JP6924344B1 - Preparation equipment and method for solid waste soil leachate in pesticide pesticide production areas - Google Patents

Preparation equipment and method for solid waste soil leachate in pesticide pesticide production areas Download PDF

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Publication number
JP6924344B1
JP6924344B1 JP2021032361A JP2021032361A JP6924344B1 JP 6924344 B1 JP6924344 B1 JP 6924344B1 JP 2021032361 A JP2021032361 A JP 2021032361A JP 2021032361 A JP2021032361 A JP 2021032361A JP 6924344 B1 JP6924344 B1 JP 6924344B1
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steam
sample container
solvent
soil
pesticide
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JP2022133598A (en
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何健
張孝飛
孔徳洋
李菊穎
豆葉枝
張悦清
許静
田豊
余佳
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生態環境部南京環境科学研究所
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Abstract

【課題】浸出液抽出装置の抽出工程は、抽出工程が煩雑で抽出が不完全であるという欠点があり、試験結果のばらつきが大きくなり、浸出液の純度と抽出の徹底性が実験の正確性に影響を与える。【解決手段】本発明は、土壤検出の技術分野に関し、具体的には、殺虫剤農薬生産地の固形廃棄土壌浸出液の調製装置および方法に関し、本発明の調製装置は、凝縮タンク、および前記凝縮タンクの上方に設けられた蒸発機構を含み、前記凝縮タンクが蒸発機構と蒸気プレス機構を介して接続され、本発明の調製方法は、高圧蒸気ジェットフロー溶解法を使用して、測定する土壤サンプル中の殺虫剤農薬を溶解・抽出し、高効率かつ高速で土壤サンプル中の抽出する組成を均一に十分に溶解できるだけでなく、高圧蒸気の温度を効果的に確保して、抽出する組成が高温によって分解されないようにし、検出実験の正確性を確保する。【選択図】図1PROBLEM TO BE SOLVED: To have a drawback that the extraction process of a leachate extraction device is complicated and the extraction is incomplete, the test results vary widely, and the purity of the leachate and the thoroughness of extraction affect the accuracy of the experiment. give. The present invention relates to a technical field of soil pot detection, specifically, an apparatus and a method for preparing a solid waste soil leachate in a pesticide pesticide production area, wherein the preparation apparatus of the present invention is a condensation tank and the condensation. Including an evaporation mechanism provided above the tank, the condensation tank is connected via an evaporation mechanism and a steam press mechanism, and the preparation method of the present invention is a soil sample to be measured using a high pressure steam jet flow melting method. Not only can the composition to be extracted in the soil sample be uniformly and sufficiently dissolved by dissolving and extracting the pesticide pesticide inside, but also the temperature of the high-pressure steam is effectively secured, and the composition to be extracted is high. Prevents decomposition by and ensures the accuracy of detection experiments. [Selection diagram] Fig. 1

Description

本発明は、土壤検出の技術分野に関し、具体的には殺虫剤農薬生産地の固形廃棄土壌浸出
液の調製装置および方法に関する。
The present invention relates to the technical field of soil pit detection, and specifically to a device and method for preparing a solid waste soil leachate in an insecticide pesticide production area.

殺虫剤農薬生産地の土壤毒性を測定する実験では、土壤浸出液を抽出する必要があるが、
現在、ある浸出液抽出装置の抽出工程は、抽出工程が煩雑で抽出が不完全であるという欠
点があり、試験結果のばらつきが大きくなり、浸出液の純度と抽出の徹底性が実験の正確
性に影響を与える。
In experiments to measure soil toxicity in pesticide pesticide production areas, it is necessary to extract soil exudate,
Currently, the extraction process of a leachate extractor has the disadvantage that the extraction process is complicated and the extraction is incomplete, the test results vary widely, and the purity of the leachate and the thoroughness of extraction affect the accuracy of the experiment. give.

上記の目的を達成するために、本発明は、殺虫剤農薬生産地の固形廃棄土壌浸出液の調製
装置、前記装置に応じて設計された対応の使用方法を提供し、低不純物および高収率の土
壤浸出液を調製し、具体的な技術的解決策は以下の通りである。
In order to achieve the above object, the present invention provides a device for preparing a solid waste soil leachate in a pesticide pesticide production area, a corresponding usage method designed according to the device, and has low impurities and high yield. The soil exudate is prepared and the specific technical solution is as follows.

一、土壤浸出液の調製装置
本発明によって設計された殺虫剤農薬生産地の固形廃棄土壌浸出液の調製装置は、凝縮タ
ンク、および前記凝縮タンクの上方に設けられた蒸発機構を含む。
前記蒸発機構は、中心軸を中心として、径方向にそって順次溶媒蒸発器および水蒸発器が
周方向に設けられ、前記溶媒蒸発器の内部に第2の加熱板および第2の熱伝達板が設けら
れ、外部に溶媒蒸気導管が連通され、前記水蒸発器の内部に第1の加熱板および第1の熱
伝達板が設けられ、外部に水蒸気導管が連通される。
前記凝縮タンクの頂部の中心に蒸気プレス機構が設けられ、前記蒸気プレス機構の位置に
対応する凝縮タンクの内壁にらせん状に延伸する凝縮板が設けられ、前記蒸気プレス機構
の位置に対応する凝縮タンクの外壁に凝縮管が設けられ、
前記蒸気プレス機構は、蒸気排気穴を備えたサンプル容器を含み、前記サンプル容器の頂
部に蒸気リングカラムが挿入され、前記サンプル容器の錐状底部の中心にくり抜いた貫通
穴を備えた液体収集カバーが接続される。
前記蒸気リングカラムの表面に蒸気微細穴が設けられ、中心軸に二次加熱カラムが設けら
れ、頂部にシールリングカバーが設けられ水蒸気導管および溶媒蒸気導管に連通する。
サンプル容器の底部に凝縮した浸出液が液体収集カバーで収集された後、凝縮板の下縁に
設けられたガイドストリップに沿って凝縮タンクの底部中心に設けられガイドカバーを備
えた溶液導出管に流入する。
ガイドストリップから滑り落ちた浸出液が前記溶液導出管の外部に設けられた環状ガイド
シェルで収集された後、環状ガイド管に流入する。
1. Soil leachate preparation device The solid waste soil leachate preparation device for the pesticide pesticide production area designed by the present invention includes a condensing tank and an evaporation mechanism provided above the condensing tank.
In the evaporation mechanism, a solvent evaporator and a water evaporator are sequentially provided in the circumferential direction with the central axis as the center, and a second heating plate and a second heat transfer plate are provided inside the solvent evaporator. Is provided, a solvent vapor conduit is communicated to the outside, a first heating plate and a first heat transfer plate are provided inside the water evaporator, and a steam conduit is communicated to the outside.
A steam press mechanism is provided at the center of the top of the condensation tank, and a condensing plate extending in a spiral shape is provided on the inner wall of the condensing tank corresponding to the position of the steam press mechanism to condense the position corresponding to the position of the steam press mechanism. A condensing tube is provided on the outer wall of the tank,
The vapor press mechanism includes a sample container with a vapor exhaust hole, a liquid collection cover having a vapor ring column inserted at the top of the sample container and a through hole hollowed out in the center of the cone-shaped bottom of the sample container. Is connected.
A steam microhole is provided on the surface of the steam ring column, a secondary heating column is provided on the central axis, and a seal ring cover is provided on the top to communicate with the steam conduit and the solvent steam conduit.
After the leachate condensed on the bottom of the sample container is collected by the liquid collection cover, it flows into the solution outlet tube provided in the center of the bottom of the condensing tank along the guide strip provided on the lower edge of the condensing plate and provided with the guide cover. do.
The leachate that has slipped off the guide strip is collected by an annular guide shell provided outside the solution outlet tube, and then flows into the annular guide tube.

