CN110487611A - A kind of pretreatment unit and preprocess method measuring Mercury In Soil content - Google Patents

A kind of pretreatment unit and preprocess method measuring Mercury In Soil content Download PDF

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Publication number
CN110487611A
CN110487611A CN201910848481.4A CN201910848481A CN110487611A CN 110487611 A CN110487611 A CN 110487611A CN 201910848481 A CN201910848481 A CN 201910848481A CN 110487611 A CN110487611 A CN 110487611A
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sample cell
pedestal
added dropwise
head
pipe holder
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CN110487611B (en
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冯艳红
张亚
王国庆
郑丽萍
应蓉蓉
杜俊洋
李勖之
孙丽
李敏
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Nanjing Institute of Environmental Sciences MEE
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Nanjing Institute of Environmental Sciences MEE
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    • 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

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  • Physics & Mathematics (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Sampling And Sample Adjustment (AREA)
  • Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)

Abstract

The invention discloses a kind of pretreatment units and preprocess method for measuring Mercury In Soil content, including the sample tube assembly for placing pedotheque, for adding the chemicals dosing plant of super water and reagent into sample, shaking device for being shaken up to the sample cell after adding medicine, and the decatize heating device for being heated;The chemicals dosing plant includes dosing pedestal and Dropping feeder, slide assemblies are provided on the dosing pedestal, the Dropping feeder includes Dropping feeder ontology and head is added dropwise, and the dropwise addition head is arranged on slide assemblies and provides super water, medicament and power by Dropping feeder ontology;Reasonable integral structure of the present invention, the degree of automation are higher.

Description

A kind of pretreatment unit and preprocess method measuring Mercury In Soil content
Technical field
The present invention relates to Soil K+adsorption technical fields, and in particular to a kind of pretreatment unit for measuring Mercury In Soil content And preprocess method.
Background technique
When carrying out analysis measurement to the heavy metal in soil, the pretreatment of sample is crucial.Pretreatment will be determined directly Concentrations, accuracy and the precision of entire analysis method.During entire test and analyze, probably there is 60% analysis Error derives from sample pretreatment, and non-instrument itself.
When currently total heavy metal content is measured in soil, the preprocess method used is wet process and two kinds of dry method Method.It is easily operated since wet digestion condition is simple, and the more common pre-treating method in laboratory at present.But it is opposite In the measurement of mercury in soils element, is easily decomposed since mercury element is heated, be not particularly suited for traditional wet digestion and carry out in advance Processing.At present when being measured to Mercury In Soil content, it is chiefly used in Boiling bath method, but since its operation is relatively complicated, Whole process is substantially manual operation process, therefore has biggish fault rate.Do not occur high degree of automation also at present For the pretreatment unit of measurement soil total mercury content.
Summary of the invention
In view of the above problems, one aspect of the present invention provides a kind of measurement Mercury In Soil of high degree of automation The pretreatment unit of content;Another aspect of the present invention proposes a kind of preprocess method for measuring Mercury In Soil content.
In order to solve the above technical problems, the technical scheme is that a kind of pretreatment for measuring Mercury In Soil content Device is used including the sample tube assembly for placing pedotheque for adding the chemicals dosing plant of super water and reagent into sample Decatize heating device in the shaking device shaken up to the sample cell after adding medicine, and for being heated;
The sample cell includes sample cell and pipe holder, the sample cell can activity be placed on pipe holder;Sample cell Using 50mL color-comparison tube;The chemicals dosing plant includes dosing pedestal and Dropping feeder, is provided with cunning on the dosing pedestal Dynamic component, the Dropping feeder include Dropping feeder ontology and head are added dropwise, and the dropwise addition head is arranged on slide assemblies and by dripping Feeder apparatus ontology provides super water, medicament and power;The medicament includes the first medicament and second medicament, and first medicament is The chloroazotic acid of 1:1, the K that the second medicament is 5%2Cr2O7Solution.
