TW200928356A - Automatic leaching test system with constant pH control - Google Patents

Automatic leaching test system with constant pH control Download PDF

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Publication number
TW200928356A
TW200928356A TW96150258A TW96150258A TW200928356A TW 200928356 A TW200928356 A TW 200928356A TW 96150258 A TW96150258 A TW 96150258A TW 96150258 A TW96150258 A TW 96150258A TW 200928356 A TW200928356 A TW 200928356A
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Taiwan
Prior art keywords
acid
automatic control
liquid
control device
test
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TW96150258A
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Chinese (zh)
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TWI352809B (en
Inventor
Chung-Chih Chen
Jinn-Shiou Hwang
Chia-Lun Kuan
Suen-Chu Hsu
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Ind Tech Res Inst
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Abstract

An automatic leaching test system with constant pH control includes an automatic control device, an acid/lye replenishing device, a stir leaching device, and a pH probe. The acid/lye replenishing device is electrically connected to the automatic control device and includes an air pump, an acid container, a lye container, an acid pressure dividing valve, and a lye pressure dividing valve. The air pump is electrically connected to the automatic control device and connects to the acid and lye containers. The acid container connects to the acid pressure dividing valve and accommodates acid. The lye container connects to the lye pressure dividing valve and accommodates lye. The acid and lye pressure dividing valves are electrically connected to the automatic control device. The stir leaching device connects to the acid and lye pressure dividing valves. The pH probe is disposed in the stir leaching device and electrically connected to the automatic control device.

Description

200928356 九、發明說明: 【發明所屬之技術領域] 本發明是有關於-種酸驗值恒定自動 統,特別是有關於一種以連續自動化 合出〃糸 料在不同且固定酸驗值下之無機或有二二析文5式樣:材 性之酸驗值悝定自動控制溶出試驗系^成份之環境溶出特 【先前技術】 ❹ 近年來,針對廢棄物與材料溶出+ 不同酸驗值下環境性溶出分析法已被4研;而言,各種 幫助全面瞭解材料在各種不同酸驗條;對,、實驗數據可 衝擊。上述之分析法乃是利用受試樣品^環境所造f之 會因不同酸驗值而有不同溶出特性之1使用過私中 品材料中無機物或有機物之溶出情形受試樣 條件下所造成之環境衝擊。然而,國内目ΐ =不同酸驗 參 毒性特性溶出程序()僅考慮單一=;=: 分析,苴I、、也. 值下之/谷出特性 有機物質反應真實環境中不同酸驗條件下無機或 是以人工、、/:!情形。此外’目前的材料溶出特性分析皆 人AM (之方式來執行,因而會造成分析上的不便及 人為te作誤差的發生。 π个便及 試驗於此,本發明提供—種酸驗值定自動控制溶出 同且固’其可以連續自動化方式分析受試樣品材料在不 疋酸鹼值下之無機或有機成份之環境溶出 【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 200928356 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、一酸液分壓閥及一鹼液分壓閥, 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 © 該鹼液分壓閥,並且容納有一受試樣品材料及一受試樣品 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。 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 7 200928356200928356 IX. Description of the invention: [Technical field to which the invention pertains] The present invention relates to a constant acid automatic test system, and more particularly to an inorganic material which is continuously automated and has a different fixed acid value. Or there are two or two analytic texts: the acidity test of the materiality, the automatic control of the dissolution test system, the environmental dissolution of the components, [previous techniques] 近年来 In recent years, the environmental and environmental properties of waste and material dissolution + different acid test The dissolution analysis method has been studied 4; in terms of various, it helps to comprehensively understand the material in various acid strips; and, the experimental data can be impacted. The above analysis method is based on the test sample ^ environment made f will have different dissolution characteristics due to different acid test values. 