TWI352809B - Automatic leaching test system with constant ph co - Google Patents

Automatic leaching test system with constant ph co Download PDF

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TWI352809B
TWI352809B TW96150258A TW96150258A TWI352809B TW I352809 B TWI352809 B TW I352809B TW 96150258 A TW96150258 A TW 96150258A TW 96150258 A TW96150258 A TW 96150258A TW I352809 B TWI352809 B TW I352809B
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acid
liquid
container
stirring
automatic control
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TW96150258A
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TW200928356A (en
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Chung Chih Chen
Jinn Shiou Hwang
Chia Lun Kuan
Suen Chu Hsu
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Ind Tech Res Inst
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1352809 九、發明說明: 【發明所屬之技術領域】 本發明是有關於一種酸鹼值恆定自動控制溶出試驗系 統,特別是有關於一種以連續自動化方式分析受試樣品材 料在不同且固定酸鹼值下之無機或有機成份之環境溶出特 性之酸驗值怪定自動控制溶出試驗系統。 【先前技術】 近年來,針對廢棄物與材料溶出性之研究而言,各種 不同酸鹼值下環境性溶出分析法已被發展,其實驗數據可 幫助全面瞭解材料在各種不同酸鹼條件下對環境所造成之 衝擊。上述之分析法乃是利用受試樣品材料在使用過程中 會因不同酸鹼值而有不同溶出特性之原理,來模擬受試樣 品材料中無機物或有機物之溶出情形,以推估在不同酸驗 條件下所造成之環境衝擊。然而,國内目前主要所採用的 毒性特性溶出程序(TCLP)僅考慮單一酸鹼值下之溶出特性 分析,其無法正確反應真實環境中不同酸鹼條件下無機或 有機物質之溶出情形。此外,目前的材料溶出特性分析皆 是以人工滴定之方式來執行,因而會造成分析上的不便及 人為操作誤差的發生。 有鑑於此,本發明提供一種酸鹼值恆定自動控制溶出 試驗糸統,其可以連績自動化方式分析受試樣品材料在不 同且固定酸鹼值下之無機或有機成份之環境溶出特性。 【發明内容】 本發明係包括一自動控制裝置;至少一酸鹼液添加裝 6 1352809 置,電性連接於該自動控制裝置,並且具有一空氣幫浦、 一酸液容器、一驗液容器、一酸液分壓閥及一驗液分壓閥, 其中,該空氣幫浦係電性連接於該自動控制裝置,並且係 連通於該酸液容器及該鹼液容器,該酸液容器係連通於該 酸液分壓閥,並且係容納有一酸液,該鹼液容器係連通於 該鹼液分壓閥,並且係容納有一鹼液,以及該酸液分壓閥 及該鹼液分壓閥係電性連接於該自動控制裝置;至少一攪 拌溶出裝置,連通於該酸鹼液添加裝置之該酸液分壓閥及 該驗液分壓閥’並且容納有'一受試樣品材料及一受试樣品 材料萃取液;以及至少一酸鹼值探針,設置於該攪拌溶出 裝置之中,並且電性連接於該自動控制裝置。 同時,根據本發明之酸鹼值恆定自動控制溶出試驗系 統,其更包括一訊號轉換器,係電性連接於該空氣幫浦與 該自動控制裝置之間、該酸液分壓閥與該自動控制裝置之 間以及該鹼液分壓閥與該自動控制裝置之間。 又在本發明中,更包括一訊號轉換器,係電性連接於 該空氣幫浦與該自動控制裝置之間、該酸液分壓閥與該自 動控制裝置之間以及該鹼液分壓閥與該自動控制裝置之 間。 又在本發明中,該酸鹼液添加裝置更具有一二氧化碳 吸附瓶,以及該二氧化碳吸附瓶係連通於該空氣幫浦與該 酸液容器之間以及該空氣幫浦與該鹼液容器之間。 又在本發明中,該攪拌溶出裝置具有一磁攪拌器、一 攪拌容器、一密封蓋及一攪拌磁石,該攪拌容器係設置於 該磁搜掉器之上,、日么六 ^ 〇 1 亚係容納有該受試樣品材料及該受試 卒取液,該密封蓋係密封覆蓋於該攪拌容器之 於哕二ί分壓閥及該鹼液分壓閥係經由該密封蓋而連通 ’該酸_探針係經由該密封蓋而設置於該 ,U中’以及該授拌磁石係設置於該麟容器之 中’亚且係轉動之方式連接於該密封蓋。 又在本發財,該密封蓋具有mi 广、=在本發明中’該㈣溶出裝置更具有—擾拌棒,該 讀盖更具有―固^架,以及該龄棒係連接於該授拌磁 石,並且係以轉動之方式連接於該固定架。· 又在本發明中,該攪拌容器係由聚乙烯、聚丙烯或聚 四氯乙烯所製成。 又在本發明中,該攪拌棒係由鐵氟龍所製成。 為使本發明之上述目的、特徵和優點能更明顯易懂, 下文特舉較佳實施例並配合所附圖式做詳細說明。 【實施方式】 ... 兹配合圖式說明本發明之較佳實施例。 本發明之酸鹼值恆定自動控制溶出試驗系統乃是依據 歐盟標準局(CEN)之參考標準 TS 14997(Characterizationof waste-Leaching behaviour tests-Influence of pH on leaching with continuous pH-control)而設計,以確實掌握受試樣品 材料在不同酸鹼值下之溶出特性,並落實TS 14997中有關 連續自動滴定酸鹼液以維持初始(目標)酸鹼值恆定之方 法,得以連續紀錄溶出液之酸驗值以及每次添加峻液 < 驗 1352809 液之單次量與最後的總量。在此,Ts 14997中規範了 "設定 目標酸驗值"、"測量酸驗值之間隔時間"、"目標酸驗值容 •許範圍”、•,初始液固比"、"最終液固比超過多少時顯示失 敗”以及”最後4小時之酸驗液添加總量大於前44小時之酸 鹼液添加總量的百分比多少時顯示失敗"等試驗條件。 ^請參閱第1圖,本實施例之酸驗值怪定自動控制溶出 試驗系統1GG主要包括有—自動控制裝置nQ、複數個酸 •鹼,添加裝置12〇、複數個搜拌溶出裝s 13〇、複數個酸驗 值棟針140 $號轉換益150及複數個酸驗值測定儀16〇。 E自動控制裝置110可以是—電腦裝置’並且自動控制 裝置110可内建有-自動控制程式或軟體。在此,自動控 制程式或軟體所呈現之操作介面可供操作者輸入”設定^ 標酸驗值"、”測量酸驗值之間隔時間”、”目標酸驗值容許 範圍(例如、,正負〇.5)"、”初始液固比”、”最終液固比超過 多少(預設為】1.0)時顯示失敗,,以及”最後4小時之酸驗液 •添加總量大於前44小時之酸鹼液添加總量的百分比多少 (預設為2%)時顯示失敗”等參數。 訊號轉換益150是電性連接於自動控制裝置1丨〇。 複數個酸鹼液添加裝置12〇皆是電性連接於自動控制 裝置110。纟本實施例之中,酸驗值恆定自動控制溶出試 驗系統100是以包括有八個酸鹼液添加裝置12〇來做舉例 說明。更詳細的來說,如第丨圖及第2圖所示,每一個酸 鹼液添加裝置12G具有-空氣幫们21、—二氧化碳吸附 瓶122、一酸液容器123、一驗液容器124、一酸液分廢閥 9 ㈣分㈣126。空氣幫浦121是電性連接於訊號 D二^ ’亚且空氣幫肖121 I連通於二氧化碳吸附瓶 哭一氧化石反吸附开瓦122是連通於酸液容器123及驗液容 ii24,亦即,二氧化碳吸附瓶122是連通於空氣幫浦121 ^液容之間以及空氣幫浦121與驗液容器124之 酉文液谷S 123是連通於酸液分壓㈤125,並且酸液容 3 ^納有一酸液(例如,具有特定濃度之而ο〗溶 二。°驗液容器124是連通於驗液分壓閥126,並且驗液容 =21内容納有一驗液(例如,具有特定濃度之NaOH溶 號闕125及驗液分壓闊126皆是電性連接於訊 ’個㈣☆出裝置13()是連通於每—個酸驗液添加 =H之酸液分壓閥125及驗液分壓閥126。更詳細的 裝置η/281、帛3圖及第4圖所示’每—個攪掉溶出 ^ 具有磁攪拌$ 131、-授拌容器132、一密封蓋 、一攪拌棒134及一攪拌磁石135。 攪拌容器132是設置於磁攪拌器131之上。在本實施 例之中’攪拌容器132可以是由聚乙烯、聚丙烯或聚四氣 乙烯所製成。 费封蓋133是密封覆蓋於攪拌容器132之上。在此, 酸液分壓閥125及鹼液分壓閥126是經由密封蓋133而連 通於攪拌容器132。更詳細的來說,如第3圖及第4圖所 不,酸液分壓閥125及鹼液分壓閥120是分別藉由一酸液 輪送官125a及一鹼液輸送管126a穿過密封蓋133上之孔 1352809 洞133a及133b而連通於攪拌容器132。此外,密封蓋133 還具有一洩氣閥133c及一固定架133d。 如第2圖及第3圖所示,攪拌磁石135是設置於攪拌 容器132之中。 攪拌棒134是連接於攪拌磁石135,並且攪拌棒134 是以轉動之方式連接於密封蓋133之固定架133d,以帶動 攪拌磁石135轉動。在本實施例之中,攪拌棒134可以是 由鐵氟龍所製成。 如第1圖、第2圖及第3圖所示,每一個酸鹼值探針 140是設置於每一個攪拌溶出裝置130之中。更詳細的來 說,每一個酸鹼值探針140是經由每一個密封蓋133而設 置於每一個攪拌容器132之中。 如第1圖及第2圖所示,每一個酸鹼值測定儀160是 電性連接於每一個酸鹼值探針140與自動控制裝置110之 間。 