CN108181373A - A kind of method of 12 kinds of metallic elements in measure soils and sediments - Google Patents
A kind of method of 12 kinds of metallic elements in measure soils and sediments Download PDFInfo
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- CN108181373A CN108181373A CN201810000712.1A CN201810000712A CN108181373A CN 108181373 A CN108181373 A CN 108181373A CN 201810000712 A CN201810000712 A CN 201810000712A CN 108181373 A CN108181373 A CN 108181373A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/62—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating the ionisation of gases, e.g. aerosols; by investigating electric discharges, e.g. emission of cathode
- G01N27/626—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating the ionisation of gases, e.g. aerosols; by investigating electric discharges, e.g. emission of cathode using heat to ionise a gas
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/286—Preparing 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
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/44—Sample treatment involving radiation, e.g. heat
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/286—Preparing 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
- G01N2001/2866—Grinding or homogeneising
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Abstract
The invention discloses a kind of methods for measuring 12 kinds of metallic elements in soils and sediments, include the following steps：S1:Acquire soil to be measured；S2:Grinder was crushed to 180 mesh sieve；S3:The soil sample in sample bottle is taken to be positioned in digestion instrument to be cleared up；S4:Acid is caught up with to digestion solution residue 8ml 10ml；S5:Standing is cooled to room temperature, and is poured into 50ml volumetric flasks, and full scale is settled to automatic volume fixing device；S6:Supernatant is taken to centrifuge after staticly settling；S7:Sample liquid is put into icp ms；S8:According to the soil sample weight weighed and detect that the concentration of digestion solution calculates the content of 12 kinds of metallic elements in pedotheque.In short, the problem of the method for the present invention is reasonable, and pipeline and atomizer block when significantly avoiding instrument detection, and the accuracy for improving resolution efficiency, reducing manually-operated error, improving Determination of Metals in soils and sediments.
Description
Technical field
The present invention relates to soil environment protection detection technique fields, are specifically related to 12 in a kind of measure soils and sediments
The method of kind metallic element.
Background technology
Heavy metal pollution of soil (heavy metal pollution of the soil) refers to due to mankind's activity, soil
The content of minor metallic element in the soil in earth is more than background value, and too high levels caused by excess deposition are referred to as soil
Earth heavy metal pollution.
Heavy metal refers to the metal that proportion is equal to or more than 5.0, such as Fe, Mn, Zn, Cd, Hg, Ni, Co；As is a kind of standard
Metal, but since its chemical property and environmental behaviour have similarity more with heavy metal, therefore frequently included when discussing heavy metal
Arsenic, some are then directly included into the range of heavy metal.Since iron and manganese content are higher in soil, thus it is generally acknowledged that them
It is not soil pollution element, but under strong reducing condition, the murder by poisoning caused by iron and manganese also causes enough attention.China is multiple
It is exceeded that the rice produced is found cadmium, and soil pollution has become " public hazards ".The appearance of " cadmium rice crisis ", beats soil pollution again
Alarm bell, the detection of soil tenor also increasingly obtain the concern of people.
Standard HJ803-2016 defines measure -- the chloroazotic acid extraction-inductance for measuring 12 kinds of metallic elements of soils and sediments
Coupled plasma mass, it is accurate that this method measures, convenient, it is unique it is insufficient for digestion solution need to after filter paper filters constant volume,
Time-consuming for the method filtering, if filter paper is damaged or misoperation easily makes particulate matter enter in filtered fluid, so as to be surveyed in instrument
Sample feeding pipe or atomizer are blocked during amount, in actual tests, it has been found that then take filtrate elder generation constant volume after the completion of resolution
The way of clear liquid centrifugation, not only saves the time, reduces the use of consumptive material, while can also largely avoid follow-up instrument
The blockage problem of device detection.
In the operation of practical Soil K+adsorption, it has been found that traditional air drying process is slow, wastes time, and then drags slow detection
Time, while it has been found that often because mixing non-uniform problem resolution occurs not exclusively in digestion process, this is right
Testing result produces large effect, and digestion time is generally longer, and efficiency is low, and in constant volume process, testing crew can
It can lead to the problem of and accidentally drip or drip less, the deviation of constant volume, also team's testing result has certain influence.
Invention content
Present invention solves the technical problem that it is：Providing one kind has detection time short, and testing result is stablized accurately, prevents
The assay method of soils and sediments metallic element that instrument detection blocks.
The technical solution adopted by the present invention is：A kind of method of 12 kinds of metallic elements in measure soils and sediments, including
Following steps：
S1:Soil to be measured is acquired, soil to be measured is put into the advanced sector-style dry-cure of soil treatment device, then carry out at sorting
Reason；The air-dried processing time is 10-20 minutes, and the sorting process time is 5-15 minutes；
S2:It, will treated that soil sample is put into that grinder was crushed to 180 mesh sieve, and was put into drying after soil sample acquisition process
It is sealed in the sample bottle of sealing；
S3:The soil sample 1-3g in sample bottle is taken to be positioned in the soil sample case of digestion instrument, by soil sample disperser several times
Soil sample is fallen into 50ml polytetrafluoroethylene beakers, while is mixed by spraying digestion solution a sprinkling and soil sample of the ring by 25-30ml
It closes, spraying time is 10 minutes, mixing periods, controls a certain temperature between 80 DEG C -100 DEG C permanent temperature by oil bath heating
Temperature 20 minutes；When mixed solution is cooled to 40 °, then the resolution of 10-15ml is instilled by autocontrol valve into the mixed solution
Liquid b, and a certain thermostatic 25 minutes between being slowly warming up to 120 DEG C -140 DEG C；
S4:Acid is caught up with then to carry out dilution constant volume in next step to digestion solution residue 8ml-10ml；
S5:Standing is cooled to room temperature, and is poured into 50ml volumetric flasks, and at least cleans volumetric flask three times with test water, most
Afterwards 50ml full scales are settled to automatic volume fixing device；
S6:After staticly settling 20-30 minutes, 9-12ml supernatants 5300r/min in 15ml centrifuge tubes is taken to centrifuge 4-6 points
Then clock carries out next step icp ms detection；
S7:Sample liquid is put into icp ms, the reality of the icp ms
Testing parameter is：Plasma flow amount 15L/min；Secondary air amount：0.4L/min；Nebulizer flow 0.7L/min；Sample introduction body
Product：2.0mL/min；Power：1500W；Lamp current 25mA；Carrier gas flux 350mL/min；Shield gas flow amount 700mL/min；Detection
Wavelength selected as 243.6nm；
S8:According to the soil sample weight weighed and detect that the concentration of digestion solution calculates 12 kinds of metallic elements in pedotheque
Content.
Further, digestion solution first shifts constant volume in the S5, then supernatant is taken to centrifuge, by filtrate elder generation constant volume then
The way that supernatant is taken to centrifuge, not only saves the time, reduces the use of consumptive material, while after can also largely avoiding
The blockage problem of continuous instrument detection.
Further, in the S3 steps, soil sample disperser is 5 times by shaking ring vibrations to add in number, is shaken every time
Time interval is 80s, and sprinkling ring can effectively be coordinated to make just to be pre-mixed with digestion solution in soil sample dropping process, disappeared compared to tradition
Solution method, effectively accelerates digestion time, shortens for 17% time, and resolution is more thorough, and resolution efficiency increases 21%.
Further, the digestion solution a is that the concentrated nitric acid of 1 volume and the concentrated hydrochloric acid of 3 volumes mix.
Further, the digestion solution b is that the nitrous acid of 2 volumes and the concentrated hydrochloric acid of 3 volumes mix.