1 The use of inorganic or organic substances in the private medium material is dissolved under the conditions of the sample. Environmental impact. However, domestically witnessed = different acid test toxicity characteristics dissolution procedure () only consider single =; =: analysis, 苴I,, also. Under the value of / grain out characteristics of organic matter reaction in the real environment under different acid conditions Inorganic or artificial, /:! In addition, the analysis of current material dissolution characteristics is performed by AM (the method is implemented, which causes the inconvenience of analysis and the occurrence of error by artificial te. π 便便 and test here, the present invention provides an acid test value automatically Controlling dissolution and solidification, which can continuously and automatically analyze the environmental dissolution of the inorganic or organic components of the test sample material under the pH value. SUMMARY OF THE INVENTION The present invention includes an automatic control device; at least one acid-base solution is added. Mounted in 200928356, electrically connected to the automatic control device, and having an air pump, an acid liquid container, a lye container, an acid pressure dividing valve and an lye partial pressure valve, wherein the air pump Electrically connected to the automatic control device, and connected to the acid liquid container and the alkali liquid container, the acid liquid container is connected to the acid liquid pressure dividing valve, and is accommodated with an acid liquid, the alkali liquid container Connected to the lye pressure dividing valve, and accommodating an alkali liquid, and the acid liquid pressure dividing valve and the lye partial pressure valve are electrically connected to the automatic control device; at least one stirring and discharging device, The acid liquid pressure dividing valve and the alkali liquid pressure dividing valve connected to the acid alkali adding device, and containing a test sample material and a test sample material extract; and at least one pH value probe, setting And in the stirring and dissolving 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 to the air gang Between the pump and the automatic control device, between the acid pressure dividing valve and the automatic control device, and between the lye partial pressure valve and the automatic control device. In the present invention, a signal converter is further included. Electrically connected between the air pump and the automatic control device, between the acid pressure dividing valve and the automatic control device, and between the lye partial pressure valve and the automatic control device. The acid test liquid adding device further has a carbon dioxide adsorption bottle, and the carbon dioxide adsorption bottle is connected between the air pump and the acid liquid container and between the air pump and the alkali liquid container. In the present invention, the stirring device having a dissolution magnetic stirrer, a stirring vessel, a stirring magnet and a sealing cover, which is provided in the mixing container based 7200928356

石,並且係以轉動之方式連接於該固定架。· 又在本發明中,該授掉容器係由聚乙烯、聚丙稀或聚 該磁 n ·*·φ 樣品 上, 於該攪拌容器, 攪拌容器之中, 中,並且係以艟 ❹密封蓋更具有一固定架 四鼠乙稀所製成。 叫衣i又具有一攪拌榉,該 以及該攪拌棒係連接於該攪拌磁 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】 / 茲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(Characterization of 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)酸驗值恆定之方 法,得以連續紀錄溶出液之酸鹼值以及每次添加酸液或驗 8 200928356 液之單次量與最後的總量。在此’ TS 14997中規範了,,設定 目標酸鹼值π、”測量酸鹼值之間隔時間”、"目標酸鹼值容 許範圍”、”初始液固比”、"最終液固比超過多少時顯示失 敗”以及”隶後4小時之酸驗液添加總量大於前44小時之酸 驗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,本實施例之酸鹼值恆定自動控制溶出 試驗系統100主要包括有一自動控制裝置11〇、複數個酸 鹼液添加裝置120、複數個攪拌溶出裝置13〇、複數個酸鹼 °值探針140、一訊號轉換器150及複數個酸鹼值測定儀160。 自動控制裝置110可以是一電腦裝置,並且自動控制 裝置110可内建有一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”設定目 標酸鹼值"、”測量酸鹼值之間隔時間"、”目標酸鹼值容許 範圍(例如、,正貞0.5)”、”初始液固比”、”最終液固比超過 多少(預設為11.0)時顯示失敗"以及,,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百分比 (預设為2%)時顯示失敗”等參數。 訊號轉換器15〇是電性連接於自動控制裝置η〇。 複數個酸驗液添加裝置12G皆是電性 裝置110。在本實施例之中,辦—A 目醫' ^ 4貝犯1夕中,酸鹼值恆定自動控 驗系統⑽是以包括有八個酸驗液添 ; 說明。更詳細_,如第心帛2目^ m 鹼液添加裝置12〇具有—空氣 一母個画 瓶】22、-酸液容器⑵、, —氧化碳吸% 驗液备m 124、一酸液分壓般 9 200928356 125及-鹼液分壓閥126。空氣幫浦121是 轉換器150,並且空氣幫浦121是連通 == r;2:氧r一122是連通於錄^ 氧化碳吸附瓶122是連通於空氣幫浦⑵ ”欠、各态123之間以及空氣幫浦121與鹼液容器^斗之 :。酸液容器123是連通於酸液分壓㈣,並:酸液容 内容納有一酸液(例如,具有特定濃度之丽〇3溶 懸 ^。^液“124是連通於驗液分㈣126,並且驗液容 二124内容納有—驗液(例如’具有特定濃度之制h溶 夜)。1液分壓閥125及鹼液分壓閥12 號轉換器150。 