接下來說明酸鹼值恆定自動控制溶出試驗系統1〇〇之 運作方式。 首先,可先分別設定複數個攪拌溶出裝置130所欲進 行溶出試驗之目標酸鹼值,亦即,分別設定複數個攪拌容 器132内之目標酸鹼值。舉例來說,由於本實施例之酸鹼 值恆定自動控制溶出試驗系統100具有八個攪拌溶出裝置 130(或攪拌容器132),故可利用此八個攪拌溶出裝置 130(或攪拌容器132)分別針對目標酸鹼值為pH4至pHll 來進行48小時的連續性溶出試驗。此外,操作者可利用自 11 動控市丨J程式或崎 攪拌容器132^ ]來將對應於每一個攪拌溶出裝置130(或 ,'、,,目標酸驗值標酸驗值"、',測量酸驗值之間隔時間 液添加總量大^!1.0時顯示失敗”以及,.最後4小時之酸驗 失敗”等灸勃&、則料小時之酸鹼液添加總量的2%時顯示 接著數自動控制裝置no之中。 入每-個攪及受試樣品材料萃取液同時置 封莒IV〜 出衣1 之攪拌容器132之中,並脾玄 二氣133密封覆蓋於攪拌容器⑴之上*之中亚將选 軚值探針14〇 θ β λ — · 上。在此,每一個酸 料及受1婵疋改母一個攪拌容器U2内之受試檨 =樣品材料萃取液岐合液_。 以樣4 办然後,利用電力驅使磁 中之授拌磁石135即;作。在此,_ <如上所述,在48小時的二二,内之丰功效。 個酸驗值探針⑽會在所性自動溶出實驗中,每--個_容器⑶内之隔時間到達時即量測每 驗值測定儀160來將所量:鹼:,並透過每-個酸 =合液的酸鹼值傳送至 =:攪拌容器132内 自動控制裝置m即可匈4:輪Π〇之中。此時, 值是否符合所設定之對應二票酸内之酸驗 〇·5)。倘若某—個攪拌容哭]32 各許叙圍(例如,正負 驗值容許範_如=能符合所設定 ^可屬、續進行後續的溶出試驗、.),則該授拌容 之,倘若某一個攪 1352809 拌容器132内之酸鹼值超出了所設定之對應目標酸鹼值容 許範圍(例如,正負0.5),則自動控制裝置110即會經由訊 號轉換器150發出訊號來驅使對應於該攪拌容器132之一 酸鹼液添加裝置120運作。舉例來說,當該攪拌容器132 内之混合液的酸驗值超出所設定之對應目標酸驗值容許範 圍(例如,該攪拌容器132内之酸鹼值過高而超出目標酸鹼 值容許範圍)時,自動控制裝置110會經由訊號轉換器150 來驅使該酸鹼液添加裝置120之空氣幫浦121進行空氣推 入以及驅使該酸鹼液添加裝置120之酸液分壓閥125開 啟。換言之,空氣幫浦121所推入之空氣會迫使酸液容器 123内之酸液經由酸液分壓閥125輸入至該攪拌容器132 内。同時,酸液分壓閥125會計算輸入的酸液量,並將輸 入的酸液量數據傳送至自動控制裝置110之中,以進行記 錄分析。在酸臉值探針140所量測得到之該授拌容器132 内之混合液的酸驗值符合所設定之對應目標酸驗值容許範 圍後,該攪拌容器132即可繼續進行後續的溶出試驗。類 似地,當該攪拌容器132内之混合液的酸鹼值超出所設定 之對應目標酸鹼值容許範圍(例如,該攪拌容器132内之酸 驗值過低而超出目標酸驗值容許範圍)時,自動控制裝置 110會經由訊號轉換器150來驅使該酸鹼液添加裝置120 之空氣幫浦121進行空氣推入以及驅使該酸鹼液添加裝置 120之鹼液分壓閥126開啟。換言之,空氣幫浦121所推 入之空氣會迫使鹼液容器124内之鹼液經由鹼液分壓閥 126輸入至該攪拌容器132内。同時,鹼液分壓閥126會 13 1.352809 計算輸入的驗液量,並將輸入的驗液量數據傳送至自動控 制裝置110之中,以進行記錄分析。 值得注意的是,由於空氣幫浦121所推入之空氣通常 會含有二氧化碳,故藉由二氧化碳吸附瓶122吸附去除二 氧化碳,即可使得二氧化碳不致於溶入酸液容器123内之 酸液、鹼液容器124内之鹼液及攪拌容器132内之混合液 之中,因而可避免干擾溶出試驗之過程或結果。此外,攪 拌容器132内所產生之各種反應氣體可經由密封蓋133上 之洩氣閥133c排出至酸鹼值恆定自動控制溶出試驗系統 100之外。 另外,值得一提的是,酸鹼值探針140除了具有量測 酸鹼值(pH值)的功能外,其還具有量測導電度的功能。更 具體而言,由酸鹼值探針140所量測到之導電度值數據可 傳送至自動控制裝置110,並且該導電度值數據可由自動 控制裝置110之一螢幕所顯示。 接著,在完成上述48.小時之連續酸鹼值測量與調整的 步驟後,自動控制裝置110會分析每一個攪拌容器132之 實驗數據。更詳細的來說,當某一個攪拌容器132内之最 終液固比未超過11.0以及最後4小時之酸鹼液添加總量未 大於前44小時之酸鹼液添加總量的2%時,該攪拌容器132 内之溶出實驗即代表成功,而可進行其他的溶出實驗分 析。反之,當某一個攪拌容器132内之最終液固比超過11.0 及/或最後4小時之酸鹼液添加總量大於前44小時之酸鹼 液添加總量的2%時,該攪拌容器132内之溶出實驗即代表 14 1352809 失敗,而必須再以上述48小時之連續酸鹼值測量與調整的 步驟來重新進行溶出實驗。 綜上所述,本發明所揭露之酸鹼值恆定自動控制溶出 試驗糸統可有效掌握整個貫驗過程的所有細卽,並可透過 自動化操作來減少人為誤差之發生,因而可避免透過人工 定時滴定時所造成之實驗操作過程的複雜與繁瑣。 雖然本發明已以較佳實施例揭露於上,然其並非用以 限定本發明,任何熟習此項技藝者,在不脫離本發明之精 神和範圍内,當可作些許之更動與潤飾,因此本發明之保 護範圍當視後附之申請專利範圍所界定者為準。1352809 IX. Description of the invention: [Technical field of the invention] The present invention relates to a constant pH control automatic dissolution test system, and more particularly to a method for continuously and automatically analyzing a test sample material in a continuous automated manner. The acid value of the environmental dissolution characteristics of the inorganic or organic components is arbitrarily determined to automatically control the dissolution test system. [Prior Art] In recent years, environmental dissolving analysis methods have been developed for the study of the dissolution of materials and materials. The experimental data can help to fully understand the materials under various acid and alkali conditions. The impact of the environment. The above analysis method is to simulate the dissolution of inorganic or organic substances in the test sample materials by using the principle that the test sample materials have different dissolution characteristics due to different pH values during use, so as to estimate the different acid tests. Environmental impact caused by conditions. However, the toxic characteristic dissolution procedure (TCLP) currently used in China only considers the dissolution characteristics analysis under a single pH value, which does not correctly reflect the dissolution of inorganic or organic substances under different acid-base conditions in the real environment. In addition, current material dissolution characteristics analysis is performed by manual titration, which causes analysis inconvenience and human error. In view of the above, the present invention provides a constant pH control automatic dissolution test system which can analyze the environmental dissolution characteristics of inorganic or organic components of a sample material under different and fixed pH values in a continuous automated manner. SUMMARY OF THE INVENTION The present invention includes