Further, further include device pedestal, be provided with linear guide on described device pedestal;The chemicals dosing plant, shake Dynamic device, decatize heating device are successively set on device pedestal from left to right, and slide unit is equipped in linear guide;Utilize device Chemicals dosing plant, shaking device, decatize heating device are once arranged pedestal, in preprocessing process, when practical operation more just It is prompt;Meanwhile the linear guide and slide unit of setting can effectively realize automation control, considerably reduce the labor of staff Momentum.
Further, the dosing pedestal is movably arranged on the left of device pedestal by mounting rack, and it includes being added dropwise that head, which is added dropwise, Head cavity body, the first inlet, the second inlet, third inlet, cylinder valve;It is added dropwise at the liquid droping port of head cavity body lower end and is provided with Internal plug;Hollow piston rod is provided in the cylinder valve;
First inlet, the second inlet, third inlet are connected to dropwise addition head cavity body respectively, and are respectively used to pass Defeated first medicament, second medicament, super water;Head cavity body upper end, and hollow piston rod and internal plug is being added dropwise in the cylinder valve setting Connection, internal plug are used to close the liquid droping port that head cavity body lower end is added dropwise;And internal plug and liquid droping port contact position are provided with washer; It head is added dropwise is internally provided with three inlets and can be realized super water, the first medicament, second medicament and dropwise addition is separated and independently performed;Simultaneously The cylinder valve of setting can further guarantee the leakproofness that head is added dropwise and selectable carry out dropwise operation.
Further, the shaking device includes mounting bracket, the first telescopic device and shaking assembly;The installation branch Frame is movably arranged on device pedestal, and the shaking assembly is arranged by first telescopic device on mounting bracket top;Benefit With
Locked groove is provided in the left and right end side surface of pipe holder;
The shaking assembly includes mounting base, vibrating motor, oscillating plate, connecting spring, electric mortise lock;The mounting base is door Character form structure, mounting base are mounted on the first telescopic device lower end;The vibrating motor is arranged in mounting base;The oscillating plate has Two, two oscillating plates pass through two connecting springs respectively and are mounted on left and right end inside mounting base;The lock tongue energy of the electric mortise lock It is enough inserted into the locked groove;It can be realized pipe holder by electric mortise lock, locked groove and be movably arranged on oscillating plate, and then realize and pass through Vibrating motor carries out the sample cell on pipe holder to shake up processing.
Further, the decatize heating device includes including outer protection shell, internal protection shell, the second flexible dress It sets and steam generation facility;
The outer protection shell is mounted on device pedestal, and the internal protection shell passes through second telescopic device It is arranged and is provided with conduit/spray assembly in external protective shell body inner tip, and on internal protection enclosure interior side;It is described to lead Pipe/spray assembly is using the stainless steel tube for being uniformly provided with stomata on tube wall, and conduit/spray assembly and steam generation facility connect It connects;Resolution processing can be carried out to sample to be tested by steam generation facility, inside and outside two protective shell bodies can be further Guarantee the safety when clearing up processing.
Further, the decatize heating device further includes steam condenser, and the steam condenser setting is protected in outside Enclosure interior is protected, steam condenser is connect by conduction pipe with internal protection enclosure interior top;Steam condenser can be into one Step to treated, steam is handled, the heat of steam is converted, steam direct emission can be effectively prevented from and made At accident.