〜注連接於訊 =_拌溶出裝置⑽是連通於每—個酸驗液添加 來說液分壓閥125及鹼液分壓閥126。更詳細的 f置^^圖、#3圖及第4圖所示,每―個授掉溶出 =置!:具有一磁㈣器131、—授拌容器132、一密封蓋 攪拌棒134及一攪拌磁石135。 Ϊ拌容器132是設置於磁攪拌器131之上。在本實施 乙烯所製成。 疋由來乙烯、承丙烯或聚四氯 密封蓋133是密封覆蓋於授掉容器132之上。在此, 酸液分壓閥125及鹼液分壓閱126是經 通於攪拌容132。f4^ _件谷益132更汗細的來說,如第3圖及第4圖所 分壓閥125及驗液分壓閥126是分別藉由-酸液 則达官125a及-驗液輸送管12如穿過密封蓋133上之孔 10 200928356 而連通於攪拌容器132。此外,密封蓋133 ^33C及一固定架133d。 第3圖所示,攪拌磁石135是設置於攪拌 日是連接於㈣磁石135,並且麟棒134 ί拌磁石135 L連接於密封蓋133之固定架133d’以帶動 搜拌磁石135轉動。太士麻 ❹ 洞 133a 及 133b 還具有一汽氣閥 如第2圖及 容器132之中。 由鐵IL龍所製成。 4例之中,麟棒134可以是 如第1圖、第2111¾當, θ 圖及第3圖所示,每一個酸驗值探針 Η0是設置於每一個搏妓、々b叫· 丨u敗赋阻休τ _ . 攪拌,奋出裝置130之中。更詳細的來 §兄,母一個酸鹼值探針丨 要认卜J ^ Τ ϋ疋經由母一個密封蓋133而設 置於每一個攪拌容器132之中。 如弟1圖及莖> 電性連接於每—個酸:值二母一個酸驗值測定儀160是 間。 们I奴值探針14〇與自動控制裝置110之 運作=來說明酸驗值怪定自動控制溶出試驗系統謂之 行溶:設定複數個授拌溶出裝置130所欲進 器分別設定複數個餅容 值恆定自馳_以糖_1(;=本錢例之酸驗 娜或_容器132),故;辦溶出裝置 130(或擦拉六。。、彳,0、ν , Ύ利用此八個攪拌溶出裝置 Am ^ AQ 刀另,針對目標酸驗值為pH4至pHll 末進盯48小時的連續性”試驗。此外,操作者可利用自 200928356 動控制程式或軟體來將對應於每一個攪拌溶出裝置 攪拌容器132)之”目標酸鹼值”、”測量酸鹼值之間隔時^ ,'、,,目標酸鹼值容許範圍(例如’正負0.5)”、”初始液固比,, "最終液固比超過11.0時顯示失敗"以及π最後4小時之酸& 液添加總量大於前44小時之酸鹼液添加總量的2%時顯= 失敗"等參數輸入至自動控制裝置110之中。 不Stone, and is connected to the holder in a rotating manner. In the present invention, the transfer container is made of polyethylene, polypropylene or a sample of the magnetic n·*·φ, in the stirring container, in the stirring container, and in a sealed lid. It has a fixed frame made of four mice. The garment i has a stirring crucible, and the stirring rod is attached to the stirring magnet. 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 behaviours-Influence of pH on leaching with continuous pH-control) It is true that the dissolution characteristics of the test sample materials under different pH values are known, and the method of continuously auto-titrating the acid-base solution in TS 14997 to maintain the initial (target) acid value constant is continuously performed, so that the pH value of the eluate can be continuously recorded. And each time you add acid or test 8 200928356 liquid single amount and the final total. It is specified in this 'TS 14997, setting the target pH value π, "measuring the interval between pH values", "target pH range allowable range", "initial liquid-solid ratio", "final liquid-solid ratio If the number of times exceeds the display failure, and the total amount of the acid test liquid added after 4 hours is greater than the percentage of the total amount of the acid test liquid added in the first 44 hours, the test condition is displayed. Referring to FIG. 1 , the pH control constant automatic control dissolution test system 100 of the embodiment mainly includes an automatic control device 11 , a plurality of acid and alkali liquid addition devices 120 , a plurality of stirring and dissolution devices 13 , and a plurality of acid and alkali. The value probe 140, a signal converter 150, and a plurality of pH indicators 160. The automatic control device 110 can be a computer device, and the automatic control device 110 can have an automatic control program or software built in. Here, the operation interface presented by the automatic control program or software can be input by the operator to "set the target pH value", "measure the interval between pH values", and the target acid-base allowable range (for example, positive贞0.5)", "initial liquid-solid ratio", "when the final liquid-solid ratio exceeds (preset to 11.0), it shows failure" and, in the last 4 hours, the total amount of acid-base solution is greater than the first 44 hours. The percentage of the total amount of acid and alkali added (preset to 2%) shows a failure and other parameters. The signal converter 15A is electrically connected to the automatic control device 〇. A plurality of acid test liquid addition devices 12G are all electrical devices 110. In the present embodiment, the laboratory--------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------- More detailed _, such as the first heart 帛 2 mesh ^ m lye addition device 12 〇 has - air a mother bottle] 22, - acid container (2), - oxidized carbon absorbing % test liquid preparation m 124, an acid solution Partial pressure like 9 200928356 125 and - lye partial pressure valve 