Further, the soil treatment device include fan, air-dry plate, sorting plate, feed inlet, discharge port, pedestal and
Power connection；The fan is equipped with 2, respectively positioned at the internal both sides in the left and right of the soil treatment device；The air-dried plate is set
There are 4, cross interval is located on the fan of both sides from top to bottom, and angle of inclination is 10 °, and the air-dried plate bottom surface is equipped with poly-
Aerofoil a, wind gathering plate b, wind gathering plate c, wind gathering plate d and wind gathering plate e, the sorting plate are located inside the soil treatment device and go to the bottom
Face, angle of inclination are 12 °, and the sorting plate is equipped with 8 baffles, the upper top surface for being equally distributed on the sorting plate, the sorting
Plate is connect by stent a and stent b with vibrating motor, and the discharge port is located on the left of the upper top surface of the soil treatment device,
The discharge port is located on the right side of the bottom surface of the soil treatment device, and the discharge port is equipped with control valve, the pedestal
The bottom surface center of the soil treatment device is fixedly connected on, the power connection is connected to the soil treatment device
Left side lower end, air-dried plate is effectively acted on by soil sample gravity and wind-force and coordinates the effect one of fan and five wind gathering plates
Grade grade, which slides, to be air-dried, and is then shaken, and baffle is coordinated to sort soil by the left and right of sorting plate, is prevented metal particulate
Soil K+adsorption is had an impact, influences the accuracy of data.
Further, it is additionally provided on the wind gathering plate a, wind gathering plate b, wind gathering plate c, wind gathering plate d and wind gathering plate e ventilative
Hole, sets that there are two set on air-permeating hole b, the wind gathering plate c there are two being set on air-permeating hole a, the wind gathering plate b on the wind gathering plate a
Have and set on air-permeating hole c, the wind gathering plate d there are two being set on air-permeating hole d, the wind gathering plate e there are two air-permeating hole e, each two is gathered
Two air-permeating holes between aerofoil are staggeredly located, and the air-permeating hole a, air-permeating hole c and air-permeating hole e positions correspond to, the air-permeating hole b
It is corresponding with air-permeating hole d positions, can be effectively by wind concentration on plate be air-dried by the setting of wind gathering plate, it will by air-permeating hole
Behind wind level-one grade passes to, avoid front wind gathering plate block behind, reducing effect.
Further, the digestion instrument includes B liquid cases, A liquid cases, soil sample case, temperature-controlled cabinet, control panel, reaction
Cup, fixator, liquid outlet and attaching plug, the B liquid cases are located at the upper left corner of the digestion instrument, the bottom of the B liquid cases
Face right end is equipped with dropper, and the dropper is equipped with autocontrol valve, filling opening B is equipped among the upper top surface of the B liquid cases；It is described
Filling opening A is equipped in A liquid cases among top surface, pipeline is connected on the left of the A liquid cases bottom surface and is connect with sprinkling ring, the sprinkling ring
Positioned at the upper inside wall of the reaction cup；The soil sample case is between the A liquid cases and B liquid cases, the soil sample case bottom surface
Center is connected to soil sample disperser, and the soil sample disperser bottom surface is evenly distributed with Process, the soil sample disperser and soil
Sample case junction is equipped with vibrations ring；The temperature-controlled cabinet is located at the interior bottom surface of the digestion instrument, the temperature-controlled cabinet
Heat block, controller and distribution box are internally provided with, the heat block is located at the interior upper top surface of the temperature-controlled cabinet, the control
Device is located at the interior left part of the temperature-controlled cabinet, and the distribution box is located at the interior right part of the temperature-controlled cabinet；The temperature control
Temperature sensor is equipped on the left of the upper top surface of case processed；The control panel is located at the leading flank of the digestion instrument, the control
The panel upper left corner is equipped with temperature display, and the lower left corner is from left to right equipped with+heat button and cooling button, and right side is opened equipped with device
It closes, the fixator is located at the interior half height of the digestion instrument, and the liquid outlet is located at the digestion instrument
At 1/5th under right side, the liquid outlet is equipped with control valve, and the attaching plug is located at the right side of the digestion instrument
Face bottom end；The controller is connect with the temperature sensor, heat block, sprinkling ring, vibrations ring and control panel, the temperature
Sensor is connect with the autocontrol valve, the distribution box and the temperature sensor, heat block, sprinkling ring, vibrations ring, control
Panel processed is connected with autocontrol valve, this digestion instrument adds in digestion solution a and digestion solution b by the two-stage stage and effectively raises
Clear up effect 27%, high degree of automation.And it can be heated evenly reaction cup, and the temperature when going out liquid using oil bath heating
It will not bad student's variation, it is ensured that go out the stabilization accuracy of liquid after resolution, sprinkling ring cooperation vibrations ring and soil sample disperser can make soil
Sample and digestion solution a mixing are abundant, shorten digestion time 17%, improve resolution efficiency 21%.
Further, the automatic volume fixing device includes telescopic rod a, control cabinet, connecting rod, titration case, buret, stretches
Bar b, beam receiver, light-beam transmitter and geometrical clamp, the telescopic rod a are located at the upper right side of the automatic volume fixing device, institute
The upper top that control cabinet is stated with the telescopic rod a is connect, and the connecting rod is connect with the left side of the control cabinet, the titration case
It is connect with the left side of the connecting rod, the buret is connected to the bottom surface center of the titration case, and the telescopic rod b is located at
The upper left side of the automatic volume fixing device, the beam receiver are located on the madial wall of the telescopic rod b, the beam emissions
Device is located on the madial wall of the telescopic rod a, and it is high that the geometrical clamp is located on the inner wall of the automatic volume fixing device 1/3rd
At degree, the control cabinet and the light-beam transmitter, beam receiver and titration case are connect, traditional constant volume be all by manually into
Row operation, this can inevitably generate certain error, by the cooperation of light-beam transmitter and beam receiver, be handled by control cabinet
Analysis and Control titration case carries out automation titration, and compared to manual operation error smaller, constant volume accuracy higher significantly reduces
The cooperation of constant volume fault rate, simultaneous retractable bar a and telescopic rod b can be according to the liquid levels for requiring constant volume different.
Compared with prior art, beneficial effects of the present invention are：
(1) digestion solution first shifts constant volume in S5 of the invention, then supernatant is taken to centrifuge, then filtrate elder generation constant volume is taken
The way of clear liquid centrifugation, not only saves the time, reduces the use of consumptive material, while can also largely avoid follow-up instrument
The blockage problem of device detection.
(2) soil treatment device of the invention, integrated degree is high, and air-dry time is short, efficient, and passes through sorting plate
Left and right vibrations, cooperation baffle sort soil, prevent metal particulate from being had an impact to Soil K+adsorption, influence the standard of data
True property.
(3) digestion procedure of the invention coordinates digestion instrument of the present invention, and digestion solution a and digestion solution are added in by the two-stage stage
B effectively raises resolution effect 27%, high degree of automation.And can be heated evenly reaction cup using oil bath heating, and
When going out liquid, temperature will not bad student's variation, it is ensured that goes out the stabilization accuracy of liquid after resolution, sprinkling ring cooperation vibrations ring and soil sample
Disperser can make soil sample and digestion solution a mixes abundant, shortening digestion time 17%, raising resolution efficiency 21%.
(4) automatic volume fixing device of the invention, compared to traditional constant volume all by manually being operated, this can inevitably be produced
Raw certain error by the cooperation of light-beam transmitter and beam receiver, handles analysis and Control by control cabinet and titrates case progress
Automation titration, compared to manual operation error smaller, constant volume accuracy higher significantly reduces constant volume fault rate.
