自动量热仪调试方法(中英文).docx

5EAC/PL自动量热仪调试方法5EAC/PL Automatic Calorimeter Debugging Method1调试目的Debugging purposes 1.1根据现场试验条件，标定仪器的热容量。According to the field test condition, demarcate the instrument heat capacity 1.2提高煤的发热量的测定数据准确度，为生产操作，成本核算提供依据。Increase the accuracy of determination data for coal calorific value, and provide the basis for production operation and cost accounting. 2编制依据Basis of compilation2.1GB/T213-2003煤的发热量的测定方法 GB/T213-2003 Determination of Calorific Value of Coal2.2煤质分析应用技术指南（2009年版） 中国标准出版社Coal Quality Analysis Application Guide (2009 edition), China Standards Press2.32009年最新煤质分析化验技术标准规范与新方法新检测设备应用指南（2009年版） 中国煤炭出版社2009 Newest Coal Quality Analysis Testing Technology Standard Specification and Application Guide for New Methods and New Testing Equipment. (2009 edition) China Coal Press2.4 GB/T483-2007煤炭分析实验方法一般规定GB/T483-2007 General Rules for Analytical and Testing Methods of Coal2.55E-AC/L自动量热仪使用说明书5EAC/PL Automatic Calorimeter Operating Manual2.6厂家提供的有关资料The information provided by the manufacturer3调试前应具备的条件Preparations before debugging3.1安装环境Installation condition3.1.1室温通常以不超过1530范围为宜，相对湿度80%。The ambient temperature should be 1530, and the relative humidity should be 80%.3.1.2周围无强烈震动、灰尘、强电磁干扰、腐蚀性气体。During analysis there should be no strong vibration, dust, strong electromagnetic interference and corrosive gas. 3.1.3试验室应设一单独房间、不得在同房间内进行其他加热类实验项目。The laboratory should be set in single room, and other heating experiments are not allowed to carry out in the same room.3.1.4室温应尽量保持恒温，每次试验室温变化不应超过1。The room temperature should try to be keeping in homoeothermic. During analysis the flowing of the room temperature should be kept within 1.3.1.5试验室应无强烈空气对流，不应有强烈的热源，应避免仪器受阳光直射，试验过程中尽量避免开门窗。During analysis there should be no violent cross-ventilation in the room, intense heat sources and fans are not allowed. The instrument should be put in the place that away from direct sunlight. During analysis doors and windows should be closed.3.1.6量热仪应放在合适的工作台面(最好是水泥台)，应平整无震动；双控立式仪器只需700mm（宽）1500mm（长）即可。Calorimeter should be put on the suitable work surface (better to be cement desk) which smooth and no vibration. For double control vertical instrument, its work surface should be 700mm1500mm.3.1.7电源要求：单相220V22V/501Hz、功率1.5KW，否则应配备UPS或稳压电源，其功率500W。Power requirement : single phase220V22V/501Hz, power 1.5KW，or stable power supply of high performance or UPS, its power 500W。3.2自备材料Material preparations3.2.1压力4Mpa、纯度99.5%的冷却氧一瓶，不得使用电解氧。Pressure 4Mpa、a bottle of cooling oxygen which purity 99.5%. The electrolyte oxygen is not allowed.3.2.2 50kg以上的蒸馏水（每个桶）。Prepare over 50kg distilled water (each bucket).3.2.3各种规格的烧杯及量筒。It should be equipped with all kinds of beaker and measuring cylinder.3.2.4热值接近实测煤样的标准煤样一瓶。Prepare a bottle of standard coal sample that the calorific value is close to the analyzed sample.3.2.5感量为0.1mg的电子天平一台。Prepare an electronic balance with 0.1mg resolution. 3.2.6普通水银温度计二支。It should be equipped with two common mercury thermometers. 3.2.7点火丝（标配）。Ignition wire (standard configuration)3.2.8量热标准物质二等或二等以上，经计量机关检定并标明热值的苯甲酸。Second class or above class calorimetric standard substances, and the standard benzoic Acid Pellets that approved by the authority and marked with the known calorific value. 3.2.9配制化学试剂所需的各种药品。Prepare all kinds of medicine for chemical reagent needs. 3.3操作人员已经过理论培训，熟知仪器的操作方法，并且有一定的计算机操作知识。