126. The air pump 121 is the converter 150, and the air pump 121 is connected == r; 2: the oxygen r-122 is connected to the recording carbon oxide adsorption bottle 122 is connected to the air pump (2) "under, each state 123 Between the air pump 121 and the lye container: the acid container 123 is connected to the acid partial pressure (4), and the acid solution contains an acid solution (for example, a certain concentration of Lishen 3 is suspended) ^液液"124 is connected to the test liquid (4) 126, and the test liquid volume 124 contains the contents of the test (for example, 'having a specific concentration of h dissolved night). 1 liquid partial pressure valve 125 and lye partial pressure Valve No. 12 converter 150. ~ Note connected to the signal = _ mixing and dissolving device (10) is connected to each acid test liquid addition liquid pressure divider valve 125 and lye pressure divider valve 126. More detailed f ^ ^ As shown in Fig. 3 and Fig. 4, each of the dispensed dissolution = set! has a magnetic (four) device 131, a mixing container 132, a sealing cap stirring rod 134 and a stirring magnet 135. 132 is disposed above the magnetic stirrer 131. It is made of ethylene in the present embodiment. The vinyl, propylene or polytetrachloride sealing cover 133 is sealed to cover the transfer container 13 2. Above, the acid partial pressure valve 125 and the lye partial pressure reading 126 are passed through the stirring capacity 132. The f4^ _ piece 谷益132 is more sweaty, as shown in Fig. 3 and Fig. 4 The pressure dividing valve 125 and the liquid pressure dividing valve 126 are respectively connected to the stirring container 132 by the -acid liquid reaching the official 125a and the liquid measuring delivery tube 12, such as through the hole 10 200928356 on the sealing cover 133. In addition, the sealing The cover 133 ^33C and a fixing frame 133d. As shown in Fig. 3, the agitating magnet 135 is disposed on the stirring day to be connected to the (four) magnet 135, and the rib 134 ф magnet 135 L is attached to the fixing frame 133d' of the sealing cover 133. In order to drive the magnet 135 to rotate, the 133a and 133b holes also have a gas valve such as the second figure and the container 132. It is made of iron IL dragon. Among the 4 cases, the lining 134 can be as In Fig. 1, 21113⁄4, θ and Fig. 3, each acid test probe Η0 is set in each beat, 々b called 丨u 赋 阻 τ τ _ . In the device 130. More detailed § brother, the mother a pH value probe to recognize the J ^ Τ ϋ疋 through the mother a sealing cover 133 and set in each mixing capacity In the middle of the device 132. If the brother 1 and the stem > are electrically connected to each acid: the value of the second mother and one acid tester 160 is between. The operation of the slave I 14 and the operation of the automatic control device 110 = to illustrate the acid test value of the automatic control of the dissolution test system is said to dissolve: set a plurality of mixing and dissolving device 130 to enter the device to set a plurality of cake values constant self-satisfaction _ with sugar _1 (; = cost example Acid chlorination or _ container 132), therefore; do the dissolution device 130 (or wipe the six. . , 彳, 0, ν, Ύ Use the eight stirring and dissolving device Am ^ AQ knife to test the target acid for the duration of pH 4 to pH □ for 48 hours. In addition, the operator can use from 200928356 The control program or software will correspond to the "target pH value" of each of the agitating and dissolving device agitating vessel 132), "measure the interval between pH values, ^, ',, the target acid-base allowable range (eg 'plus or minus 0.5 "," initial liquid-solid ratio, "final liquid-solid ratio exceeds 11.0, showing failure" and π last 4 hours of acid & total addition of liquid is greater than 2% of the total amount of acid and alkali added in the first 44 hours The parameters such as time = failure " are input to the automatic control device 110. Do not