Further, utilize described device measurement Mercury In Soil content preprocess method, which is characterized in that including with Lower step:
Step 1: 0.5g pedotheque to be measured is placed in sample cell, sample cell is placed on pipe holder;Then will Pipe holder be placed on dosing pedestal by be added dropwise head the super water of a few drops are added dropwise into sample cell will be after soil to be measured soaks;Xiang Run again The chloroazotic acid of 10mL1:1 is added in soil after wet;It jumps a queue;
Step 2: pipe holder is placed on slide unit, is slid into immediately below shaking device, is adjusted by the first telescopic device Shaking assembly moves down, then will be in the lock tongue insertion locked groove of electric mortise lock;The first telescopic device is adjusted to rise so that pipe holder is outstanding It after sky, opens vibrating motor and sample cell is carried out to shake up processing, specifically shaking up the time is 5~15min;It is then shut off vibration electricity Machine, closes lock tongue after pipe holder is placed on slide unit by the first telescopic device, then adjusts the rising of the first telescopic device To initial position;
Step 3: pipe holder is slid into immediately below protection shell by slide unit, by the second telescopic device by protective shell Body is dropped to be contacted with device pedestal;It opens steam generation facility and makes steam persistently to sample cell using conduit/spray assembly Heat 1.5h after, steam off generating device and will using the second telescopic device by protect shell restore to initial position;It is cooling After 20~30min;
Step 4: sliding into initial position for pipe holder using slide unit, and then pipe holder is placed on dosing pedestal and is led to It crosses dropwise addition head and 1~2 drop K is added dropwise into sample cell2Cr2O7Solution;Then super water is added into sample cell using dropwise addition head to be settled to After the graticule of sample cell, repeat to stand after step 2 is shaken up.
Compared with prior art, beneficial effects of the present invention: reasonable integral structure of the present invention, the degree of automation is higher, energy Enough amounts of labour for effectively mitigating staff in laboratory;Also, the present invention is cleared up using steam heating, entire to clear up Time is shorter, and can be realized multiple groups sample using apparatus of the present invention while carrying out;It can effectively be kept away using chemicals dosing plant Exempt from staff to contact in preprocessing process with reagent, efficiently avoids corrosive reagent bring risk; The measurement for carrying out mercury element after handling using pretreatment unit of the present invention and method sample has higher accuracy, all It is obtained in error range in a sample guarantee value, is suitble to large-scale popularization.
Detailed description of the invention
Fig. 1 is schematic diagram of internal structure of the invention;
Fig. 2 is external structure schematic diagram of the invention;
Fig. 3 is the structural schematic diagram of bracket of the invention;
Fig. 4 is the structural schematic diagram of shaking assembly of the invention;
Fig. 5 is the structural schematic diagram of dropwise addition head of the invention;
Wherein, 1- sample tube assembly, 11- sample cell, 12- pipe holder, 120- locked groove, 2- chemicals dosing plant, 21- dosing bottom Head is added dropwise in seat, 210- slide assemblies, 22- Dropping feeder, 221-, head cavity body, the first inlet of 2211-, 2212- is added dropwise in 2210- Second inlet, 2213- third inlet, 2214- internal plug, 2215- washer, 3- shaking device, 31- mounting bracket, 32- first Telescopic device, 33- and shaking assembly, 331- mounting base, 332- vibrating motor, 333- oscillating plate, 334- connecting spring, 335- Electric mortise lock, 4- decatize heating device, 41- outer protection shell, 42- internal protection shell, 420- conduit/spray assembly, 43- Two telescopic devices, 44- steam generation facility, 5- device pedestal, 51- linear guide, 6- cylinder valve, 61- hollow piston rod.
Specific embodiment
Embodiment: a kind of pretreatment unit of measurement Mercury In Soil content as shown in Figure 1, 2, including for placing soil The sample tube assembly 1 of earth sample, for adding the chemicals dosing plant 2 of super water and reagent into sample, for the sample after adding medicine The shaking device 3 that quality control 1 is shaken up, the decatize heating device 4 for being handled;And for installing chemicals dosing plant 2, shake The device pedestal 5 of dynamic device 3, heating device 4;It is provided with linear guide 51 on device pedestal 5, cunning is installed in linear guide 51 Platform 52;