本発明の一態様として、前記凝縮タンクの下方に支持ベースが設けられ、上方に支持板が
設けられ、外側に支持カラムを介して支持ベースに接続された支持リングが設けられ、前
記支持リングの頂部に支持油圧シリンダーが設けられ、前記支持油圧シリンダー内の油圧
ロッド頂部が前記支持板の底部に固定的に接続される。
本発明の一態様として、前記サンプル容器の頂部に可動シールカバーが設けられ、前記サ
ンプル容器の内部、蒸気リングカラムに嵌設された環状サンプル押し板が設けられ、前記
蒸気リングカラムの水蒸気導管および溶媒蒸気導管との接続部に溶媒連通リングが設けら
れる。
As one aspect of the present invention, a support base is provided below the condensing tank, a support plate is provided above, and a support ring connected to the support base via a support column is provided on the outside of the support ring. A support hydraulic cylinder is provided at the top, and the top of the hydraulic rod in the support hydraulic cylinder is fixedly connected to the bottom of the support plate.
As one aspect of the present invention, a movable seal cover is provided at the top of the sample container, an annular sample push plate fitted to the steam ring column is provided inside the sample container, and the steam conduit of the steam ring column and the steam conduit of the steam ring column are provided. A solvent communication ring is provided at the connection with the solvent vapor conduit.

本発明の一態様として、前記可動シールカバーと同一平面にあるサンプル容器の外壁に外
側シールリングが設けられ、前記外側シールリングの下端に外側シールリング溝が設けら
れ、前記凝縮タンクの頂部に外側シールリング溝内にしっかりと拘束されたシールフィッ
トリングが設けられる。
As one aspect of the present invention, an outer seal ring is provided on the outer wall of the sample container which is flush with the movable seal cover, an outer seal ring groove is provided at the lower end of the outer seal ring, and the outer side is provided on the top of the condensing tank. A tightly restrained seal fit ring is provided in the seal ring groove.

本発明の一態様として、前記水蒸発器上に第1の定圧弁、第1の電気制御弁および第1の
空気圧センサーが設けられ、前記溶媒蒸発器上に第2の定圧弁、第2の電気制御弁および
第2の空気圧センサーが設けられる。
As one aspect of the present invention, a first constant pressure valve, a first electric control valve and a first air pressure sensor are provided on the water evaporator, and a second constant pressure valve and a second constant pressure valve are provided on the solvent evaporator. An electric control valve and a second air pressure sensor are provided.

本発明の一態様として、前記支持板上に蒸気管固定穴が設けられる。 As one aspect of the present invention, a steam pipe fixing hole is provided on the support plate.

本発明の一態様として、前記凝縮タンクの頂部に圧力逃がし弁が固定的に設けられ、前記
凝縮タンクの外壁に凝縮管を被覆する凝縮保護シェルが設けられ、前記凝縮タンクの内壁
に疎水性耐摩耗コート層がメッキされる。
As one aspect of the present invention, a pressure release valve is fixedly provided on the top of the condensation tank, a condensation protection shell for covering the condensation tube is provided on the outer wall of the condensation tank, and the inner wall of the condensation tank is hydrophobically resistant. The wear coat layer is plated.

本発明の一態様として、前記可動シールカバーの内壁の下端に内側密封リングが設けられ
、前記内側密封リングが可動シールカバーの下端よりも低くなるように下向きに延伸し、
前記内側密封リングの外側面にシールリングを備えた内側密封リング溝が設けられる。
As one aspect of the present invention, an inner sealing ring is provided at the lower end of the inner wall of the movable seal cover, and the inner sealing ring is extended downward so as to be lower than the lower end of the movable seal cover.
An inner sealing ring groove provided with a sealing ring is provided on the outer surface of the inner sealing ring.

二、土壤浸出液の調製方法
本発明によって設計された土壤浸出液調製の方法は、
S1、土壤サンプルを30〜45℃の低温で乾燥させ、粉末状に粉砕し、砂利雑草の粒子
を濾過し除去するステップと、
S2、処理された土壤サンプルを前記サンプル容器の内部に入れ、蒸気リングカラムをサ
ンプル容器内に押し込み、環状サンプル押し板によりサンプル頂部をしっかりと押圧する
ステップと、
S3、前記水蒸発器内に純水を注入し、溶媒蒸発器の内部に混合液を注入し、前記混合液
は質量濃度50〜95%のアルコールと質量濃度10〜20%のアセトンが5:1の質量
比で混合されて構成されるステップと、
S4、第1の加熱板および第2の加熱板を始動して加熱し、水蒸発器内の圧力を0.18
〜0.22MPaに制御し、溶媒蒸発器内の圧力を0.14〜0.16MPaに制御する
ステップと、
S5、まず水蒸発器の第1の電気制御弁を開き、サンプル容器内に高圧蒸気を10〜15
min通気し、次に溶媒蒸発器の第2の電気制御弁を開き、サンプル容器内に蒸発溶媒を
通気するステップと、
S6、高圧蒸気および蒸発溶媒を混合してサンプル容器内に30〜45min通気し、こ
のときサンプル容器の温度を75〜85℃に制御するステップと、
S7、順次第2の電気制御弁、第1の電気制御弁を閉じ、15〜20min冷却するステ
ップと、
S8、外側排液管と導出排液管から排出した浸出液を収集し、静置し遠心分離して上澄み
液を得、標準を満たす浸出液を取得するステップと、を含む。
2. Method for preparing soil leachate The method for preparing soil leachate designed by the present invention is as follows.
S1, the step of drying the soil pot sample at a low temperature of 30 to 45 ° C., crushing it into powder, and filtering and removing the particles of gravel weeds.
S2, the step of putting the treated earthenware sample into the sample container, pushing the steam ring column into the sample container, and firmly pressing the sample top with the annular sample push plate.
S3, pure water is injected into the water evaporator, and a mixed solution is injected into the solvent evaporator. The mixed solution contains alcohol having a mass concentration of 50 to 95% and acetone having a mass concentration of 10 to 20%. A step composed of being mixed at a mass ratio of 1 and
S4, the first heating plate and the second heating plate are started and heated, and the pressure in the water evaporator is 0.18.
The step of controlling the pressure in the solvent evaporator to 0.14 to 0.16 MPa by controlling the pressure to ~ 0.22 MPa, and the step of controlling the pressure in the solvent evaporator to 0.14 to 0.16 MPa.
S5, First, open the first electric control valve of the water evaporator, and put high-pressure steam in the sample container for 10 to 15
The step of venting the evaporative solvent into the sample container by opening the second electric control valve of the solvent evaporator after min aeration,
S6, a step of mixing high-pressure steam and an evaporation solvent and aerating the sample container for 30 to 45 minutes, at which time controlling the temperature of the sample container to 75 to 85 ° C.
S7, the step of closing the second electric control valve and the first electric control valve in sequence and cooling for 15 to 20 minutes, and
S8 includes a step of collecting the exudate discharged from the outer drainage pipe and the outlet drainage pipe, allowing it to stand and centrifuging to obtain a supernatant, and obtaining an exudate satisfying the standard.