Description of the drawings
Fig. 1 is the soil treatment device overall structure diagram of the present invention.
Fig. 2 is the air-permeating hole location map of the wind gathering plate of the present invention.
Fig. 3 is the digestion instrument overall structure diagram of the present invention.
Fig. 4 is the automatic volume fixing device overall structure diagram of the present invention.
Wherein, 1- soil treatments device, 11- fans, 12- air-dry plate, 121- wind gathering plate a, 1211- air-permeating holes a, 122- gather
Aerofoil b, 1221- air-permeating hole b, 123- wind gathering plate c, 1231- air-permeating hole c, 124- wind gathering plate d, 1241- air-permeating hole d, 125- gathers
Aerofoil e, 1251- air-permeating hole e, 13- sorting plate, 131- vibrating motors, 132- stent a, 133- stent b, 134- baffle, 14- into
Material mouth, 15- discharge ports, 151- control valves, 16- pedestals, 17- power connections, 2- digestion instruments, 21-B liquid cases, 211- are automatic
Control valve, 212- droppers, 213- filling opening b, 22-A liquid case, 221- sprinklings ring, 222- filling opening a, 23- soil samples case, 231- shakes
Rotating ring, 232- soil samples disperser, 24- temperature-controlled cabinets, 241- heat blocks, 242- controllers, 243- temperature sensors, 244- match
Electronic box, 25- control panels, 251- temperature displays, 252-+heat buttons, 253- cooling buttons, 254- devices switch, 26- are anti-
Answer cup, 27- fixators, 28- liquid outlets, 281- control valves, 29- attaching plugs, 3- automatic volume fixing devices, 31- telescopic rods a, 32-
Control cabinet, 33- connecting rods, 34- titration case, 35- burets, 36- telescopic rod b, 37- beam receiver, 38- light-beam transmitters,
39- geometrical clamps.
Specific embodiment
With reference to embodiment come to the present invention be further described in detail, preferably to embody this hair
Bright advantage.
Embodiment 1
The method of 12 kinds of metallic elements, includes the following steps in a kind of measure soils and sediments：
S1:Soil to be measured is acquired, soil to be measured is put into the feed inlet 14 of soil treatment device 1, by fan 11, is air-dried
The cooperation of plate 12 and five wind gathering plates, which is realized, air-dries processing, then drive sorting plate 13 by vibrating motor 131 and pass through baffle 134
And gravity, soil is sorted；It is 10 minutes to air-dry processing time, and the sorting process time is 5 minutes；
S2:It, will treated that soil sample is put into that grinder was crushed to 180 mesh sieve, and was put into drying after soil sample acquisition process
It is sealed in the sample bottle of sealing；
S3:The soil sample 1g in sample bottle is taken to be positioned in the soil sample case 23 of digestion instrument 2, shakes soil by shaking ring 231
Sample disperser 232 falls into soil sample in 50ml polytetrafluoroethylene beakers, and it is 5 times to add in number, shakes time interval every time and is
80s, while mixed by spraying digestion solution a sprinkling and soil sample of the ring 221 by 25ml, spraying time is 10 minutes, mixing periods,
Oil bath heating is controlled by control panel 25 and temperature-controlled cabinet 24, by temperature control at 80 DEG C, constant temperature after twenty minutes, stops adding
Heat, when mixed solution is cooled to 40 °, autocontrol valve 211 receives the data information of temperature sensor 243, control dropper to
The digestion solution b of 10ml is instilled in the mixed solution, subsequent temperature controller 24 is slowly warming up to 120 DEG C automatically, constant temperature 25 minutes,
After, it opens control valve 281 and collects digestion solution, carry out in next step；
S4:Acid is caught up with then to carry out dilution constant volume in next step to digestion solution residue 8ml；
S5:Standing is cooled to room temperature, and is poured into 50ml volumetric flasks, and volumetric flask three is at least cleaned with test water before pouring into
It is secondary, finally volumetric flask is fixed on automatic volume fixing device 3, by the cooperation of light-beam transmitter 38 and beam receiver 37, is led to
It crosses the control titration case 34 of control cabinet 32 and 50ml full scales is settled to it；
S6:It staticly settles after twenty minutes, takes 9ml supernatants 5300r/min centrifugations 4 minutes in 15ml centrifuge tubes, then
Carry out next step icp ms detection；
S7:Sample liquid is put into icp ms, the experiment ginseng of icp ms
Number is：Plasma flow amount 15L/min；Secondary air amount：0.4L/min；Nebulizer flow 0.7L/min；Sampling volume：
2.0mL/min；Power：1500W；Lamp current 25mA；Carrier gas flux 350mL/min；Shield gas flow amount 700mL/min；Detect wave
Long selected as 243.6nm；
S8:According to the soil sample weight weighed and detect that the concentration of digestion solution calculates 12 kinds of metallic elements in pedotheque
Content.
Digestion solution a is that the concentrated nitric acid of 1 volume and the concentrated hydrochloric acid of 3 volumes mix.
Digestion solution b is that the nitrous acid of 2 volumes and the concentrated hydrochloric acid of 3 volumes mix.
As illustrated in fig. 1 and 2, soil treatment device 1 includes fan 11, air-dries plate 12, sorting plate 13, feed inlet 14, discharging
Mouth 15, pedestal 16 and power connection 17；Fan 11 is equipped with 2, respectively positioned at the internal both sides in the left and right of soil treatment device 1；Wind
Dry plate 12 is equipped with 4, and cross interval is located on both sides fan 11 from top to bottom, and angle of inclination is 10 °, air-dries plate 12 and goes to the bottom
Face is equipped with wind gathering plate a 121, wind gathering plate b 122, wind gathering plate c 123, wind gathering plate d 124 and wind gathering plate e 125, wind gathering plate a
121st, air-permeating hole, wind gathering plate a are additionally provided on wind gathering plate b 122, wind gathering plate c 123, wind gathering plate d 124 and wind gathering plate e 125
Air-permeating hole b 1221 there are two being set on air-permeating hole a 1211 there are two being set on 121, wind gathering plate b 122, wind gathering plate c 123 to be equipped with
Air-permeating hole e there are two being set on air-permeating hole d 1241 there are two being set on air-permeating hole c 1231, wind gathering plate d 124, wind gathering plate e 125
1251, two air-permeating holes between each two wind gathering plate are staggeredly located, air-permeating hole a 1211, air-permeating hole c1231 and air-permeating hole e
1251 positions correspond to, and air-permeating hole b 1221 is corresponding with 1241 positions of air-permeating hole d, by the setting of wind gathering plate can effectively by
Behind wind concentration passes to wind level-one grade on air-dried plate 12, by air-permeating hole, avoid front wind gathering plate block behind, drop
Inefficient fruit.Sorting plate 13 is located at 1 inside bottom surface of soil treatment device, and angle of inclination is 12 °, and sorting plate 13 is equipped with 8 baffles
134th, the upper top surface of sorting plate 13 is equally distributed on, sorting plate 13 passes through stent a 132 and stent b 133 and vibrating motor 131
Connection, discharge port 15 are located on the left of the upper top surface of soil treatment device 1, and discharge port 15 is located at the bottom surface of soil treatment device 1
Right side, discharge port 15 are equipped with control valve 151, and pedestal 16 is fixedly connected on the bottom surface center of soil treatment device 1,
Power connection 17 is connected to the left side lower end of soil treatment device 1, effectively acts on air-dried plate by soil sample gravity and wind-force
12 and the effect level-one grade of fan 11 and five wind gathering plates is coordinated to slide air-dry, then shake by the left and right of sorting plate 13, and
Cooperation baffle 134 sorts soil, prevents metal particulate from being had an impact to Soil K+adsorption, influences the accuracy of data.
