TW567090B - Method and device for preparing acid-base solution - Google Patents

Method and device for preparing acid-base solution Download PDF

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TW567090B
TW567090B TW91105782A TW91105782A TW567090B TW 567090 B TW567090 B TW 567090B TW 91105782 A TW91105782 A TW 91105782A TW 91105782 A TW91105782 A TW 91105782A TW 567090 B TW567090 B TW 567090B
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solute
acid
value
volume
base solution
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TW91105782A
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Chinese (zh)
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Tzu-Jen Yang
Wei-Jen Li
Sheng-Hung Jeng
Shuen-Shiu Du
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Asia Ic Mic Process Inc
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Abstract

A technique for preparing an acid-base solution uses a variation of the mole concentrations of a solute and a solvent. The solute is fed in two stages and an accurate pH value can be obtained, thereby reducing the preparation time and avoiding the drawback of an excessive addition of the solute.

Description

567090 案號 911057S?567090 Case No. 911057S?

五、發明說明(1) 發明領域 ,—本發明係關於一種酸鹼溶液調配技術,特別指一種可 穩定、、準確及容易的調配出所設走酸鹼值溶液之調配技術 ’以滿足化學製程上所需不同酸鹼值之溶液。 發明背景 > 在化學製程上往往須要不同"酸鹼值的混合溶液,如積 ,電路製造的晶圓製作過程中,於化學機械研磨(CMp)的 衣程中須加注ό又疋目標範圍内酸驗值的混合溶液,如第一 圖所不,化學機械研磨裝置包含有研磨墊丨〗以研磨晶圓 1 2,在晶圓1 2的研磨過程中混合溶液丨3須持續加注於研磨 墊11上,而該混合溶液13之酸鹼值須控制在所設定之目標 值,以使晶圓有非常平坦的表面。 以往混合/谷液的調配技術中,通常以固定體積的溶劑 (水)緩慢加入經驗值的溶質,待反應平衡或攪拌均勻後, 再加入微量溶質,並待反應平衡或攪拌均勻後,判斷是否 須再加入微量溶質,如此藉由重複添加微量溶質之方式, ,混合溶液的酸鹼值緩慢達到所設定之目標值,此傳統技 術,由於須添加多次的溶質,而造成時間的延宕外,另往 往因溶質添加過置,而須放棄整桶混合溶液,而造成成 費。 發明概要 —本發明主要目的係在提供一種針對化學製程上所需不 合溶液^^,本#明剎用溶質(劑)莫 567090 月 曰 修正 案號 91105782 五、發明說明(2) 爾濃度的變化而設計,溶質分二次 定目標的酸鹼值,不僅縮短調製,間P :精確達到所設 量的缺點。 ]亦避免溶質添加過 本發日丹另一目的係在提供一藉 同酸鹼值的混合溶液之調配裝'置,本笋學製程上所需不 用的可程式控制器配合人機介面般工業常 定量泵浦、泣旦呌;^f凡成,並選用精密的 尺’甫 /瓜里计及酸鹼計,提丨供籍定 _ ^ 作方式,可你ρ a , ^ %疋、準確及容易的操 F乃A ’可使刼作人在使 置。 优用及g丨丨練上更為容易之調配裝 之酸 發明詳細說明 一般而言,影響調配混 主要包括有溶質(劑)莫爾濃 合速率等等,在不同的化學 ,不同的環境、容器或溫度 (物理)變化,在一混合溶液 原有莫爾濃度值計算所需溶 合溶液的實際酸鹼值與理論 本發明混合溶液之調配方法 >辰度的變化而設計,使混合 氧)離子莫爾濃度變化影響 驗值。 根據實驗在2 5 °C的室溫 合溶液之酸鹼值的因素很多, 度值、溶質(劑)衰減速度、混 液體本身具有不同的衰滅速率 等都有可能造成不同的化學 的混合或稀釋過程中,若利用 貝及溶劑的體積,往往造成7¾ 酸驗值之間有相當大的誤羞, ,主要就是針對溶質(劑)莫爾 溶液不受溶質(劑)中的氮(氮 ,並能精確的達成所設定 下,任何水溶液中, 〔H+〕X〔OH-〕=ι〇,Μ2V. Description of the invention (1) Field of invention, the present invention relates to an acid-base solution preparation technology, in particular, a preparation technology capable of stably, accurately, and easily preparing the pH-base solution provided to meet the chemical process Solution with different pH value required. BACKGROUND OF THE INVENTION > Chemical processes often require different " mixed solutions of pH ", such as product, circuit manufacturing wafer manufacturing process, chemical mechanical polishing (CMp) clothing process must be added and target range The mixed solution of the internal acid test value is not shown in the first figure. The chemical mechanical polishing device includes a polishing pad to grind the wafer 12. During the polishing