従来の土壤浸出液の調製装置と比較すると、本発明の有益な効果は以下の通りである。
本発明は、高圧蒸気ジェットフロー溶解法を使用して、測定する土壤サンプル中の殺虫剤
農薬溶解を抽出し、高効率かつ高速で土壤サンプル中の抽出組成を均一かつ十分に溶解す
ることができるだけでなく、高圧蒸気の温度を良好に制御し、抽出組成が高温によって分
解されないようにして、検出実験の正確性を確保する。
Compared with the conventional soil exudate preparation device, the beneficial effects of the present invention are as follows.
The present invention can extract the pesticide pesticide dissolution in the soil sample to be measured by using the high-pressure steam jet flow dissolution method, and can uniformly and sufficiently dissolve the extraction composition in the soil sample at high efficiency and high speed. Instead, the temperature of the high-pressure steam is well controlled so that the extraction composition is not decomposed by the high temperature to ensure the accuracy of the detection experiment.

本発明の正面図である。It is a front view of this invention. 図1の上面図である。It is a top view of FIG. 図1のA-A断面図である。FIG. 1 is a cross-sectional view taken along the line AA of FIG. 図1の部分図Bである。FIG. 1 is a partial view B of FIG. 図1の部分図Cである。FIG. 1 is a partial view C of FIG. 図1の部分図Dである。FIG. 1 is a partial view D of FIG. 図1の部分図Eである。FIG. 1 is a partial view E of FIG.

[符号の説明]
10 支持ベース
11 支持リング
12 支持カラム
13 支持油圧シリンダー
14 支持板
141 蒸気管固定穴
20 凝縮タンク
201 サンプル収容固定穴
202 シールフィットリング
21 凝縮板
22 凝縮保護シェル
23 凝縮管
24 環状ガイドシェル
25 環状ガイド管
251 外側排液管
26 溶液導出管
261 導出排液管
27 ガイドカバー
271 ガイドカバー貫通穴
28 ガイドストリップ
29 圧力逃がし弁
30 蒸気プレス機構
31 サンプル容器
311 蒸気排気穴
32 可動シールカバー
33 蒸気リングカラム
331 シールリングカバー
332 蒸気進入ポート
333 蒸気微細穴
34 二次加熱カラム
35 環状サンプル押し板
36 溶媒連通リング
361 溶媒進入ポート
37 液体収集カバー
371 くり抜いた貫通穴
38 内側密封リング
381 内側密封リング溝
39 外側シールリング
391 外側シールリング溝
40 蒸発機構
41 水蒸発器
411 第1の加熱板
412 第1の熱伝達板
413 蒸気排出ポート
414 第1の空気圧センサー
415 第1の定圧弁
42 溶媒蒸発器
421 第2の加熱板
422 第2の熱伝達板
423 溶媒排出ポート
424 第2の空気圧センサー
425 第2の定圧弁
43 水蒸気導管
431 第1の電気制御弁
44 溶媒蒸気導管
441 第2の電気制御弁
[Explanation of code]
10 Support base 11 Support ring 12 Support column 13 Support hydraulic cylinder 14 Support plate 141 Steam pipe fixing hole 20 Condensing tank 201 Sample storage fixing hole 202 Seal fit ring 21 Condensing plate 22 Condensing protection shell 23 Condensing tube 24 Circular guide shell 25 Circular guide Pipe 251 Outer liquid drain pipe 26 Liquid outlet pipe 261 Derived liquid drain pipe 27 Guide cover 271 Guide cover through hole 28 Guide strip 29 Pressure relief valve 30 Steam press mechanism 31 Sample container 311 Steam exhaust hole 32 Movable seal cover 33 Steam ring column 331 Seal ring cover 332 Vapor entry port 333 Steam fine hole 34 Secondary heating column 35 Circular sample push plate 36 Solvent communication ring 361 Solution entry port 37 Liquid collection cover 371 Hollow through hole 38 Inner seal ring 381 Inner seal ring groove 39 Outer seal Ring 391 Outer seal Ring groove 40 Evaporation mechanism 41 Water evaporator 411 First heating plate 412 First heat transfer plate 413 Steam discharge port 414 First air pressure sensor 415 First constant pressure valve 42 Solvent evaporator 421 Second Heating plate 422 Second heat transfer plate 423 Solvent discharge port 424 Second air pressure sensor 425 Second constant pressure valve 43 Steam conduit 431 First electric control valve 44 Solvent steam conduit 441 Second electric control valve

本発明によって達成される方法および効果をさらに説明するために、以下、本発明の技術
的解決策を、添付の図面と併せて明確かつ完全に説明する。
In order to further illustrate the methods and effects achieved by the present invention, the technical solutions of the present invention will be described below clearly and completely in conjunction with the accompanying drawings.

実施例1
実施例1は、主に本発明によって設計された土壤浸出液調製装置の具体的な構造を説明す
るが、具体的な内容は以下の通りである。
図1に示すように、本発明によって設計された殺虫剤農薬生産地の固形廃棄土壌浸出液の
調製装置は、凝縮タンク20、および前記凝縮タンク20の上方に設けられた蒸発機構4
0を含む。
Example 1
Example 1 mainly describes the specific structure of the soil leachate preparation device designed by the present invention, and the specific contents are as follows.
As shown in FIG. 1, the device for preparing the solid waste soil leachate in the pesticide pesticide production area designed by the present invention includes a condensing tank 20 and an evaporation mechanism 4 provided above the condensing tank 20.
Includes 0.

