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SQL服务器9003错误的解决 MS SQL错误: 9003,严重度: 20,状态: 1 The LSN (4:272:1) passed to log scan in database 'model' is invalid.近日,开机发现Sql Server服务不能正常启动,于是打开事件查看器,发现错误一项内容为:"错误: 9003,严重度: 20,状态: 1 The LSN (4:272:1) passed to log scan in database 'model' is invalid.".大意好像是在数据库中检测日志Model是无效的.于是我首先将Sqlserver的三个服务停掉;找来Sql Server安装盘,将X86\Data\ Model.mdf,ModelLog.ldf两个文件复到C:\Program Files\Microsoft SQL Server\MSSQL\Data目录下,将Model.mdf,modellog.ldf两个文件覆盖.再启动Sql Server服务.问题得以解决.sql server 错误9003:LSN无效(日志扫描号无效),对数据库的修复.--sql server 错误9003:LSN无效(日志扫描号无效)--今天,从朋友那儿接到一个有问题的数据库文件与日志文件,在使用sql2000与sql2005进行数据库附加时,--sql server报错,错误信息: "传递给数据库'POS' 中的日志扫描操作的日志扫描号(2806:120:1) 无效。
--此错误可能指示数据损坏,或者日志文件(.ldf)与数据文件(.mdf)不匹配。
--如果此错误是在复制期间出现的,请重新创建发布。
否则,如果该问题导致启动期间出错,请从备份还原。
--无法打开新数据库'POS'。
CREATE DATABASE 中止。
June 2009Rev – 1.1Photodetector Sensor BoardSP1202S03RB User’s Guide© 2009 National Semiconductor Corporation.Table of Contents1.0 Introduction (3)2.0 Board Assembly (3)3.0 Quick Start (3)4.0 Functional Description (5)4.1 Operational Modes (5)4.1.1 The Computer Mode (5)4.1.2 The Stand-Alone Mode (5)4.2 Signal Conditioning Circuitry (5)4.2.1 The Transimpedance Amplifier (5)4.2.2 Light Source (5)4.3 Power Supply (5)4.4 ADC Reference Circuitry (5)4.5 ADC clock (6)4.6 Digital Data Output (6)4.7 Power Requirements and Settings (6)5.0 Installing and Using the Photodetector Sensor Board (6)5.1 Board Set-up (6)5.2 Quick Check of Analog Functions (6)5.3 Quick Check of Software and Computer Interface Operation (6)5.4 Troubleshooting (7)6.0 Board Specifications (7)7.0 Example Hardware Schematic (8)8.0 Example Bill of Materials (9)Appendix: Summary Tables of Test Points and Connectors (10)Summary Tables of Test Points and Connectors (cont'd) (11)1.0 IntroductionThe Photodiode Sensor Board (SP1202S03RB), along with the Sensor Signal Path Control Panel (Sensor Panel) software and SPUSI2 USB Interface Dongle are designed to ease the design of circuits using various photodiodes with National’s amplifiers and Analog-to-Digital converters (ADCs). Use the WEBENCH® Photodiode Sensor Designerto determine appropriate ICs and passives to achieve your signal path requirements:/analog/webench/sensors/p hotodiodeSee Figure 1 for component placement and Figure2 for the example board schematic. The circuit for the photodiode sensor consists of a transimpedance amplifier (current to voltage converter) for operation in the photoconductive mode. Also, the board has circuitry to drive a light source (LED) which can be mounted in close proximity to the photodiode. The LED current can be either continuous or switched with the current level adjustable using a multi turn potentiometer.The values for the LED driver are not calculated by Sensor Designer. The idea here is to provide a generic driver stage, allow the user to select a light source and adjust the current accordingly. The light source is not included in the kit. It should be chosento be commensurate with the photodiode wavelength and optical sensitivity.The outputs are a voltage output for the photocurrent (received optical power and a voltage output for the LED current (transmitted optical power). 2.0 Board AssemblyThis Photodetector Sensor Board comes as a bare board that must be assembled. Refer to the example Bill of Materials for a description of component values. The values for the photodiode circuit are calculated using WEBENCH Sensor Designer. The values for the LED driver are not calculated by Sensor Designer.3.0 Quick StartRefer to Figure 1 for locations of test points and major components. This Quick Start procedure provides 5V excitation for the sensor.1. Place the J1 jumper across pins 2 & 3. Thisapplies a negative 5VDC bias to thephotodiode.2. Place the J3 jumper across pins 2 &3. Thissets the ADC reference voltage to 4.096VDC. 3. Place the J4 jumper across pins 2 & 3. Thissets the –VCC to -5VDC. Do not use thissetting for an Op Amp that has a VCC of 5VDCor less.4. Connect the Differential Pressure Sensor Boardto the SPUSI2 board via 14-pin header J2.5. Connect a USB cable between the SPUSI2board and a PC USB port. GRN LED D1 on the Photodiode Sensor Board and D1 on the SPUSI2 board should come on if the PC is on. 6. If not already installed, install the Sensor Panelsoftware on the PC. Run the software.Figure 1. Component and Test Point Locations4.0 Functional DescriptionThe Photodiode Sensor Board component and test point locations are shown in Figure 1. The board schematic is shown in Figure 2.4.1 Operational ModesThis board may be use in one of two modes: the Computer Mode using the SPUSI2 USB Interface Dongle or the Stand-Alone Mode without the use of the SPUSI2 USB Interface Dongle and a PC.4.1.1 The Computer ModeThe board is intended for use in the Computer Mode, where a SPUSI2 board is used with it and the SPUSI2 board is connected to a PC via a USB port. Power to both boards is provided via USB.4.1.2 The Stand-Alone ModeThe Stand-Alone Mode does not use the SPUSI2 board to capture data and upload it to a PC. To use the board this way, the user must provide +5V at pin 14 of header J2 as well as provide ADC clock and Chip Select signals to the ADC at pins 3 and 1, respectively, of J24. ADC data output is available at pin 5 of J2. Test Points may also be used to insert/read these signals. The range of frequencies for the ADC clock is 500KHZ to 1 MHz. The CS rate can be as low as desired, as but no faster than 17 times the ADC clock rate.4.2 Signal Conditioning CircuitryThe output of the TIA (transimpedance amplifier) is on TP1. This is a voltage that is proportional to photocurrent. The values for RF and CF are calculated by the WEBENCH Sensor Designer. RF is determined by the full scale input voltage of the ADC and the maximum output photocurrent of the photodiode. CF is