an automatic control device; at least one acid and alkali solution is installed 6 1352809, electrically connected to the automatic control device, and has an air pump, an acid liquid container, a test liquid container, An acid liquid partial pressure valve and an inspection liquid partial pressure valve, wherein the air pump is electrically connected to the automatic control device, and is connected to the acid liquid container and the alkali liquid container, and the acid liquid container is connected The acid liquid partial pressure valve, and is provided with an acid liquid, the alkali liquid container is connected to the alkali liquid pressure dividing valve, and is provided with an alkali liquid, and the acid liquid partial pressure valve and the alkali liquid pressure dividing valve Electrically connected to the automatic control device; at least one agitating and dissolving device, the acid liquid partial pressure valve and the liquid pressure dividing valve connected to the acid-alkali adding device and containing a sample material and a test sample The test sample material extract; and at least one pH detector are disposed in the agitation dissolution device and electrically connected to the automatic control device. Meanwhile, the pH control constant automatic control dissolution test system according to the present invention further includes a signal converter electrically connected between the air pump and the automatic control device, the acid liquid pressure dividing valve and the automatic Between the control devices and between the lye partial pressure valve and the automatic control device. In the present invention, the invention further includes a signal converter electrically connected between the air pump and the automatic control device, between the acid pressure dividing valve and the automatic control device, and the lye pressure dividing valve. Between this automatic control device. In the present invention, the acid-base addition device further has a carbon dioxide adsorption bottle, and the carbon dioxide adsorption bottle is connected between the air pump and the acid container, and between the air pump and the alkali container. . In the present invention, the stirring and dissolving device has a magnetic stirrer, a stirring vessel, a sealing cap and a stirring magnet, and the stirring vessel is disposed on the magnetic pick-up device, and the day is six 〇1 The test sample material and the test sample liquid are accommodated, and the seal cover is sealed on the stirring container and the lye pressure regulating valve is connected via the sealing cover. The acid probe is disposed through the sealing cover, and the U-shaped 'and the mixed magnet are disposed in the collar container and are connected to the sealing cover in a manner of being rotated. In addition, in the present invention, the sealing cover has a wide width, and in the present invention, the (four) dissolution device further has a disturbing rod, the reading cover further has a "fixing frame", and the age bar is connected to the mixed magnet. And connected to the holder in a rotating manner. In still another aspect of the invention, the agitating vessel is made of polyethylene, polypropylene or polytetrachloroethylene. Also in the present invention, the stirring rod is made of Teflon. The above described objects, features and advantages of the present invention will become more apparent from the description of the appended claims. [Embodiment] A preferred embodiment of the present invention will be described with reference to the drawings. The pH-constant automatic control dissolution test system of the present invention is designed according to the European Standards Agency (CEN) reference standard TS 14997 (Characterization of waste-Leaching behaviour tests-Influence of pH on leaching with continuous pH-control) Master the dissolution characteristics of the tested sample materials under different pH values, and implement the method of continuous automatic titration of acid and alkali in TS 14997 to maintain the initial (target) pH value, and continuously record the acid value of the eluate and Each time you add Juncus < Check the single amount of 1352809 liquid