Operating personnel have been take part in the theoretical training, well know about the operating methods of instrument and have some knowledge of computer operation. 4量热仪主要技术参数和各部件功能Calorimeter main technical parameters and component functions4.1主要技术参数Main technical parameters4.1.1测温范围：535 Temperature measuring range: 5354.1.2温度分辨率：0.0001 Temperature resolution: 0.00014.1.3测试时间：约 16 min个 Analysis time: about 16 minutes / pc4.1.4试样重量：1g（煤） Sample weight: 1g(coal)4.1.5精密度：RSD0.2% Precision RSD 0.2%4.1.6准确度：在标准样品的允许范围之内Accuracy: within the allowance of the standard sample.4.1.7电源：220V22V、50Hz1Hz Power supply: 220V22V、50Hz1Hz4.1.8功率：计算机300W,仪器主机500W Power : Computer:300W, Calorimeter500W4.2仪器各部件功能Components and functions4.2.1 自动恒温桶（包含搅拌器、点火装置等），属立式桶。用于放置氧弹并将其与外界环境隔离，提供水循环系统及自动进水、放水控制。 Automatic constant temperature bucket (including stirrer, ignition equipment), belong to vertical type. Used to setup oxygen bomb and isolate it with the outside world. Provide water circulation system, automatic control inflow and drain off.4.2.2精密感温探头（已装于自动恒温桶内），温度传感器用于测量内桶水温度。 Precision probe (already installed inside the bucket): used to measure the temperature of the inner bucket.4.2.3主板负责桶与计算机之间的接口，读取温度信号，接收并识别控制命令。控制板提供系统电源并控制泵阀、搅拌、点火等执行部件。 Main board in charge of the interface between bucket and computer, and converts the temperature signals, into digital signals, receive and identify control order. Control panel provides system power and control pump valve, stir, ignition, etc.4.2.4氧弹：待测物质的燃烧室。 Oxygen bomb: combustion chamber for the samples to be determined.4.2.5手持式自动充氧仪：用于向氧弹中充氧。Hand-held automatic bomb charger: for the bomb to charge with oxygen.4.2.6测试软件：控制测试过程按要求进行。Testing software: control all the measuring process.4.2.7计算机（含显示器、键盘、鼠标等）：运行测试软件，存储、打印结果、数据处理等。Computer (including the monitor, keyboard and mouse): is used to run the testing software, save and print the analysis results, and process the data. 4.2.8电子天平：称量样品重量。Electronic balance: weigh the sample.4.2.9可调定量加液器：向氧弹内注水（可用量筒代替）。Adjustable bottle-top dispenser: filling water into oxygen bomb (can instead by measuring cylinder)4.2.10减压阀：将钢瓶压力降到规定压力。Oxygen pressure regulator： is used to reduce the tank pressure to authorized pressure.5调试的项目、方法和步骤Debugging Items, Methods and Steps5.1仪器和附件的摆放Instruments and accessories set out5.1.1把电脑放在工作台上，仪器(立式桶）直接放在地上,根据现场情况尽量摆放整齐,仪器的摆放应避免阳光直射和空调直吹。Put the computer on the working table, direct put the instrument (vertical bucket) on the floor in order by according to the field condition. The instrument should be put in the place that away from direct sunlight or direct blow by air-condition 5.1.2把充氧仪、充氧导管、减压阀、氧气瓶连接好，开启氧气瓶并保证减压阀的二次压力为2.8-3.0Mp。把氧弹和氧弹支架、点火丝、坩埚、摆放在合适的位置，以便操作。Well connecting the bomb charger, oxygen tube, reducing valve and oxygen tank, then open the oxygen tank and keep the second pressure of reducing valve within 2.8-3.0Mp. Put the oxygen bomb, support, ignition wire and crucible on the suitable place for convenient use. 5.2软件的安装将安装盘插入软驱中，点击“我的电脑”中“A”盘，再点击该安装盘中的“Setup.exe”文件，然后按操作提示即可完成系统的安装。默认安装目录一般选择为：“C5E-ACNew”Software installationInsert optical disc in the floppy drive, and open the “A disc” in My Computer, and double click on “Steup.exe” to start installation, and continue the following steps as indications. The default installation directory is “C5E-ACNew”5.3万分卡（PCI卡）的安装和软件的设置PCI card installation and software setting5.3.1PCI卡的安装PCI card installation5.3.1.1在安装前要分别记录下两块PCI卡上的系数。