determined based on photodiode capacitance and an estimate of stray capacitance on the inverting input of OP Amp U1. The current flowing in the LED is measured and scaled by Op Amp U2 and appears on TP3. These voltages appear on the inputs of ADC U4. The digital output of the ADC appears on J2 Pin 5.4.2.1 The Transimpedance AmplifierIn the photoconductive mode, the cathode of the photodiode is connected to the inverting pin of an op amp with the non inverting pin grounded. To maintain the virtual ground on the inverting pin, the op amp must provide current from its output through the RF to the photodiode.So: V out = I PHOTODIODE * RF.RF is determined by knowing the maximum photocurrent, sometimes referred to as I SHORT CIRCUITof the photodiode, and the full scale input value of the ADC.So: RF = VFS/I SHORT CIRCUIT Because the photodiode has capacitance, RF andC DIODE form a pole in the noise gain transfer function. This can create stability issues and is compensated for by CF. WEBENCH Sensor Designer calculates the value of CF for a 45 0 phase margin to insure stability.4.2.2 Light SourceProvisions for a light source for test purposes are on the board.The user can select an LED with appropriate wavelength and output power to compliment the photodiode selection. It may be necessary to modify component values in the LED driver to optimize performance.S1 is provided as an ON/OFF control for the LED drive circuit. It controls the gate voltage of an NCH MOSFET. In the open position, the mosfet is conducting and the current source is enabled.Also connected to the gate of the mosfet is a connector for a signal generator. A switching signal can be connected here to observe the transient response of the transimpedance amplifier. The rise times and switching frequencies are somewhat limited by the current source components and the mosfet switch so the user may want to install different components to achieve higher performance for the current source in this mode.The current source consists of U3, Q1, VR1 andR7. The op amp will make sure the voltage at the CT of VR1 appears on the inverting pin. This voltage then appears across R7 (minimal V ON forQ2). I LED = VR1CT/R7. Turning VR1 clockwise increases LED current. The differential amplifier U2 measures the current flowing in the LED by measuring the Voltage drop across R4. This voltage drop is scaled by the gain setting resistors.I LED = Analog_V2/(R3/(R2*R4))4.3 Power SupplyIn the computer mode, power to this board is supplied through header J2 and ultimately from the host PC via USB. In most cases, the only voltage needed for the Photodetector Sensor board is the+5V from the USB connection.The supply voltage source for the ADC (VREF on the schematic) is selected with J3 to be either the 4.1V from U5, or +5V from J2.4.4 ADC Reference CircuitryThe single-ended ADC122S101 uses its supply voltage as its reference, so it is important that its supply voltage be stable and quiet. A 4.1V reference voltage is provided by U5, an accurate LM4120-4.1.4.5 ADC clockThe ADC clock signal is provided external to the board at header J2. The frequency of this clock should be in the range of 500KHZ MHz to 1 MHz. A CS (Chip Select) signal is also required at J2. See the ADC data sheet for timing requirements.4.6 Digital Data Output.The digital output data from the ADC is available at 14-pin header J2. All digital signals to and from the ADC are present at this connector socket.4.7 Power Requirements and SettingsVoltage and current requirements for the Photodetector Sensor Board are:∙Pin 14 of J2: +5.0V at 30 mA∙Pins 2 and 4 of J2: GroundWith J4 connected from pin 2 to pin 3, the op amps in the circuit have a -5VDC on the -VCC terminals. This will yield a more accurate result for zero current flow in the LED and zero light level received in the photodiode. J4 pin 1 to pin 2 places GND on the –VCC pin.The Photodiode can be reversed biased by connecting J1 from pin 2 to pin 3. This will reverse bias the photodiode by -5VDC and reduce the diode capacitance. This will reduce the effects of noise gain peaking due to capacitance on the inverting input of the transimpedance amplifier. J1 pin 1 to pin 2 connects the photodiode anode to GND.5.0 Installing and Using the Photodetector Sensor BoardThis Photodetector Sensor board requires power as described above.5.1 Board Set-upRefer to Figure 1 for locations of connectors, test points and jumpers on the board.1. Connect the Photodetector Sensor board to aSPUSI2 USB Interface Dongle.2.Be sure all jumpers are in place per Table 1,below.Table 1 - Jumper Default PositionsJumperPinsShortedFUNCTIONJ1 2-3 Neg. Photodiode BiasJ3 2 - 3 4.1V ADC ReferenceJ4 2 - 3 -5VDC for -VCC3. Connect a USB cable to the SPUSI2 board anda PC. 4. Confirm that GRN LED D1 on thePhotodetector Sensor board is on, indicatingthe presence of power to the board.5. Be sure that the correct light source is installedin close proximity to the photodiode.6. Be sure the current source values are chosen todrive the Light Source with the correct currentlevels.7. For more accurate light power measurements itmay be necessary to fashion a light shield tocover both the light source and the photodiode.Sufficient room around these two componentshas been provided for a light shield.5.2 Quick Check of Analog FunctionsRefer to Figure 1 for locations of connectors and test points and jumpers on the board. If at any time the expected response is not obtained, see Section 5.4 on Troubleshooting.1. Perform steps 1 through 7 of Section 5.1.2. Check for 5.0V on VCC and for 4.1V at TP8.3. Check for -5V at J4 pin 3.4. Turn S1 ON.5. Monitor the voltage on TP3.6. As the potentiometer is adjusted, the DC voltageon TP3 will vary. Verify the LED current is in thecorrect range.7. As the potentiometer is adjusted, the voltage onTP1 should also vary based on the amount oflight the source is generating.This completes the quick check of the analog portion of the evaluation board.5.3 Quick Check of Software and Computer Interface Operation1. Perform steps 1 through 7 of Section 5.1.2. Run the Sensor Panel software on the PC.3. Select the SPI202S03RB Board.4. Manually enter the following data:∙Responsivity of the photodiode under test.