with the final total amount. Here, Ts 14997 specifies the "set target acid test value","measures the interval between acid test values","target acid test value range,•, initial liquid-solid ratio" , "Failure when the final liquid-solid ratio exceeds the total" and "The total amount of acid test liquid added in the last 4 hours is greater than the percentage of the total amount of acid-base solution added in the first 44 hours." Referring to FIG. 1 , the acid test value automatic control dissolution test system 1GG of the present embodiment mainly includes an automatic control device nQ, a plurality of acid and alkali, an adding device 12〇, a plurality of searching and mixing devices, 13〇, The plurality of acid test pins 140$ converts 150 and the plurality of acid testers 16〇. The E automatic control device 110 can be a computer device and the automatic control device 110 can have an internal control program or software. Here, the operation interface presented by the automatic control program or software can be input by the operator to "set the calibration value of the acid value", "the interval between the measurement of the acid value", and the allowable range of the target acid value (for example, Positive and negative 〇.5)& “, “initial liquid-solid ratio”, “when the final liquid-solid ratio exceeds (preset to 1.0), it shows failure, and “the last 4 hours of acid test • the total amount of acid and alkali added is greater than the first 44 hours Add a percentage of the total amount (preset to 2%) and display a failure. The signal conversion benefit 150 is electrically connected to the automatic control device 1丨〇. A plurality of acid-base addition devices 12 are electrically connected to the automatic control device 110. In the present embodiment, the acid value constant automatic control dissolution test system 100 is exemplified by including eight acid-base addition devices 12A. More specifically, as shown in the first and second figures, each of the acid-base addition devices 12G has an air plenum 21, a carbon dioxide adsorption bottle 122, an acid liquid container 123, and a test liquid container 124. One acid liquid waste valve 9 (four) points (four) 126. The air pump 121 is electrically connected to the signal D2' and the air shield 121I is connected to the carbon dioxide adsorption bottle. The crystone anti-adsorption open tile 122 is connected to the acid container 123 and the test liquid ii24, that is, The carbon dioxide adsorption bottle 122 is connected to the air pump 121 ^ between the liquid volume and the air pump 121 and the test liquid container 124. The liquid liquid valley S 123 is connected to the acid partial pressure (five) 125, and the acid liquid capacity is 3 ^ There is an acid solution (for example, having a specific concentration). The test solution container 124 is connected to the test liquid pressure dividing valve 126, and the test liquid volume = 21 contains a test liquid (for example, a specific concentration of NaOH) The solution 阙125 and the test liquid partial pressure width 126 are electrically connected to the signal 'a (four) ☆ out device 13 () is connected to each acid test liquid addition = H acid liquid partial pressure valve 125 and test liquid Pressure valve 126. More detailed devices η / 281, 帛 3 and Figure 4 - each of the stirring dissolution ^ with magnetic stirring $ 131, - mixing container 132, a sealing cover, a stirring rod 134 and a stirring magnet 135. The stirring container 132 is disposed above the magnetic stirrer 131. In the present embodiment, the stirring container 132 may be It is made of polyethylene, polypropylene or polytetraethylene. The cover 133 is sealed over the agitating vessel 132. Here, the acid partial pressure valve 125 and the alkaline partial pressure valve 126 are via the sealing cover 133. And connected to the agitating vessel 132. In more detail, as shown in Figs. 3 and 4, the acid liquid partial pressure valve 125 and the alkaline liquid pressure dividing valve 120 are respectively provided by an acid liquid to the officer 125a and one. The lye delivery tube 126a communicates with the agitating vessel 132 through the holes 1352809 in the holes 135a and 133b of the sealing