図4に示すように、前記蒸発機構40は中心軸を中心として径方向にそって順次溶媒蒸発
器42および水蒸発器41が周方向に設けられ、前記溶媒蒸発器42の内部に第2の加熱
板421および第2の熱伝達板422が設けられ、外部に溶媒蒸気導管44が連通され、
前記水蒸発器41の内部に第1の加熱板411および第1の熱伝達板412が設けられ、
外部に水蒸気導管43が連通される。
図1に示すように、前記凝縮タンク20の頂部中心に蒸気プレス機構30が設けられ、前
記蒸気プレス機構30の位置に対応する凝縮タンク20の内壁にらせん状に延伸する凝縮
板21が設けられ、前記蒸気プレス機構30の位置に対応する凝縮タンク20の外壁に凝
縮管23が設けられ、
前記蒸気プレス機構30は、蒸気排気穴311を備えたサンプル容器31を含み、前記サ
ンプル容器31の頂部に蒸気リングカラム33が挿入され、前記サンプル容器31の錐状
底部中心に、くり抜いた貫通穴371を備えた液体収集カバー37が接続される。
前記蒸気リングカラム33の表面に蒸気微細穴333が設けられ、中心軸に二次加熱カラ
ム34が設けられ、頂部にシールリングカバー331が設けられ水蒸気導管43および溶
媒蒸気導管44と連通する。
サンプル容器31の底部から凝縮した浸出液が液体収集カバー37で収集された後、凝縮
板21の下縁に設けられたガイドストリップ28に沿って凝縮タンク20の底部中心に設
けられガイドカバー27を備えた溶液導出管26に流入する。
ガイドストリップ28から滑り落ちた浸出液は、前記溶液導出管26の外部に設けられた
環状ガイドシェル24で収集された後、環状ガイド管25に流入する。
具体的には、前記凝縮タンク20の下方に支持ベース10が設けられ、上方に支持板14
が設けられ、外側に支持カラム12を介して支持ベース10に接続された支持リング11
が設けられ、前記支持リング11の頂部に支持油圧シリンダー13が設けられ、前記支持
油圧シリンダー13内の油圧ロッド頂部が前記支持板14の底部に固定的に接続される。
具体的には、前記サンプル容器31の頂部に可動シールカバー32が設けられ、前記サン
プル容器31の内部に蒸気リングカラム33に嵌設された環状サンプル押し板35が設け
られ、前記蒸気リングカラム33の水蒸気導管43および溶媒蒸気導管44との接続部に
溶媒連通リング36が設けられる。
As shown in FIG. 4, in the evaporation mechanism 40, a solvent evaporator 42 and a water evaporator 41 are sequentially provided in the circumferential direction along the radial direction about the central axis, and a second solvent evaporator 42 is provided inside the solvent evaporator 42. A heating plate 421 and a second heat transfer plate 422 are provided, and a solvent vapor conduit 44 is communicated to the outside.
A first heating plate 411 and a first heat transfer plate 412 are provided inside the water evaporator 41.
The steam conduit 43 is communicated to the outside.
As shown in FIG. 1, a steam press mechanism 30 is provided at the center of the top of the condensation tank 20, and a condensing plate 21 extending spirally is provided on the inner wall of the condensation tank 20 corresponding to the position of the steam press mechanism 30. A condensing tube 23 is provided on the outer wall of the condensing tank 20 corresponding to the position of the steam press mechanism 30.
The steam press mechanism 30 includes a sample container 31 provided with a steam exhaust hole 311, and a steam ring column 33 is inserted into the top of the sample container 31, and a hollow through hole is formed in the center of the cone-shaped bottom of the sample container 31. A liquid collection cover 37 with 371 is connected.
A steam microhole 333 is provided on the surface of the steam ring column 33, a secondary heating column 34 is provided on the central axis, and a seal ring cover 331 is provided on the top thereof to communicate with the steam conduit 43 and the solvent steam conduit 44.
After the leachate condensed from the bottom of the sample container 31 is collected by the liquid collection cover 37, the guide cover 27 is provided at the center of the bottom of the condensing tank 20 along the guide strip 28 provided on the lower edge of the condensing plate 21. It flows into the solution outlet pipe 26.
The leachate that has slipped off the guide strip 28 is collected by the annular guide shell 24 provided outside the solution outlet pipe 26, and then flows into the annular guide pipe 25.
Specifically, a support base 10 is provided below the condensation tank 20, and a support plate 14 is provided above.
Is provided, and the support ring 11 is connected to the support base 10 via the support column 12 on the outside.
Is provided, a support hydraulic cylinder 13 is provided at the top of the support ring 11, and the top of the hydraulic rod in the support hydraulic cylinder 13 is fixedly connected to the bottom of the support plate 14.
Specifically, a movable seal cover 32 is provided on the top of the sample container 31, and an annular sample push plate 35 fitted in the steam ring column 33 is provided inside the sample container 31, and the steam ring column 33 is provided. A solvent communication ring 36 is provided at a connection portion between the steam conduit 43 and the solvent vapor conduit 44.

具体的には、図5を参照して、前記可動シールカバー32と同一平面にあるサンプル容器
31外壁に外側シールリング39が設けられ、前記外側シールリング39の下端に外側シ
ールリング溝391が設けられ、前記凝縮タンク20の頂部に外側シールリング溝391
内にしっかりと拘束されたシールフィットリング202が設けられる。
具体的には、前記水蒸発器41上に第1の定圧弁415、第1の電気制御弁431および
第1の空気圧センサー414が設けられ、前記溶媒蒸発器42上に第2の定圧弁425、
第2の電気制御弁441および第2の空気圧センサー424が設けられる。
具体的には、前記支持板14上に蒸気管固定穴141が設けられる。
具体的には、前記凝縮タンク20の頂部に圧力逃がし弁29が固定的に設けられ、前記凝
縮タンク20の外壁に凝縮管23を被覆する凝縮保護シェル22が設けられ、前記凝縮タ
ンク20の内壁に疎水性の耐摩耗コート層がメッキされる。
具体的には、前記可動シールカバー32の内壁の下端に内側密封リング38が設けられ、
前記内側密封リング38が可動シールカバー32の下端よりも低くなるように下向きに延
伸し、前記内側密封リング38の外側面にシールリングを備えた内側密封リング溝381
が設けられる。
Specifically, with reference to FIG. 5, an outer seal ring 39 is provided on the outer wall of the sample container 31 which is flush with the movable seal cover 32, and an outer seal ring groove 391 is provided at the lower end of the outer seal ring 39. The outer seal ring groove 391 is formed on the top of the condensation tank 20.
A tightly constrained seal fit ring 202 is provided inside.
Specifically, a first constant pressure valve 415, a first electric control valve 431, and a first air pressure sensor 414 are provided on the water evaporator 41, and a second constant pressure valve 425 is provided on the solvent evaporator 42. ,
A second electrical control valve 441 and a second air pressure sensor 424 are provided.
Specifically, the steam pipe fixing hole 141 is provided on the support plate 14.
Specifically, a pressure release valve 29 is fixedly provided on the top of the condensation tank 20, a condensation protection shell 22 for covering the condensation tube 23 is provided on the outer wall of the condensation tank 20, and an inner wall of the condensation tank 20 is provided. Is plated with a hydrophobic wear-resistant coat layer.
Specifically, an inner sealing ring 38 is provided at the lower end of the inner wall of the movable seal cover 32.
The inner sealing ring groove 381 is extended downward so that the inner sealing ring 38 is lower than the lower end of the movable seal cover 32, and the inner sealing ring 38 is provided with a sealing ring on the outer surface.
Is provided.