（本仪器为双控，有两个恒温桶分别称为A、B桶）Before installation, write down the coefficients of two PCI cards. (This instrument is double control, which have two constant temperature buckets and names bucket A and bucket B)5.3.1.2把万分卡插入电脑主机对应的插槽里面，万分卡（PCI卡）的接线要参照仪器说明正确连接。Inset the PCI card into the suitable slots in the computer and correct connect by according to the instrument introductions, 5.3.1.3连接仪器、电脑、信号线,再把仪器、电源线接好。Connect the instrument, computer and signal line, and then connect the instrument and power line. 5.3.1.4打开计算机电源，右击“我的电脑”“属性”“硬件”“设备管理”安装PCI卡驱动程序 (双控重复操作即可)。Turn on the computer power, right-click My Computer-Properties -Hardware- Equipment Management; install PCI card drivers (repeat the steps for double control type)5.3.2软件的设置Software Setting5.3.2.1在软件所在的根目录下找到“GetCardAddress”软件，打开它。如图5-1所示 Find out and open the “GetCardAddress” software in the root directory. As shown in Figure 5-1 图5-1 图5-2点击“获取卡地址”卡1、卡2的地址就会显示出来，记录卡1、卡2的地址。Click GetCardAddress and the Card1 and Card 2 address will be display, and then record them. 5.3.2.2打开已安装好的软件，在“设置”“卡设置”中输入记录的卡地址、卡系数并且选择好寄存器方式，密码是“csky”（注意卡地址前加上“”）。如图5-2、5-3所示Open the installed software, in the “Settings”“Card Settings”, input the recorded cards address and card coefficient, set up the register type, the password is “csky” (note: dont forget input a “” in front of card address). As shown in Figure 5-2, 5-3 图5-3完成以上设置后点击“保存”。Click “Save” after finish the above setting.5.4硬件的检测Hardware Debugging打开仪器电源开关，通电检查仪器的泵、阀是否能正常工作。可通过仪器测试软件中的“功能”里面的“硬件调试”逐个测试，阀的通断可以听声音，泵的通断必须靠手接触，由于仪器目前无水，泵阀开的时间不宜太长。如图5-4所示Turn of the instrument power switch, check whatever the pump and valve is working normally. Check one by one by the “Hardware Debugging” of the “Functions” of Instrument Testing Software. Check the valve On-Off by Voice-listening; check the pump On-Off by hand touch. At the moment, as the instrument without water, the operation time for pump and valve not suitable to be too long. As shown in Figure 5-4图5-45.5仪器加水、放水步骤Feeding and Draining5.5.1加水Feeding water5.5.1.1准备50L的蒸馏水或去离子水，再准备一个盛水容器放在溢流口处。Prepare 50L distilled water or deionized water and a large container at the overflow port.5.5.1.2运行测试程序进入“功能”“硬件调试”，首先选择对应的桶类型（分为立式和台式，选择立式）和“A、B”桶，打开“放水阀”。Run the test program to “Functions”“Hardware debugging”, first select the buckets type (vertical and table type, select Vertical type) and “Bucket A or “Bucket B, and switch on “Drain Valve”.5.5.1.3用引水管从内桶加入蒸馏水或去离子水至溢流口有水溢出，此时说明备用水箱水已加满。注意不要使水进入内、外桶之间的垫圈，以免影响测试结果。Feed distilled water or deionized water from the bucket with diversion conduit unit water overflowing from the gate, at this moment, the buffer tank will be full of water. Pay attention not let the water get into the gasket between inside and outside bucket, in order to avoid influence the test result. 5.5.1.4关闭“放水阀”，打开“进水阀”和“进水泵”（仪器会自动从水箱往外桶加水），至听到溢流声后（说明外桶水已加满）。关闭“进水阀”、“进水泵”。Switch off “Drain Valve”, and switch on the “Inlet Valve” and “Inlet Pump” (the instrument will auto add water from water tank to outer bucket), after hearing overflow voice (means outside bucket is full of water), switch off “Inlet Valve” and “Inlet Pump”.5.5.1.5打开“放水阀”继续从内桶加水至溢流口再次有水溢出（说明水箱水已补充满），撤去引水管，停止加水。Switch on “Inlet Valve”, continue to feed water from inner bucket until water overflow from the overflow port again (means the water tank make up full of water), and then remove the diversion conduit, stop feeding water.5.5.1.6关闭“放水阀”。