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(英)KZDL-8A型快速智能定硫儀操作規(guī)程

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更新時間:2024-11-26
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 一、儀器安裝
I. Instrument Installation

打開包裝箱,儀器包括控制器,爐體和凈化吸收器三部分:
Open the packing case, you will see the three parts of the instrument, i.e. controller, furnace body and purification absorber.

1、安裝爐體部分,首先安裝硅碳管、兩個金屬片要離硅碳管邊有3mm,金屬片中間墊有兩個瓷片,一定要靠中間,目的是防止短路和損壞硅碳管。

1、Furnace body installation: First install the silicon carbide tube. Be sure that the two sheet metals are 3mm away from the edge of silicon carbide tube. Put two ceramic pads in the middle of the sheet metal for preventing short circuit and silicon carbide tube damage. 

螺絲上的瓷片要放好,否則會短路。然后緊固螺絲,兩邊的螺絲要同步擰緊,保持兩邊間隙一致,螺絲的松緊一定掌握好,太松容易打火,太緊容易擰爛硅碳管。最好使用一個月再緊固一下,或者金屬片中間再加個螺絲帽。然后將兩個硅碳管連線擰上,用螺絲帽固定緊。如果絕緣瓷碗較松,要把線皮擰一下,將瓷碗頂緊沒有間隙。避免裸露銅線漏電。
Correctly position the ceramic pads of the screw, or else short circuit may be caused. Then fasten the screw. The screws on both sides shall be simultaneously fastened with the same space kept. The degree of screw tightness must be proper. If too loose, sparking may occur, if too tight, the silicon carbide tube may break. The best practice is to refasten them after one month of use, or add a screw cap between the sheet metals. Then screw the wires of the two silicon carbide tubes and secure them with screw cap. If the insulation bowl is loose, screw the wire to tighten it until there is no space. Avoid bare copper wire from electric leakage.

2、把左側(cè)圓形擋片取下,看爐體內(nèi)是否有雜物,清潔干凈。然后將硅碳管送入爐體內(nèi),推到頭后其實沒有到位,要抬一下,使硅碳管再進去一點兒上了臺階才算安裝到位。把左側(cè)擋片安裝上,緊固螺絲時,要同時晃動硅碳管,防止卡住硅碳管,將硅碳管擠爛。4條螺絲都擰緊后,保證硅碳管還是可以活動的。然后插入異經(jīng)管,同樣抬一下,使異經(jīng)管再進去一點兒上了臺階。再緊固左側(cè)的固定螺絲,固定異經(jīng)管。還要注意右側(cè)送樣口異經(jīng)管與爐體本身是否一致,不要錯位,否則做實驗時送樣容易卡住。
2、Take down the left round shied to see whether there are sundries in the furnace body and whether it is clean. Then feed the silicon carbide tube into the furnace body until it can not move forward. Then slightly lift it up to movie it inward more until it is on a step. Then install the left shied and fasten its screw while shaking the silicon carbide tube to prevent blocking and breaking the latter. Ensure that after 4 screws are tightened, the silicon carbide tube is also movable. Then insert the reducing pipe, also slightly lift it up to move it inward more onto the step. Then fasten the left retaining screw to secure the reducing pipe. Also pay attention that whether the reducing pipe at right feed port is consistent with the furnace body itself. Avoid dislocation, or the sample may be blocked in the experiment.

把熱電偶的連線接好,將熱電偶的幾個螺絲都擰緊,再將熱電偶插入爐體中間的熱電偶孔內(nèi),用手抬一下硅碳管,看熱電偶是否會動,如果沒有動,說明沒有插到位。最后將插到位的熱電偶退回1mm。緊固螺絲固定好熱電偶。
Connect the wire of thermocouple and screw the several screws of the thermocouples tight. After that, insert the thermocouple into the thermocouple hole in the furnace body. Then lift the silicon carbide tube by hand to see whether the thermocouple moves. If not, it means the thermocouple is not in place. At last, after it is in place, draw it back for 1mm. Fasten the screw to secure it.