実施例2
実施例2は実施例1に記載の調製装置を基になされたものであり、その目的は本発明によ
って設計された土壤浸出液の調製方法を説明することである。
本発明によって設計された土壤浸出液調製の方法は、
S1、土壤サンプルを30℃の低温で乾燥させ、粉末状に粉砕し、砂利雑草の粒子を濾過
し除去するステップと、
S2、処理された土壤サンプルを前記サンプル容器31の内部に入れ、蒸気リングカラム
33をサンプル容器31内に押し込み、環状サンプル押し板35によりサンプルの頂部を
しっかりと押圧するステップと、
S3、前記水蒸発器41内に純水を注入し、溶媒蒸発器42の内部に混合液を注入し、前
記混合液は、質量濃度50%のアルコールと質量濃度10%のアセトンが5:1の質量比
で混合されて構成されるステップと、
S4、第1の加熱板411および第2の加熱板421を始動して加熱し、水蒸発器41内
の圧力を0.18MPaに制御し、溶媒蒸発器42内の圧力を0.14MPaに制御する
ステップと、
S5、まず水蒸発器41の第1の電気制御弁431を開き、サンプル容器31内に高圧蒸
気を10min通気し、次に溶媒蒸発器42の第2の電気制御弁441を開き、サンプル
容器31内に蒸発溶媒を通気するステップと、
S6、高圧蒸気と蒸発溶媒を混合してサンプル容器31内に30min通気し、このとき
サンプル容器31の温度を75℃に制御するステップと、
S7、順次第2の電気制御弁441、第1の電気制御弁431を閉じ、15min冷却す
るステップと、
S8、外側排液管251および導出排液管261から排出された浸出液を収集し、静置し
遠心分離して上澄み液を得、標準を満たす浸出液を取得するステップと、を含む。
Example 2
Example 2 is based on the preparation apparatus described in Example 1, and an object of the present invention is to explain a method for preparing a soil leachate designed by the present invention.
The method of soil exudate preparation designed by the present invention is:
S1, the step of drying the soil pot sample at a low temperature of 30 ° C., crushing it into powder, and filtering and removing the particles of gravel weeds.
S2, a step of putting the treated earthenware sample into the sample container 31, pushing the steam ring column 33 into the sample container 31, and firmly pressing the top of the sample with the annular sample push plate 35.
S3, pure water is injected into the water evaporator 41, and a mixed solution is injected into the solvent evaporator 42. The mixed solution contains 5: 1 alcohol having a mass concentration of 50% and acetone having a mass concentration of 10%. And the steps that are mixed in the mass ratio of
S4, the first heating plate 411 and the second heating plate 421 are started and heated, the pressure in the water evaporator 41 is controlled to 0.18 MPa, and the pressure in the solvent evaporator 42 is controlled to 0.14 MPa. Steps to do and
S5, First, the first electric control valve 431 of the water evaporator 41 is opened, high-pressure steam is ventilated into the sample container 31 for 10 minutes, then the second electric control valve 441 of the solvent evaporator 42 is opened, and the sample container 31 is opened. With the step of aerating the evaporative solvent inside,
S6, a step of mixing high-pressure steam and an evaporation solvent and aerating the sample container 31 for 30 minutes, at which time controlling the temperature of the sample container 31 to 75 ° C.
S7, a step of sequentially closing the second electric control valve 441 and the first electric control valve 431 and cooling for 15 minutes,
S8 includes a step of collecting the exudate discharged from the outer drainage pipe 251 and the lead drainage pipe 261 and allowing it to stand and centrifuge to obtain a supernatant to obtain a leachate that meets the standards.

実施例3
実施例3は実施例2に記載の調製方法を基になされたものであり、主に別の異なるパラメ
ータ下での調製方法を説明する。
本発明によって設計された別のパラメータ下での土壤浸出液の調製方法は、
S1、土壤サンプルを45℃の低温で乾燥させ、粉末状に粉砕し、砂利雑草の粒子を濾過
し除去するステップと、
S2、処理された土壤サンプルを前記サンプル容器31の内部に入れ、蒸気リングカラム
33をサンプル容器31内に押し込み、環状サンプル押し板35によりサンプルの頂部を
しっかりと押圧するステップと、
S3、前記水蒸発器41内に純水を注入し、溶媒蒸発器42内に混合液を注入し、前記混
合液は質量濃度95%のアルコールと質量濃度20%のアセトンが5:1の質量比で混合
されて構成されるステップと、
S4、第1の加熱板411および第2の加熱板421を始動し加熱して、水蒸発器41内
の圧力を0.22MPaに制御し、溶媒蒸発器42内の圧力を0.16MPaに制御し、
S5、まず水蒸発器41の第1の電気制御弁431を開き、サンプル容器31内に高圧蒸
気を15min通気し、次に溶媒蒸発器42の第2の電気制御弁441を開き、サンプル
容器31内に蒸発溶媒を通気するステップと、
S6、高圧蒸気と蒸発溶媒を混合してサンプル容器31内に45min通気し、このとき
サンプル容器31の温度を85℃に制御するステップと、
S7、順次第2の電気制御弁441、第1の電気制御弁431を閉じ、20min冷却す
るステップと、
S8、外側排液管251および導出排液管261から排出した浸出液を収集し、静置し遠
心分離して上澄み液を得、標準を満たす浸出液を取得するステップと、を含む。
Example 3
Example 3 is based on the preparation method described in Example 2, and mainly describes the preparation method under different different parameters.
The method of preparing the soil leachate under another parameter designed by the present invention is:
S1, the step of drying the soil pot sample at a low temperature of 45 ° C., crushing it into powder, and filtering and removing the particles of gravel weeds.
S2, a step of putting the treated earthenware sample into the sample container 31, pushing the steam ring column 33 into the sample container 31, and firmly pressing the top of the sample with the annular sample push plate 35.
S3, pure water is injected into the water evaporator 41, and a mixed solution is injected into the solvent evaporator 42. The mixed solution has a mass ratio of alcohol having a mass concentration of 95% and acetone having a mass concentration of 20% in a mass ratio of 5: 1. Steps that are mixed in proportion and
S4, the first heating plate 411 and the second heating plate 421 are started and heated to control the pressure in the water evaporator 41 to 0.22 MPa and the pressure in the solvent evaporator 42 to 0.16 MPa. death,
S5, First, the first electric control valve 431 of the water evaporator 41 is opened, high-pressure steam is ventilated into the sample container 31 for 15 minutes, then the second electric control valve 441 of the solvent evaporator 42 is opened, and the sample container 31 is opened. With the step of aerating the evaporative solvent inside,
S6, a step of mixing high-pressure steam and an evaporation solvent and aerating the sample container 31 for 45 minutes, at which time controlling the temperature of the sample container 31 to 85 ° C.
S7, a step of sequentially closing the second electric control valve 441 and the first electric control valve 431 and cooling for 20 minutes,
S8 includes a step of collecting the exudate discharged from the outer drainage pipe 251 and the lead drainage pipe 261 and allowing it to stand and centrifuge to obtain a supernatant to obtain an exudate that meets the standards.

実験例
本実験例は、上記実施例2に記載の調製方法を基になされたものであり、発明の実際の応
用効果を説明することを目的とする。土壤中の殺虫剤の浸出効率は、土壤中の残存殺虫剤
の量によって示され得、殺虫剤の残存量が少ないほど、浸出液の抽出効率が高くなる。殺
虫剤の残存量は動物実験で直観に表現することができるため、試験方法はこのような考え
に基づいて設計される。
本実験例で使用される土壤は人工的に調製した実験土壤であり、その組成は具体的に表1
に示される。
表1 実験土壤の組成および割合
Experimental Example This experimental example is based on the preparation method described in Example 2 above, and an object of the present invention is to explain the actual application effect of the invention. The leaching efficiency of the pesticide in the soil can be indicated by the amount of the residual insecticide in the soil, and the smaller the residual amount of the insecticide, the higher the extraction efficiency of the exudate. Since the residual amount of pesticide can be intuitively expressed in animal experiments, the test method is designed based on this idea.
The soil used in this experimental example is an artificially prepared experimental soil, and its composition is specifically shown in Table 1.
Shown in.
Table 1 Composition and proportion of experimental soil