process of the wafer 12, the mixed solution must be continuously filled in The polishing pad 11 and the pH value of the mixed solution 13 must be controlled at a set target value so that the wafer has a very flat surface. In the past, the mixing / valley preparation technology usually used a fixed volume of solvent (water) to slowly add empirical solutes. After the reaction was balanced or stirred well, a small amount of solute was added, and after the reaction was balanced or stirred well, determine whether It is necessary to add a small amount of solute, so by repeatedly adding the solute, the pH value of the mixed solution slowly reaches the set target value. This traditional technology requires the addition of multiple solutes, which causes time delay. In addition, due to the excessive addition of solutes, the entire barrel of mixed solution must be abandoned, resulting in cost. Summary of the Invention—The main purpose of the present invention is to provide a solution that is incompatible with chemical processes. ^^ This solute (agent) for Mingcha Mo 567090 month amendment number 91105782 5. Description of the invention (2) Changes in concentration And the design, the solute content of the secondary target pH value, not only shorten the modulation, the interval P: the disadvantage of accurately reaching the set amount. ] Also avoid the addition of solutes. The other purpose is to provide a blending equipment with a mixed solution with the same pH value. The programmable controller that is not used in the bamboo processing process is compatible with the human-machine interface industry. Constant volume pumping and weeping; ^ f Fancheng, and choose a precise ruler 'Fu / Guali meter and acid-base meter, to provide the method of _ _ _ _ _ ^, ^ a, ^% 疋, accurate And the easy operation of F is A 'can make the person make use of it. Optimal use and g 丨 丨 It is easier to mix and match the acid. Detailed description of the invention In general, the effect of mixing mainly includes solute (agent) Mohr concentration rate, etc., in different chemistry, different environments, The container or the temperature (physical) is changed, and the actual pH value of the fused solution is calculated from the original Moire concentration value of a mixed solution and the theory. The method for preparing the mixed solution of the present invention is designed to change the degree of mixed oxygen. ) Changes in ion moire concentration affect the test value. According to the experiment, the pH value of the solution at room temperature of 2 5 ° C has many factors. The degree value, the solute (agent) decay rate, and the mixed liquid itself have different decay rates, etc. may cause different chemical mixing or In the process of dilution, if the volume of shellfish and solvent is used, there is often a considerable misunderstanding between the 7¾ acid test values, which is mainly for the solute (agent) Moore solution is not affected by the nitrogen (nitrogen in the solute (agent), And can accurately achieve the set, in any aqueous solution, [H +] X [OH-] = ι〇, M2