3、安裝凈化器和電解池,注意膠管的連接順序,異經(jīng)管和兩通閥之間用硅膠管連接,兩通閥最好用凡士林涂抹,密封更好。兩通閥連接電解池其中一個有溶板的接口,另一個口連接凈化器上。電解池底部接口連上一截膠管,并用止水夾夾住。凈化器上左邊兩個干燥管上下兩端堵上脫脂棉,中間放入變色硅膠,將膠塞擰緊,不要漏氣。
3、Installation of purifier and electrolytic tank: Pay attention to the connection order of rubber tubes. The reducing pipe and two-way valve are linked with silicone tube. It would be best to apply vaseline over the two-way valve, so that it will be sealed better. Connect the two-way valve with one of connector with solution plate of the electrolytic tank at one way, and with the purifier at the other way. The bottom port of the electrolytic tank is connected with a section of rubber tube and clamped with a water sealing clip. Both ends of the two drying tubes on the left of purifier are plugged with degreasing cotton with allochroic silicagel in the middle. Screw the rubber plug tight to avoid air leakage.

4、配制電解液:稱取5克碘化鉀、5克溴化鉀、溶于250~300毫升蒸餾水中,再加入10毫升冰乙酸攪拌至完全溶解即可。電解液可重復(fù)使用,當(dāng)PH<1需重新配制。
Preparation of electrolyte: Take 5g of potassium iodide and 5g of potassium bromide, dissolve both in 250~300mlof distilled water. Then add 10 ml of glacial acetic acid into the solution, mix them until they are completely dissolved. The electrolyte may be used repeatedly. It shall be re-prepared in case of PH<1.

 二、操作步驟
Ⅱ 、Operating steps

1、升溫:打開儀器右邊送樣窗口,合上電源開關(guān),打印機自檢,送樣電機自動復(fù)位,處待命狀態(tài)。儀器便自動升溫(不用手工調(diào)節(jié)),初次使用最好使?fàn)t溫升到800℃時恒溫30min(請使用面板“控溫”鍵),關(guān)掉電源開關(guān),冷卻到室溫。再重新開機,升到工作溫度1050℃。
1、Warming up: Open the feed window on the right side of the instrument and switch on. Then the printer will check itself and the feed motor will reset automatically to be on standby. The instrument will warm up automatically (without manual adjustment). For first use, it would be best to let the furnace warm up to 800℃and keep the temperature for 30min (please use the“Temperorature control” key on the panel. ). Then switch off and let the furnace cool to the room temperature. Start the instrument again and let the furnace warm up to the operating temperature of 1050℃.

2、倒入或吸入電解液,打開二通閥,氣泵,調(diào)節(jié)流量計達到1000毫升/分,打開攪拌器,緩慢調(diào)節(jié)轉(zhuǎn)速到融板所出的氣泡與電解液完全混合均勻即可,儀器進入待實驗狀態(tài)。
2、Pour into or absorb electrolyte. Open the two-way valve and air pump. Adjust the flowmeter to 1000 ml/min.. Open the mixer and slowly adjust its rotating speed until the bubbles from solution plate are fully mixed with the electrolyte. Then the instrument enters the status of ready for experiment.

3、在瓷舟中稱取50mg±0.2mg左右混合均勻的試樣,于煤樣上鋪蓋一薄層三氧化鎢,將瓷舟放入石英托盤上,打開 “電解開關(guān)”,按“啟動”鍵,輸入三位數(shù)樣重(小數(shù)點不用輸入),再按“啟動”鍵,試樣自動被送入燃燒爐,分別在500℃和1050℃處停留已設(shè)定好的時間,自動返回,自動打印,整個實驗過程由程序自動執(zhí)行。

3、Take about 50mg±0.2mg of uniformly mixed sample from the porcelain boat. Cover a thin layer of tungsten trioxide over the coal sample. Put the porcelain boat on the quartz tray. Open“Electrolytic switch”press"start" key, input three-digit sample weight (no need to input digits after the decimal point), press"start" key again, the sample will be sent to combustion furnace again. Remain at 500℃and 1050℃respectively for the set durations. After then, return and print automatically. The whole experiment is executed by procedure automatically.  