Sample cell 1 include sample cell 11 and pipe holder 12, sample cell 11 can activity be placed on pipe holder 12;Sample cell 11 use 50mL color-comparison tube;
Chemicals dosing plant 2 includes dosing pedestal 21 and Dropping feeder 22, is provided with slide assemblies 210 on dosing pedestal 21, is dripped Feeder apparatus 22 includes Dropping feeder ontology and head 221 is added dropwise, and head 221 is added dropwise and is arranged on slide assemblies 210 and by Dropping feeder Ontology provides super water, medicament and power;
Dropping feeder ontology includes liquid reserve tank and metering pump;Medicament includes the first medicament and second medicament, and the first medicament is The chloroazotic acid of 1:1, the K that second medicament is 5%2Cr2O7Solution;Liquid reserve tank includes the first liquid reserve tank, the second liquid reserve tank and third liquid storage Case, and the first liquid reserve tank, the second liquid reserve tank and third liquid reserve tank are respectively used to place the first medicament, second medicament and super water;
As shown in Figure 1,5, dosing pedestal 21 is movably arranged on 5 left side of device pedestal by mounting rack, and head 221 is added dropwise and includes Head cavity body 2210, the first inlet 2211, the second inlet 2212, third inlet 2213, cylinder valve 6 is added dropwise;Head is added dropwise Internal plug 2214 is provided at 2210 lower end liquid droping port of cavity;Hollow piston rod 61 is provided in cylinder valve 6;
First inlet 2211, the second inlet 2212, third inlet 2213 are connected to dropwise addition head cavity body 2210 respectively, And it is connect respectively with the first liquid reserve tank, the second liquid reserve tank and third liquid reserve tank by independent metering pump;The setting of cylinder valve 6 exists 2210 upper end of head cavity body is added dropwise, and hollow piston rod 61 is connect with internal plug 2214, internal plug 2214 is used for dropwise addition head cavity body 2210 The liquid droping port of lower end is closed;And internal plug 2214 and liquid droping port contact position are provided with washer 2215;
Shaking device 3 includes mounting bracket 31, the first telescopic device 32 and shaking assembly 33;31 activity of mounting bracket is set It sets on device pedestal 5, shaking assembly 33 is arranged by the first telescopic device 32 on 31 top of mounting bracket;
As shown in figure 3, being provided with locked groove 120 in the left and right end side surface of pipe holder 12;
As shown in Fig. 1,4, shaking assembly 33 includes mounting base 331, vibrating motor 332, oscillating plate 333, connecting spring 334, electric mortise lock 335;Mounting base 331 is door word structure, and mounting base 331 is mounted on 32 lower end of the first telescopic device;Vibrating motor 332 are arranged in mounting base 331;There are two oscillating plates 333, and two oscillating plates 333 are installed by two connecting springs 334 respectively At the 331 left and right end in inside of mounting base;The lock tongue of electric mortise lock 335 is inserted into locked groove 120;
Decatize heating device 4 includes including outer protection shell 41, internal protection shell 42, the second telescopic device 43 and steaming Vapour generating device 44;
Outer protection shell 41 is mounted on device pedestal 5, and internal protection shell 42 is arranged by the second telescopic device 43 Conduit/spray assembly 420 is provided in external 41 inner tip of protective shell body, and in 42 inner side of internal protection shell;It leads Pipe/spray assembly 420 uses the stainless steel tube that stomata is uniformly provided on tube wall, and conduit/spray assembly 420 and steam generation Device 44 connects;
Wherein, decatize heating device 4 further includes steam condenser, and the steam condenser is arranged in external protective shell body 41 Inside, steam condenser are connect by conduction pipe with 42 inner tip of internal protection shell;
It should be understood that PLC controller of the present embodiment using the model GCAN-PLC extensively produced at science and technology, and this Device needs are connect with external power supply.