∙ RF∙Number of bits∙Input Optical Power. This value is determined by setting the LED current,going to the LED datasheet and reading thepower out at that LED current and at thephotodiode wavelength.∙ Reference VoltageThe software will measure the photocurrent ofthe photodiode and the LED current.The software knows the input power, calculatesthe received power and estimates the opticalloss between the LED and the photodiode.This completes the quick check of the software and computer interface.5.4 TroubleshootingIf there is no output from the board, check the following:∙Be sure that the proper voltages and polarities are present.∙Be sure there is a clock signal at TP11 when trying to capture data.∙Be sure there is a voltage at TP3 that varies with light source current adjust.∙Be sure that the voltage on TP1 varies with light source current adjust. If the ADC output is zero or a single code, check the following:∙Be sure that the proper voltages and polarities are present.∙Be sure that J2 is properly connected to a SPIUSI-2 USB Interface Dongle.6.0 Board SpecificationsBoard Size: 2.6" x 2.5" (6.6 cm x 6.35 cm) Power Requirements:+5V (30mA) at J2 pin 147.0 Example Hardware SchematicAPPENDIXSummary Tables of Test Points and ConnectorsTest Points on the Photodetector Sensor BoardIdentifier Name FunctionTP 1 Analog_V1 TIA Analog OutputTP 2 GND GroundTP 3 Analog_V2 Current Meter Analog OutputTP 4 GND GroundTP 5 Isense + Current Sense Resistor +TP 6 Isense - Current Sense Resistor -TP 7 J5 Pin 1 Waveform Generator InputTP 8 VREF ADC VDCTP 9 CS* CS* input for ADCTP 10 GND GroundTP 11 SCLK SCLK Input to ADCTP 12 DOUT SDATA output from ADCTP 13 VCC_3V3 3.3VDC from SPUSI2 BoardTP 14 DIN ADC DIN from SPUSI2 BoardJ1 Jumper – Photodiode Bias SelectShorted Positions Results1 -2 GND on Photodiode Anode2 -3 -5VDC on Photodiode AnodeJ3 Jumper - VADC_SELShorted Positions Results1 -2 +5V for ADC Supply and Reference Voltage2 -3 +4.1V for ADC Supply and Reference VoltageJ4 Jumper - -VCC SelectShorted Positions Results1 -2 -VCC = GND2 -3 -VCC = -5VDCSummary Tables of Test Points and Connectors (cont'd) J2 Connector - Connection to SPUSI2 BoardJ2 Pin Number Voltage or Signal1 CS* input to ADC2 Ground3 SCLK input to ADC4 Ground5 SDATA output from ADCconnection6 no7 DIN to ADCconnection8 no9 noconnectionconnection10 noconnection11 no12 noconnection13 +3.3V from SPUSI2 USB Interface Dongle14 +5V from SPUSI2 USB Interface DongleThe Photodetector Sensor Board is intended for product evaluation purposes only and is not intended for resale to end consumers, is not authorized for such use and is not designed for compliance with European EMC Directive 89/336/EEC.National does not assume any responsibility for use of any circuitry or software supplied or described. 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免疫组化操作步骤一、实验原理与意义免疫组织化学又称免疫细胞化学,是指带显色剂标记的特异性抗体在组织细胞原位通过抗原抗体反应和组织化学的呈色反应,对相应抗原进行定性、定位、定量测定的一项新技术。
它把免疫反应的特异性、组织化学的可见性巧妙地结合起来,借助显微镜(包括荧光显微镜、电子显微镜)的显像和放大作用,在细胞、亚细胞水平检测各种抗原物质(如蛋白质、多肽、酶、激素、病原体以及受体等)。
(一)、仪器设备1. 18cm不锈钢高压锅或电炉或用微波炉.2.水浴锅(二)、试剂1. PBS缓冲液(ph7."2―7."4):NaC137mmol/L,KCl2."7mmol/L ,Na2HPO44."3mmol/L, KH2PO41."4mmol/L.2."0.01mol/L柠檬酸钠缓冲液(CB,ph6."0,1000ml):柠檬酸三钠3g,柠檬酸0."4g。
3.0."5mol/L EDTA缓冲液(ph8."0):700ml水中溶解186."1g EDTA& 8226;2H2O,用10mmol/L NaOH调至ph 8."0,加水至1000ml.4. 1mol/L的TBS缓冲液(ph8."0):在800ml水中溶解121gTris碱,用1N的HCl调至pH 8."0,加水1000ml。
5.酶消化液:a.0."1%胰蛋白酶:用0."1%CaCl 12(ph7."8)配制。
b.0."4%胃蛋白酶液:用0."1N的HCl配制。
6. 3%甲醇―H2O2溶液:用30%H2O2和80%甲醇溶液配制7.风裱剂:a.甘油和0."5mmol/L碳酸盐缓冲液(pH9."0–9."5)等量混合b油和TBS(PBS)配制8."TBS/PBS PH9."0–9."5,适用于荧光纤维镜标本;ph7."0-7."4适合光学纤维标本(三)、操作流程1、脱蜡和水化:脱蜡前应将组织芯片在室温中放置60分钟或60℃恒温箱中烘烤20分钟。
免疫组化实验步骤免疫组化操作步骤一、实验原理与意义免疫组织化学又称免疫细胞化学,是指带显色剂标记的特异性抗体在组织细胞原位通过抗原抗体反应和组织化学的呈色反应,对相应抗原进行定性、定位、定量测定的一项新技术。
它把免疫反应的特异性、组织化学的可见性巧妙地结合起来,借助显微镜(包括荧光显微镜、电子显微镜)的显像和放大作用,在细胞、亚细胞水平检测各种抗原物质(如蛋白质、多肽、酶、激素、病原体以及受体等)。
(一)、仪器设备1. 18cm不锈钢高压锅或电炉或用微波炉.2. 水浴锅(二)、试剂1. PBS缓冲液(ph7.2―7.4):NaC137mmol/L,KCl2.7mmol/L ,Na2HPO4 4.3mmol/L, KH2PO4 1.4mmol/L. 2.0.01mol/L柠檬酸钠缓冲液(CB,ph6.0,1000ml):柠檬酸三钠3g,柠檬酸0.4g。
3.0.5mol/L EDTA缓冲液(ph8.0):700ml水中溶解186.1g EDTA& 8226;2H2O,用10mmol/L NaOH调至ph8.0,加水至1000ml.4. 1mol/L的TBS缓冲液(ph8.0):在800ml水中溶解121gTris 碱,用1N的HCl调至pH8.0, 加水1000ml。
5. 酶消化液:a.0.1%胰蛋白酶:用0.1%CaCl 12(ph7.8)配制。
b.0.4%胃蛋白酶液:用0.1N的HCl配制。
6. 3%甲醇―H2O2溶液:用30%H2O2和80%甲醇溶液配制7. 风裱剂:a.甘油和0.5mmol/L碳酸盐缓冲液(pH9.0–9.5)等量混合 b 油和TBS(PBS)配制8.TBS/PBS PH9.0–9.5,适用于荧光纤维镜标本;ph7.0-7.4适合光学纤维标本(三)、操作流程1、脱蜡和水化:脱蜡前应将组织芯片在室温中放置60分钟或60℃恒温箱中烘烤20分钟。
a 组织芯片置于二甲苯中浸泡10分钟,更换二甲苯后在浸泡10分钟b 无水乙醇中浸泡五分钟c 95%乙醇中浸泡五分钟d 75%乙醇中浸泡五分钟2、抗原修复:用于福尔马林固定的石蜡包埋组织芯片:A 抗原热修复a 高压热修复在沸水中加入EDTA(ph8.0)或0.01m枸橼酸钠缓冲溶液(ph6.0).盖上不锈钢锅盖,但不能锁定。
免疫组化操作步骤一、实验原理与意义免疫组织化学又称免疫细胞化学,是指带显色剂标记的特异性抗体在组织细胞原位通过抗原抗体反应和组织化学的呈色反应,对相应抗原进行定性、定位、定量测定的一项新技术。
它把免疫反应的特异性、组织化学的可见性巧妙地结合起来,借助显微镜(包括荧光显微镜、电子显微镜)的显像和放大作用,在细胞、亚细胞水平检测各种抗原物质(如蛋白质、多肽、酶、激素、病原体以及受体等)。
(一)、仪器设备1. 18cm不锈钢高压锅或电炉或用微波炉.2. 水浴锅(二)、试剂1. PBS缓冲液(ph7.2―7.4):NaC137mmol/L,KCl2.7mmol/L ,Na2HPO4 4.3mmol/L, KH2PO4 1.4mmol/L. 2.0.01mol/L柠檬酸钠缓冲液(CB,ph6.0,1000ml):柠檬酸三钠3g,柠檬酸0.4g。
3.0.5mol/L EDTA缓冲液(ph8.0):700ml水中溶解186.1g EDTA& 8226;2H2O,用10mmol/L NaOH调至ph8.0,加水至1000ml.4. 1mol/L的TBS缓冲液(ph8.0):在800ml水中溶解121gTris碱,用1N的HCl调至pH8.0, 加水1000ml。
5. 酶消化液:a.0.1%胰蛋白酶:用0.1%CaCl 12(ph7.8)配制。
b.0.4%胃蛋白酶液:用0.1N的HCl配制。
6. 3%甲醇―H2O2溶液:用30%H2O2和80%甲醇溶液配制7. 风裱剂:a.甘油和0.5mmol/L碳酸盐缓冲液(pH9.0–9.5)等量混合 b 油和TBS(PBS)配制8.TBS/PBS PH9.0–9.5,适用于荧光纤维镜标本;ph7.0-7.4适合光学纤维标本(三)、操作流程1、脱蜡和水化:脱蜡前应将组织芯片在室温中放置60分钟或60℃恒温箱中烘烤20分钟。
