一、概述：
根據(jù)新標(biāo)準(zhǔn)GB/T176-2017《水泥化學(xué)分析方法》中氯離子電位滴定法研制的一款用于氯離子濃度測量儀器。該儀器適用于各水泥企業(yè)，檢測機構(gòu)，攪拌站，科研所及高等院校等行業(yè)試驗室。
本設(shè)備采用7寸觸摸屏，參數(shù)輸入操作簡單，直觀。頁面實時顯示滴定容量和電極電位。
滴定裝置采用25ml大容量進樣器，0.1ml的滴定頭，保證滴定準(zhǔn)確。設(shè)備進樣采用高精度耐腐蝕的三通電磁閥，方便進樣吸液和試驗滴定。
本機具有自動空白試驗滴定功能，自動測量記錄并存儲相關(guān)試驗數(shù)據(jù)，操作員可隨時調(diào)用試驗數(shù)據(jù)，且試驗前可對參數(shù)進行修改。
I. Overview:
According to the new standard GB/T176-2017 "Methods for Chemical Analysis of Cement", a chloride ion concentration measurement instrument developed by the chloride ion potentiometric titration method. This instrument is suitable for industrial laboratories such as cement companies, testing institutions, mixing stations, scientific research institutes and universities.
The device uses a 7-inch touch screen, and the parameter input operation is simple and intuitive. The page displays the titration capacity and electrode potential in real time.
The titration device uses a 25ml large-capacity sampler and a 0.1ml titration head to ensure accurate titration. The equipment uses a high-precision, corrosion-resistant three-way solenoid valve for sample injection, which is convenient for sample injection and test titration.
This machine has an automatic blank test titration function, automatic measurement records and storage of related test data, the operator can call the test data at any time, and the parameters can be modified before the test.
二、技術(shù)參數(shù)：
★滴定分析重復(fù)性：0.2%。
★滴定容量允許誤差：±0.035ml。
★滴定管分辨率：2/10000。
★滴定管排液或吸液速度：30±10s。
★電位測量范圍：-500~2500mV。
★電位分辨率：0.1mV。
★電位基本誤差：±0.03%FS。
★電位穩(wěn)定性：±0.1mV。
★輸入電源：AC220V/50HZ。
★大功率：50W。
★大記錄：200條。
2. Technical parameters:
★Repeatability of titration analysis: 0.2%.
★The allowable error of titration volume: ±0.035ml.
★ Burette resolution: 2/10000.
★Drain or suction speed of burette: 30±10s.
★Potential measuring range: -500~2500mV.
★Potential resolution: 0.1mV.
★Basic error of potential: ±0.03%FS.
★Potential stability: ±0.1mV.
★Input power: AC220V/50HZ.
★High power: 50W.
★L(fēng)arge records: 200 records.
三、試驗操作過程：
★化學(xué)試劑制備
1.1氯離子標(biāo)準(zhǔn)溶液【C（NaCl）=0.02mol/L】
稱取0.5844已于105℃--110℃烘干2小時的氯化鈉*至0.0001g，置于燒杯中，加水溶解后，移入500ml容量瓶中，用蒸餾水稀釋至刻度搖勻。
1.2*銀標(biāo)準(zhǔn)溶液【C（AgNO3）=0.02mol/L】
稱取1.70g*銀（AgNO3），*至0.0001g，置于燒杯中，加水溶解后，移入500ml容量瓶中，用水稀釋至刻度線搖勻，存儲于棕色瓶中，避光保持。
1.3*（1:1）。
1.4過氧化氫（1.11g/cm3,質(zhì)量分?jǐn)?shù)30%）。
1.5飽和*鉀。
3. Test operation process:
★Chemical reagent preparation
1.1 Chloride ion standard solution [C(NaCl)=0.02mol/L]
Weigh 0.5844 sodium chloride that has been dried at 105°C-110°C for 2 hours to the nearest 0.0001g, place it in a beaker, add water to dissolve, transfer it to a 500ml volumetric flask, dilute to the mark with distilled water and shake it well.
1.2 Silver nitrate standard solution [C(AgNO3)=0.02mol/L]
Weigh 1.70g of silver nitrate (AgNO3), accurate to 0.0001g, place it in a beaker, add water to dissolve, transfer to a 500ml volumetric flask, dilute with water to the mark, shake well, store in a brown bottle, and keep away from light.