As shown in figure 3, digestion instrument 2 includes B liquid cases 21, A liquid cases 22, soil sample case 23, temperature-controlled cabinet 24, control panel
25th, reaction cup 26, fixator 27, liquid outlet 28 and attaching plug 29, B liquid cases 21 are located at the upper left corner of digestion instrument 2, B liquid cases
21 bottom surface right end is equipped with dropper 212, and dropper 212 is equipped with autocontrol valve 211, is equipped among the upper top surface of B liquid cases 21
Filling opening B 213；Filling opening A 222 is equipped in A liquid cases 22 among top surface, pipeline and sprinkling are connected on the left of 22 bottom surface of A liquid cases
Ring 221 connects, and sprinkling ring 221 is located at the upper inside wall of reaction cup 26；Soil sample case 23 is between A liquid cases 22 and B liquid cases 21, soil
23 bottom surface center of sample case is connected to soil sample disperser 232, and 232 bottom surface of soil sample disperser is evenly distributed with Process, soil sample
Disperser 232 is equipped with vibrations ring 231 with 23 junction of soil sample case；Temperature-controlled cabinet 24 is located at the interior bottom surface of digestion instrument 2, temperature
Degree control cabinet 24 is internally provided with heat block 241, controller 242 and distribution box 244, and heat block 241 is located at temperature-controlled cabinet 24
Interior upper top surface, controller 242 are located at the interior left part of temperature-controlled cabinet 24, and distribution box 244 is located at the interior right part of temperature-controlled cabinet 24；
Temperature sensor is equipped on the left of the upper top surface of temperature-controlled cabinet 24；Control panel 25 is located at the leading flank of digestion instrument 2, control plane
25 upper left corner of plate is equipped with temperature display 251, and the lower left corner is from left to right equipped with+heat button 252 and cooling button 253, and right side is set
There is device to switch 254, fixator 27 is located at the interior half height of digestion instrument 2, and liquid outlet 28 is located at digestion instrument 2
At 1/5th under right side, liquid outlet 28 is equipped with control valve 281, and attaching plug 29 is located at the right side bottom of digestion instrument 2
End；Controller 242 is connect with temperature sensor 243, heat block 241, sprinkling ring 221, vibrations ring 231 and control panel 25, temperature
Degree sensor 243 is connect with autocontrol valve 211, distribution box 244 and temperature sensor 243, heat block 241, spray ring 221,
Vibrations ring 231, control panel 25 and autocontrol valve 211 connect, this digestion instrument 2 by the two-stage stage add in digestion solution a and
Digestion solution b effectively raises resolution effect 27%, high degree of automation.And reaction cup 26 can be made heated using oil bath heating
Uniformly, temperature will not bad student's variation and when going out liquid, it is ensured that goes out the stabilization accuracy of liquid, the sprinkling cooperation shake of ring 221 after resolution
Rotating ring 231 and soil sample disperser 232 can make soil sample and digestion solution a mixes abundant, shortening digestion time 17%, raising resolution effect
Rate 21%.
As shown in figure 4, automatic volume fixing device 3 includes telescopic rod a31, control cabinet 32, connecting rod 33, titration case 34, titration
Pipe 35, telescopic rod b 36, beam receiver 37, light-beam transmitter 38 and geometrical clamp 39, telescopic rod a 31 are located at automatic constant volume dress
3 upper right side is put, control cabinet 32 is connect with the upper top of telescopic rod a 31, and connecting rod 33 is connect with the left side of control cabinet 32, drop
The left side for determining case 34 with connecting rod 33 is connect, and buret 35 is connected to the bottom surface center of titration case 34, and telescopic rod b 36 is located at
The upper left side of automatic volume fixing device 3, beam receiver 37 are located on the madial wall of telescopic rod b 36, and light-beam transmitter 38, which is located at, to be stretched
On the madial wall of contracting bar a 31, geometrical clamp 39 is located on the inner wall of automatic volume fixing device 3 1/3rd height and locates, control cabinet 32 and
Light-beam transmitter 38, beam receiver 37 and titration case 34 connect, and traditional constant volume is all by manually being operated, this is inevitably
Certain error can be generated, by the cooperation of light-beam transmitter 38 and beam receiver 37, analysis and Control is handled by control cabinet 32
Titration case 34 carries out automation titration, and compared to manual operation error smaller, constant volume accuracy higher significantly reduces constant volume mistake
Accidentally rate, the cooperation of simultaneous retractable bar a 31 and telescopic rod b 36 can be according to the liquid level for requiring constant volume different.
Embodiment 2
The method of 12 kinds of metallic elements, includes the following steps in a kind of measure soils and sediments：
S1:Soil to be measured is acquired, soil to be measured is put into the feed inlet 14 of soil treatment device 1, by fan 11, is air-dried
The cooperation of plate 12 and five wind gathering plates, which is realized, air-dries processing, then drive sorting plate 13 by vibrating motor 131 and pass through baffle 134
And gravity, soil is sorted；It is 15 minutes to air-dry processing time, and the sorting process time is 10 minutes；
S2:It, will treated that soil sample is put into that grinder was crushed to 180 mesh sieve, and was put into drying after soil sample acquisition process
It is sealed in the sample bottle of sealing；
S3:The soil sample 2g in sample bottle is taken to be positioned in the soil sample case 23 of digestion instrument 2, shakes soil by shaking ring 231
Sample disperser 232 falls into soil sample in 50ml polytetrafluoroethylene beakers, and it is 5 times to add in number, shakes time interval every time and is
80s, while mixed by spraying digestion solution a sprinkling and soil sample of the ring 221 by 27ml, spraying time is 10 minutes, mixing periods,
Oil bath heating is controlled by control panel 25 and temperature-controlled cabinet 24, by temperature control at 90 DEG C, constant temperature after twenty minutes, stops adding
Heat, when mixed solution is cooled to 40 °, autocontrol valve 211 receives the data information of temperature sensor 243, control dropper to
The digestion solution b of 13ml is instilled in the mixed solution, subsequent temperature controller 24 is slowly warming up to 130 DEG C automatically, constant temperature 25 minutes,
After, it opens control valve 281 and collects digestion solution, carry out in next step；
S4:Catching up with acid, to digestion solution residue then 9ml carries out dilution constant volume in next step；
S5:Standing is cooled to room temperature, and is poured into 50ml volumetric flasks, and volumetric flask three is at least cleaned with test water before pouring into
It is secondary, finally volumetric flask is fixed on automatic volume fixing device 3, by the cooperation of light-beam transmitter 38 and beam receiver 37, is led to
It crosses the control titration case 34 of control cabinet 32 and 50ml full scales is settled to it；
S6:After staticly settling 25 minutes, 11ml supernatants 5300r/min centrifugations 5 minutes in 15ml centrifuge tubes are taken, then
Carry out next step icp ms detection；
S7:Sample liquid is put into icp ms, the experiment ginseng of icp ms
Number is：Plasma flow amount 15L/min；Secondary air amount：0.4L/min；Nebulizer flow 0.7L/min；Sampling volume：
2.0mL/min；Power：1500W；Lamp current 25mA；Carrier gas flux 350mL/min；Shield gas flow amount 700mL/min；Detect wave
Long selected as 243.6nm；
S8:According to the soil sample weight weighed and detect that the concentration of digestion solution calculates 12 kinds of metallic elements in pedotheque
Content.
Digestion solution a is that the concentrated nitric acid of 1 volume and the concentrated hydrochloric acid of 3 volumes mix.