Figure 0006924344
Figure 0006924344

本実験例で使用される動物モデルの構築方法は次の通りである。
天津大環ミミズ工場から導入されたシマミミズ(E.fetida)を、人工環境(温度
20±2℃、湿度80%±2、光照射400〜800Lux、明暗比10:14)で7日
間飼育した。実験中、明らかな生殖リングを備えた300〜500mgの健康な生後6ヶ
月のミミズを使用した。
本実験では、ネオニコチノイド系殺虫剤に含まれるイミダクロプリドを実験用殺虫剤とし
て使用し、その情報は表2に示される。
表2 殺虫剤情報
The method for constructing the animal model used in this experimental example is as follows.
Eisenia fetida introduced from the Tianjin Great Ring Earthworm Factory was bred in an artificial environment (temperature 20 ± 2 ° C., humidity 80% ± 2, light irradiation 400 to 800 Lux, light-dark ratio 10:14) for 7 days. During the experiment, 300-500 mg of healthy 6-month-old earthworms with obvious reproductive rings were used.
In this experiment, imidacloprid contained in neonicotinoid insecticides was used as an experimental insecticide, and the information is shown in Table 2.
Table 2 Insecticide information

Figure 0006924344
Figure 0006924344

比較組:
本実験例では、従来の抽出方法で調製された土壤浸出液を比較組とし、具体的な調製方法
は次の通りである。
実験土壤と濃度2mg/kgのイミダクロプリドを混合し土壤サンプルとして、60℃で
0.5h乾燥した。乾燥した後の土壤サンプルを乳鉢で粉砕し、次に20メッシュのふる
いにかけ、ふるいに残った土壌を再度粉砕してから再びふるいにかけた。十分に粉砕し均
一に混合した土壤サンプルに水を加えて混合し、超音波で15min浸出・抽出した後、
4000r/minの速度で10min遠心分離し、上澄み液を0.22μmのフィルタ
に通過させた。
浸出液を抽出した土壤サンプル500gを1Lのビーカーに入れ、無薬人工土壌に24時
間飼いならしたミミズ10匹を入れ、最後に人工気候ボックスに入れ、14日後ミミズの
死亡数と中毒状況を確認した。
Comparison group:
In this experimental example, the soil pit leachate prepared by the conventional extraction method is used as a comparative group, and the specific preparation method is as follows.
The experimental soil pot and imidacloprid having a concentration of 2 mg / kg were mixed and dried as a soil pot sample at 60 ° C. for 0.5 h. The dried clay pot sample was crushed in a mortar, then sifted through a 20 mesh sieve, and the soil remaining on the sieve was crushed again and then sifted again. Water is added to the clay pot sample that has been thoroughly crushed and mixed uniformly, mixed, and leached and extracted for 15 minutes by ultrasonic waves.
Centrifugation was carried out at a rate of 4000 r / min for 10 min, and the supernatant was passed through a 0.22 μm filter.
500 g of a clay pot sample from which the exudate was extracted was placed in a 1 L beaker, 10 earthworms domesticated for 24 hours were placed in a drug-free artificial soil, and finally placed in an artificial climate box. 14 days later, the number of earthworm deaths and poisoning status were confirmed. ..

実験組:
本実験例では、本願の調製方法で調製された土壤浸出液を実験組とし、実験組の実験土壤
も濃度2mg/kgのイミダクロプリドと混合し、異なる浸出液調製パラメータに応じて
、実験組を以下の3組に分けた:
実験組1:水蒸発器41内の圧力を0.18MPaに制御し、溶媒蒸発器42内の圧力を
0.14MPaに制御し、高圧蒸気の換気時間を10minとし、混合蒸気の通気時間を
30minとする、
実験組2:水蒸発器41内の圧力を0.22MPaに制御し、溶媒蒸発器42内の圧力を
0.16MPaに制御し、高圧蒸気の換気時間を10minとし、混合蒸気の通気時間を
30minとする、
実験組3:水蒸発器41内の圧力を0.22MPaに制御し、溶媒蒸発器42内の圧力を
0.16MPaに制御し、高圧蒸気の換気時間を15minとし、混合蒸気の通気時間を
45minとする。
各実験組では、浸出液を抽出した土壤サンプル500gをビーカー1Lに入れ、無薬人工
土壌で24時間飼育したミミズ10匹を入れ、最後に人工気候ボックスに入れ、14日後
ミミズの死亡数と中毒状況を確認した。
浸出液を抽出した実験土壤中の殺虫剤の抽出率を計算し、結果を表3に示す。
Experimental group:
In this experimental example, the soil exudate prepared by the preparation method of the present application is used as the experimental group, and the experimental soil of the experimental group is also mixed with imidacloprid having a concentration of 2 mg / kg. Divided into groups:
Experimental group 1: The pressure in the water evaporator 41 is controlled to 0.18 MPa, the pressure in the solvent evaporator 42 is controlled to 0.14 MPa, the ventilation time of the high-pressure steam is set to 10 min, and the ventilation time of the mixed steam is 30 min. To
Experimental group 2: The pressure in the water evaporator 41 is controlled to 0.22 MPa, the pressure in the solvent evaporator 42 is controlled to 0.16 MPa, the ventilation time of the high-pressure steam is set to 10 min, and the ventilation time of the mixed steam is 30 min. To
Experimental group 3: The pressure in the water evaporator 41 is controlled to 0.22 MPa, the pressure in the solvent evaporator 42 is controlled to 0.16 MPa, the ventilation time of the high-pressure steam is set to 15 min, and the ventilation time of the mixed steam is 45 min. And.
In each experimental group, 500 g of a clay pot sample from which the exudate was extracted was placed in a beaker, 10 earthworms bred in drug-free artificial soil for 24 hours were placed in the beaker, and finally placed in an artificial climate box. It was confirmed.
The extraction rate of the insecticide in the experimental soil from which the exudate was extracted was calculated, and the results are shown in Table 3.

Figure 0006924344
Figure 0006924344

浸出液を抽出した実験土壤中の残存殺虫剤のミミズ成長と繁殖に対する影響の具体的なデ
ータを表4に示す。
表4 残存殺虫剤のミミズの成長と繁殖に対する影響
Table 4 shows specific data on the effects of residual insecticides on earthworm growth and reproduction in the experimental soil from which the exudate was extracted.
Table 4 Effects of residual pesticides on earthworm growth and reproduction