1.3 Nitric acid (1:1).
1.4 Hydrogen peroxide (1.11g/cm3, mass fraction 30%).
1.5 Saturated potassium nitrate.
★開啟和預(yù)熱
2.1儀器開機
用電源線連接上電源，打開儀器開關(guān)，儀器開機后進入初始化過程。
2.2系統(tǒng)預(yù)熱
儀器初始化完成后，觸摸屏顯示主菜單界面，因電器件需要預(yù)熱一定時間后方可達到穩(wěn)定狀態(tài)，所以儀器需要預(yù)熱約為半小時。
加注溶液和電極活化
3.1 注入溶液
打開儀器右側(cè)蓋板，取出棕色儲液瓶，用已準(zhǔn)備好的*銀標(biāo)準(zhǔn)溶液清洗存儲液瓶，并將*銀標(biāo)準(zhǔn)溶液注入棕色儲液瓶中。
3.2雙鹽橋*電極填充溶液
取出雙鹽橋*電極，拆下內(nèi)外橋之間的橡皮帽，使用蒸餾水和飽和*鉀溶液清洗外僑，并在外僑注入飽和*鉀溶液，溶液高度不低于2/3,裝好電極。
3.3電極活化
將裝好的雙鹽橋*電極和氯離子電極，浸入蒸餾水中活化，時間約為2小時，活化完成后在進行后續(xù)實驗。（每天試驗前都需要活化）
*銀標(biāo)準(zhǔn)滴定溶液標(biāo)定
4.1 標(biāo)定溶液配制
吸取10.00ml氯離子標(biāo)準(zhǔn)溶液放入200ml燒杯中，加入2ml*（1+1），加水稀釋至150ml，放入一顆磁力攪拌子。
4.2*銀濃度標(biāo)定
4.2.1在主菜單頁面點擊“AgNO3標(biāo)定”，進入頁面后，點擊“吸液”等待溶液吸滿，溶液吸滿后點擊“排液”排空溶液，重復(fù)操作一次，達到清洗管路和排除氣泡的作用。然后再點擊“吸液”按鈕，溶液吸滿后儀器自動將溶液連續(xù)排除且無氣泡殘留在滴定頭*后停止。
5.2.2 將5.2中準(zhǔn)備好的溶液連同燒杯放入儀器托盤中，將兩個電極都插入溶液，點擊“開始”，等待屏幕顯示測量完成。從溶液中移出電極，并用蒸餾水清洗電極，擦干，濾紙擦拭電極頭截面。點擊“吸液”待溶液吸滿后儀器自動溶液排出且無氣泡后停止。
★Turn on and warm up
2.1 Turn on the instrument
Connect the power supply with the power cord, turn on the instrument switch, and enter the initialization process after the instrument is turned on.
2.2 System warm-up
After the instrument is initialized, the touch screen displays the main menu interface. Because the electrical components need to be warmed up for a certain period of time before reaching a stable state, the instrument needs to be warmed up for about half an hour.
Filling solution and electrode activation
3.1 Inject solution
Open the cover on the right side of the instrument, take out the brown liquid storage bottle, clean the storage liquid bottle with the prepared silver nitrate standard solution, and pour the silver nitrate standard solution into the brown liquid storage bottle.
3.2 Double salt bridge calomel electrode filling solution
Take out the double salt bridge calomel electrode, remove the rubber cap between the inner and outer bridges, clean the alien with distilled water and saturated potassium nitrate solution, and inject saturated potassium nitrate solution into the alien, the height of the solution is not less than 2/3, install the electrode.
3.3 Electrode activation
The installed double salt bridge calomel electrode and chloride ion electrode are immersed in distilled water for activation for about 2 hours. After activation, follow-up experiments will be performed. (It needs to be activated every day before the test)
Calibration of silver nitrate standard titration solution
4.1 Preparation of calibration solution
Pipette 10.00ml chloride ion standard solution into a 200ml beaker, add 2ml nitric acid (1+1), dilute to 150ml with water, and put a magnetic stir bar.
4.2 Calibration of silver nitrate concentration
4.2.1 Click "AgNO3 Calibration" on the main menu page. After entering the page, click "Aspirate" and wait for the solution to be full. After the solution is full, click "Drain" to empty the solution. Repeat the operation once to clean the pipeline and remove it. The role of bubbles. Then click the "Aspirate" button, the instrument will automatically remove the solution continuously after the solution is full, and stop after no bubbles remain on the tip of the titration head.
5.2.2 Put the solution prepared in 5.2 and the beaker into the instrument tray, insert both electrodes into the solution, click "Start", and wait for the screen to display the measurement is complete. Remove the electrode from the solution, clean the electrode with distilled water, wipe it dry, and wipe the section of the electrode tip with filter paper. Click "Aspirate" and wait until the solution is full and the instrument will automatically discharge the solution and stop when there are no bubbles.