Digestion solution b is that the nitrous acid of 2 volumes and the concentrated hydrochloric acid of 3 volumes mix.
As illustrated in fig. 1 and 2, soil treatment device 1 includes fan 11, air-dries plate 12, sorting plate 13, feed inlet 14, discharging
Mouth 15, pedestal 16 and power connection 17；Fan 11 is equipped with 2, respectively positioned at the internal both sides in the left and right of soil treatment device 1；Wind
Dry plate 12 is equipped with 4, and cross interval is located on both sides fan 11 from top to bottom, and angle of inclination is 10 °, air-dries plate 12 and goes to the bottom
Face is equipped with wind gathering plate a 121, wind gathering plate b 122, wind gathering plate c 123, wind gathering plate d 124 and wind gathering plate e 125, wind gathering plate a
121st, air-permeating hole, wind gathering plate a are additionally provided on wind gathering plate b 122, wind gathering plate c 123, wind gathering plate d 124 and wind gathering plate e 125
Air-permeating hole b 1221 there are two being set on air-permeating hole a 1211 there are two being set on 121, wind gathering plate b 122, wind gathering plate c 123 to be equipped with
Air-permeating hole e there are two being set on air-permeating hole d 1241 there are two being set on air-permeating hole c 1231, wind gathering plate d 124, wind gathering plate e 125
1251, two air-permeating holes between each two wind gathering plate are staggeredly located, air-permeating hole a 1211, air-permeating hole c 1231 and air-permeating hole e
1251 positions correspond to, and air-permeating hole b 1221 is corresponding with 1241 positions of air-permeating hole d, by the setting of wind gathering plate can effectively by
Behind wind concentration passes to wind level-one grade on air-dried plate 12, by air-permeating hole, avoid front wind gathering plate block behind, drop
Inefficient fruit.Sorting plate 13 is located at 1 inside bottom surface of soil treatment device, and angle of inclination is 12 °, and sorting plate 13 is equipped with 8 baffles
134th, the upper top surface of sorting plate 13 is equally distributed on, sorting plate 13 is connected by stent a132 and stent b133 with vibrating motor 131
It connects, discharge port 15 is located on the left of the upper top surface of soil treatment device 1, and the bottom surface that discharge port 15 is located at soil treatment device 1 is right
Side, discharge port 15 are equipped with control valve 151, and pedestal 16 is fixedly connected on the bottom surface center of soil treatment device 1, electricity
Source connector 17 is connected to the left side lower end of soil treatment device 1, effectively acts on air-dried plate 12 by soil sample gravity and wind-force
And the effect level-one grade of fan 11 and five wind gathering plates is coordinated to slide and is air-dried, then shaken, and match by the left and right of sorting plate 13
It closes baffle 134 to sort soil, prevents metal particulate from being had an impact to Soil K+adsorption, influence the accuracy of data.
As shown in figure 3, digestion instrument 2 includes B liquid cases 21, A liquid cases 22, soil sample case 23, temperature-controlled cabinet 24, control panel
25th, reaction cup 26, fixator 27, liquid outlet 28 and attaching plug 29, B liquid cases 21 are located at the upper left corner of digestion instrument 2, B liquid cases
21 bottom surface right end is equipped with dropper 212, and dropper 212 is equipped with autocontrol valve 211, is equipped among the upper top surface of B liquid cases 21
Filling opening B 213；Filling opening A 222 is equipped in A liquid cases 22 among top surface, pipeline and sprinkling are connected on the left of 22 bottom surface of A liquid cases
Ring 221 connects, and sprinkling ring 221 is located at the upper inside wall of reaction cup 26；Soil sample case 23 is between A liquid cases 22 and B liquid cases 21, soil
23 bottom surface center of sample case is connected to soil sample disperser 232, and 232 bottom surface of soil sample disperser is evenly distributed with Process, soil sample
Disperser 232 is equipped with vibrations ring 231 with 23 junction of soil sample case；Temperature-controlled cabinet 24 is located at the interior bottom surface of digestion instrument 2, temperature
Degree control cabinet 24 is internally provided with heat block 241, controller 242 and distribution box 244, and heat block 241 is located at temperature-controlled cabinet 24
Interior upper top surface, controller 242 are located at the interior left part of temperature-controlled cabinet 24, and distribution box 244 is located at the interior right part of temperature-controlled cabinet 24；
Temperature sensor is equipped on the left of the upper top surface of temperature-controlled cabinet 24；Control panel 25 is located at the leading flank of digestion instrument 2, control plane
25 upper left corner of plate is equipped with temperature display 251, and the lower left corner is from left to right equipped with+heat button 252 and cooling button 253, and right side is set
There is device to switch 254, fixator 27 is located at the interior half height of digestion instrument 2, and liquid outlet 28 is located at digestion instrument 2
At 1/5th under right side, liquid outlet 28 is equipped with control valve 281, and attaching plug 29 is located at the right side bottom of digestion instrument 2
End；Controller 242 is connect with temperature sensor 243, heat block 241, sprinkling ring 221, vibrations ring 231 and control panel 25, temperature
Degree sensor 243 is connect with autocontrol valve 211, distribution box 244 and temperature sensor 243, heat block 241, spray ring 221,
Vibrations ring 231, control panel 25 and autocontrol valve 211 connect, this digestion instrument 2 by the two-stage stage add in digestion solution a and
Digestion solution b effectively raises resolution effect 27%, high degree of automation.And reaction cup 26 can be made heated using oil bath heating
Uniformly, temperature will not bad student's variation and when going out liquid, it is ensured that goes out the stabilization accuracy of liquid, the sprinkling cooperation shake of ring 221 after resolution
Rotating ring 231 and soil sample disperser 232 can make soil sample and digestion solution a mixes abundant, shortening digestion time 17%, raising resolution effect
Rate 21%.
As shown in figure 4, automatic volume fixing device 3 includes telescopic rod a 31, control cabinet 32, connecting rod 33, titration case 34, titration
Pipe 35, telescopic rod b36, beam receiver 37, light-beam transmitter 38 and geometrical clamp 39, telescopic rod a 31 are located at automatic volume fixing device
3 upper right side, control cabinet 32 are connect with the upper top of telescopic rod a 31, and connecting rod 33 is connect with the left side of control cabinet 32, titration
Case 34 is connect with the left side of connecting rod 33, and buret 35 is connected to the bottom surface center of titration case 34, and telescopic rod b 36 is located at certainly
The upper left side of dynamic volume fixing device 3, beam receiver 37 are located on the madial wall of telescopic rod b 36, and light-beam transmitter 38 is located at flexible
On the madial wall of bar a 31, geometrical clamp 39 is located on the inner wall of automatic volume fixing device 3 at 1/3rd height, control cabinet 32 and light
Beam transmitter 38, beam receiver 37 and titration case 34 connect, and traditional constant volume is all by manually being operated, this inevitably meeting
Certain error is generated, by the cooperation of light-beam transmitter 38 and beam receiver 37, analysis and Control is handled by control cabinet 32 and is dripped
Determine case 34 and carry out automation titration, compared to manual operation error smaller, constant volume accuracy higher significantly reduces constant volume error
Rate, the cooperation of simultaneous retractable bar a 31 and telescopic rod b 36 can be according to the liquid level for requiring constant volume different.