第5頁 567090 、發明說 车 月一 曰 修正 其中 日月(3) 〔Η+〕 〔OH-〕 Μ 氫離子濃度 氫氧離子濃度 莫爾濃度 而奮〔Η+〕=101,即定義酸鹼^ρΗ 一 7·〇 —由上,混合溶液酸驗值的精痛度關鍵在於溶質(劑)中 氣離子與氫惠離子含量的莫爾濃度值’本發明調配方法 • Θ由此二者間的莫爾濃度變化而設計,其包含下列步驟 ·: 傷預定體積X的溶劑(水)及求取溶質原有的莫爾濃度 b ·从 應有 質原有的莫爾濃度值計算出達到設定之目標酸驗值 μ的體積γ ; c. 將Υ骼往 檢列Α積的溶質加入X體積的溶劑攪拌使之均勻混合,並 d. 。峻鹼值Ζ ; 體積vlf值ζ回推溶質實際的莫爾濃度,再計算溶劑目桿 e 、所需實際溶質的體積Yi ; ^入溶質差值(γ「γ)、加入溶劑差值(ν—X),如此,即 凡成所需混合溶液之酸鹼目標值。Page 5 567090, the invention said that the first month of the moon and the moon (3) [Η +] [OH-] M hydrogen ion concentration hydroxide ion concentration Moore concentration [奋 +] = 101, that is to define the acid and base ^ ρΗ 7 · 〇—From above, the key point of the pain value of the acid value of the mixed solution is the Mohr concentration value of the gas ions and hydrogen ions in the solute (agent). It is designed to change the Moire concentration, which includes the following steps: Solvent (water) that damages the predetermined volume X and the original Moire concentration b of the solute. The volume of the target acid test value μ is γ; c. Add X volume of the solute to the test column A volume and add X volume of solvent to stir to mix uniformly, and d. Jun base number Z; volume vlf value ζ back to the actual Moore concentration of the solute, and then calculate the solvent eye e, the required actual solute volume Yi; ^ enter the solute difference (γ "γ", add the solvent difference (ν —X), so that it becomes the target value of acid and base of the required mixed solution.

藉由上述方法,本發明溶質分為二次投入即可精確達 到所設定目標值的酸鹼值,相較習知技術,不僅大幅地縮 翅了調製時間,也避免溶質添加過量的缺點,為便於瞭解 f發明之調配方法,兹進一y由下述實例說明: 567090 _案號911Q5782_年月日 修正 五、發明說明(4) " · · '^^ 由濃度為45%的Κ0Η溶液,稀釋成酸鹼目標值pHll 5 、目標體積為80公升的Κ0Η溶液^ ’ a·準備預定體積40公升的水,並根據Κ0Η供應商的資料(45 %Κ0Η的比重為i.442g/ml)將重量百〗分濃度(45%)換算成 體積莫爾濃度 —11.56M, " ^ 重量百分濃度(%) =溶質的重量(g) /溶液的重量(g), 體積莫爾濃度(Μ)=溶質的莫爾數/溶液的體積(L), 溶質的莫爾數 =溶質的重量/溶質的分子量,故可得By the above method, the solute of the present invention can be divided into two inputs to accurately reach the set pH value of the target value. Compared with the conventional technology, not only the preparation time is greatly reduced, but the disadvantage of excessive solute addition is also avoided. It is easy to understand the method of formulating the invention of f, which is illustrated by the following examples: 567090 _Case No. 911Q5782_ Year Month Day Amendment V. Description of the Invention (4) " Dilute to a K0Η solution with a target pH of pH 5 and a target volume of 80 liters ^ a. Prepare a predetermined volume of 40 liters of water, and according to the data of the K0Η supplier (the specific gravity of 45% K0Η is i.442g / ml) Weight percent concentration (45%) converted to volumetric Moire concentration — 11.56M, " ^ weight percent concentration (%) = weight of solute (g) / weight of solution (g), volume moire concentration (Μ ) = Moore number of solute / volume of solution (L), Moore number of solute = weight of solute / molecular weight of solute, so we can get