接著,將受試樣品材料及受試樣品材料萃取液同時 入每一個攪拌溶出裝置130之攪拌容器132之中,並=六 封蓋133密封覆蓋於攪拌容器132之上。在此,每—個^ 鹼值探針140是浸入每一個攪拌容器132内之受試樣尸 料及受試樣品材料萃取液的混合液中。 然後,利用電力驅使磁攪拌器131運作。在此,攪拌 容器132中之攪拌磁石135即會因磁攪拌器131之磁場交 替變化而轉動,因而可達成攪拌容器132内之攪拌功效二 如上所述,在48小時的連續性自動溶出實驗中,每一 個酸鹼值探針140會在所設定之間隔時間到達時即量測每 一個攪拌容器132内之混合液的酸鹼值,並透過每一個酸 鹼值測定儀160來將所量測得到之每一個攪拌容器132内 之混合液的酸鹼值傳送至自動控制袭置11〇之中。此時, 自動控制裝置11G gp可判讀每—個㈣容器132内之酸驗 值疋否符合所没疋之對應目標酸鹼值容許範圍(例如,正負 〇.5)。倘若某-侧拌容器132内之酸鹼值能符合所設定 之對應目標酸鹼值容許範圍(例如,正負〇5),則該攪拌容 器m可繼續進行後續的溶出試驗。反之,倘若某一個授 200928356 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。在酸鹼值探針140所量測得到之該攪拌容器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 200928356 計算輸入的鹼液量’並將輸入的鹼液量數據傳送至自動控 制裝置110之中,以進行記錄分析。 值付注思的疋’由於空氣奮浦121所推入之空氣通常 會含有一氧化奴,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=,因而可避免干擾溶出試驗之過程或結果。此外,攪 ❾芈谷:132内所產生之各種反應氣體可經由密封蓋133上 洩氣閥133c排出至酸鹼值恆定自動控制溶出試驗系統 1〇〇之外。 另外’值得一提的是,酸驗值探針14〇除了具有量測 敲鹼值(pH值)的功能外’其還具有量測導電度的功能。更 ” s ’由酸鹼值探針14〇所量測到之導電度值數據可 傳送至自動控制裝置11〇,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。 ❹ 接著’在完成上述48小時之連續酸鹼值測量與調整的 二驟後’自動控制裝置110會分析每一個攪拌容器132之 二驗數據。更詳細的來說,當某一個攪拌容器132内之最 終液,比未超過11〇以及最後4小時之酸鹼液添加總量未 大於如44小時之酸驗液添加總量的2%時,該攪拌容器132 '谷出Λ驗即代表成功,而可進行其他的溶出實驗分 析反之’當某—個攪拌容器132内之最終液固比超過η.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 200928356 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 試驗系統可有效掌握整個實驗過程的所有細節,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 ❿ 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。 ❿ 15 200928356 【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鹼值恆定自動控制溶出試驗 系統之攪拌溶出裝置之侧視示意圖;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 ❹ 系統之攪拌溶出裝置之俯視示意圖。 【主要元件符號說明】 100〜酸驗值恒_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 125a〜酸液輸送管 126〜驗液分壓閥 126a〜驗液輸送管 130〜攪拌溶出裝置 131〜磁攪拌器 132〜攪拌容器 16 200928356 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 ❹ 160〜酸鹼值測定儀Next, the test sample material and the test sample material extract are simultaneously introduced into the agitation vessel 132 of each of the agitation dissolution apparatus 130, and the six seals 133 are sealed to cover the agitating vessel 132. Here, each of the alkalinity probes 140 is a mixture of the sample carcass and the test sample material extract immersed in each of the agitating vessels 132. Then, the magnetic stirrer 131 is operated by electric power. Here, the agitating magnet 135 in the agitating vessel 132 is rotated by the alternating magnetic field of the magnetic agitator 131, so that the stirring effect in the agitating vessel 132 can be achieved as described above in the 48-hour continuous automatic dissolution test. Each of the pH detectors 140 measures the pH value of the mixture in each of the stirred vessels 132 at the set interval time and passes the measurement through each of the pH analyzers 160. The pH value of the mixture in each of the obtained agitating vessels 132 is transferred to the automatic control set 11〇. At this time, the automatic control device 11G gp can determine whether the acid test value in each of the (four) containers 132 meets the corresponding target acid-base allowable range (for example, plus or minus 5.5). If the pH in the side-mixing vessel 132 can meet the set target acid-base allowable range (e.g., plus or minus 5), the agitating vessel m can continue the subsequent dissolution test. On the other hand, if the pH value of a given 200928356 mixing container 132 exceeds the set target corresponding pH value (for example, plus or minus 0.5), the automatic control device 110 will send a signal via the signal converter 150 to drive The acid-base addition device 120 corresponding to one of the agitating 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 adding device 120 to perform air push-in and the acid-pressure dividing valve 125 of the acid-base adding device 120 is turned on. 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. The agitating vessel 132 can continue the subsequent dissolution test after the acidity of the mixture in the stirred vessel 132 as measured by the pH probe 140 meets the set tolerance range for the corresponding target acid. Similarly, when the pH value of the mixture in the agitating vessel 132 exceeds the set target corresponding pH value (for example, the acid value in the agitating vessel 132 is too low to exceed the target acid value tolerance) In the range, 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 calculates the amount of lye input as '200928356' and transmits the input lye amount data to the automatic control device 110 for recording analysis.