a 组织芯片置于二甲苯中浸泡10分钟,更换二甲苯后在浸泡10分钟b 无水乙醇中浸泡五分钟c 95%乙醇中浸泡五分钟d 75%乙醇中浸泡五分钟2、抗原修复:用于福尔马林固定的石蜡包埋组织芯片:A 抗原热修复a 高压热修复在沸水中加入EDTA(ph8.0)或0.01m枸橼酸钠缓冲溶液(ph6.0).盖上不锈钢锅盖,但不能锁定。
2010-01-2920:48各种彩电遥控器型号及代换大全熊猫遥控器遥控器型号遥控器芯片对应CPU芯片适应机型备注YKF-1 M50462AP M50436-560SP C3615C3631B C3631C YKF-1A M50462AP M50436-560SP C3615D C3631D C3640BC3658C3642AC51P3C51P1M YKF-1B M50462AP M50436-560SP C3651C3653 C64P88Y KF-1C M50462APM50436-560SP C3659 YKF-2 M708LB1 M494B1 C3617YK F-2AM708L B1 M494B1C47P1YKF-2A M708LB1 M494B1 C3608A交流关机YKF-3 TC9012F-011MP47C430NC3615B C3632 C3643 YKF-3A TC9012F-011 M P47C430N C3615C C3640YK F-5 S AA3010 PCA84C640 C74P2Y KF-7M50560-003P M37210M3-508S P C2118 C2119 C2128C49P4C54P4C54P11C54P19 C54P26YKF-9 M50462A P M50436-560SPC2120 C2138 C54P3C54P10 YKF-11 M50462AP M50436-560SP C64P1C64P88 C74P2Y KF-12 TC9012F-011 MP47C430N C37P4 C44P3C47P1C49P2YKF-13 T C9012F-011 MP47C430N C54P12Y KF-15 SAA3010TPCA84C440C54P5 C54P37 C64P2C64P4 C74P2MYKF-16 M50560-003P M37210M3-508SP C2528 C54P18 C64P6YKF-18 TC9012F-011MP47C837NC54P4A C54P4L C54P22 C64P8YK F-20M50560-003P M37210M3-508S P C54P24 YKF-21 LC7461 H S0038 C54P32 C74P4 YKF-22 LTD001CR LC84012LC54P32 C74P2 C74P4 东芝机芯RCE1M50560-001P M37210M3-508S P C3632 21C1R CE2 T C9012F-011 MP47C430N C14C3YK F-24TC9028-012SP C2518 C2918YKF-26 M50560-003 M37210M3-508SP C2138A C54P29BC54P35C54P37YK F-27TC9012F-011 MP47C837N C44P5Y KF-28 TC9012F-011 C54P4554P8 M3004 C54P8 C54P9 QDF-5D4B M50560-003P C64P2YK F30 M50560-003PYKF-33 T C9028-012YKF-39Y KF-40 TC9028-023厦华遥控器遥控器型号遥控器型号对应C PU芯片适应机型备注R CF 01 TC9012F011 TMP47C634-2465 3781A 1020/SRCF02 TC9012F011 RCF 03 M34300N4-0126698T H 7698TH RCF 05 TC9012F011 TM P47C634-384 XT-3770R C/RN/RZ5151R 5170RK/RZ 5160RC/RR/R Z 5180RZ 5650R5670R R/RZ5660R/RN/R R/RZ5680R C/RK/RN/RR/RZ 5690RZ 6687RCF 10 X T-5661SR CF 16 M3004LABST6378 XT-37715661/T 5670RT 5680RA/RT RCF-20 TC9012F011 TM P47C634-384 XT-3770R 5160R 5660R 5680R RC-K21 TC9028-021 CT S763B XT-2195T2555T2965T 3465TRC F 22TC9012F011 KY84C94 X T-6667T/TZ 6698TA 71220TA 7687T7698TA 6687SRCF27 TC9012F011 K Y84C94 XT-6668T/TC 7128TRCF-30 TC9012-011 RCF 31 M50560-008P M37211M2-704SP RCF 36 TC9012F011 KL84C94 XT-7688T/TC 7128T RCF 37 TC9012F011 KL84C94 XT-6687THRCF 42 M50560-008P M37211M2-704SP XT3770RF5160R F 5170RF 5180RF 5660RF 5670RF5680R F 5690RF 6667TL/TJ/T N 6687TN/T J XT-7687RCF45 TC9012F011 K L84C94 XT-6687T G 7687TG RCF 46 M50560-008P M37211M2-704SP X T-6668TL/T M 6688TL 7688TL/TM/T VRC F 47M50560-008P M37211M2-704S P XT-6667T L/TM6687T L 7687TL/T MRC F 51TC9012F011 TMP47C634-RC18 XT-5660RY 5670RY 5680RY5690R Y/RRRCF52 TC9012F011 W ST98A01 XT-6637TB 6507TB7687T B DM-2522TRCF 54 T C9012F011WST98A01 X T-7688T/TG 7128TRC F56 M3004L B1 ST6387XT-2080II2197I I 21K82570II 5670RXRCF57 TC9012F-011 W ST98A01 XT-7687TGR C-K58 TC9012-023RC F59 S AA3010T TV222-P R XT-2560257029602970 2980 RCF60 M3004LB1ST9291 XT-2167217721872197/RRC-E04 D1986UPD1937CUP C1362 XT3701/A3702/A3751B 1902 51015102 MTV-137MT V-147RC-E03 T C9012F-011 TMP47C432N-8094 XT5103/P/NR C-E06 TC9012F-011 TM P47C634N-2465 X T-3751 3902 51405103DA 5622R C-D04 M50560-001P M34300N4-012 XT5653T 6698T7103T/TA/K7120T/TZ7698T/T R/TZRC-K21 TC9028-021 C TS763B XT-2195T 2555T 2965T 3465T金星遥控器遥控器型号遥控器芯片对应CPU芯片适应机型备注射器JY F-2C1YH-F2C M708LB1M491B1 C514J-HYF-03JYF-2C2 M708LB1 M491B1 C512 C513 C564 JYF-3C3J-H YF-08 M50462APM50436-560SP C542 C541 C491J-HYF-04 M50560-123 M34300N4-555SP C514 C515 C518 YH-F4BJ-HY F-06J YF-3C M50462APM50436-560SP C4717 CT-9679 UP D6125AG-76E C7428J-HYF-10 SA A3010 PCA84C640/641C498J-HY F-10B SAA3010 P CA84C640/641 C5128BJ-HY F-11TC9012F-011 C518 C548 C5418C546-1 J-HYF-12 M50462AP M50436-560SP C4717A C543-1J-HY F-15TC9012F-011 C5418J-HYF-16 M50462A P M50436-560SPC6418J-H YF-17 SAA3010TPCA84C640/641 C498-1J-H YF-18 M50462APM50436-560SP C718J-HYF-U18 M50462AP M50436-560SP C648J-H YF-19 TC9012F-011 TM P47C432/433 C546-1 C5428C79650 UP D6125A CXP80420-139S C6428035/5 L C7462-8167N M34300N4-628M34300N4-721 C5438 C5488 C5458NC15A BU5777FC6438G335051M50462AP M50436-560S P C648-1 UPD1943G C471-1 C478 C2110MN6014A MN15245KW C C4718 C4918 G33512 M50467-001P/F P M37102M8 C6438 C6468 C7411 8C LC7462G328051 M50462APG328052 M50462APG328061SAA3010T G328111 PC F84C122A093G329000 LC7461G330081 LC7462 G335122 M50467-001PG329003 L C7461G327740TC9028-023Re:各种彩电遥控器型号及代换大全赣新遥控器遥控器型号遥控器芯片对应CPU芯片适应机型备注M50462 M50436-560S P KG-4701470247034706 KG-5106 5116 5186-25186-3KG-2156 5401 540654165426KG-5436 5446 MN6014A MN15287KW KG-6409 2909M37102MB-509S P KG-6401M3700MB4-506SP KG-5415 5425 54352158M37211M2-604SP K G-2518 2528 2918SA A3010T CTV222SKG-5428K D9218 KG-6402 M50560-003PM50560-008PM50467-001P 同5D4 KG-6401北京遥控器遥控器型号遥控器芯片对应CP U芯片适应机型备注释M50462AP 8316/-2 8329 541/YHY DF-15AHYDF-15AD KS51840-D0 2102 2113Q 2120Q2122Q 2129Q2182Q2183Q 2184Q 2191Q5422S 5429S HYDF-51A K S51840-D02516T 2518T 2922T 2925T 2903 29052913/T2915T29AT57A HYDF-57A K S51810-D02505G 2506G 2903G2905G 2911G 2912GHYDF-57B1 2506G 2508 2511G2513GH YDF-201D HYDF-2162KS51810-02 PCN84C444P/504 2162C/H 8346 8348-18348-2DH YDF-2163 K S51810-54216321645083HYDF-2181 KS51840-D0 2181 8346-1 HYDF-A3 LC74621401N 1801N 2131M2132NA 8310A8312N8316A 8320A8327A8336A/N8353A 8355AHY DF-A3-1 BU2483-13 2010 2101 21028356/C 8366 HYDF-A3-2BU2483-1321032104/A 8366CH YDF-A6 LC7462 2102 2501 25022503 2901 29022903HY DF-B1 M50462 2106/C2107/A 5418HY DF-B2 M50462 2108 2109 21102903HY DF-B3 TC9012 8320/G/N 8320-18320-28320-3 8353G8320-IN8320-2H8351G H YDF-B3K 2531 8368H YDF-B3K 2531 8368H YDF-F91 D6125A766 2931/H8361/HHY DF-FP5J KS51810-02 2162/C 8348HYD F-TC9650 D6125A766 2931 8340 8361 M50462 511A 541/Y 83138316 8316-2 83278329 8343M50560-0018348AA59-00097A KS51840-D0 AA59-00098A KS51840-D0福日遥控器遥控器型号遥控器芯片对应CPU芯片适应机型备注FH211 2998FI112 D6124A F21 2552 FI 113 1260 2553FH211 D6124A F212998FN112 D6124A F21ZSD DD` FM321 M50467-001P M372102M8-530SP H FC2586 2587 29862987FN111 D6124AF21 29816 29910P1P6 SAA3010T21P60VD101 