit (2) left side is set There are feed inlet (23), drying unit (2) right side to be equipped with discharge port (24), feed inlet (23) lower end is equipped with infrared biography Sensor (4), the infrared sensor (4) are connect with the heating plate controller (22) by data line, the heating plate control Device (22) is located at the leading flank of the drying unit (2), and the heating plate controller (22) is for receiving infrared sensor (4) Data open heating plate (21);The grinding device (3) includes splicing slideway (31), master (32) and bracket panel (33), described to connect Material slideway (31) is located at the upper left side of the grinding device (3), and the master (32) is located at the upper top surface of the grinding device (3) Right part, the bracket panel (33) are located on the Right Inboard face of the grinding device (3), and closely with the master (32), described to grind Mill apparatus (3) position corresponding with the right end of master (32) is equipped with level-one sieve plate (35), the grinding device (3) and bracket panel (33) the corresponding position in bottom is equipped with two level sieve plate (36), and splicing slideway (31) inlet is equipped with infrared sensor (4), the infrared sensor (4) is connect with the grinding control device (34) by data line, grinding control device (34) position On the left of the leading flank of the grinding device (3), the data that the grinding control device (34) is used to receive infrared sensor (4) are opened Open the motor of master (32) and bracket panel (33);Conveyer belt (51), the biography are equipped with before mercury vapourmeter device (5) the detection mouth entrance Send plane on band (51) left side to be placed with sampling cup (52), the discharging port strobe (18) of the washer box (11) by pipeline with it is described The feed inlet (23) of drying unit (2) connects, the discharge port (24) of the drying unit (2) and connecing for the grinding device (3) Material slideway (31) is connected by pipeline.
2. a kind of integrated apparatus measuring mercury in agricultural product according to claim 1, which is characterized in that the level-one sieve Plate (35) is the level-one sieve pore (351) of 60 mesh, and the two level sieve plate (36) is the two level sieve pore (361) of 100 mesh.
3. a kind of integrated apparatus measuring mercury in agricultural product according to claim 1, which is characterized in that the master (32) bottom end is equipped with spiral helicine crushing tooth (321), and the bracket panel (33) and the contact surface of the grinding device (3) are equipped with carefully Helical teeth (331).
4. a kind of integrated apparatus measuring mercury in agricultural product according to claim 1, which is characterized in that the master (32) and bracket panel (33) is respectively equipped with crushing tooth (321) and thin helical teeth (331).
5. a kind of method measuring mercury in agricultural product, which is characterized in that mainly include the following steps that:
S1:Sample collection and keeping:In sampling and preparation process, it should be noted that do not make sample contamination;By agricultural samples from adding Material mouth (16) is added, triggering infrared sensor (4), and controlling power bin (13) by electric machine controller (15) starts to work, simultaneously Agricultural samples add medicine catch (121) by being triggered when charge door (16), and removal liquid falls into washer box (11), when 5-10 points of cleaning Zhong Hou, electric machine controller (15) send out instruction control liquid outlet floodgate motor (171) and open liquid outlet gate (17), exclude waste liquid Afterwards, electric machine controller (15) sends out instruction control discharge port floodgate motor (181) and opens discharging port strobe (18), makes agricultural product sample Product go out from discharging port strobe (181), enter drying unit (2) by pipeline, triggering infrared sensor (4) passes through heat block control Device (22) control heat block (21) processed is started to work, after 20-30 DEG C of drying unit (2) low temperature drying 10-15 minutes, into grinding Device (3), triggering infrared sensor (4) control master (32) and bracket panel (33) rotation to agricultural production by grinding control device (34) Product sample crushes, and carries out the control of grain size to the sample after crushing by level-one sieve plate (35) and two level sieve plate (36), grinds Mill 15-20 minute to grain size be 100 mesh, after the completion of grinding, fall into sampling cup (52), by conveyer belt (51) by sample be sent into survey Mercury instrument device (5);Sample segment is fitted into clean polyethylene bottle simultaneously, is sealed spare;
S2:The flow of mercury vapourmeter device (5) detection:
A) preparation of standard solution:Mercury Standard Stock solutions are taken, being diluted to concentration step by step with 0.5% salpeter solution is respectively 0.1,0.2,0.5,1.0,10.0,20.0,50.0,100.0ppb standard working solution;
B) a ten thousandth balance is used to weigh sample;
C) mercury vapourmeter examination criteria working solution and sample are used;
S3:Interpretation of result:Go out the content of mercury in sample according to the example weight weighed and the Mass Calculation for detecting mercury;
W is sample metal content, measurement unit:ug/kg;
mhgTo read the quality of mercury, measurement unit in mercury vapourmeter:μg;
mSampleTo weigh the quality of sample, measurement unit:g.
6. a kind of method measuring mercury in agricultural product according to claim 4, which is characterized in that the agricultural samples tool Body is grain beans.
7. a kind of method measuring mercury in agricultural product according to claim 4, which is characterized in that the polyethylene bottle is with dense The salpeter solution of degree 0.3% impregnates 3-4 hours.
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