Embodiment 3
The method of 12 kinds of metallic elements, includes the following steps in a kind of measure soils and sediments：
S1:Soil to be measured is acquired, soil to be measured is put into the feed inlet 14 of soil treatment device 1, by fan 11, is air-dried
The cooperation of plate 12 and five wind gathering plates, which is realized, air-dries processing, then drive sorting plate 13 by vibrating motor 131 and pass through baffle 134
And gravity, soil is sorted；It is 20 minutes to air-dry processing time, and the sorting process time is 15 minutes；
S2:It, will treated that soil sample is put into that grinder was crushed to 180 mesh sieve, and was put into drying after soil sample acquisition process
It is sealed in the sample bottle of sealing；
S3:The soil sample 1-3g in sample bottle is taken to be positioned in the soil sample case 23 of digestion instrument 2, is shaken by shaking ring 231
Soil sample disperser 232 falls into soil sample in 50ml polytetrafluoroethylene beakers, and it is 5 times to add in number, shakes time interval every time and is
80s, while mixed by spraying digestion solution a sprinkling and soil sample of the ring 221 by 30ml, spraying time is 10 minutes, mixing periods,
Oil bath heating is controlled by control panel 25 and temperature-controlled cabinet 24, by temperature control at 100 DEG C, constant temperature after twenty minutes, stops
Heating, when mixed solution is cooled to 40 °, autocontrol valve 211 receives the data information of temperature sensor 243, controls dropper
The digestion solution b of 15ml, a certain temperature between subsequent temperature controller 24 is slowly warming up to 140 DEG C automatically are instilled into the mixed solution
Constant temperature 25 minutes are spent, after, it opens control valve 281 and collects digestion solution, carry out in next step；
S4:Acid is caught up with then to carry out dilution constant volume in next step to digestion solution residue 10ml；
S5:Standing is cooled to room temperature, and is poured into 50ml volumetric flasks, and volumetric flask three is at least cleaned with test water before pouring into
It is secondary, finally volumetric flask is fixed on automatic volume fixing device 3, by the cooperation of light-beam transmitter 38 and beam receiver 37, is led to
It crosses the control titration case 34 of control cabinet 32 and 50ml full scales is settled to it；
S6:After staticly settling 30 minutes, 12ml supernatants 5300r/min centrifugations 6 minutes in 15ml centrifuge tubes are taken, then
Carry out next step icp ms detection；
S7:Sample liquid is put into icp ms, the experiment ginseng of icp ms
Number is：Plasma flow amount 15L/min；Secondary air amount：0.4L/min；Nebulizer flow 0.7L/min；Sampling volume：
2.0mL/min；Power：1500W；Lamp current 25mA；Carrier gas flux 350mL/min；Shield gas flow amount 700mL/min；Detect wave
Long selected as 243.6nm；
S8:According to the soil sample weight weighed and detect that the concentration of digestion solution calculates 12 kinds of metallic elements in pedotheque
Content.
Digestion solution a is that the concentrated nitric acid of 1 volume and the concentrated hydrochloric acid of 3 volumes mix.
Digestion solution b is that the nitrous acid of 2 volumes and the concentrated hydrochloric acid of 3 volumes mix.
As illustrated in fig. 1 and 2, soil treatment device 1 includes fan 11, air-dries plate 12, sorting plate 13, feed inlet 14, discharging
Mouth 15, pedestal 16 and power connection 17；Fan 11 is equipped with 2, respectively positioned at the internal both sides in the left and right of soil treatment device 1；Wind
Dry plate 12 is equipped with 4, and cross interval is located on both sides fan 11 from top to bottom, and angle of inclination is 10 °, air-dries plate 12 and goes to the bottom
Face is equipped with wind gathering plate a 121, wind gathering plate b 122, wind gathering plate c 123, wind gathering plate d 124 and wind gathering plate e 125, wind gathering plate a
121st, air-permeating hole, wind gathering plate a are additionally provided on wind gathering plate b 122, wind gathering plate c 123, wind gathering plate d 124 and wind gathering plate e 125
Air-permeating hole b 1221 there are two being set on air-permeating hole a 1211 there are two being set on 121, wind gathering plate b 122, wind gathering plate c 123 to be equipped with
Air-permeating hole e there are two being set on air-permeating hole d 1241 there are two being set on air-permeating hole c 1231, wind gathering plate d 124, wind gathering plate e 125
1251, two air-permeating holes between each two wind gathering plate are staggeredly located, air-permeating hole a 1211, air-permeating hole c 1231 and air-permeating hole e
1251 positions correspond to, and air-permeating hole b 1221 is corresponding with 1241 positions of air-permeating hole d, by the setting of wind gathering plate can effectively by
Behind wind concentration passes to wind level-one grade on air-dried plate 12, by air-permeating hole, avoid front wind gathering plate block behind, drop
Inefficient fruit.Sorting plate 13 is located at 1 inside bottom surface of soil treatment device, and angle of inclination is 12 °, and sorting plate 13 is equipped with 8 baffles
134th, the upper top surface of sorting plate 13 is equally distributed on, sorting plate 13 passes through stent a 132 and stent b 133 and vibrating motor 131
Connection, discharge port 15 are located on the left of the upper top surface of soil treatment device 1, and discharge port 15 is located at the bottom surface of soil treatment device 1
Right side, discharge port 15 are equipped with control valve 151, and pedestal 16 is fixedly connected on the bottom surface center of soil treatment device 1,
Power connection 17 is connected to the left side lower end of soil treatment device 1, effectively acts on air-dried plate by soil sample gravity and wind-force
12 and the effect level-one grade of fan 11 and five wind gathering plates is coordinated to slide air-dry, then shake by the left and right of sorting plate 13, and
Cooperation baffle 134 sorts soil, prevents metal particulate from being had an impact to Soil K+adsorption, influences the accuracy of data.
As shown in figure 3, digestion instrument 2 includes B liquid cases 21, A liquid cases 22, soil sample case 23, temperature-controlled cabinet 24, control panel
25th, reaction cup 26, fixator 27, liquid outlet 28 and attaching plug 29, B liquid cases 21 are located at the upper left corner of digestion instrument 2, B liquid cases
21 bottom surface right end is equipped with dropper 212, and dropper 212 is equipped with autocontrol valve 211, is equipped among the upper top surface of B liquid cases 21
Filling opening B 213；Filling opening A 222 is equipped in A liquid cases 22 among top surface, pipeline and sprinkling are connected on the left of 22 bottom surface of A liquid cases
Ring 221 connects, and sprinkling ring 221 is located at the upper inside wall of reaction cup 26；Soil sample case 23 is between A liquid cases 22 and B liquid cases 21, soil
23 bottom surface center of sample case is connected to soil sample disperser 232, and 232 bottom surface of soil sample disperser is evenly distributed with Process, soil sample
Disperser 232 is equipped with vibrations ring 231 with 23 junction of soil sample case；Temperature-controlled cabinet 24 is located at the interior bottom surface of digestion instrument 2, temperature
Degree control cabinet 24 is internally provided with heat block 241, controller 242 and distribution box 244, and heat block 241 is located at temperature-controlled cabinet 24
Interior upper top surface, controller 242 are located at the interior left part of temperature-controlled cabinet 24, and distribution box 244 is located at the interior right part of temperature-controlled cabinet 24；
Temperature sensor is equipped on the left of the upper top surface of temperature-controlled cabinet 24；Control panel 25 is located at the leading flank of digestion instrument 2, control plane
25 upper left corner of plate is equipped with temperature display 251, and the lower left corner is from left to right equipped with+heat button 252 and cooling button 253, and right side is set
There is device to switch 254, fixator 27 is located at the interior half height of digestion instrument 2, and liquid outlet 28 is located at digestion instrument 2
At 1/5th under right side, liquid outlet 28 is equipped with control valve 281, and attaching plug 29 is located at the right side bottom of digestion instrument 2
End；Controller 242 is connect with temperature sensor 243, heat block 241, sprinkling ring 221, vibrations ring 231 and control panel 25, temperature
Degree sensor 243 is connect with autocontrol valve 211, distribution box 244 and temperature sensor 243, heat block 241, spray ring 221,
Vibrations ring 231, control panel 25 and autocontrol valve 211 connect, this digestion instrument 2 by the two-stage stage add in digestion solution a and
Digestion solution b effectively raises resolution effect 27%, high degree of automation.And reaction cup 26 can be made heated using oil bath heating
Uniformly, temperature will not bad student's variation and when going out liquid, it is ensured that goes out the stabilization accuracy of liquid, the sprinkling cooperation shake of ring 221 after resolution
Rotating ring 231 and soil sample disperser 232 can make soil sample and digestion solution a mixes abundant, shortening digestion time 17%, raising resolution effect
Rate 21%.