2175 2176V M101M50560-123 M34300N4-555SP 1814R 2014R 2111RGB3701VM201 M50462APVM222 M50462A P 2122 2125 2024RV M2312998VM301 M50560-170FP216821692188VP101 SAA3010TVP112 2174V P121SAA3010P 2173 VP151 2179VP153 2178V P202M50462AP VS141 M3004LB121082109FN111 MDT2005D LRC-F05TC9012F-011VM321 M50560-170F P 2582 2591P1-P6 S AA3010T 21P60 P2-P6 SAA3010T海信遥控器遥控器型号遥控器芯片对应CPU芯片适应机型备注HYD FSR-0002 D6125A766CXP80420-139 2525 2919 2929 H YDFSR-0010 D600A B88HYD FSR-0011 P CA84C122A/093 P C2143 360S FRH YDFSR-0016 D6600A B88 2958HY DFSR-A0011L 6122-001 2968HYD FSR-0023 P T2214HYD FSR-0013 P T2212HYD FSR-2020 T C9028-021HYDF SR-0041H YDFSR-A001HYD FSR-A0112HYDF SR-0035 BE2483-13H YDFSR-0037 TC9012-011HY DFSR-0041TC9012-011HYD FSR-0043 HYDFS R-0043L 8521BT/040SIHYD FSR-0046 L C7461-103HYDF SR-0048 LC7461-103 HYDFS R-0048L LC7461-103 HYDFS R-0035HY DFSR-328111 PCF84C122-0937461系列遥控器遥控器型号遥控器芯片对应CPU芯片适应机型备注7E1 LC7461-8103 LC864012L-54637EA LC7461- LC864012L-57118EA LC7461- L C864912L-5G13菲利浦遥控器遥控器型号遥控器芯片对应CPU芯片适应机型备注RC7802SSAA3010T 21A9221B9RC7812S S AA3010T 21D9 25B9 29B9 21D8R C7952 21V8 25V7RC7953 21V9 25V8 RC7594 29V8RC795929V921K8 PCA84C122AT1 25A6 29A6 21V7 21B8索尼遥控器遥控器型号遥控器芯片对应CPU芯片适应机型备注RM-626A C X523-110PC X522-063/054 M50119KV1423CH 1882CH 2062CHR M-643 M50460-012P 2090 2092CHRM-656A B U2483-2P(G S5053-002) M50431-513SP K V2181DC 2182D 2182DCRM-677 B U3780F 2553RM-679KV2900RM-681RM-687C B U5810F KV2184TV 2510CRM-821RM-827S 6600(H D9601) 2593V1A2825296529662593KV1485 2185F25MF1 K V2565 2189 2585RM-845PKV29RM-845S 2189 2189TCRM-849SM34302MB-612S 2189 2189TCRM-857SK25 K29 F25MF1RM-857A K V21845MTJRM-870R M-873 D6133 544RM- M34280R e:各种彩电遥控器型号及代换大全夏普遥控器遥控器型号遥控器芯片对应CP U芯片适应机型备注G0676CE SA IX0733IX0981CE C V2100 2102 2106VLA 2122 2122DK 2162CK 5404 21S11 A121S11-A221S21-A1 G0756CESAIX1741 C573 2121DK G0933PESA14D-C MG1077PE SA 2500G1069P ESA I X1560CEG1602P ESA 3714 G1084PESA6600A E70 G1021PESGIX1560CE 0615C ESA 2X0773CE 同0676CE SA三星遥控器遥控器型号遥控器芯片对应CPU芯片适应机型备注3F14-00038-0933F14-00038-3403F14-00038-9003F14-00034-A11 KS51900-52 3F14-00034-270KS519000-22 M50439-214SP三星21993F14-00038-311 KS51810-78 3F14-00034-B90KS51810-023F14-00038-420 同北京21813F14-00038-450 KS51840-D0 同北京21813F14-00038-150 KS51800-383F14-00050-050 KS51800-80 3F14-00038-121KS51800-52AA59-10041R K S51810-79SMM-201 4C5401松下遥控器遥控器型号遥控器芯片对应CP U芯片适应机型备注2140 9012 EU R501325 TC214021102150 TC2150 21602185 M N141542TEA50560-200TNQ2645 TC2185187018711872 1873 207020902163 21702125 2172 21732186 2187 D21C D25C2188 M50560-001P TN Q10408 TC2188 2588 2530 2550TC2550M25 M50560-117 TN Q2678 M25263626722687MV29C小画王 M50560-001P 21L3R 21-10R 21-E1NB T0009M2485-20 2148牡丹遥控器遥控器型号遥控器芯片对应CP U芯片适应机型备注HY DFMID-7 TC9012F011 54C10HYDF MD1005 TC9012F011H YDFMD1009TC9012F011HYD FMD-P281 M50560-008PRC-007 L C7462 54C5HYD FMDP25D SA A3010T50560-003 64C1 64C2 74C2日立遥控器遥控器型号遥控器芯片对应CPU芯片适应机型备注CLE-821 UP D1943 CADD-161D CTP-233D237D18381838D CMT-208520832083D CEP-3210323D327DCRD-451D H FC-238DX 2024 CLE-860 CP T1801 2001 2008CLE-862UPD1943G M50432-551S P 1803 1910 2024 2038 2038D 2103 2110 21252403 2403SFCLE-862ED6124A511CLE-865 M50560-123F P 2157SF/D U 同VM101 CLE-865A M50560-123F P GMT2138CPT2150 同V M101CLE-865B21752157S F/DUCLE-866AD6124A 620 2159 2177SF/DC 2408 2518CLE-866B 2700 2908 2918 3300CLE-866C 2901CLE-866E D6124A 679 2918CL E-878 M50560-170FP 2992 21D8C2159CMT2195 25D8C 2192 CLE-886 D6114A355 C25M8A 21D8A 25D8A 29M8A CLE-891 M50560-170FP 2992 21D8C 2159 CMT219525D8C 2192CLE-893A D6124 2118 2518 21M8CC LE-894 D6124A C SC23CLE-898 50560-170FP 2195CLE-900A D6124A B24CL E-904 D6124ACSC46C LE-907 D6124ACS C47VM101 CPT-1435 1888 2105东芝遥控器C T-9199 198D6C 218D6C 218R8C2 2185 289C T-9200 288X6M CT-9335 219D8MCT-9369 M34300N-587P 219R9C CT-9396 21R92 CT-9430 188D6C198D6C 218D6C 2500XH 2806 289X6N 289X8MCT-9507 2104 9507 CT-9599 TC2518K B 2518KTVCT-9631 2929KT PCT-9640 2125 2128CT-9643CT-9687 2940 CT-9612 28W3DSH 28W3ME 28W3DXH三洋遥控器R C700CTP69510 6953 697华强三洋C MK2089 2169 2176DK-00 2176DK-01 2179-002179-50 2179-60 21812189 CME2143C-00 CK P2161D-00CTP6951D-00 6069R e:各种彩电遥控器型号及代换大全[值得收藏]一(代号SN-101)M50462AP(BU5905)对应CP U: M50436-560SP, 30频道,常用机型熊猫 (Y KF-1YKF-1A/B/C YKF-9 YKF-11)2120213836153615D 3631 3631A 3631B 3631C 3631D3631M 3635 3636 3640B 36423642B3642A 3651 3653 3658 3659 54L2 54L5 54L2A54P354P17 54P10(带交流关机) C51P1M C51P1Z C51P3 C64P1C64P88北京 541Y 2103C 2104C 8313 8316 8316-28343长虹C K49A53A 2141 2421 上海 Z247-5C 249-1A 249-2A249-5A 254-5A 254-5A1 651-1A 654-2A 654-4A 654-4A1 656-5A 海燕 CS54E-3-R CS54E-4-R CS54E-5-R CS54B-3-R CS54B-4-R HC-9012黄河HC-47 47-V1 47A VI 4402 4703 4708 4901 5401 5405 5405A 54065425560244FS-1 44F S-II54FS-I 54F S-II韶峰C AD8903 SFC47-5B SFC54-4 长城(画龙) 8148赣新 KQ5106 5186-354015401A 5406 5409 5416 5426金星(J-HY F-3CJ-HYF-4B J-HYF-05 J-HYF-06 J-H YF-08 J-HY F-16J-HYF-18 Y KF-U18)C491 512 541 542 543543-1 648648-1 71847174717A 5438 5458 5488 6418飞跃(FY2FY21FY22) FY4701 5401 6402 6405 6405K47C2Y2X-147C2Y2-6 54EY249C2Y21-1 51C2Y2-251C2Y21-254C2Y2-1 54C2Y-2 4C2Y21-1 54C2Y21-2福日(VP202) HF C1425 1725 1824 1824R 1925 2024R 2025 2125凯歌 4C4401 5101 5104 5401 5401-1 5404 5405孔雀(KQ-Y KF-1KQ-YK F-3 K Q-YKF-6 KQ-YKF-8 KQ-YKF-9)KQ44-38-1 47-39-5 49-39-1 51-38-451-39-5 51-39-7 54-38 54-38-154-39 54-39-254-39-5 54-39-5A 54-39-654-39-8A 64-39198821502188D 2188G环宇 47C-2R 51C-4R54C-2R 54C-2RA牡丹47C1049C151C151C551C5A 54C3 54C3A 54C4 54C4A宝声 21388 21389 2168821688A 21689 21689A25588 25689西湖(YKF-4L Y KF-4P YKF-10)51CD5A 51CD5C 54CD6 54CD8A 63CD1A 6403 成都 C47-851F 47-851FA47-851K 51-851K 53-871 54-87156-871A美乐 DS44C-147C-3 47C-3A1 51C-351CD5 51CD5A 53C-2 54C-254CD6 1808 2108 2188B 4F3A2B1虹美(YKF-3B YKF-4C)477451556403乐华(YKF-3)TC541-2PD 511-3PD(R)III三元44SYC-3 54S YC-3青岛S R5417 4426长风C FC54-3FR 54-3FR1 54-7FR 泰山 TS54C10 44C13 红岩SC-543彩虹 CAD8903 3909 8913 春笋 CSD541 黄山 AH5353C AH5353R 南声 ZY-5401如意S GC-4403 5403A 5403C菊花 FS531AFS531B金凤 