把空氧弹放入内桶，打开“平衡阀”，把外桶的水平衡到内桶（进行模拟实验，溢出多余的水）。然后关闭“平衡阀”，打开“放水阀”（内桶水会自动排放到水箱中），水箱水慢后溢流（如果进行模拟试验后，溢流口没有水流出，则说明备用水箱的水还不足够，需继续按5.5.1.3操作加水，直到模拟试验后有水从溢流口溢出为止）。Switch off “drain valve”, and then put the empty bomb in the inner bucket, switch on the “Balance valve”, balance the outer bucket water to the inner bucket （carry out the simulation test, overflow the unwanted water）. And then switch off “Balance valve”, switch on “Drain Valve” (inner bucket water will auto drain to the water tank), the water tank water will be overflow slowly (after simulation test, if there are no water flow from the port, it means buffer tank have not enough water and should keep feeding water by according to step 5.5.1.3, until there have water overflow from the overflow port after simulation test)5.5.2放水（如果发现水箱水脏，应把水放掉，重新加水）Draining. (If water of the tank water is dirty, if should be changed immediately.)5.5.2.1用软管将放水口连到地漏口直接排水。Connect the relief outlet to floor drain with a flexible tube to drain directly. 5.5.2.2运行测试程序进入“硬件调试”，打开“平衡阀”、“放水阀”。Run the Test Program, and enter into “Hardware Debugging”, switch on “Balance Valve”, “Drain Valve”.5.5.2.3放水完毕后关闭“平衡阀”、“放水阀”，退出程序，拧紧放水螺帽。After finishing draining, switch off “Balance Valve”, “Drain Valve” and then exit this program and tighten the screw cap of the drain port.5.5.3自动恒温桶内的水温与室温之差应小于1.5，一般加水后需放置一晚上，即可平衡。在完成以上工作后，就可以开始试验了。The difference between room and water temperature in the automatic bucket should be kept within 1.5.Usually it should be balance after add water and place over night. The analysis would be beginning after finish all the above works. 5.6热容量的标定（精密度检验）Heat capacity calibration (accuracy test)5.6.1标定的要求Calibration requirements5.6.1.1用苯甲酸(C6H5COOH)连续进行 5 次热容量试验，若其相对标准偏差在 0.20%以内，则其精密度合格，若其相对标准偏差超过 0.20%，可再补做 1 次热容量试验，取符合要求的 5 次结果的平均值作为该仪器的热容量值填入测试软件的“系统设置”中。After analyzing the heat capacity for five times continuously by using benzoic acid (C6H5COOH), if the RSD (relative standard deviation) is within 0.20%, the accuracy should be regarded as qualified. If the RSD is more than 0.20%, one more analysis should be performed, and then select five acceptable results to get the mean value , which will take as the instrument heat capacity value and input into the “System Setting” of the testing software.5.6.1.2如果补做后任何 5 次结果的相对标准偏差仍然不能满足要求，则应对仪器各部件，试验环境条件，操作技术仔细检查，并纠正存在的问题后再重新进行试验，而舍弃已有的全部结果。After making up analysis, if the RSD of any five results still cannot meet the requirements, and the instrument, test condition and operating technology should be checked before running. Correct the existing problems and retest, all the existing results should be abandon.5.6.2标定的方法与步骤Calibration methods and steps5.6.2.1依次打开量热仪主机、计算机电源和主机的开关。预热半小时后方可正常测试。Turn on the calorimeter, computer power and host computer in proper order. Start testing after preheating for half an hour.5.6.2.2运行量热仪测试程序，进入主界面。如图5-5所示Running the calorimeter analysis system and enter the main interface in the screen. As shown in Figure 5-5 图5-55.6.2.3打开“设置”菜单下的“系统设置”窗口，对实验内容和相关参数进行设置。在系统设置中输入苯甲酸的热值、氧弹数、点火丝热值和添加物热值，选择测试内容“为苯甲酸标热容量”，高低位热值为不计算，点击“确定”按钮返回主界面。如图5-6、5-7所示。