Figure 0006924344
Figure 0006924344

表3と表4のデータから分かるように、従来の土壤浸出液抽出法を使用した比較組では、
殺虫剤の抽出率は約46.6%であるのに対して、本発明によって設計された土壤浸出液
の抽出法を使用した実験組では、殺虫剤の抽出率が85%を上回り、実験結果が最も良い
実験組3では、殺虫剤の抽出率が93.2%に達した。これは、従来の土壤浸出液の抽出
法と比較して、本発明の抽出効率が大幅に改善されることを示している。
表4中の実験組1と実験組2のデータを比較すると、換気時間が同じである場合、通気圧
力が大きいほど、ミミズの体重と繁殖に対する影響が小さくなり、これは、実験土壤中の
殺虫剤の残存量が空気圧力の増加に従って減少することが分かる。
表4中の実験組2と実験組3のデータを比較すると、通気圧力が同じである場合、換気時
間が長いほど、ミミズの体重と繁殖に対する影響が小さくなり、これは、実験土壤中の殺
虫剤の残存量が換気時間の増加に従って減少することが分かる。
As can be seen from the data in Tables 3 and 4, in the comparative group using the conventional soil leachate extraction method,
The pesticide extraction rate is about 46.6%, whereas in the experimental group using the soil pit leachate extraction method designed by the present invention, the pesticide extraction rate exceeds 85%, and the experimental results are In the best experimental group 3, the pesticide extraction rate reached 93.2%. This indicates that the extraction efficiency of the present invention is significantly improved as compared with the conventional method for extracting soil effluent.
Comparing the data of Experimental Group 1 and Experimental Group 2 in Table 4, when the ventilation time is the same, the larger the ventilation pressure, the smaller the effect on the weight and reproduction of earthworms, which is the insecticidal activity in the experimental soil. It can be seen that the residual amount of the agent decreases as the air pressure increases.
Comparing the data of Experimental Group 2 and Experimental Group 3 in Table 4, when the ventilation pressure is the same, the longer the ventilation time, the smaller the effect on the weight and reproduction of earthworms, which is the insecticidal activity in the experimental soil. It can be seen that the residual amount of the agent decreases as the ventilation time increases.

要するに、以上の実験データから分かるように、本発明によって設計された土壤浸出液抽
出方法は、従来方法と比較すると、殺虫剤の抽出率がより高く、処理された土壤中の殺虫
剤残存量がより少ないため、高い応用価値がある。
In short, as can be seen from the above experimental data, the soil exudate extraction method designed by the present invention has a higher pesticide extraction rate and a higher residual amount of pesticide in the treated soil as compared with the conventional method. Since there are few, it has high application value.

Claims (6)