C51S Y C54SZ C54SZ1天鹅 CS47-C3 54-S1沈阳 SDSY51-254-2山茶 SC-L54E Y1金鹊 53D C1 53DC13华利 5140 5410日电 NEC5260P DH 5460PDH 5488PDH 飞鹿 54C2 54C3赛格 5140PDH 5410PD H 长飞附注:1,M50462AP遥控器模拟量的调节方式有两种:其一是模拟量分开单独调节,此类使用较多,如长虹熊猫北京等;其二是菜单调节方式,如康佳等;注意区别选用2,少量机型多几种功能,如孔雀KQ54-39-6带交流关机,KQ64-39带立体声二(SN-101A)M50462AP 对应CPU:M50436-560S P 或C PU:Z86227系统 30频道,30键,模拟量菜单调节方式康佳(KK-Y01 KK-Y07KK-Y08 KK-Y19)KK-T920D920DI 953P 953P I 953PIII953PI I 953II 953III953B1826 1926 2109 2110 2126 2128 2188 5402优拉纳斯 U49-39-1B U54-39-5B三(SN-102)3010TCTV222,CTV320S,CTV322系统,对应CP U:PCA84C440/444/504/640/641,90频道,32键,常用机型,熊猫(YK F-5 Y KF-15) C54P5 C54P6 C54P37 C64P2 C64P4 C74P2 C74P2M北京2162C 28”8346-1菲利蒲(RC7802) 4703F 21A9 21B9 25”虹美(YKF-1A)4703 5109 5306 5445 5456 5456C飞跃(FY3 F Y31)44C3Y3-1 47C3-3 51C3-1 51C3F 51C3Y-2 51C3F3-2 FY4702 5402凯歌 4C3705 4705-2 5105 5405 5405-3 5405-46405牡丹44C1 C T-54G1D-G54G1P-G 54G1P1-C乐华 TC374-2PD 542A-2PD(R) 542A-2P D/I(R) 542A-1RCP4928W5428W 5438W孔雀K Q-54-38-221882188A 2529 2588 2588A 7188 7188A 7188B 如意 SG C-4703 4703F 5303 5403 5403C 5403F上海Z654-19A 664-1A664-2A 664-3A 671-1A 671-1A1 671-1B 674-1A 674-2A674-2A1 674-D 创维 CT V-8298WF T C-2140 莺歌Y5412 C71-1海燕 CS47E-6B-R 金星498 498-15128美乐2508 西湖 54C D7 54CD9 54CD10黄河HF51-V 长城画龙 G8153YFG8253YN环宇 47C-3 54C-3RA黄山5481C5481R三元54SYC-4B 菊花 FS531 531A 531B赣新 5418 百合花 CD47-6 49-6优拉纳斯U2529永固 C2108 C2118C2189BP金塔 JW-D542康立 CE5306梦寐M9081D四(S N102B) SAA3010T CTV222S,C TV320S,CTV322系统,对应CPU:P CA84C440/444/504/640/641,90频道,29键,模拟量菜单方式调节长虹 C2115 C2191C2521 C2588Z C2591 C2591A C2591V C2591AVC2591AZC2592 C2592AV C2593C2991 C2992康佳(KK-Y05 K K-Y17 KK-Y52)KK-T963A T963AI II T2101 T2103T2104 T2105 T9121 T9421 福日(V P101) HCF1475 1775 1975 2076 2101 2104 2111A21132176王牌T CL9321 9325 9329 9421。
sql server 错误9003:LSN无效(日志扫描号无效),对数据库的修复sql server 错误9003:LSN无效(日志扫描号无效)今天,从朋友那儿接到一个有问题的数据库文件与日志文件,在使用sql2000与sql2005进行数据库附加时,sql server报错,错误信息: "传递给数据库 'POS' 中的日志扫描操作的日志扫描号 (2806:120:1) 无效。
此错误可能指示数据损坏,或者日志文件(.ldf)与数据文件(.mdf)不匹配。
如果此错误是在复制期间出现的,请重新创建发布。
否则,如果该问题导致启动期间出错,请从备份还原。
无法打开新数据库 'POS'。
CREATE DATABASE 中止。
(Microsoft SQL Server,错误: 9003)"一看是9003错误,就想到可能是由于日志文件的原因,再看数据库文件可能损坏,于是想到dbcc checkdb指令.方法如下:1.我们使用默认方式建立一个供恢复使用的数据库(如pos)。
可以在SQ Server Enterprise Manager里面建立。
2.停掉数据库服务器。
3.将刚才生成的数据库的日志文件pos_log.ldf删除,用要恢复的数据库mdf文件覆盖刚才生成的数据库数据文件pos_data.mdf。
4.启动数据库服务器。
此时会看到数据库pos的状态为“置疑”。
这时候不能对此数据库进行任何操作。
5.设置数据库允许直接操作系统表。
此操作可以在SQ Server Enterprise Manager里面选择数据库服务器,按右键,选择“属性”,在“服务器设置”页面中将“允许对系统目录直接修改”一项选中。
也可以使用如下语句来实现。
use mastergoexec sp_configure 'allow updates',1goreconfigure with overridego6.设置pos为紧急修复模式 update sysdatabases set status=-32768 where dbid=DB_ID('pos')此时可以在SQL Server Enterprise Manager里面看到该数据库处于“只读\置疑\脱机\紧急模式”可以看到数据库里面的表,但是仅仅有系统表7.下面执行真正的恢复操作,重建数据库日志文件godbcc rebuild_log('pos','D:\Program Files\Microsoft SQL Server\MSSQL\Data\pos_log.ldf') go。
夏普复印机代码进入维修代码方式进入工厂代码方式SF1118/1025/AR161/AR200C 插入0 插入 C Ca 0 CAR275/AR255# 插入 C 插入# 插入0 CM350/M450P * C * P * 0 CAR158C 浓度 C 浓度 C 浓度 C 倍率AR2818 m160 m205 m276# 插入 C 插入* 插入CA 插入夏普便携复印机鼓计数清零方法1、按曝光开机,现在除准备灯外所以指示灯都会点亮2、按住曝光约十秒钟直到三个灯同时点亮,松开曝光3、重新开机故障代码U(主板电池电压低) L(原稿台未回到规定位置)H(热辊定影器故障) F(暴光灯或定影灯温度保险断掉)维修方式:按清除键-重复键-加法键-减法键进入1 解除故障2 读出主计数器内容3 读出总计数器内容4读出维修计数器内容5 维修计数器复位SIM46-1暴光强度调整执行模式时,开始预热并在复印数量显示器上显示当前手动设定上限值(ME) 要选择显示,按放大倍率显示键复印数量显示屏第1位第2第3位显示数据A 1----99 手动(ME)上限值b 1----99 手动(M)下限值c 1----99 手动(ME)色粉节省上限值d 1---99 手动(ME)色粉节省下限值E 1---99 照片(PE)上限值F 1---99 照片(PE)下限值G 1---99 自动(AE)倾斜H 1---99 自动(AE)下限值I 1---99 自动(AE)色粉节省倾斜J 1---99 自动(AE)色粉节省下限值设定范围为1---99,减小数值则加大浓度,如出现底灰时可加大对应的数值。
调完后按CA键取消调整方式(注)对于自动(AE)倾斜和自动(AE)色粉节省倾斜,一定要设定“0”。
夏普模拟复印机维修代码维进:C-插入- 0-插入或清除键-插入键-0键-插入键-清除键厂进:C- Ca - 0- C 纸盒键按4秒进用户模式1-01:反光镜动作检测1-02:光学系统传感器检查(缺纸灯、卡纸灯)1-03:镜头动作检查1-04:镜头动作老化检查2-01:ADF进行原稿输送动作2-02:ADF传感器检查2-03:ADF单独装纸动作检查(给纸电机反向旋转)2-04:ADF单独装纸动作检查(给纸电机正向旋转)2-05:ADF单独装纸动作检查(输纸电机正向旋转)2-06:ADF单独装纸动作检查(输纸电机反向旋转)2-07:ADF单独装纸动作检查(原稿限位器电磁阀接通)2-08:ADF单独装纸动作检查(送纸限位器)2-10:ADF单独装纸动作检查3-02:分页器传感器检查3-03:分页器单独装纸动作检查(输纸电机)3-04:分页器单独装纸动作检查(纸库电机)3-05:分页器单独装纸动作检查(蜂鸣器)3-06:分页器单独装纸动作检查(直线马达)(只适用于SF-S54)3-07:分页器单独装纸动作检查(钳夹马达)(只适用于SF-S54)5-01:操作面板显示检查(LED灯全亮5秒)5-02:加热灯检查(以0.5秒间隔亮灭加热灯)5-03:复印灯点亮检查5-04:DL 光度检查(放电灯亮30秒)5-05:BL 光度检查(消电灯以5秒间隔亮灭)6-01:输纸系统装纸动作(离合器/ 电磁阀)通断30次6-02:给纸电机动作检查(仅SP-2118)6-10:主纸盒半圆辊动作7-01:预热时间显示和老化预热计时并显示(秒)7-04:预热省略7-06:间歇老化7-08:预热时间显示8-01:显影偏压输出(30秒)8-02:主/ 转印充电输出/ 栅极检查(ME)8-03:主/ 转印充电输出/ 栅极检查(PE)8-04:主/ 转印充电输出/ 栅极检查(T / S)8-07:分离充电器输出(30秒)9-02 ADU传感器检查测试指令9-05 门电磁铁启动10 :色粉电机转动14 :故障消除(除U2故障外)15 废色粉装满(小人灯闪亮)取消16 U2 故障取消17 消除PF故障20-01 保养计数器(小人灯亮)清零21-01 保养周期设定0=50000张1=2500张2=5000张3=10000张4=25000张5=关闭21-02 显影器小修设置0=80000张1=5000张2=10000张21-03 彩色显影器小修设置0=10000张1=5000张22-01:保养计数器显示22-02:保养预置计数器显示22-03:卡纸存储器显示22-04:总卡纸存储器显示22-05:总计数器显示22-06:DV 计数器显示22-07:DV 预置计数器显示(载体更换周期)22-08:ADF 送纸数显示22-10:装订计数显示22-15:故障记忆显示(显示最近20个错误代码)24-01:卡纸存储器/ 总卡纸计数器清零24-02:故障记忆清除24-04:ADF 计数器清零24-05:装订计数清零24-06:显影剂调整时间清零24-07:鼓调整时间清零24-06:纸盒计数器清零25-01:主驱动系统检查25-02:自动显影剂调整(更换载体后执行)(厂代中80-2调浓度与漏粉)26-01:选购件设定(输入选购件所表数值之和)26-05:计数器方式设定( 0 A3计数 3 A4计数)26-06:目的地设定(设为10)26-07:转鼓灵敏度设定校正复印灯电压(1-3 初始为2)26-10:AE 原稿浓度设定(1低浓度原稿2正常浓度原稿)26-13:预热方式设定(0 正常1主电机转至预热结束)26-20:后缘空白设定(0 有空白1无空白)26-29:交流电压调整(0 100V 1 200V)30-01:复印机传感器检查(纸检测)42-01:清除小太阳符号换载体后43-01:定影温度设定(倍率键选择)44-01:成像控制动作设定(输入校正方式代码总和,栅压校正+1 光学尘埃校正+2 鼓磨损校正+4)44-05:栅极电压较正(显示图介浓度传感器A/D输入值)44-06:栅极电压较正强行执行44-07:图像浓度/ 转鼓标记传感器动作试验(F-J中0表示鼓标不能检测,1表示能检到)44-08:成像控制数据显示44-09:成像控制数据显示(最新值)44-10:栅极电压较正(转鼓表面/ 斑纹)数据显示44-11:初级栅极偏压设定44-12:中央控制处理器关闭时对复印功能进行检测主代码子代码内容46-01:曝光调整47 :AE 传感器增益自动调整(先在稿台上放几张A3白纸)48-01:前/ 后(垂直)放大倍率调整(A值调100% B调200% C调50%)48-02:输纸方向放大倍率调整(反光镜速度校正)50-01:复印件前缘调整50-02:前缘调整(简单型)(C值为245 显示为A45)51-02:阻力量调整(A 托盘阻力B手动给纸)53-01:ADF 停止位置调整值(普通纸)设定53-03:ADF 停止位置调整值(薄纸)设定53-04:ADF 阻力传感器、宽度传感器调整53-05:ADF出纸传感器调整53-06:ADF 时间传感器调整54-03:除去蜂鸣装置57 删边量调整58 -1 纸头调整58-2 空白区调整60 原稿尺寸检测97 补粉夏普模拟复印机故障代码L1-00:反光镜进给故障(传感器坏、主板坏、反光镜传动索缺油)L3-00:反光镜返回故障L4-01:主电机故障L5-00:镜头初始误差检测L5-02:镜头故障L5-03 第4/5反光镜电机故障L5-04 第4/5反光镜电机MHPS故障L5-05 