Using the device of the present embodiment to the technique of the soil pretreatment of total mercury content to be determined, comprising the following steps:
Step 1: 0.5g pedotheque to be measured is placed in sample cell 11, sample cell 11 is placed on pipe holder 12; Then pipe holder 12 is placed on dosing pedestal 21 and a few super water of drop is added dropwise into sample cell 11 by soil to be measured by the way that head 221 is added dropwise After earth wetting;The chloroazotic acid of 10mL1:1 is added into the soil after wetting again;It jumps a queue;
Step 2: pipe holder 12 is placed on slide unit 52, is slid into immediately below shaking device 3, and the first flexible dress is passed through It sets 32 adjusting shaking assemblies 33 to move down, then will be in the lock tongue insertion locked groove 120 of electric mortise lock 335;Adjust the first telescopic device It after 32 rise so that pipe holder 12 is hanging, opens vibrating motor 332 and sample cell 11 is carried out to shake up processing, specifically shaking up the time is 10min;It is then shut off vibrating motor 332, by lock tongue after pipe holder 12 is placed on slide unit 52 by the first telescopic device 32 It closes, then adjusts the first telescopic device 32 and rise to initial position;
Step 3: pipe holder 12 is slid into immediately below protection shell 42 by slide unit 52, passes through the second telescopic device 43 Protection shell 42 is dropped to and is contacted with device pedestal 5;Steam generation facility 44 is opened to make using conduit/spray assembly 420 After steam persistently heats 1.5h to sample cell 11, steam off generating device 44 and will be using the second telescopic device 43 by protective shell Body 42 restores to initial position;After cooling 25min;
Step 4: pipe holder 12 is slid into initial position using slide unit 52, pipe holder 12 is then placed on dosing bottom 2 drop K are added dropwise into sample cell 11 by the way that head 221 is added dropwise on seat 212Cr2O7Solution;Then it utilizes and head 221 is added dropwise to sample cell 11 After the middle super water of addition is settled to the graticule of sample cell 11, repeat to stand after step 2 is shaken up.
Test example: using the present embodiment device and method to tri- kinds of pedotheques of collected ESS-1, ESS-2, ESS-3 ICP-MS is recycled to carry out the measurement of mercury element after being pre-processed.Mercury Determination in sample the result is as follows:
Conclusion: using the present embodiment pretreatment unit and method to mercury member in sample under pedotheque progress pretreatment mode Cellulose content is all in a sample guarantee value error range, as a result, acceptable.

Claims (7)

1. a kind of pretreatment unit for measuring Mercury In Soil content, including the sample tube assembly (1) for placing pedotheque, Shake for adding the chemicals dosing plant (2) of super water and reagent into sample, for being shaken up to the sample cell (1) after adding medicine Dynamic device (3), and the decatize heating device (4) for being heated;
It is characterized in that, the sample cell (1) includes sample cell (11) and pipe holder (12), the sample cell (11) being capable of activity It is placed on pipe holder (12);Sample cell (11) uses 50mL color-comparison tube;
The chemicals dosing plant (2) includes dosing pedestal (21) and Dropping feeder (22), is provided with cunning on the dosing pedestal (21) Dynamic component (210), the Dropping feeder (22) include Dropping feeder ontology and head (221) are added dropwise, dropwise addition head (221) setting Super water, medicament and power are provided on slide assemblies (210) and by Dropping feeder ontology;The medicament include the first medicament and Second medicament, first medicament are the chloroazotic acid of 1:1, the K that the second medicament is 5%2Cr2O7Solution.
2. a kind of pretreatment unit for measuring Mercury In Soil content according to claim 1, which is characterized in that further include Device pedestal (5) is provided with linear guide (51) on described device pedestal (5);The chemicals dosing plant (2), shaking device (3), Decatize heating device (4) is successively set on from left to right on device pedestal (5), and slide unit (52) are equipped in linear guide (51).
3. a kind of pretreatment unit for measuring Mercury In Soil content according to claim 2, which is characterized in that described to add Medicine pedestal (21) is movably arranged on the left of device pedestal (5) by mounting rack, and it includes that head cavity body is added dropwise that head (221), which are added dropwise, (2210), the first inlet (2211), the second inlet (2212), third inlet (2213), cylinder valve (6);Head is added dropwise Internal plug (2214) are provided at the liquid droping port of cavity (2210) lower end;Hollow piston rod (61) are provided in the cylinder valve (6);
First inlet (2211), the second inlet (2212), third inlet (2213) respectively be added dropwise head cavity body (2210) it is connected to, and is respectively used to transmission the first medicament, second medicament, super water;Head cavity is being added dropwise in cylinder valve (6) setting Body (2210) upper end, and hollow piston rod (61) is connect with internal plug (2214), internal plug (2214) is used for dropwise addition head cavity body (2210) liquid droping port of lower end is closed;And internal plug (2214) and liquid droping port contact position are provided with washer (2215).