cap 133. Further, the sealing cap 133 has a deflation valve 133c and a holder 133d. As shown in Fig. 2 and Fig. 3 As shown, the agitating magnet 135 is disposed in the agitating vessel 132. The agitating bar 134 is coupled to the agitating magnet 135, and the agitating bar 134 is rotatably coupled to the fixing frame 133d of the sealing cap 133 to drive the agitating magnet 135 to rotate. In the present embodiment, the stirring rod 134 may be made of Teflon. As shown in Figures 1, 2 and 3, each pH probe 140 is provided for each stirring. In the dissolution device 130. In more detail, each of the pH probes 140 is via A sealing cover 133 is disposed in each of the agitating containers 132. As shown in Figures 1 and 2, each of the pH indicators 160 is electrically connected to each of the pH sensors 140 and is automatically controlled. Between the devices 110. Next, the operation mode of the constant pH control automatic dissolution test system will be described. First, the target pH values of the plurality of agitation dissolution devices 130 to be subjected to the dissolution test may be separately set, that is, The target pH values in the plurality of stirred vessels 132 are set separately. For example, since the pH-constant automatic control dissolution test system 100 of the present embodiment has eight agitation dissolution devices 130 (or agitation vessels 132), the eight agitation dissolution devices 130 (or the agitation vessels 132) can be utilized, respectively. A 48-hour continuous dissolution test was carried out for the target pH value from pH 4 to pH 11. In addition, the operator can use the 11 dynamic control system or the kneading container 132^] to correspond to each of the agitation dissolution devices 130 (or, ',,, the target acid value is the acid value ", ' At the interval between the measurement of the acid value, the total amount of the liquid addition is large, the value of the liquid addition is ^, 1.0, and the failure of the last 4 hours of the acid test, etc., and the amount of the acid and alkali solution added for the hour is 2%. The following is displayed in the automatic control device no. Into each of the stirred sample material extracts, the argon IV~ clothes 1 is stirred in the agitating container 132, and the spleen and the second gas 133 are sealed and covered in the stirring container. (1) Above * Central Asia will select the 軚 value probe 14 〇 θ β λ — ·. Here, each acid material and one tamper is tested in a stirred vessel U2 = sample material extract 岐The liquid mixture _. Take the sample 4 and then use the electric power to drive the magnetic 135 in the magnetic field; here, _ < as described above, in the 48 hours of the second, the effect of the abundance. The probe (10) will measure each tester when it arrives in each of the _ containers (3) in the automatic dissolution test. 160 to measure the amount: alkali:, and through the acid value of each acid = mixture to the = =: the automatic control device m in the mixing container 132 can be hungry 4: rim. At this time, the value is It meets the acid test in the corresponding two-voort acid set. 5). If a certain kind of stirring and crying] 32 Xu Xuan (for example, the positive and negative test allowable _ _ = can meet the set ^ can be, continue to carry out the subsequent dissolution test, .), then the mix, if If the pH value of the stirred 1352809 mixing container 132 exceeds the set target corresponding pH value (for example, plus or minus 0.5), the automatic control device 110 sends a signal via the signal converter 150 to drive the corresponding value. The acid-base addition device 120 of one of the agitation vessels 132 operates. For example, when the acid value of the mixed solution in the stirring vessel 132 exceeds the set target acid tolerance value (for example, the pH value in the stirring vessel 132 is too high and exceeds the target acid-base allowable range). When the automatic control device 110 drives the air pump 121 of the acid-base addition device 120 to push the air through the signal converter 150 and drive the acid partial pressure valve 125 of the acid-base addition device 120 to open. In other words, the air pushed in by the air pump 121 