镜头电机故障L5-06 镜头原位检测出错L5-8 镜头原位传感器故障L6 加粉电机故障L8-01:零交叉脉冲故障L8-03:AE传感器故障(执行47时,AE输入无变化)L9 分页器故障H2-00:定影热敏电阻开路故障(热敏电阻输入超过3.81V)H3-00:定影高温故障(定影温达240度,热敏电阻输入在0.36V下)H4-00:定影低温故障U1 存储器电池电压底于2.2V,指令“13”,复位U2-01:后备储存器故障U3-8 镜架驱动电机检测异常U3-10 镜架原位传感器故障U3-20 反光镜电机锁定U3-21 反光镜原始位置出错U3-40 时钟脉冲故障U4-02 ADU对位板操作错误检测U4-04 ADU后端板故障U5-00:ADF通信错误U5-01:A马达错误检测U5-03 时序传感器故障U5-04 空传感器故障U5-11:给纸电机故障U5-12:输纸电机故障U6-00:机架通信错误U6-01:1纸盒电机错误U6-02:2纸盒电机错误U6-03:3纸盒电机错误U6-08:机架24V线路出错U6-10:机架送纸电机错误U6-09:机架LCC电机过电流检测F1-00:分页器通信错误F1-02:输纸电机故障F1-04:纸库上限/下限故障F1-05:纸库原位传感器故障F1-06:纸库电机故障F1-14:输纸电势故障F2-02:色粉粉斗电机错误F2-31:图象浓度传感器故障(传感器脏、删边灯脏、鼓处插线坏)F2-32:鼓标记传感器故障F2-35:栅级电压校正故障F3-12 上纸盒升起电机故障F3-22 下纸盒升起电机故障C2 高压发生器故障电极丝短路或断路CC 原稿尺寸传感器误检测EE-EU:色粉不足EE-EL:色粉过多CH:亮是盖打开闪烁是显影组件安装不到位夏普数码复印机维修代码1-1 确认反射镜装置动作1-2 确认光学系传感器动作1-6 反光镜扫描连续动作2-1 SPF连续动作2-2 确认SPF传感器动作2-3 确认SPF电动机正转方向动人2-4 确认SPF电动机逆转方向动作2-8 确认SPF进纸电磁阀动作2-9 RSPF翻转电磁铁动作检查2-10 RSPF出纸门电磁铁动作检查2-11 确认SPF PS释放电磁阀动作3-2 确认移动分离传感器动作3-3 确认分页器移动动人3-4 确认分离板动作(检测是否正常转动)3-11 确认配页器原位动作5-1 确认扣作部显示(面板LED灯全亮秒)5-2 确认加热灯亮(定影灯50秒间隔亮5次)5-3 确认复印机灯亮(10秒浓度键改亮度)6-1 确认进纸电磁阀动作(50秒间隔驱动20次)6-10 驱动主盒半圆辊7-1 预热时间表示有JAM老化7-4 预热省略7-6 间歇老化有纸7-8 预热时间表示8-1 复印模式的显影偏压输出8-2 复印模式的主充电器栅极电压(High状态高)输出8-3 复印模式的主充电器栅极电压(Low状态低)输出8-6 转印电压输出8-10 打印模式的显影偏压以及控制回路的动作确认和调整8-11 打印模式的主充电器栅极电压(High状态)以及控制回路的动作确认8-12 打印模式的主充电器栅极电压(Low状态)以及控制回路的动作确认8-13 FAX模式的显影偏压以及控制回路的动作确认和调整8-14 FAX模式的主充电器栅极电压(High状态)以及控制回路的动作确认8-15 FAX模式的主充电器栅极电压(Low状态)以及控制回路的动作确认9-1 双面器负载(马达)正转测试9-2 双面器负载(马达)反转测试9-4 双面器马达的转速调整9-5 双面器马达的把向转换时间调整10 确认墨粉电动机动作14 解除U2以外的故障16 解除U2故障20-1 清除保养计数21-1 保养循环的设定(0=2500张1=5000张2=15000张3=30000张4=150000张5=999999张)22-1 保养计数器的显示22-2 保养预置值显示(SIM20-1设定值)22-3 卡纸储存的显示(最近30次卡纸)22-4 总卡纸计数显示22-5 总计数显示22-6 显影计数器显示22-8 SPF计数器显示22-9 进纸计数器显示22-12 光鼓计数器显示22-13 CRUM类型显示22-14 FLASH ROM的版本22-15 故障储存器显示(最近15次故障)22-16 双面打印计数显示22-17 复印计数器显示22-18 打印计数器显示22-19 电子分类计数器显示22-21 扫描计数器显示22-22 SPF卡纸计数器显示24-1 卡纸储存器清除24-2 故障储存器清除24-4 SPF计数器清除24-5 双面打印计数清除24-6 进纸计数器清除24-7 光鼓计数器清除24-8 复印计数器清除24-9 印刷计数器清除24-10 电子类计数器清除24-13 扫描计数器清除24-14 SPF卡纸计数清除24-15 扫描模式计数器清除25-1 确认主电机机劝作(30秒)25-10 确认LSU多面镜电动机动作(30秒)26-1 选件开关的显示(选购件对应灯亮)26-3 部门管理器的设定(0:计数模式1:投币模式)26-4 本机双面动作设置(0:无双面1:有双面功能)26-5 计数器方式设定(0:双面计数1:单面计数)26-6 发送地设定(5:中国6:台湾)26-7 直接显示CPM旋转速度26-10 网络扫描的试用设定26-18 节粉方式(0:节粉关闭1打开)26-22 语言设定(打印卡面板语言)(0:日语1:英语……)26-30 CE标记对应控制设定(0:CE标记OFF 1:ON)26-32 风扇旋转状况变化26-36 (0:保养计数到停机1:不停)26-37 (0:载体计数到停机1:不停)26-38 光鼓超寿命停止设定(0停机1不停机)26-39 内存容量检测(16:16M内存32:32M内存)26-42 转印时间调整(R系列:1:240MS 3:260MS 9:320MS)(M系列机子取值1-99 默认值50)26-43 上下端空白设置(自动灯表下端,手动灯表上端)26-50 黑白转换功能设定(0:可转1:不可转)26-51 复印机暂停功能设定(0:不停1:停)26-60 未装载FAX时,设定FAX模式键是否有效27-1 设定有元PC/调制解调器的通信故障27-5 输入机器的机号30-1 确认本体传感器动作30-2 确认给纸部的传感、检测器及相关回路的动作40-1 确认手动托盘的纸张尺寸检测器及相关回路的动作41-2 调整OC原稿检测传感器41-3 原稿检测传感器受光电平显示41-4 OC盖板20度时的检测电平调整42-1 载体记数清除43-1 定影温度设定(倍率键调)43-10 明信片纸张进纸周期设置(取值1-99)43-11 明信片纸定影温度设置43-12 待机模式定影风扇转动设置(0:低速1:高速)43-13 定影纸张间隙控制(0:禁止1:允许)44-34 转印电流设定44-40 墨粉补充前转动时间设置(取值1-99)46-1 复印浓度300dpi电平调整46-2 复印曝光600dpi浓度等级调整46-7 分别调整复印曝光浓度等级(超级照片)46-9 复印浓度等级单独调整手动300dpi等级(文字)46-10 复印浓度等级单独调整手动600dpi(文字/照片)46-11 复印浓度等级单独调整(照片)46-18 复印对比度调整300dpi46-19 曝光时的图像质量调整46-20 SPF的曝光浓度校正46-29 复印对比度调整600dpi46-30 进行AE设定(取值0-30)46-31 图像锐度调整(0:黑白校正2:清晰)46-39 调整传真模式对比度46-45 调整传真模式的图像浓度48-1 主(前后)扫描方向倍率调整48-2 复印时OC方式副扫描方向倍率调整48-3 自动调整前端.副扫描倍率48-5 复印时SPF方式副扫描方向倍率调整49-1 FLASH ROM程序写入模式50-1 复印画像位置调整(左右方向,值加减1移动0.127MM)50-5 调整图像先端位置50-6 调整复印模式SPF/RSPF原稿图像位置50-10 用纸中心偏移调整(上下方向)50-12 调整复印模式原稿图像中心位置50-13 OC方式原稿中心偏50-16 SPF方式原稿中心偏听偏信移调整50-18 双面复印时反面图像位置调整50-19 双面复印时后端空白调整51-02 对位量调整51-8 设定禁止感光鼓分离爪动作53-8 SPF扫描位置调整56-1 传送MFP控制器数据61-1 检测LSU的动作61-2 调复印模式激光功率(绝对值)61-3 六棱镜电机检测62-1 格式化硬盘62-3 检测硬盘读写操作62-8 格式化硬盘(除系统数据区域)62-10 删除完成作业列表(同时删除作业日志)63-1 确认黑白校正数据63-2 执行黑白校正63-7 自动调整SPF白校正开始的像素位置64-1 自我打印功能65-5 进行操作面板的检测66-22 调传真听筒音量66-23 下载传真程序66-24 清除传真数据内存66-39 设定发货地规格66-60 设定ACR数据67-11 用于设定“select-in“信号67-14 进行flash programs写入/比较检测67-17 进行NVROM的清除67-18 清除FLASH ROM 的NETwork Scanner Application(网络扫描应用软件)用数据区域67-20 装载网络扫描组件时,检测网络连接夏普数码复印机故障代码H2 00 热敏电阻断开(电阻到MCU板的连接、SIM14清)H3 00 定影部高温故障(温超240度、SIM5-2灯闪时:查接线。
相同皮带轮直径下:应用SP 型皮带的,宽度和装置空间都可以节省节距长度(mm)外周长(mm)节距长度(mm)56257516126126251637630/3V2506431650670/3V2656851662710/3V28072516877307431700/3V6707507631737670/3V300775176277578817877878001800/3V710800/3V31581318128258381837850/3V33586418628758881887900/3V3559131900/3V7509259381937950/3V37596019879759882000100010132030/3V8001010/3V400102520371030104320871047106021201080/3V42510902137112011332160/3V8501140/3V45011502187115011632240SP 型皮带和传统三角皮带的性能比较同样的传输马力比较:应用SP 型皮带的,皮带轮的中央距离、直径和宽度都只需普通的3/4。
SPZ (9.5x8)(※86 个规格)公司简介经销商证书产品目录联系我们SPA SPB SPCSPZ※个规格12821300253213001318258213201338260713321350263213571375265013821400268214001418273214321450278214501468280014571475283215001518288215071525293215571575298215821600300016001618303216071625308216321650315016571675318216821700328217001718335017071725338217321750348217571775355017821800375018001818400018071825426518321850450018571875节距长度(mm)外周长(mm)节距长度(mm)125012713340/5V13201260/5V50012823550/5V14001340/5V53013623750140014223800/5V1500※如有需求,可提供其他尺寸。