值 疋 疋 由于 由于 由于 由于 由于 由于 由于 由于 由于 由于 由于 由于 由于 由于 由于 由于 由于 由于 由于 由于 由于 由于 由于 由于 由于 由于 由于 由于 由于 由于 由于 由于 由于 由于 由于 由于 由于 由于 由于 由于 由于 由于 由于 由于 由于 由于 由于 由于The lye in the liquid or lye 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 crucible: 132 can be discharged to the pH-constant automatic control dissolution test system via the vent valve 133c on the sealing cover 133. Further, it is worth mentioning that the acid test probe 14 has a function of measuring conductivity in addition to the function of measuring the knockout value (pH). Further, the conductivity value data measured by the pH detector 14 can be transmitted to the automatic control device 11A, and the conductivity value data can be displayed by one of the screens of the automatic control device 110. ❹ Next After the completion of the above-mentioned 48 hours of continuous pH measurement and adjustment, the automatic control device 110 analyzes the data of each of the agitating containers 132. In more detail, when the final liquid in one of the agitating containers 132 When the total amount of acid-base solution added is less than 11% 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 test solution added, such as 44 hours, the stirred container 132's test is successful, and can be performed. Other dissolution experiments analyze the other words when the final liquid-solid ratio in a certain stirred vessel 132 exceeds η.0 and/or the total amount of acid-base solution added in the last 4 hours is greater than the total amount of acid-base solution added in the first 44 hours. At %, the dissolution test in the agitating vessel 132 represents 14 200928356 failure, and the dissolution test must be repeated with the above-mentioned 48 hours continuous pH measurement and adjustment step. In summary, the present invention discloses Constant pH The automatic control dissolution test system can effectively grasp all the details of the whole experimental process, and can reduce the occurrence of human error through automatic operation, thereby avoiding the complexity and cumbersomeness of the experimental operation process caused by manual timing titration. The present invention has been disclosed in its preferred embodiments, and it is not intended to limit the present invention. Any one skilled in the art can 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. ❿ 15 200928356 [Simplified description of the drawings] Fig. 1 is a schematic plan view showing the constant pH control automatic dissolution test system of the present invention; 2 is a schematic plan view showing the pH control constant automatic controlled dissolution test system of the present invention; FIG. 3 is a side view showing the stirring and dissolution device of the pH constant constant automatic dissolution test system of the present invention; 4 is a graph showing the constant pH control of the present invention for the dissolution test ❹ the system of stirring and dissolution Schematic diagram of the top view. [Main component symbol description] 100~acid test value constant_determination automatic control dissolution test system 110~ automatic control device 120~ acid-base addition device 121~ air pump 122~carbon dioxide adsorption bottle 123~ acid container ® 124~ lye container 125~acid partial pressure valve 125a~acid delivery tube 126~test liquid pressure dividing valve 126a~test liquid delivery tube 130~stirring and discharging device 131~magnetic stirrer 132~stirring container 16 200928356 133~ Sealing cap 133a, 133b - hole 133c - vent valve 133d - holder 134 - stirring rod 135 ~ stirring magnet 140 ~ pH probe 150 ~ signal converter ❹ 160 ~ pH meter

Claims (1)