(1. 44 2g/ml X100 0mlx45%)/56.098 )/lL = 11 · 56J b ·將溶質Κ Ο Η原有莫爾濃度(11 · 5 6 Μ )計算到達酸驗目標值 (ρΗ11·5)所需應有的體積 —l〇.94ml, 由KOH稀釋於40公升水的混合溶液之酸驗值為pH11.5, 得知氫離子的莫爾濃度Ji為〔H+〕=l〇-ii.5GM,根據 〔H+〕X 〔OH-〕=10_14M2,則知 〔OH-〕=10_2·5°Μ ,又 ΚΟΗ溶於水中將完全解離為鉀離子(〇及氫氧離子(〇Η_), 其離子方程式 ΚΟΗ — Κ+ + ΟΗ_ ,藉此些資料則可得知須 在40公升水加入10. 94ml的ΚΟΗ, ( 40 0 0 0 Χ10_2·50)/11· 56 =l〇. 94ml (註:添加KOH後,混合溶液體積變化量很小) C·將10· 94ml的K0H溶於40公升水中之混合溶液,其酸鹼值 測得為 ρΗ11·26(即〔OH-〕=1〇ΐ74Μ)'(1. 44 2g / ml X100 0mlx45%) / 56.098) / lL = 11 · 56J b · Calculate the original Moore concentration of the solute κ Ο (11 · 5 6 Μ) to reach the target value for acid test (ρΗ11 · 5) The required volume-10.94 ml, the acid value of the mixed solution diluted with KOH in 40 liters of water was pH 11.5, and the Mole concentration Ji of the hydrogen ion was [H +] = 10-ii. 5GM, according to [H +] X [OH-] = 10_14M2, then we know that [OH-] = 10_2 · 5 ° M, and K0Η dissolved in water will completely dissociate into potassium ions (0 and hydroxide ions (〇Η_), which Ionic equation ΚΟΗ— Κ + + ΟΗ_. From this information, we can know that 10.94ml of ΚΟΗ must be added to 40 liters of water, (40 0 0 0 Χ10_2 · 50) / 11 · 56 = l〇. 94ml (Note: After adding KOH, the volume change of the mixed solution is small) C. A mixed solution of 10.94 ml of KOH dissolved in 40 liters of water, the pH value of which was measured as ρΗ11 · 26 (that is, [OH-] = 1〇ΐ74Μ) '

第7頁 567〇9〇 7^—~911〇5782_年—J 曰 心 瓦、發明說明(5) ---- 嘗=該酸驗值pHl 1.26回推溶質KOH實際的莫爾濃度,再計 异〉容劑目標體積V所需實際溶質的1體積, K〇H 莫爾濃度= (40000 XI 0-2.74)/2 〇. 94 KOH 體積=(800 0 0 X l〇-25G)/6· 653 = 38 02ml \ —:- 汝加入ί谷質差值(38.02-10.94)、加入溶劑差值(8〇一4〇), ^此’即可完成所需混合溶液之酸鹼目標值(測得K〇I1溶液 的駿鹼值為ΡΗ11· 51)。 請參閱第二圖、第三圖所示,其係為根據本發明調配 法所提供之裝置,為便於人員操作,該本發明使用一般 工業常用的可程式控制器(PLC)配合人機介面(HMI)設計而 $ ’以提供穩定、準確及容易操作的操作方式,該裝置包 二y程式控制器21、人機介面22、流量計23、酸鹼計24及 疋里系满2 5 ’該可程式控制器2 1主要用以訊號收集、訊號 $理、資料計算等任務,酸鹼目標值可由人機介面讀入設 定’該流量計2 3以控制溶劑注入桶槽2 6之量,該定量泵浦 以控制溶質2 5加入之量,該酸驗計2 4以檢測混合溶液之酸 驗值並送出回饋訊號以達成酸鹼值精確度的要求,其操作 控制流程包含下列程序步驟(請配合第四圖所示)·· 步驟301 :讀入設定之酸鹼目標值; 步驟30 2 :加入預定體積X之溶劑; 步驟3 0 3 :加入以溶質原有的莫爾濃度計算到達酸鹼目標 值的溶質體積;Page 7567〇9〇7 ^ — ~ 911〇5782_ 年 —J Yue Xin tile, description of the invention (5) ---- taste = the acid test value pHl 1.26 back to the actual Moore concentration of solute KOH, and then Differentiation> 1 volume of the actual solute required for the target volume V of the container, K〇H Moore concentration = (40000 XI 0-2.74) / 2 〇. 94 KOH volume = (800 0 0 X l〇-25G) / 6 · 653 = 38 02ml \ —:-Add the difference in grain quality (38.02-10.94) and the difference in solvent (80-40), and you can complete the target value of the acid and base of the required mixed solution ( The alkaloid value of the KOI1 solution was determined to be pH 11.51). Please refer to the second and third figures, which are the devices provided according to the deployment method of the present invention. In order to facilitate the operation of the personnel, the present invention uses a programmable controller (PLC) commonly used in industry to cooperate with a human-machine interface ( HMI) is designed to provide a stable, accurate and easy-to-operate operation. The device includes two program controllers 21, human-machine interface 22, flow meter 23, pH meter 24, and full-line 2 5 'The Programmable controller 21 is mainly used for signal collection, signal processing, data calculation and other tasks. The target value of acid and alkali can be read and set by the man-machine interface. 'The flow meter 2 3 is used to control the amount of solvent injected into the tank 26. Quantitative pumping to control the amount of solute 25 added. The acid meter 24 detects the acid value of the mixed solution and sends a feedback signal to achieve the accuracy of the pH value. The operation control process includes the following program steps (please Match with the fourth figure). · Step 301: Read the set acid-base target value; Step 302: Add a predetermined volume of X solvent; Step 303: Add the moire concentration calculated from the original solute to reach the acid-base Target solute volume;