★空白試驗
5.1、空白溶液配制
吸取2.00ml氯離子標(biāo)準(zhǔn)溶液放入200ml燒杯中，加水稀釋至100ml，加入2ml*（1+1）和2ml 蓋上表面皿，加熱沸煮，微沸1-2min，冷卻至室溫，用水沖洗表面皿，放入一顆磁力攪拌子。
5.2、空白滴定
將5.1中準(zhǔn)備好的溶液連同燒杯放入儀器托盤中，將兩個電極都插入溶液，點擊“開始”，等待屏幕顯示測量完成。從溶液中移出電極，并用蒸餾水清洗電極，擦干，濾紙擦拭電極頭截面。點擊“吸液”待溶液吸滿后儀器自動溶液排出且無氣泡后停止。
★Blank test
5.1. Preparation of blank solution
Draw 2.00ml chloride ion standard solution into a 200ml beaker, add water to dilute to 100ml, add 2ml nitric acid (1+1) and 2ml hydrogen peroxide solution. Cover the watch glass, heat and boil for 1-2 minutes, cool to room temperature, rinse the watch glass with water, and put in a magnetic stir bar.
5.2 Blank titration
Put the solution prepared in 5.1 and the beaker into the instrument tray, insert both electrodes into the solution, click "start", and wait for the screen to display the measurement is complete. Remove the electrode from the solution, clean the electrode with distilled water, wipe it dry, and wipe the section of the electrode tip with filter paper. Click "Aspirate" and wait until the solution is full and the instrument will automatically discharge the solution and stop after no bubbles.
★氯離子測量
6.1 待測樣品配制
稱取待測試樣5.0000g（允許有少許誤差，實際稱量的質(zhì)量輸入到試樣質(zhì)量）置于200ml燒杯中，加人20ml水，攪拌使試樣*分散，然后在攪拌一下加入25ml*（1+1），加水稀釋至100ml，加入2.00ml氯離子標(biāo)準(zhǔn)溶液和2ml*，蓋上表面皿，加入沸煮，微沸1-2min冷卻至室溫，用水沖洗表面皿和玻璃棒，并從燒杯中去玻璃棒，加入磁力攪拌子。
6.2 CL-測量
將6.1中準(zhǔn)備好的溶液連同燒杯放入儀器托盤中，將兩個電機都插入溶液，輸入實際稱量的試樣質(zhì)量，點擊“開始”，等待測量完成。測量完成后，從溶液中移出電極，并用蒸餾水清洗電極，擦干，濾紙擦拭電極頭截面。點擊“吸液”待溶液吸滿后儀器自動溶液排出且無氣泡后停止。
★Chloride ion measurement
6.1 Preparation of samples to be tested
Weigh 5.000g of the sample to be tested (a little error is allowed, the actual weighed mass is entered into the mass of the sample), put it in a 200ml beaker, add 20ml of water, stir to disperse the sample completely, and then add 25ml of nitric acid while stirring (1+1), add water to dilute to 100ml, add 2.00ml chloride ion standard solution and 2ml hydrogen peroxide solution, cover the watch glass, add to boiling, boil slightly for 1-2min to cool to room temperature, rinse the watch glass and glass rod with water , And remove the glass rod from the beaker, add a magnetic stir bar.
6.2 CL-Measure
Put the solution prepared in 6.1 and the beaker into the instrument tray, insert both motors into the solution, enter the actual weighed sample mass, click "start", and wait for the measurement to be completed. After the measurement is completed, remove the electrode from the solution, clean the electrode with distilled water, wipe it dry, and wipe the electrode tip section with filter paper. Click "Aspirate" and wait until the solution is full and the instrument will automatically discharge the solution and stop after no bubbles.
★電極的保養(yǎng)
7.1試驗結(jié)束后需用蒸餾水對兩個電極進行充分清洗，將雙鹽橋*電極的外橋*鉀溶液倒掉，并沖洗內(nèi)外橋之間的部分，用橡膠帽將內(nèi)橋蓋好，恢復(fù)使用前。沖洗后用濾紙擦干電極，防止有水泥殘留。
★Maintenance of electrodes
7.1 After the test, the two electrodes need to be fully cleaned with distilled water. Pour the potassium nitrate solution of the outer bridge of the double salt bridge calomel electrode, and rinse the part between the inner and outer bridges, and cover the inner bridge with a rubber cap to restore it. before use. After rinsing, dry the electrode with filter paper to prevent cement residue.
五、裝箱清單：
1、主機
2、雙鹽橋*電極
3、氯離子電極
4、燒杯
5、電源線
6、調(diào)零端子
7、攪拌子
8、保險管
5. Packing list:
1. Host
2. Double salt bridge calomel electrode
3. Chloride ion electrode
4. Beaker
5. Power cord
6. Zero adjustment terminal
7, stir bar
8. Insurance tube