凝縮タンク(20)と、および前記凝縮タンク(20)の上方に設けられた蒸発機構(4
0)と、を含む殺虫剤農薬生産地の固形廃棄土壌浸出液の調製装置であって、
前記蒸発機構(40)は、中心軸を中心として、径方向に沿って順次溶媒蒸発器(42)
および水蒸発器(41)が周方向に設けられ、前記溶媒蒸発器(42)の内部に第2の加
熱板(421)および第2の熱伝達板(422)が設けられ、外部に溶媒蒸気導管(44
)が設けられ、前記水蒸発器(41)の内部に第1の加熱板(411)および第1の熱伝
達板(412)が設けられ、外部に水蒸気導管(43)が連通し、
前記凝縮タンク(20)の頂部の中心に蒸気プレス機構(30)が設けられ、前記蒸気プ
レス機構(30)の位置に対応する凝縮タンク(20)の内壁にらせん状に延伸する凝縮
板(21)が設けられ、前記蒸気プレス機構(30)の位置に対応する凝縮タンク(20
)の外壁に凝縮管(23)が設けられ、
前記蒸気プレス機構(30)に蒸気排気穴(311)が設けられたサンプル容器(31)
が設けられ、前記サンプル容器(31)の頂部に蒸気リングカラム(33)が挿入され、
前記サンプル容器(31)の錐状の底部中心にくり抜いた貫通穴(371)を備えた液体
収集カバー(37)が接続され、
前記蒸気リングカラム(33)の表面に蒸気微細穴(333)が設けられ、中心軸に二次
加熱カラム(34)が設けられ、頂部にシールリングカバー(331)が設けられ水蒸気
導管(43)と溶媒蒸気導管(44)が連通し、
サンプル容器(31)の底部から凝縮した浸出液は、液体収集カバー(37)で収集され
た後、凝縮板(21)の下縁に設けられたガイドストリップ(28)に沿って、凝縮タン
ク(20)の底部中心に設けられガイドカバー(27)が設けられた溶液導出管(26)
に流入し、
ガイドストリップ(28)から滑り落ちた浸出液は、前記溶液導出管(26)の外部に設
けられた環状ガイドシェル(24)で収集された後、環状ガイド管(25)に流入する、
ことを特徴とする殺虫剤農薬生産地の固形廃棄土壌浸出液の調製装置。
A condensation tank (20) and an evaporation mechanism (4) provided above the condensation tank (20).
0) and a solid waste soil leachate preparation device for pesticide pesticide production areas, including
The evaporation mechanism (40) is a solvent evaporator (42) sequentially along the radial direction with the central axis as the center.
A water evaporator (41) is provided in the circumferential direction, a second heating plate (421) and a second heat transfer plate (422) are provided inside the solvent evaporator (42), and solvent vapor is provided outside. Conduit (44
) Is provided, a first heating plate (411) and a first heat transfer plate (412) are provided inside the water evaporator (41), and a steam conduit (43) communicates with the outside.
A steam press mechanism (30) is provided in the center of the top of the condensation tank (20), and a condensing plate (21) spirally extends to the inner wall of the condensation tank (20) corresponding to the position of the steam press mechanism (30). ) Is provided, and the condensing tank (20) corresponding to the position of the steam press mechanism (30) is provided.
) Is provided with a condensing tube (23) on the outer wall.
A sample container (31) provided with a steam exhaust hole (311) in the steam press mechanism (30).
Is provided, and the steam ring column (33) is inserted into the top of the sample container (31).
A liquid collection cover (37) having a hollowed-out hole (371) is connected to the center of the cone-shaped bottom of the sample container (31).
A steam microhole (333) is provided on the surface of the steam ring column (33), a secondary heating column (34) is provided on the central axis, and a seal ring cover (331) is provided on the top of the steam conduit (43). And the solvent vapor conduit (44) communicate with each other.
The leachate condensed from the bottom of the sample container (31) is collected by the liquid collection cover (37) and then along the guide strip (28) provided on the lower edge of the condensing plate (21) in the condensing tank (20). ) With a guide cover (27) provided in the center of the bottom of the solution outlet tube (26).
Inflow to
The leachate that has slid off the guide strip (28) is collected by the annular guide shell (24) provided outside the solution outlet tube (26), and then flows into the annular guide tube (25).
A device for preparing solid waste soil leachate in pesticide pesticide production areas.
前記凝縮タンク(20)の下方に支持ベース(10)が設けられ、上方に支持板(14)
が設けられ、外側に支持カラム(12)を介して支持ベース(10)に接続された支持リ
ング(11)が設けられ、前記支持リング(11)の頂部に支持油圧シリンダー(13)
が設けられ、前記支持油圧シリンダー(13)内の油圧ロッドの頂部が前記支持板(14
)の底部に固定的に接続される、ことを特徴とする請求項1に記載の調製装置。
A support base (10) is provided below the condensation tank (20), and a support plate (14) is provided above.
Is provided, and a support ring (11) connected to a support base (10) via a support column (12) is provided on the outside, and a support hydraulic cylinder (13) is provided on the top of the support ring (11).
Is provided, and the top of the hydraulic rod in the support hydraulic cylinder (13) is the support plate (14).
The preparation apparatus according to claim 1, wherein the preparation apparatus is fixedly connected to the bottom of the).
前記サンプル容器(31)の頂部に可動シールカバー(32)が設けられ、前記サンプル
容器(31)の内部に蒸気リングカラム(33)に嵌設された環状サンプル押し板(35
)が設けられ、前記蒸気リングカラム(33)と水蒸気導管(43)および溶媒蒸気導管
(44)との接続部に溶媒連通リング(36)が設けられる、ことを特徴とする請求項2
に記載の調製装置。
A movable seal cover (32) is provided on the top of the sample container (31), and an annular sample push plate (35) fitted in a steam ring column (33) inside the sample container (31).
2), And a solvent communication ring (36) is provided at a connection portion between the steam ring column (33), the steam conduit (43) and the solvent vapor conduit (44).
The preparation device described in.
前記可動シールカバー(32)と同一平面にあるサンプル容器(31)の外壁に外側シー
ルリング(39)が設けられ、前記外側シールリング(39)の下端に外側シールリング
溝(391)が設けられ、前記凝縮タンク(20)の頂部に外側シールリング溝(391
)内に拘束されたシールフィットリング(202)が設けられる、ことを特徴とする請求
項3に記載の調製装置。
An outer seal ring (39) is provided on the outer wall of the sample container (31) which is flush with the movable seal cover (32), and an outer seal ring groove (391) is provided at the lower end of the outer seal ring (39). , Outer seal ring groove (391) on the top of the condensation tank (20)
The preparation apparatus according to claim 3, wherein a seal fit ring (202) constrained in the) is provided.
前記水蒸発器(41)に第1の定圧弁(415)、第1の電気制御弁(431)および第
1の空気圧センサー(414)が設けられ、前記溶媒蒸発器(42)に第2の定圧弁(4
25)、第2の電気制御弁(441)および第2の空気圧センサー(424)が設けられ
る、ことを特徴とする請求項1に記載の調製装置。
The water evaporator (41) is provided with a first constant pressure valve (415), a first electric control valve (431) and a first air pressure sensor (414), and the solvent evaporator (42) is provided with a second. Constant pressure valve (4
25) The preparation apparatus according to claim 1, wherein a second electric control valve (441) and a second air pressure sensor (424) are provided.
請求項1から5のいずれか1項に記載の調製装置を使用して土壤浸出液を調製する方法で
あって、
S1、土壤サンプルを30〜45℃の低温で乾燥させ、粉末状に粉砕し、砂利雑草の粒子
を濾過し除去するステップと、
S2、処理された土壤サンプルを前記サンプル容器(31)の内部に入れ、蒸気リングカ
ラム(33)をサンプル容器(31)内に押し込み、次に環状サンプル押し板(35)に
より土壤サンプルの頂部を押圧するステップと、
S3、前記水蒸発器(41)内に純水を注入し、溶媒蒸発器(42)の内部に混合液を注
入し、前記混合液は質量濃度50〜95%のアルコールと質量濃度10〜20%のアセト
ンが5:1の質量比で混合されて構成されるステップと、
S4、第1の加熱板(411)および第2の加熱板(421)を始動して加熱を開始し、
水蒸発器(41)内の圧力を0.18〜0.22MPaに制御し、溶媒蒸発器(42)内
の圧力を0.14〜0.16MPaに制御するステップと、
S5、まず水蒸発器(41)の第1の電気制御弁(431)を開き、サンプル容器(31
)内に高圧蒸気を10〜15min通気し、そして溶媒蒸発器(42)の第2の電気制御
弁(441)を開き、サンプル容器(31)内に蒸発溶媒を通気するステップと、
S6、高圧蒸気を蒸発溶媒を混合してサンプル容器(31)内に30〜45min通気し
、このときサンプル容器(31)温度を75〜85℃に制御するステップと、
S7、順次第2の電気制御弁(441)、第1の電気制御弁(431)を閉じ、15〜2
0min冷却するステップと、
S8、外側排液管(251)と導出排液管(261)によって浸出液を収集し、静置し遠
心分離して上澄み液を取得し、標準を満たす浸出液を得るステップと、
を含むことを特徴とする方法。
A method for preparing a soil exudate using the preparation device according to any one of claims 1 to 5.
S1, the step of drying the soil pot sample at a low temperature of 30 to 45 ° C., crushing it into powder, and filtering and removing the particles of gravel weeds.
S2, the treated soil sample is placed inside the sample container (31), the steam ring column (33) is pushed into the sample container (31), and then the top of the soil sample is pressed by the annular sample push plate (35). The step to press and
S3, pure water is injected into the water evaporator (41), a mixed solution is injected into the solvent evaporator (42), and the mixed solution contains alcohol having a mass concentration of 50 to 95% and a mass concentration of 10 to 20. A step composed of% acetone mixed in a mass ratio of 5: 1 and
S4, the first heating plate (411) and the second heating plate (421) are started to start heating,
A step of controlling the pressure in the water evaporator (41) to 0.18 to 0.22 MPa and a step of controlling the pressure in the solvent evaporator (42) to 0.14 to 0.16 MPa.
S5, First, the first electric control valve (431) of the water evaporator (41) is opened, and the sample container (31) is opened.
), And the second electric control valve (441) of the solvent evaporator (42) is opened to ventilate the evaporative solvent into the sample container (31).
S6, a step of mixing an evaporative solvent with high-pressure steam and aerating the sample container (31) for 30 to 45 minutes, and controlling the temperature of the sample container (31) to 75 to 85 ° C.
S7, sequentially close the second electric control valve (441) and the first electric control valve (431), 15 to 2
The step of cooling for 0 min and
S8, the step of collecting the exudate by the outer drainage pipe (251) and the outlet drainage pipe (261), allowing it to stand and centrifuging to obtain the supernatant liquid, and obtaining the exudate that meets the standard.
A method characterized by including.
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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114323880A (en) * 2021-12-23 2022-04-12 生态环境部华南环境科学研究所 Leaching device for toxicity samples of solid wastes with different particles
CN115541648A (en) * 2022-12-05 2022-12-30 埃森农机常州有限公司 Plant protection machine mixes medicine concentration on-line measuring device
CN116296695A (en) * 2023-05-12 2023-06-23 北京建工环境修复股份有限公司 Soil detection device and soil detection method
CN117491127A (en) * 2023-11-09 2024-02-02 湖南科睿思仪器设备有限公司 Acid-dispelling treatment equipment
CN118649431A (en) * 2024-08-16 2024-09-17 潍坊晶润化工有限公司 Rectification and purification device for diethyl malonate preparation

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114323880A (en) * 2021-12-23 2022-04-12 生态环境部华南环境科学研究所 Leaching device for toxicity samples of solid wastes with different particles
CN115541648A (en) * 2022-12-05 2022-12-30 埃森农机常州有限公司 Plant protection machine mixes medicine concentration on-line measuring device
CN115541648B (en) * 2022-12-05 2023-03-10 埃森农机常州有限公司 Plant protection machine mixes medicine concentration on-line measuring device
CN116296695A (en) * 2023-05-12 2023-06-23 北京建工环境修复股份有限公司 Soil detection device and soil detection method
CN117491127A (en) * 2023-11-09 2024-02-02 湖南科睿思仪器设备有限公司 Acid-dispelling treatment equipment
CN118649431A (en) * 2024-08-16 2024-09-17 潍坊晶润化工有限公司 Rectification and purification device for diethyl malonate preparation

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