567090 五、發明說明(6) 步驟304 :循環攪拌; 步驟305 :偵測酸鹼值; 步驟30 6 ··以步驟30 5偵測之酸鹼值回推實際溶質莫爾濃度 並計算溶劑目標體積V所需的溶質體積; 步驟3 0 7 :加入溶劑體積差值; 步驟3 0 & ··加入溶質體積差值; 、‘ 步驟309 :循環攪拌; 〇 步驟31 0 ·偵測pH值,即得完成所需之混合溶液。步驟3工〇 所偵測之pH值正常都可符合所設定酸鹼目標值的範圍内, 混合溶液即可進入等待輸出供應步驟3丨】,若有值在酸 鹼目標值的範圍外,即進入步驟312得利用警報提示而不 輸出供應,藉此,所有調配過程均採自動化流程,降低操 作錯誤發生的機會,使得調配混合溶液獲得精確的酸鹼值 萨=此糟由本發明之調配技術,溶質分二次投入即可 精確的酸鹼值,大幅縮短了調製時 量的缺點。 避充岭貝添加過 睛再參閱第三圖所示,該調配裝置循 用循環用泵浦27以驅使混合溶液的循環攪拌=㈣係利 雖本發明已以一具體實施例揭露如上,麸二 限定本發明,任何熟悉此技藝者,在不脫:^非用以 ^範圍内,當可作各種之更動與潤飾,因 二明之精神 範圍當視後附之申請專利範圍所界定者為準。&明之保護 第9頁 567090 案號 91105782 曰 修正 圖式簡單說明 ^ 圖式說明 第一圖為化學機械研磨裝置加乂混合溶液之實施例示意 圖。 第二圖為本發明調配裝置之硬體架構方塊示意圖。 第三圖為本發明調配裝置之硬體架構實施例示意圖。 第四圖為本發明調配裝置實施之控制流程圖。 1 2.晶圓 22.人機介面 2 4 ·酸驗計 26.桶槽 圖號說明 11.研磨墊 1 3.混合溶液 2 1.可程式控制器 2 3.流量計 2 5.定量泵浦 27.泵浦 3 0 1.讀入設定之酸鹼目標值 3 0 2.加入預定體積X之溶劑 3 0 3.加入以溶質原有的莫爾濃度計算到達酸鹼目標值的 溶質體積。 304.循環攪拌 3 0 5.偵測酸驗值 3 0 6.以步驟3 0 5偵測之酸鹼值回推實際溶值莫爾濃度並計 算溶劑目標體積V所需的溶質體積。 3 0 7.加入溶劑體積差值 308.加入溶質體積差值 3 0 9.循環攪拌 ^567090 V. Description of the invention (6) Step 304: Cyclic stirring; Step 305: Detect pH value; Step 30 6 ·· Use the pH value detected in Step 30 5 to push back the actual solute Moore concentration and calculate the target volume of the solvent V required solute volume; Step 3 0 7: Add solvent volume difference; Step 30 & · Add solute volume difference; 'Step 309: Cyclic stirring; 〇 Step 31 0 · Detect pH value, ie To obtain the required mixed solution. In step 3, the detected pH value can normally meet the set range of the target value of acid and alkali, and the mixed solution can enter the waiting output and supply step 3]. If any value is outside the range of the target value of acid and base, that is, Go to step 312 to use the alarm prompt instead of output supply, so that all the deployment processes are automated, reducing the chance of operating errors, so that the mixed solution can obtain an accurate pH value. This is the technology of the invention, The accurate pH value can be obtained by the second input of solute, which greatly shortens the disadvantage of the amount of preparation. Avoid filling the oysters and see the third figure again. The blending device uses a circulating pump 27 to drive the circulating stirring of the mixed solution = ㈣ 系 利 Although the present invention has been disclosed as a specific embodiment above, bran two To limit the present invention, anyone familiar with the art can make various modifications and retouching within the scope of: ^ Not used ^, because the spiritual scope of Erming shall be defined by the scope of the attached patent application. & Protection of the Ming Page 9 567090 Case No. 91105782 Amendment Brief Description of the Drawings ^ Description of the Drawings The first drawing is a schematic view of an embodiment of a chemical mechanical polishing device with a mixed solution of rhenium. The second figure is a block diagram of the hardware structure of the deployment device of the present invention. The third figure is a schematic diagram of an embodiment of the hardware architecture of the deployment device of the present invention. The fourth figure is a control flowchart of the deployment device of the present invention. 1 2. Wafer 22. Human-machine interface 2 4 Acid tester 26. Bucket slot number description 11. Polishing pad 1 3. Mixed solution 2 1. Programmable controller 2 3. Flow meter 2 5. Dosing pump 27. Pump 3 0 1. Read the set target value of acid and base 3 0 2. Add a predetermined volume X of solvent 3 0 3. Add the solute volume calculated to reach the target value of acid and base based on the original Moire concentration of the solute. 304. Cyclic stirring 3 0 5. Detect acid test value 3 0 6. Use the acid-base value detected in step 3 5 to push back the actual solubilized Moore concentration and calculate the required solute volume of the solvent target volume V. 3 0 7. Add volume difference of solvent 308. Add volume difference of solute 3 0 9. Cyclic stirring ^