Click on “System Settings” of the “Settings”, and the user is requested to make setting on analysis content and relative parameters. Input the “Calorific Value of Benzoic Acid”, “Bomb Quantity”, “Calorific Value of Ignition Wire” and “Calorific Value of Additive”. Choose “Calibrating Heating Capacity of Benzoic Acid” for the Analysis Content. Choose “Not Calculate” for the Gross and Net Calorific Value. Click “OK” back to the main interface. As shown in Figure 5-6, 5-7 图5-6图5-7 “系统设置”设置好后即可开始标定热容量。Start heat capacity calibration after finish select the “System Settings”.5.6.2.4从“测试”菜单进入“ 开始测试”窗口，输入试样重量，点击开始进行测试。如图5-8、5-9所示。Click on “Start Analysis” of the “Analysis”, input the” Sample Wight”, press “Start Analysis” to start analysis. As shown in figure 5-9 图5-8 图5-9 系统会自动完成整个测试过程。The system will finish the test procedure automatic. 5.6.2.5实验结束后，将弹出实验结果显示界面。点击“继续实验” 按钮，回到开始界面，进行下一次实验。Once the analysis finish, it wills popup out the Analysis results. Click “Continue Analysis” back to the start interface and carry on the next analysis. 5.6.2.6用苯甲酸标定热容量时要按照仪器的日常操作和国标GB/T213-2003中的有关标定热容量的方法进行试验。When use Benzoic Acid to calibrating heat capacity, it should be according to the Instrument Daily Operation and relevant methods of GB/T213-20035.6.2.7按照上述步骤连续做57个苯甲酸样后。在“功能”“计算平均热容量”窗口，选取符合条件的结果进行计算。保存结果，系统会自动保存计算后得到的仪器热容量。如图5-10所示。如果补做后任何5次测定结果的相对标准偏差仍然不能满足要求，则应对仪器各部件，实验环境条件，操作技术仔细检查，并纠正存在的问题后重新进行实验，而舍弃已有的全部结果。After carry out 5-7 Benzoic Acid samples continuously by the above stepsClick on “Calculate the Average Heat Capacity” of the “Functions”, carry out the calculation by choosing the eligible results. Save the results, and the system will autosave the instrument heat capacity by calculation. As shown in figure 5-10.After making up analysis, if the RSD of any five results still cannot meet the requirements, and the instrument, test condition and operating technology should be checked before running. Correct the existing problems and retest, all the existing results should be abandon. 图5-10 热容量检定技术指标J/KHeat Capacity Calibration Technical Index J/K热容量Heat Capacity15009000110001400015000极差Range940605.7准确度实验Accuracy Test5.7.1实验要求标准煤样测试结果与标准值之差都在不确定度范围内，并且重复性不能超过120J/g(空气干燥基)；或者用苯甲酸作为样品进行 5 次发热量测定，其平均值与标准值之差不超过 50J/g（除燃料燃烧不完全的结果外，所有测试结果不能随意舍弃）。Test Requirements The difference between standard coal sample test results and standard values are all in the uncertainty range, and its repeatability cannot exceed 120J/g (air dry basis); or carry out 5 times calorific value test by using benzoic acid as sample, the difference between average valves and standard values less than 50J/g (except the results of incomplete combustion fuels, all test results should not be abandon at will.5.7.2标准煤样发热量的测定步骤Testing steps of standard coal sample calorific value 5.7.2.1依次打开5E-AC/L量热仪主机、计算机的电源开关。Successively turn on power switch of the 5E-AC/L calorimeter and computer 5.7.2.2运行测试程序，打开“设置”菜单下的“系统设置”窗口，把“测试内容”修改为“煤的发热量”，点击“确定”按钮返回主界面。Run the analysis system, click “System Settings” of the “Settings”, and change the “Analysis Content” to “Calorific Value of the Coal”5.7.2.3从“测试”菜单进入“开始测试”工作界面。往氧弹中装入一个废样进行试验。注意观察点火前水温与室温之差应在1.5以内,否则测试结果会有偏差。 Enter “Start Analysis” work interface from “Analysis”. Carry out the test by putting a waste sample into the oxygen bomb. Before ignition up, pay attention to observe the difference between water temperature and room temperature which should be within 1.5. Otherwise the test results will have deviation. 5.7.2.4半个小时后用坩埚称取标准煤样（样重1g左右，称准到0.0001g）。 Half an hour later, use crucible to weight standard coal sample (the weigh is about 1g with resolution 0.0001g）5.7.2.5装样：将氧弹头挂于氧弹支架上，将装有样