forces the acid in the acid container 123 to be introduced into the agitating vessel 132 via the acid pressure dividing valve 125. At the same time, the acid partial pressure valve 125 calculates the amount of acid input and transmits the input acid amount data to the automatic control unit 110 for recording analysis. After the acid test value of the mixed liquid in the mixing container 132 measured by the acid face value probe 140 meets the allowable range of the corresponding target acid test value, the stirring container 132 can continue the subsequent dissolution test. . Similarly, when the pH value of the mixed liquid in the stirring vessel 132 exceeds the set target corresponding pH value (for example, the acid value in the stirring vessel 132 is too low and exceeds the target acid value tolerance range) At this time, the automatic control device 110 drives the air pump 121 of the acid-base addition device 120 to push the air through the signal converter 150 and drive the alkali partial pressure valve 126 of the acid-base addition device 120 to open. In other words, the air pushed in the air pump 121 forces the lye in the lye container 124 to be introduced into the agitating vessel 132 via the lye pressure dividing valve 126. At the same time, the lye partial pressure valve 126 13 13 352 809 calculates the input test volume, and transmits the input test volume data to the automatic control device 110 for recording analysis. It is to be noted that since the air pushed in the air pump 121 usually contains carbon dioxide, the carbon dioxide adsorbing bottle 122 adsorbs and removes carbon dioxide, so that the carbon dioxide is not dissolved in the acid liquid or the lye in the acid container 123. The lye in the container 124 and the mixture in the agitating vessel 132 are such that the process or result of the dissolution test can be avoided. Further, various reaction gases generated in the agitating vessel 132 can be discharged to the pH-constant automatic control dissolution test system 100 via the bleed valve 133c on the sealing cover 133. In addition, it is worth mentioning that the pH sensor 140 has a function of measuring conductivity in addition to the function of measuring pH (pH). More specifically, the conductivity value data measured by the pH sensor 140 can be communicated to the automatic control device 110, and the conductivity value data can be displayed by one of the screens of the automatic control device 110. Next, after completing the above-described 48 hours of continuous pH measurement and adjustment steps, the automatic control unit 110 analyzes the experimental data of each of the agitating vessels 132. In more detail, when the final liquid-solid ratio in a certain agitating vessel 132 is less than 11.0 and the total amount of acid-base solution added in the last 4 hours is not more than 2% of the total amount of acid-base solution added in the first 44 hours, The dissolution test in the agitating vessel 132 represents success and other dissolution experiments can be performed. On the other hand, when the total liquid-solid ratio in a certain agitating vessel 132 exceeds 11.0 and/or the total amount of acid-base solution added in the last 4 hours is greater than 2% of the total amount of acid-base solution added in the first 44 hours, the stirring vessel 132 is inside. The dissolution test represents 14 1352809 failure, and the dissolution test must be repeated with the above 48 hours of continuous pH measurement and adjustment steps. In summary, the constant pH-controlled automatic dissolution test system disclosed in the present invention can effectively grasp all the details of the entire inspection process, and can reduce the occurrence of human error through automatic operation, thereby avoiding manual timing. The experimental operation caused by the titration is complicated and cumbersome. Although the present invention has been disclosed in its preferred embodiments, it is not intended to limit the present invention, and it is possible to make some modifications and refinements without departing from the spirit and scope of the present invention. The scope of the invention is defined by the scope of the appended claims.