第10頁 567090Page 10 567090

Claims (1)

567090 _案號911Q5782_年月日__ 六、申請專利範圍 3. 如申請專利範圍第1項所述之實施於半導體CMP製程之酸 鹼溶液調配裝置,其中該調配裝"置混合溶液之循環攪拌係 利用循環用泵浦以驅使實施者。' 4. 如申請專利範圍第1項所述之實施於半導體CMP製程之酸 鹼溶液調配裝置,其中該操作程序f驟c之溶質原有的莫 爾濃度,係利用該溶質之重量百分遠度換算而成。 5. 如申請專利範圍第1項所述之實施於半導體CMP製程之酸 鹼溶液調配裝置,其中該預定體積X係為目標體積V之一 半0567090 _Case No. 911Q5782_Year Month Date__ VI. Patent Application Range 3. The acid-base solution deployment device implemented in the semiconductor CMP process as described in item 1 of the scope of the patent application, where the deployment device " The circulating stirring system uses a circulating pump to drive the practitioner. '4. The acid-base solution preparation device implemented in the semiconductor CMP process as described in item 1 of the scope of the patent application, wherein the original Moire concentration of the solute in the operation procedure f step c is based on using the weight of the solute far away. Degree conversion. 5. The acid-base solution deployment device implemented in the semiconductor CMP process as described in item 1 of the scope of the patent application, wherein the predetermined volume X is one and a half of the target volume V 第13頁Page 13
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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112630131A (en) * 2020-12-01 2021-04-09 深圳供电局有限公司 Device and method for testing waterproof performance of cable intermediate joint

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112630131A (en) * 2020-12-01 2021-04-09 深圳供电局有限公司 Device and method for testing waterproof performance of cable intermediate joint

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