As shown in figure 4, automatic volume fixing device 3 includes telescopic rod a 31, control cabinet 32, connecting rod 33, titration case 34, titration
Pipe 35, telescopic rod b 36, beam receiver 37, light-beam transmitter 38 and geometrical clamp 39, telescopic rod a 31 are located at automatic constant volume dress
3 upper right side is put, control cabinet 32 is connect with the upper top of telescopic rod a 31, and connecting rod 33 is connect with the left side of control cabinet 32, drop
The left side for determining case 34 with connecting rod 33 is connect, and buret 35 is connected to the bottom surface center of titration case 34, and telescopic rod b 36 is located at
The upper left side of automatic volume fixing device 3, beam receiver 37 are located on the madial wall of telescopic rod b 36, and light-beam transmitter 38, which is located at, to be stretched
On the madial wall of contracting bar a 31, geometrical clamp 39 is located on the inner wall of automatic volume fixing device 3 1/3rd height and locates, control cabinet 32 and
Light-beam transmitter 38, beam receiver 37 and titration case 34 connect, and traditional constant volume is all by manually being operated, this is inevitably
Certain error can be generated, by the cooperation of light-beam transmitter 38 and beam receiver 37, analysis and Control is handled by control cabinet 32
Titration case 34 carries out automation titration, and compared to manual operation error smaller, constant volume accuracy higher significantly reduces constant volume mistake
Accidentally rate, the cooperation of simultaneous retractable bar a 31 and telescopic rod b 36 can be according to the liquid level for requiring constant volume different.
Getting off, we make the method for the present invention verification by experiment：
A) preparation of standard solution：Hybrid standard stock solution is taken, concentration point is diluted to step by step with 0.5% salpeter solution
Not Wei 0.1,0.2,0.5,1.0,10.0,20.0,50.0,100.0ppb standard working solution；
B) sample liquid handled using icp ms examination criteria working solution and the method for the present invention；
Interpretation of result：According to the soil sample weight weighed and detect that the concentration of digestion solution calculates chromium arsenic cadmium in pedotheque
The content of lead；
W=cV/1000m
W be soil sample tenor, mg/kg；
C be digestion solution in metal concentration, μ g/kg；
V be digestion solution constant volume, mL；
M is the quality for weighing soil, g.
Comparative result is as shown in table 1.
1 filter method of table and centrifugal method Comparative result (mg/Kg)
In the soils and sediments that are detected of the present invention method of metallic element on experimental result without influence, and detection range
Section is narrower, and effect is more accurate.
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
The present invention is described in detail with reference to the foregoing 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 carry out equivalent replacement to which part technical characteristic；And
These modifications are replaced, 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 (9)
- A kind of 1. method for measuring 12 kinds of metallic elements in soils and sediments, which is characterized in that include the following steps：S1:Soil to be measured is acquired, soil to be measured is put into the advanced sector-style dry-cure of soil treatment device (1), then carry out at sorting Reason；The air-dried processing time is 10-20 minutes, and the sorting process time is 5-15 minutes；S2:It, will treated that soil sample is put into that grinder was crushed to 180 mesh sieve, and was put into dry sealing after soil sample acquisition process Sample bottle in be sealed；S3:The soil sample 1-3g in sample bottle is taken to be positioned in the soil sample case of digestion instrument (2), passes through soil sample disperser (232) point Repeatedly soil sample is fallen into 50ml polytetrafluoroethylene beakers, while sprayed the digestion solution a of 25-30ml by spraying ring (221) With soil sample mix, spraying time be 10 minutes, mixing periods, by oil bath heating by temperature control between 80 DEG C -100 DEG C certain One thermostatic 20 minutes；When mixed solution is cooled to 40 °, then instilled into the mixed solution by autocontrol valve (211) The digestion solution b of 10-15ml, and a certain thermostatic 25 minutes between being slowly warming up to 120 DEG C -140 DEG C；S4:Acid is caught up with then to carry out dilution constant volume in next step to digestion solution residue 8ml-10ml；S5:Standing is cooled to room temperature, and is poured into 50ml volumetric flasks, and at least cleans volumetric flask three times with test water, is finally used Automatic volume fixing device (3) is settled to 50ml full scales；S6:After staticly settling 20-30 minutes, 9-12ml supernatants 5300r/min in 15ml centrifuge tubes is taken to centrifuge 4-6 minutes, Then next step icp ms detection is carried out；S7:Sample liquid is put into icp ms, the experiment ginseng of the icp ms Number is：Plasma flow amount 15L/min；Secondary air amount：0.4L/min；Nebulizer flow 0.7L/min；Sampling volume： 2.0mL/min；Power：1500W；Lamp current 25mA；Carrier gas flux 350mL/min；Shield gas flow amount 700mL/min；Detect wave Long selected as 243.6nm；S8:According to the soil sample weight weighed and detect that the concentration of digestion solution calculates in pedotheque containing for 12 kinds of metallic elements Amount.
- 2. according to the method for 12 kinds of metallic elements in a kind of measure soils and sediments described in claim 1, feature exists In digestion solution first shifts constant volume in the S5, then supernatant is taken to centrifuge.
- 3. according to the method for 12 kinds of metallic elements in a kind of measure soils and sediments described in claim 1, feature exists In digestion solution first is shifted constant volume, after staticly settling, supernatant is taken to centrifuge.
- 4. according to the method for 12 kinds of metallic elements in a kind of measure soils and sediments described in claim 1, feature exists In in the S3 steps, soil sample disperser (232) is 5 times by shaking ring (231) vibrations to add in number, shakes the time every time Between be divided into 80s.
- 5. according to the method for 12 kinds of metallic elements in a kind of measure soils and sediments described in claim 1, feature exists In the digestion solution a is that the concentrated nitric acid of 1 volume and the concentrated hydrochloric acid of 3 volumes mix.
- 6. according to the method for 12 kinds of metallic elements in a kind of measure soils and sediments described in claim 1, feature exists In the digestion solution b is that the nitrous acid of 2 volumes and the concentrated hydrochloric acid of 3 volumes mix.
- 7. according to the method for 12 kinds of metallic elements in a kind of measure soils and sediments described in claim 1, feature exists In the soil treatment device (1) includes fan (11), air-dried plate (12), sorting plate (13), feed inlet (14), discharge port (15), pedestal (16) and power connection (17)；The fan (11) is equipped with 2, respectively positioned at the soil treatment device (1) The internal both sides in left and right；Equipped with 4, cross interval is located on both sides fan (11) the air-dried plate (12) from top to bottom, is inclined Rake angle is 10 °, and air-dried plate (12) bottom surface is equipped with wind gathering plate a (121), wind gathering plate b (122), wind gathering plate c (123), gathers Aerofoil d (124) and wind gathering plate e (125), the sorting plate (13) are located at the internal bottom surface of the soil treatment device (1), tilt Angle is 12 °, the sorting plate (13) equipped with 8 baffles (134), be equally distributed on the upper top surface of the sorting plate (13), institute It states sorting plate (13) to connect with vibrating motor (131) by stent a (132) and stent b (133), the discharge port (15) is located at On the left of the upper top surface of the soil treatment device (1), the discharge port (15) is positioned at the bottom surface of the soil treatment device (1) Right side, the discharge port (15) are equipped with control valve (151), and the pedestal (16) is fixedly connected on the soil treatment device (1) bottom surface center, the power connection (17) are connected to the left side lower end of the soil treatment device (1).