4、用鑷子(勿用手)取下瓷舟,重復(fù)步驟3進行第二個樣試驗。

注意:〈1〉每次試驗前必須做幾個廢樣,使電解液達到平衡,即右顯示窗開始計數(shù)為止,也就是在正式測試試樣之前所作的廢樣結(jié)果不是零才可以。
Take down the porcelain boat with tweezers (not by hand). Repeat step 3 for the second sample

Note: 〈1〉Prepare several waste samples before each test to balance the electrolyte, i.e. the right display window becomes to count, that is to say, the waste sample result is not zero before normal sample testing.

〈2〉實驗時"電解開關(guān)"必須打開,否則,永遠不會電解。嚴(yán)禁在電解液攪拌狀態(tài)關(guān)閉下打開“電解開關(guān)”。只有在攪拌時才可。否則會污染電極,影響測試精度。
〈2〉During experiment, the“electrolytic switch” must be switched on, or no electrolysis will occur. It is prohibited to switch on the“electrolytic switch” when the electrolyte mixing is closed. It can only be switched on when the electrolyte is being mixed. Or else, it will pollute the electrode and affect the test precision.

〈3〉試驗最好連續(xù)進行,如中間間隔時間太長,在做試樣前應(yīng)加燒一個廢樣。
〈3〉It would be best to carry out the test continuously. If there is a long interval between two tests, an additional waste sample shall be burnt before the latter test.

〈4〉 、實驗結(jié)束,按“電解開關(guān)”鍵,關(guān)掉電解,關(guān)閉二通閥、攪拌器、氣泵,放出電解液(最好保存在棕色磨口瓶內(nèi))以備下用。用蒸餾水洗凈電解池,關(guān)掉電源開關(guān)。
〈4〉 、After the experiment is over, press the“electrolytic switch”and close electrolysis, two-way valve, mixer and air pump. Discharge the electrolyte (best saved in brown grinding jar) for future use. Clean the electrolytic tank with distilled water. Switch off.  

三、常見故障維修
III. Common Troubleshooting

1、ERR1—熱電偶接反,將連線反過來
1、ERR1—Inversed connection of thermocouple: Inverse the connection.

      ERR2—熱電偶開路,連線斷了或者熱電偶損壞
      ERR2— Open circuit of thermocouple: The connection is broken or the thermocouple is damaged.

      ERR3—可控硅失控,加熱控制元器件固態(tài)繼電器損壞或者其本身損壞
      ERR3— Silicon-controlled rectifier (SCR) is out of control: Solid-state relay of the heating control component is damaged or the heating control component itself is damaged.

      ERR4—可控硅觸發(fā)后沒有加熱電流,一般是硅碳管老化,需更換
      ERR4— No heating current is generated after triggering SCR: Usually because the silicon carbide tube is aged and needs changing.

      ERR5—電解池問題,電解液有問題或者液體太少,或者是電解池損壞
      ERR5—Problem of electrolytic tank: The electrolyte has a problem or the liquid is too little, or the electrolytic tank is damaged.

      ERR6—送樣卡,送樣棒卡住,皮帶松動或者電機不轉(zhuǎn)
      ERR6—Feeding blocked: The feed bar is blocked, the belt is loose or the motor does not rotate.

      ERR7-送樣器問題,送樣位置檢測元件,霍爾損壞
      ERR7-Feeder problem: The feed position detection Hall element is damaged.

2、凈化器部分氣路引起的實驗結(jié)果做不準(zhǔn)的故障分析
2、Troubleshooting for incorrect experimental result caused by gas circuit of purifier part

 故障原因的幾點,凈化器干燥管上端的膠塞和下端的氣咀,是否松動或堵塞。電解池的溶板,電解池下端的放液口,二通閥,干燥管和所有的連接膠管都要檢查。
Several causes: Whether the upper rubber plug and lower nozzle of dry pipe of the purifier are loose or blocked. Check the solution plate and the lower discharge outlet of the electrolytic tank, the two-way valve, dry pipe and all connection rubber tubes.