200928356 十、申請專利範圍: 1·一種酸驗值衫自動控制溶出試驗系統,包括: 一自動控制裝置; 、,/豸l n加裝置’電性連接於該自動控制裝 並且具有-空氣幫浦、—酸液容器、一驗液容器、一 酸液分壓閥及-驗液分壓閥,其中,該空氣幫浦係電性連 該自動控制裝置’並且係連通於該酸液容器及該驗液 谷益’該酸液容器係連通於該酸液分壓閥,並且係容納有 ® 一酸液,該較容㈣連通於該錄分㈣,並且係容納 有-驗液’以及該酸液分壓閥及祕液分壓閥係電性連接 於該自動控制裝置; 至)一攪拌溶出裝置,連通於該酸鹼液添加裝置之該 酉夂液分壓閥及歸液分壓閥,並且容納有—受試樣品材料 及一受試樣品材料萃取液;以及 至少一酸鹼值探針,設置於該攪拌溶出裝置之中,並 β 且電性連接於該自動控制裝置。 w 2·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,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 制裝置之間以及該驗液分壓閥與該自動控制裝置之間。 3.如申請專利範圍第1項所述之酸鹼值值定自動控制 ;谷出试驗系統,更包括一酸驗值測定儀,係電性連接於今 酸鹼值探針與該自動控制裝置之間。 4.如申請專利範圍第1項所述之酸鹼值值定自動控制 18 200928356 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 ❿ 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,該密封蓋具有一泡氣閥。 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 溶出試驗系統,其中,該攪拌棒係由鐵氟龍所製成。 19200928356 X. Patent application scope: 1. An acid test shirt automatic control dissolution test system, comprising: an automatic control device; , / / 豸 ln plus device 'electrically connected to the automatic control device and has - air pump, - an acid liquid container, a test liquid container, an acid liquid partial pressure valve and a liquid pressure dividing valve, wherein the air pump is electrically connected to the automatic control device 'and is connected to the acid liquid container and the test The liquid reservoir is connected to the acid pressure dividing valve and contains an acid solution which is connected to the recording (four) and which contains the liquid test and the acid liquid. a pressure dividing valve and a secret liquid pressure dividing valve are electrically connected to the automatic control device; a) a stirring dissolution device connected to the liquid pressure dividing valve and the liquid returning pressure dividing valve of the acid alkali adding device, and The test sample material and the test sample material extract are contained; and at least one pH detector is disposed in the stirring and dissolving device, and is β and electrically connected to the automatic control device. w 2· The constant pH automatic dissolution test system according to claim 1 of the patent application, further comprising a signal converter electrically connected between the air pump and the automatic control device, the acid solution Between the partial pressure valve and the automatic control device and between the test fluid pressure valve and the automatic control device. 3. The automatic control of the pH value as described in item 1 of the patent application scope; the grain outlet test system further includes an acid value tester electrically connected to the present pH value probe and the automatic control device between. 4. The automatic control of the pH value according to the first application of the patent scope 18 200928356 dissolution test system, wherein the acid test liquid addition device further 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 And disposed on the magnetic stirrer, and containing the test sample material and the test sample material extract, the sealing cover is sealed on the crucible of the stirring container, the acid liquid partial pressure valve and the alkali The liquid partial pressure valve communicates with the agitating vessel via the sealing cap, the pH sensor is disposed in the agitating vessel via the sealing cap, and the agitating magnet is disposed in the agitating vessel, and 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 bubble 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 system is connected. The magnet is stirred and connected to the holder in a rotating 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 pH-controlled constant automatic controlled dissolution test system of claim 7, wherein the stir bar is made of Teflon. 19
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CN105021670A (en) * 2015-02-09 2015-11-04 浙江工商大学 Apparatus and method for analyzing concentration of cycloheximide based on surface acoustic wave series resonator biological tongue
CN105004768B (en) * 2015-02-09 2017-11-17 浙江工商大学 Phenylthiourea concentration analysis device and method based on surface acoustic wave series resonator biology tongue
CN105021670B (en) * 2015-02-09 2018-08-07 浙江工商大学 Cycloheximide concentration analysis device and method based on surface acoustic wave series resonator biology tongue

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