- 8. according to the method for 12 kinds of metallic elements in a kind of measure soils and sediments described in claim 6, feature exists In on the wind gathering plate a (121), wind gathering plate b (122), wind gathering plate c (123), wind gathering plate d (124) and wind gathering plate e (125) also Equipped with air-permeating hole, set on the wind gathering plate a (121) there are two air-permeating hole a (1211), set on the wind gathering plate b (122) there are two Air-permeating hole b (1221), the wind gathering plate c (123) are equipped with air-permeating hole c (1231), set on the wind gathering plate d (124) there are two Air-permeating hole d (1241) is set on the wind gathering plate e (125) there are two air-permeating hole e (1251), two between each two wind gathering plate Air-permeating hole is staggeredly located, and the air-permeating hole a (1211), air-permeating hole c (1231) are corresponding with air-permeating hole e (1251) position, described Air holes b (1221) is corresponding with air-permeating hole d (1241) position.
- 9. according to the method for 12 kinds of metallic elements in a kind of measure soils and sediments described in claim 1, feature exists In the digestion instrument (2) includes B liquid cases (21), A liquid cases (22), soil sample case (23), temperature-controlled cabinet (24), control panel (25), reaction cup (26), fixator (27), liquid outlet (28) and attaching plug (29), the B liquid cases (21) are positioned at the resolution The upper left corner of device (2), the bottom surface right end of the B liquid cases (21) are equipped with dropper (212), and the dropper (212) is equipped with certainly Dynamic control valve (211), the upper top surface centre of the B liquid cases (21) are equipped with filling opening B (213)；On the A liquid cases (22) in top surface Between be equipped with filling opening A (222), pipeline is connected on the left of A liquid cases (22) bottom surface and is connect with spraying ring (221), the sprinkling Ring (221) is positioned at the upper inside wall of the reaction cup (26)；The soil sample case (23) is positioned at the A liquid cases (22) and B liquid cases (21) between, soil sample case (23) the bottom surface center is connected to soil sample disperser (232), soil sample disperser (232) bottom Face is evenly distributed with Process, and the soil sample disperser (232) is equipped with vibrations ring (231) with soil sample case (23) junction；Institute Interior bottom surface of the temperature-controlled cabinet (24) positioned at the digestion instrument (2) is stated, the temperature-controlled cabinet (24) is internally provided with heating Block (241), controller (242) and distribution box (244), the heat block (241) positioned at the temperature-controlled cabinet (24) it is interior on Top surface, the controller (242) is positioned at the interior left part of the temperature-controlled cabinet (24), and the distribution box (244) is positioned at the temperature Spend the interior right part of control cabinet (24)；Temperature sensor is equipped on the left of the upper top surface of the temperature-controlled cabinet (24)；The control plane Plate (25) positioned at the digestion instrument (2) leading flank, control panel (25) upper left corner be equipped with temperature display (251), The lower left corner is from left to right equipped with+heat button (252) and cooling button (253), and right side is equipped with device and switchs (254), the fixation Device (27) is at the interior half height of the digestion instrument (2), and the liquid outlet (28) is positioned at the digestion instrument (2) Right side under at 1/5th, the liquid outlet (28) is equipped with control valve (281), and the attaching plug (29) is positioned at described The right side bottom end of digestion instrument (2)；The controller (242) and the temperature sensor (243), heat block (241), sprinkling Ring (221), vibrations ring (231) and control panel (25) connection, the temperature sensor (243) and the autocontrol valve (211) it connects, the distribution box (244) and the temperature sensor (243), heat block (241), sprinkling ring (221), vibrations ring (231), control panel (25) and autocontrol valve (211) connection.
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Cited By (8)
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| CN108507821A (en) * | 2018-06-20 | 2018-09-07 | 温州新鸿检测技术有限公司 | A kind of soil pollution detection method |
| CN109115577A (en) * | 2018-09-29 | 2019-01-01 | 中国地质大学（武汉） | A kind of portable soil heavy metal leaching device and leaching method based on STM32 |
| CN109470535A (en) * | 2018-11-12 | 2019-03-15 | 崔维佳 | The Microwave Pretreatment device and microwave method for preprocessing of heavy metal-polluted soil detection |
| CN109884036A (en) * | 2019-03-08 | 2019-06-14 | 国家硅材料深加工产品质量监督检验中心东海研究院 | A kind of sampling method using microelement in inductive coupling plasma emission spectrograph measurement quartz |
| CN111948007A (en) * | 2020-09-17 | 2020-11-17 | 中国环境监测总站 | Method for measuring various metal elements in soil |
| CN111982636A (en) * | 2020-09-17 | 2020-11-24 | 中国环境监测总站 | Sample processing method and device for determining metal elements in soil |
| CN112730020A (en) * | 2020-12-21 | 2021-04-30 | 广东贝源检测技术股份有限公司 | Soil heavy metal digestion device |
| CN115586061A (en) * | 2022-10-12 | 2023-01-10 | 生态环境部南京环境科学研究所 | Soil sample pretreatment equipment and method for soil cadmium detection |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108507821A (en) * | 2018-06-20 | 2018-09-07 | 温州新鸿检测技术有限公司 | A kind of soil pollution detection method |
| CN109115577A (en) * | 2018-09-29 | 2019-01-01 | 中国地质大学（武汉） | A kind of portable soil heavy metal leaching device and leaching method based on STM32 |
| CN109470535A (en) * | 2018-11-12 | 2019-03-15 | 崔维佳 | The Microwave Pretreatment device and microwave method for preprocessing of heavy metal-polluted soil detection |
| CN109470535B (en) * | 2018-11-12 | 2021-06-01 | 吉林小德川农业科技有限公司 | Microwave pretreatment device and microwave pretreatment method for soil heavy metal detection |
| CN109884036A (en) * | 2019-03-08 | 2019-06-14 | 国家硅材料深加工产品质量监督检验中心东海研究院 | A kind of sampling method using microelement in inductive coupling plasma emission spectrograph measurement quartz |
| CN111948007A (en) * | 2020-09-17 | 2020-11-17 | 中国环境监测总站 | Method for measuring various metal elements in soil |
| CN111982636A (en) * | 2020-09-17 | 2020-11-24 | 中国环境监测总站 | Sample processing method and device for determining metal elements in soil |
| CN111948007B (en) * | 2020-09-17 | 2023-04-07 | 中国环境监测总站 | Method for measuring various metal elements in soil |
| CN112730020A (en) * | 2020-12-21 | 2021-04-30 | 广东贝源检测技术股份有限公司 | Soil heavy metal digestion device |
| CN115586061A (en) * | 2022-10-12 | 2023-01-10 | 生态环境部南京环境科学研究所 | Soil sample pretreatment equipment and method for soil cadmium detection |
| CN115586061B (en) * | 2022-10-12 | 2023-04-21 | 生态环境部南京环境科学研究所 | Soil sample pretreatment equipment and method for detecting soil cadmium |
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