干燥管的變色硅膠要經(jīng)常更換,否則凈化器的流量計和氣泵進水后會很快損壞。
The allochroic silicagel in the dry pipe shall be replaced frequently, or the flowmeter and air pump of purifier will be damaged soon if any water enters.

漏氣的檢查,分別捏住電解池的左右兩個接口,看流量計指示是否會下降,從而判斷哪部分漏氣
Air leakage check: Pinch the left and right connectors of the electrolytic tank respectively. Observe the flowmeter to see whether its indication drops and determine which part leaks.

例如流量計指示正常,但發(fā)現(xiàn)溶板沒有氣泡,說明爐體的氣體根本沒有進入電解池。一般為電解池膠塞或干燥管膠塞沒有塞緊,
For example: If the flowmeter indication is normal but no bubble is found on the solution plate, it means the gas in the furnace body does not enter the electrolytic tank. It is generally because the rubber plug of electrolytic tank or dry pipe is not tight.

3、當(dāng)儀器結(jié)果出現(xiàn)偏差后的調(diào)整
3、Adjustment of instrument in case of deviation

儀器本身沒有故障,但隨著儀器常年使用、各元器件老化后,測試結(jié)果可能會有所偏差,這時就需要重新校正儀器。
The instrument itself has no trouble. However, after being used all year round, the components become aged and the test result may have deviations. Then it is necessary to re-calibrate the instrument.

首先選擇與平時測試的煤樣硫含量相接近的煤標(biāo)樣來校正儀器,這樣校正結(jié)果更準(zhǔn)確。儀器內(nèi)部的調(diào)整范圍較大為粗調(diào)。面板按鍵的調(diào)整為細調(diào),但調(diào)整范圍較小,一般盡量調(diào)整內(nèi)部。內(nèi)部通過線路板上的一個沒有點紅漆的電位器調(diào)整。面板則是修改精度鍵的數(shù)據(jù),按精度鍵,顯示“J”,這是調(diào)整整體系數(shù),范圍是0900~1100之間。“U”是調(diào)整高硫,范圍是109~009之間,109中的1代表的是負號的意思,并不是數(shù)值1,切勿搞錯。“N”是調(diào)整低硫,范圍同“U”。
First calibrate the instrument using the coal standard sample with similar sulfur content with normally tested coal sample. In this way, the calibration result is more correct. The internal adjustment range of the instrument is large (rough adjustment). While the adjustment range of panel keys is small (fine adjustment), usually adjusting the internal part as much as possible. The internal part is adjusted via a red-paint-free potentiometer on the circuit board. For adjustment of panel, modify the precision data by pressing the precision key (“J”is displayed). This is to adjust the overall coefficient in the range of 0900~1100. When “U” is displayed, it is to adjust high sulfur in the range of 109~009. The 1 of the109 represents negative sign, not the numeric 1. Do not mix it up. When “N” is displayed, it is to adjust low sulfur in the same range as that of “U”.

修正方法:按“精度”鍵調(diào)整顯示到項目,比如U,按數(shù)字鍵輸入數(shù)據(jù),按“確認(rèn)”鍵,按“退出”鍵,修改結(jié)束。
Method of correcting: Press “precision”key to adjust the corresponding item, for example U. Then press numeric keys to input data and press “OK”. After that, press “return”key. The correction is over.

修正過再次做一個標(biāo)準(zhǔn)樣,看結(jié)果是否已經(jīng)達到國標(biāo)范圍內(nèi),否則再次調(diào)整

After correction, prepare an additional standard sample to see whether the result meets the national standard range. If not, correct again.

附:全硫的精密度
Attachment: Precision of total sulfur

(此表格出至國家標(biāo)準(zhǔn)GB/T214-2007煤中全硫的測定方法)
(This table is abstracted from GB/T214-2007 Determination of total sulfur in coal.)

 

全硫質(zhì)量分?jǐn)?shù)Mass faction of total sulfur

St--%

重復(fù)性限Repeatability limit

St,ad--%

再現(xiàn)性限Reproducibility limit

St,d--%

≤1.50

0.05

0.15

1.50(不含Not inclusive)~4.00

0.10

0.25

﹥4.00

0.20

0.35

 

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