4. a kind of pretreatment unit for measuring Mercury In Soil content according to claim 2, which is characterized in that the shake Dynamic device (3) include mounting bracket (31), the first telescopic device (32) and shaking assembly (33);The mounting bracket (31) is living Dynamic to be arranged on device pedestal (5), the shaking assembly (33) is arranged by first telescopic device (32) in mounting bracket (31) top;
Locked groove (120) are provided in the left and right end side surface of the pipe holder (12);
The shaking assembly (33) include mounting base (331), vibrating motor (332), oscillating plate (333), connecting spring (334), Electric mortise lock (335);The mounting base (331) is character "door" form structure, and mounting base (331) is mounted under the first telescopic device (32) End;The vibrating motor (332) is arranged on mounting base (331);There are two the oscillating plates (333), two oscillating plates (333) The internal left and right end of mounting base (331) is mounted on by two connecting springs (334) respectively;The lock tongue energy of the electric mortise lock (335) It is enough inserted into the locked groove (120).
5. a kind of pretreatment unit for measuring Mercury In Soil content according to claim 2, which is characterized in that the vapour Steaming heating device (4) includes including outer protection shell (41), internal protection shell (42), the second telescopic device (43) and steam Generating device (44);
The outer protection shell (41) is mounted on device pedestal (5), and the internal protection shell (42) passes through described second Telescopic device (43) setting is provided in external protective shell body (41) inner tip, and in internal protection shell (42) inner side Conduit/spray assembly (420);Conduit/the spray assembly (420) uses the stainless steel tube that stomata is uniformly provided on tube wall, And conduit/spray assembly (420) is connect with steam generation facility (44).
6. using the preprocess method of claim 1-5 any one described device measurement Mercury In Soil content, feature exists In, comprising the following steps:
Step 1: 0.5g pedotheque to be measured is placed in sample cell (11), and sample cell (11) is placed on pipe holder (12) On;Then pipe holder (12) is placed on dosing pedestal (21) and several drops is added dropwise into sample cell (11) by the way that head (221) are added dropwise After super water soaks soil to be measured;The chloroazotic acid of 10mL1:1 is added into the soil after wetting again;It jumps a queue;
Step 2: pipe holder (12) is placed on slide unit (52), is slid into immediately below shaking device (3), flexible by first Device (32) adjusts shaking assembly (33) and moves down, then will be in lock tongue insertion locked groove (120) of electric mortise lock (335);Adjust the After one telescopic device (32) rises so that pipe holder (12) is hanging, opens vibrating motor (332) and sample cell (11) is shaken up Processing, specifically shaking up the time is 5~15min;Vibrating motor (332) are then shut off, by the first telescopic device (32) by pipe branch Frame (12) closes lock tongue after being placed on slide unit (52), then adjusts the first telescopic device (32) and rises to initial position;
Step 3: pipe holder (12) is slid into immediately below protection shell (42) by slide unit (52), passes through the second telescopic device (43) protection shell (42) is dropped to and is contacted with device pedestal (5);It opens steam generation facility (44) and utilizes conduit/sprinkling group After part (420) makes steam persistently heat 1.5h to sample cell (11), steam off generating device (44) and it will stretch using second Compression apparatus (43) will protect shell (42) to restore to initial position;After cooling 20~30min;
Step 4: pipe holder (12) is slid into initial position using slide unit (52), pipe holder (12) is then placed on dosing 1~2 drop K is added dropwise into sample cell (11) by the way that head (221) are added dropwise on pedestal (21)2Cr2O7Solution;Then dropwise addition head is utilized (221) it after into sample cell (11), the super water of addition is settled to the graticule of sample cell (11), repeats to stand after step 2 is shaken up .
7. a kind of pretreatment unit for measuring Mercury In Soil content according to claim 1, which is characterized in that described K2Cr2O7The concentration of solution is 5%.
CN201910848481.4A 2019-09-09 2019-09-09 Pretreatment device and pretreatment method for measuring total mercury content in soil Expired - Fee Related CN110487611B (en)

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