15 1-352809 【圖式簡單說明】 第1圖係顯示本發明之酸鹼值恆定自動控制溶出試驗 系統之一種平面示意圖; 第2圖係顯示本發明之酸鹼值恆定自動控制溶出試驗 系統之另一種平面示意圖; 第3圖係顯示本發明之酸驗值怪定自動控制溶出試驗 系統之攪拌溶出裝置之側視示意圖;以及 第4圖係顯示本發明之酸鹼值恆定自動控制溶出試驗 系統之攪拌溶出裝置之俯視示意圖。 【主要元件符號說明】 100〜酸驗值恆定自動控制溶出試驗系統 110〜自動控制裝置 120〜酸鹼液添加裝置 121〜空氣幫浦 122〜二氧化碳吸附瓶 123〜酸液容器 124〜鹼液容器 125〜酸液分壓閥 125 a〜酸液輸送管 126〜驗液分壓閥 126a〜驗液輪送管 130〜攪拌溶出裝置 131〜磁攪拌器 132〜攪拌容器 16 L352809 133〜密封蓋 133a、133b〜孔洞 133c〜洩氣閥 133d〜固定架 134〜攪拌棒 135〜攪拌磁石 140〜酸鹼值探針 150〜訊號轉換器 160〜酸鹼值測定儀15 1-352809 BRIEF DESCRIPTION OF THE DRAWINGS Fig. 1 is a schematic plan view showing a constant automatic controlled dissolution test system for pH and pH of the present invention; Fig. 2 is a view showing a constant automatic controlled dissolution test system for pH of the present invention. Another schematic plan view; Fig. 3 is a side view showing the stirring and dissolving device of the acid test value automatic control dissolution test system of the present invention; and Fig. 4 is a view showing the constant pH automatic control dissolution test system of the present invention. A schematic plan view of the stirring and dissolving device. [Description of main component symbols] 100 to acid constant constant automatic control dissolution test system 110 to automatic control device 120 to acid-base addition device 121 to air pump 122 to carbon dioxide adsorption bottle 123 to acid container 124 to alkali solution container 125 ~ Acid liquid pressure dividing valve 125 a - acid liquid conveying pipe 126 - liquid measuring pressure dividing valve 126a - liquid measuring wheel feeding pipe 130 - stirring and discharging device 131 - magnetic stirring device 132 - stirring container 16 L352809 133 - sealing cover 133a, 133b ~ Hole 133c ~ vent valve 133d ~ holder 134 ~ stirring rod 135 ~ stirring magnet 140 ~ pH probe 150 ~ signal converter 160 ~ pH meter

Claims (1)

1-352809 十、申請專利範園: 1.一種酸鹼值恆定自動控制溶出試驗系統,包括 一自動控制裝置; 至少-酸驗液添加裝置,電性連接於該自動控制裝 置,並且具有一空氣幫浦、一酸液容器、一鹼液容器、一 酸液分壓閥及-驗液分壓閥,其中,該空氣幫浦係^性連 接=該自動控㈣置,並且係連通於該酸液容器及該驗液 容器,該酸液容器係連通於該酸液分壓閥,並且係容納有 一酸液,該鹼液容器係連通於該鹼液分壓閥,並且係容納 有一鹼液,以及該酸液分壓閥及該鹼液分壓閥係電性捲 於該自動控制裝置; 至少一攪拌溶出裝置,連通於該酸鹼液添加裝置之哼 酸液分壓閥及⑽液分㈣,並且容财—钱樣品材^ 及一受試樣品材料萃取液;以及1-352809 X. Patent application garden: 1. A constant pH control automatic dissolution test system, including an automatic control device; at least an acid test liquid addition device electrically connected to the automatic control device and having an air a pump, an acid liquid container, an lye container, an acid liquid pressure dividing valve and a liquid pressure dividing valve, wherein the air pumping system is connected to the automatic control (four) and is connected to the acid a liquid container and the liquid test container, wherein the acid liquid container is connected to the acid liquid pressure dividing valve, and is provided with an acid liquid, the alkali liquid container is connected to the alkaline liquid partial pressure valve, and is provided with an alkali liquid, And the acid liquid pressure dividing valve and the alkali liquid pressure dividing valve are electrically wound on the automatic control device; at least one stirring and discharging device, the tannic acid partial pressure valve connected to the acid alkali adding device, and (10) liquid (4) And a wealth of money-money sample material ^ and a test sample material extract; 至少一酸鹼值探針,設置於該攪拌溶出裝置之中,並 且電性連接於該自動控制裝置。 、’ 一 ^如申請專利範圍第i項所述之酸鹼值惺定自動控制 溶出試驗系統,更包括—訊號轉換^,係電性連接於該空 氣幫浦與該自動控制裝置之間、該酸液分壓_該自動= 制裝置之間以及该驗液分壓閥與該自動控制裝置之間。 水如申請專利範圍第1項所述之酸鹼值恆定自動控制 岭出系統,更包括一酸鹼值測定儀,係電性 酸鹼值探針與該自動控制裝置之間。 ;' 申明專利範圍第1項所述之酸驗值丨互定自動控制 18 1352809 溶出試驗系統,其中,該酸驗液添加裝置更具有一二氧化 碳吸附瓶,以及該二氧化碳吸附瓶係連通於該空氣幫浦與 該酸液容器之間以及該空氣幫浦與該鹼液容器之間。 5. 如申請專利範圍第1項所述之酸鹼值恆定自動控制 溶出試驗系統,其中,該攪拌溶出裝置具有一磁攪拌器、 一攪拌容器、一密封蓋及一攪拌磁石,該攪拌容器係設置 於該磁攪拌器之上,並且係容納有該受試樣品材料及該受 試樣品材料萃取液,該密封蓋係密封覆蓋於該攪拌容器之 上,該酸液分壓閥及該鹼液分壓閥係經由該密封蓋而連通 於該攪拌容器,該酸鹼值探針係經由該密封蓋而設置於該 攪拌容器之中,以及該攪拌磁石係設置於該攪拌容器之 中,並且係以轉動之方式連接於該密封蓋。 6. 如申請專利範圍第5項所述之酸鹼值恆定自動控制 溶出試驗系統,其中,該密封蓋具有一洩氣閥。 7. 如申請專利範圍第5項所述之酸鹼值恆定自動控制 溶出試驗系統,其中,該攪拌溶出裝置更具有一攪拌棒, 該密封蓋更具有一固定架,以及該攪拌棒係連接於該攪拌 磁石,並且係以轉動之方式連接於該固定架。 8. 如申請專利範圍第5項所述之酸鹼值恆定自動控制 溶出試驗系統,其中,該攪拌容器係由聚乙烯、聚丙烯或 聚四氯乙烯所製成。 9. 如申請專利範圍第7項所述之酸鹼值恆定自動控制 溶出試驗糸統’其中’該授掉棒係由鐵氣龍所製成。 19At least one pH probe is disposed in the agitation dissolution device and electrically connected to the automatic control device. [1] The acid-base determination automatic control dissolution test system described in item i of the patent application scope, further includes a signal conversion ^, electrically connected between the air pump and the automatic control device, Acid partial pressure _ this automatic = between the devices and between the test fluid pressure valve and the automatic control device. Water, as described in the first paragraph of the patent application, has a constant pH control automatic control system, and further includes a pH detector, between the electrical pH sensor and the automatic control device. ; 'Declaration of the acid range described in the first paragraph of the patent range 丨 mutual automatic control 18 1352809 dissolution test system, wherein the acid test liquid addition device has a carbon dioxide adsorption bottle, and the carbon dioxide adsorption bottle is connected to the air Between the pump and the acid container and between the air pump and the lye container. 5. The pH control constant automatic controlled dissolution test system according to claim 1, wherein the agitation dissolution device has a magnetic stirrer, a stirring vessel, a sealing cap and a stirring magnet, and the stirring vessel is Provided on the magnetic stirrer, and containing the test sample material and the test sample material extract, the seal cover is sealed on the stirring container, the acid partial pressure valve and the alkali solution a pressure dividing valve is connected to the stirring container via the sealing cover, the pH sensor is disposed in the stirring container via the sealing cover, and the stirring magnet is disposed in the stirring container, and is It is connected to the sealing cover in a rotating manner. 6. The pH control constant automatic controlled dissolution test system of claim 5, wherein the sealing cap has a bleed valve. 7. The pH control constant automatic controlled dissolution test system according to claim 5, wherein the agitation dissolution device further comprises a stirring rod, the sealing cover further has a fixing frame, and the stirring rod is connected to the stirring rod The agitating magnet is coupled to the holder in a rotational manner. 8. The pH-controlled constant automatic controlled dissolution test system according to claim 5, wherein the stirred vessel is made of polyethylene, polypropylene or polytetrachloroethylene. 9. The constant pH control of the pH value as described in item 7 of the patent application. The dissolution test system 'where' the transfer rod is made of iron gas dragon. 19
TW96150258A 2007-12-26 2007-12-26 Automatic leaching test system with constant ph co TWI352809B (en)

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