JournalofChromatography∗通讯联系人.Tel:(0535)20109130ꎬE ̄mail:lxchen@yic.ac.cn.基金项目:国家自然科学基金项目(21275158ꎬ21105117)ꎻ山东省自然科学基金项目(ZR2010BQ027)ꎻ山东省优秀中青年科学家奖励基金项目(BS2009CL055)ꎻ烟台市科技发展项目(2010158).收稿日期:2012 ̄09 ̄03摘要:建立了采用超声辅助分散液液微萃取技术结合高效液相色谱法(UA ̄DLLME ̄HPLC)对4种邻苯二甲酸酯(PAEs)进行富集㊁检测的方法ꎬ并成功应用于实际水样分析ꎮ实验中采用富集因子来评价萃取效率ꎬ考察并优化了影响萃取效率的主要因素ꎬ包括萃取剂类型和用量㊁分散剂类型和用量㊁超声时间㊁离子强度㊁萃取时间和pH值等ꎮ结果表明:在最佳萃取条件下ꎬ该法对4种PAEs(邻苯二甲酸二甲酯㊁邻苯二甲酸二乙酯㊁邻苯二甲酸二丁酯和邻苯二甲酸二正辛酯)具有较高的富集能力ꎬ富集因子分别为71㊁144㊁169和159ꎻ检出限分别为3 78㊁1 77㊁3 07和3 30μg/Lꎮ对实验室自来水㊁某品牌矿泉水以及湖水分别加标50㊁200及500μg/L的回收率为82 99%~114 47%ꎬ相对标准偏差为1 93%~8 31%ꎮ该法简便㊁快速㊁环保ꎬ可以用于测定实际水样中的PAEs类增塑剂ꎮ关键词:分散液液微萃取ꎻ超声辅助ꎻ高效液相色谱ꎻ邻苯二甲酸酯ꎻ水样中图分类号:O658㊀㊀㊀文献标识码:A㊀㊀㊀文章编号:1000 ̄8713(2013)02 ̄0155 ̄07Simultaneousdeterminationoffourphthalateestersinwatersamplesusingultrasound ̄assisteddispersiveliquid ̄liquidmicroextractioncoupledwithhighperformanceliquidchromatographyMAYanling1ꎬ2ꎬCHENLingxin1ꎬ2∗ꎬDINGYangjun1ꎬMINGYongfei3ꎬLIJinhua2(1.CollegeofChemistryandChemicalEngineeringꎬQufuNormalUniversityꎬQufu273165ꎬChinaꎻ2.KeyLaboratoryofCoastalZoneEnvironmentalProcessesꎬYantaiInstituteofCoastalZoneResearchꎬChineseAcademyofSciencesꎬYantai264003ꎬChinaꎻ3.CollegeofLifeScienceꎬLudongUniversityꎬYantai264025ꎬChina)Abstract:Ultrasound ̄assisteddispersiveliquid ̄liquidmicroextractioncoupledwithhighper ̄formanceliquidchromatography(UA ̄DLLME ̄HPLC)wasdevelopedforthedeterminationoffourtypicalphthalateesters(PAEs).TheanalyzedPAEsincludeddimethylphthalate(DMP)ꎬdiethylphthalate(DEP)ꎬdibutylphthalate(DBP)anddi ̄n ̄octylphthalate(DnOP).TheUA ̄DLLMEparameterssuchastypes/volumesofextraction/dispersionsolventsꎬultrasonictimeꎬionicstrengthandextractiontimeꎬwereinvestigated.Enrichmentfactor(EF)wasem ̄ployedtoevaluatetheextractionefficiency.Theconditionswerefinallychosen:CCl4(40μL)/acetonitrile(1 0mL)asextraction/dispersionsolventsꎻ30g/LNaClꎻultrasound/centrifuga ̄tionof5min.UndertheoptimizedextractionconditionsꎬUA ̄DLLMEexhibitedstrongenrich ̄mentabilityforthefourPAEs.TheEFsforDMPꎬDEPꎬDBPandDnOPobtainedwere71ꎬ144ꎬ169and159ꎬrespectively.Thelimitsofdetectionwere3 78ꎬ1 77ꎬ3 07and3 30μg/LforDMPꎬDEPꎬDBPandDnOPꎬrespectively.Thesatisfactoryrecoveriesforthreewatersam ̄plesatthreespikedlevelsrangedfrom82 99%-114 47%ꎬwiththerelativestandarddeviations色谱第31卷of1 93%-8 31%.ItisaconvenientꎬspeedyꎬenvironmentallybenignmethodfortheroutineanalysisofPAEsinwatersamples.Keywords:dispersiveliquid ̄liquidmicroextraction(DLLME)ꎻultrasound ̄assisted(UA)ꎻhighperformanceliquidchromatography(HPLC)ꎻphthalateesters(PAEs)ꎻwatersample㊀㊀邻苯二甲酸酯类化合物(PAEs)ꎬ又称酞酸酯ꎬ一般为无色油状黏稠液体ꎬ是目前最广泛使用的增塑剂ꎬ在塑料制品中的添加量达20%~50%[1]ꎮ此类化合物在环境中难以降解ꎬ已成为全球最普遍的环境污染物之一ꎮ同时ꎬ它们也是一类内分泌破坏性物质ꎬ并表现出生物累积性ꎮ它们可以改变人体激素中的雌激素水平ꎬ从而导致严重的健康问题[2ꎬ3]ꎮ商品化使用的PAEs约有14种ꎬ其中6种被美国环保局列为重点控制污染物[4]ꎬ包括邻苯二甲酸二甲酯(DMP)㊁邻苯二甲酸二乙酯(DEP)㊁邻苯二甲酸二丁酯(DBP)㊁邻苯二甲酸二正辛酯(DnOP)㊁邻苯二甲酸丁基苄基酯(BBP)和邻苯二甲酸(2 ̄乙基己基)酯(DEHP)[5]ꎮ其中DMP㊁DBP与DnOP已列入我国环境优先控制污染物名单ꎮ㊀㊀鉴于PAEs对人类生命安全存在极大的潜在危害性ꎬ因而对于PAEs的安全卫生性检测显得十分必要和迫切ꎮ目前ꎬPAEs的测定方法主要有高效液相色谱法(HPLC)[6-8]㊁气相色谱法[9]㊁气相色谱 ̄质谱联用[10ꎬ11]㊁液相色谱 ̄质谱联用[12ꎬ13]以及毛细管电泳法[14ꎬ15]ꎮ而在实际样品检测中ꎬ因样品基质具有组分复杂㊁干扰物质多以及目标物含量低等特点ꎬ通常需要采用适当前处理技术才能进行分析测定ꎮ传统的PAEs类样品前处理方法主要有固相萃取[16]和液相萃取[17]ꎬ然而ꎬ这些技术不但存在操作冗繁㊁萃取时间长的缺点ꎬ大量有毒溶剂的使用也对实验操作人员和环境造成不利的影响ꎮ于是ꎬ人们不断致力于将上述萃取技术微型化ꎬ建立不用或者少用有毒有机溶剂㊁成本低㊁操作简单㊁应用范围广的样品前处理技术ꎬ于是ꎬ固相微萃取(SPME)[18ꎬ19]和液相微萃取(LPME)[20]也越来越多地被应用于PAEs类的富集浓缩前处理中ꎮ由于SPME装置的萃取头成本较高ꎬ且萃取涂层易磨损ꎬ使用寿命短ꎬ多次使用还存在交叉污染问题ꎬ而LPME技术因其具有有机溶剂用量少㊁快速㊁价廉且操作简单的优势ꎬ成为一种环境友好型的样品前处理新技术ꎮ近些年ꎬ分散液液微萃取(dispersiveliquid ̄liquidmicroextractionꎬDLLME)因其具有所需萃取溶剂量小㊁萃取速度快ꎬ萃取效率和富集倍数高㊁操作简便㊁消耗低和环境友好等优点ꎬ已发展成为一种极具潜力的分离富集技术[21]ꎬ并已在水样中的磺胺类药物[22]㊁重金属[23]及多环芳烃[24]㊁人体血清中的姜黄素[25]等分析前处理过程中得以成功应用ꎮ同时ꎬ此技术在PAEs类的前处理中也得到了应用[7ꎬ26ꎬ27]ꎮ㊀㊀本文以4种典型的PAEs类物质(DMP㊁DEP㊁DBP㊁DnOP)为研究对象ꎬ采用DLLME并加以超声辅助(ultrasound ̄assistedꎬUA)对样品进行富集浓缩前处理ꎬ加速了不互溶的两相之间的质量传递ꎬ使得萃取效率可在最小的溶剂使用量和最短的时间内得到快速的提高ꎻ随后ꎬ采用HPLC进行分离测定ꎮ建立了一种简便㊁快捷㊁实用的测定自来水㊁瓶装水和湖水中PAEs类增塑剂的分析方法ꎮ1㊀实验部分1.1㊀仪器与试剂㊀㊀LC310高效液相色谱仪(江苏天瑞仪器股份有限公司)ꎻTG16 ̄WS台式高速离心机(湖南湘仪实验室仪器开发有限公司)ꎻKQ ̄400KDE型高功率数控超声波清洗器(昆山市超声仪器有限公司)ꎻ电子天平(赛多利斯科学仪器(北京)有限公司)ꎻ雷磁PHS ̄3CpH计(上海精密科学仪器有限公司)ꎻMilli ̄Q超纯水系统(美国Millipore公司)ꎮ㊀㊀DMP㊁DEP㊁DBP和DnOP标准品均购自阿拉丁试剂公司ꎮ甲醇和乙腈均为色谱纯ꎬ购于北京百灵威科技有限公司ꎻ四氯化碳(CCl4)为色谱纯ꎬ购于阿拉丁试剂公司ꎻ其他试剂均为分析纯ꎬ购于国药集团化学试剂有限公司ꎻ实验用水均为Milli ̄Q水ꎮ1.2㊀标准溶液的配制与实际水样㊀㊀精密称取DMP㊁DEP㊁DBP和DnOP标准品各0 0100g置于4个10mL容量瓶中ꎬ用甲醇溶解并定容ꎬ配成1000mg/L的4种PAEs储备液ꎮ准确移取4种PAEs储备液各2 00mLꎬ置于同一10mL容量瓶中ꎬ用水定容ꎬ配成200mg/LPAEs混合标准溶液ꎮ储备液和混合标准溶液均置于4ħ冰箱中保存备用ꎮ将200mg/LPAEs混合标准溶液用水逐级稀释至所需浓度得到工作溶液ꎮ㊀㊀实际水样分别为实验室自来水㊁某品牌矿泉水以及湖水ꎮ使用前经过0 45μm滤膜过滤ꎬ待富集浓缩前处理ꎮ1.3㊀HPLC分析条件㊀㊀色谱分离柱:WatersSymmetryC18柱(250mm651第2期马燕玲ꎬ等:超声辅助分散液液微萃取 ̄高效液相色谱测定水样中的4种邻苯二甲酸酯类增塑剂ˑ4 6mmꎬ5μm)ꎮ流动相:甲醇(A) ̄水(B)ꎮ梯度洗脱程序:0~3minꎬ85%Aꎻ3~10minꎬ85%A线性变化至100%Aꎻ10~20minꎬ100%Aꎮ流速:1 0mL/minꎮ进样量:10μLꎮ检测波长:225nmꎮ1.4㊀样品前处理过程㊀㊀将4种PAEs质量浓度均为2mg/L的混合标准溶液5 00mL置于10mL尖底玻璃离心管中ꎬ加入30g/LNaCl溶液ꎮ将1 00mL乙腈(分散剂)和40μLCCl4(萃取剂)混合ꎬ用1mL的玻璃注射器迅速注入上述溶液中ꎬ轻晃离心管形成液滴ꎬ超声辅助萃取5min后ꎬ以4000r/min离心5minꎮ离心后的下层溶液用20μL微型注射器取10μLꎬ进行HPLC检测ꎮ1.5㊀标准曲线与工作曲线的建立㊀㊀取4种PAEs质量浓度分别为1㊁2㊁5㊁10㊁20㊁25㊁50和100mg/L的混合标准溶液各10μLꎬ在选定的波长和梯度洗脱条件下进行HPLC分离检测ꎬ以目标分析物的峰面积A为纵坐标ꎬ以质量浓度C(mg/L)为横坐标ꎬ绘制标准曲线ꎮ㊀㊀取4种PAEs质量浓度分别为0 005㊁0 02㊁0 05㊁0 1㊁0 2㊁0 5㊁1 0㊁2 0和5 0mg/L的混合标准溶液5 00mL置于10mL尖底玻璃离心管中ꎬ加入30g/LNaCl溶液ꎮ用1mL的玻璃注射器将1 00mL乙腈和40μLCCl4的混合溶液迅速注入上述溶液中ꎬ轻晃离心管形成液滴ꎬ超声辅助萃取5min后以4000r/min离心5minꎮ离心后的下层溶液用微型注射器取10μLꎬ进行HPLC分离检测ꎮ以目标分析物的峰面积A对质量浓度C(mg/L)绘制工作曲线ꎬ平行实验3次ꎬ取A的平均值ꎬ外标法定量ꎮ2㊀结果与讨论2.1㊀DLLME条件优化㊀㊀影响DLLME萃取效率的主要因素包括萃取剂类型和用量㊁分散剂类型和用量㊁超声时间㊁离子强度㊁pH值和萃取时间等ꎮ为了获得最佳的萃取条件ꎬ采用下述公式计算富集因子(enrichmentfac ̄torꎬEF)ꎬ以此参数来评价不同萃取条件下的萃取效率ꎮEF=Csed/C0(1)式(1)中ꎬCsed为萃取沉积相中PAEs的质量浓度(g/L)ꎻC0为水样中PAEs的质量浓度(g/L)ꎮ㊀㊀本实验研究了影响DLLME萃取效率的诸多因素并对其进行了优化ꎬ从而实现对4种PAEs的快速高效的测定ꎮ2.1.1㊀萃取剂的选择㊀㊀萃取剂的选择需满足:密度大于水且与水不互溶ꎬ对待测物有强溶解能力等要求ꎮ选择4种萃取剂(CCl4㊁CHCl3㊁氯苯和CS2)进行实验比较ꎬ分散剂选择为乙腈㊁甲醇㊁乙醇和丙酮ꎮ考察所有组合ꎬ结果发现ꎬCHCl3只在与乙腈组合时ꎬ才能形成稳定的两相ꎻ氯苯的色谱峰与分析物的色谱峰重叠在一起ꎬ分离不开ꎻCS2的萃取效果很小ꎬ且与DBP的色谱峰重叠在一起ꎮ而CCl4与4种分散剂均能形成稳定的两相ꎬ生成的下层溶液能够很容易地由微型注射器取出ꎬ而且色谱峰不干扰分析物的检测ꎮ因此最终选择CCl4作为样品处理的萃取剂ꎮ2.1.2㊀分散剂的选择㊀㊀分散剂的类型是影响萃取效率的又一重要因素ꎬ所选分散剂应能与萃取剂及水有良好的混溶性ꎬ而在分相时又能形成两相ꎬ并且对目标化合物的分析不产生干扰ꎮ选择符合上述条件的4种分散剂:乙腈㊁甲醇㊁乙醇和丙酮ꎬ体积均为1 00mLꎬ萃取剂CCl4体积为40μLꎬ经萃取离心检测之后ꎬ获得的EF值如图1所示ꎮ相对于其他3种萃取剂ꎬ乙腈对目标分析物(除DBP外)的富集倍数均最高ꎬ所以最终选择乙腈作为分散剂ꎮ图1㊀不同分散剂对4种PAEs富集因子的影响Fig.1㊀EffectofdifferentdispersionsolventsontheenrichmentfactorsofthefourPAEs㊀Extractionconditions:samplevolumeꎬ5 0mLꎻextractionsolventꎬCCl4ꎻvolumeofextractionsolventꎬ40μLꎻvolumeofdispersionsolventꎬ1 0mLꎻultrasonictimeꎬ5minꎻionicstrengthꎬ30g/LNaCl.2.1.3㊀萃取剂的用量㊀㊀在固定分散剂乙腈的加入量为1 00mL的情况之下ꎬ考察了不同CCl4用量对萃取效率的影响ꎬ体积分别选择为30㊁40㊁50㊁60㊁70㊁80㊁90和100μLꎬ由此获得不同萃取剂用量之下的EF值ꎬ如图2a所示ꎮ当CCl4的体积为40μL时ꎬ所获得的DEP㊁DBP和DnOP的EF均最高ꎬ而获得的DMP的EF稍低于50μL时的值ꎬ综合考虑ꎬ选择萃取剂的用量751色谱第31卷为40μLꎮ图2㊀(a)萃取剂用量㊁(b)分散剂用量㊁(c)超声时间和(d)离子强度对4种PAEs富集因子的影响Fig.2㊀Effectsof(a)extractionsolventvolumeꎬ(b)dispersionsolventvolumeꎬ(c)ultrasonictimeand(d)ionicstrengthontheenrichmentfactorsofthefourPAEs㊀Extractionconditions:samplevolumeꎬ5 0mL.a.dispersionsolventꎬACNꎬ1 0mLꎻultrasonictimeꎬ5minꎻionicstrengthꎬ30g/LNaCl.b.extractionsolventꎬCCl4ꎬ40μLꎻultrasonictimeꎬ5minꎻionicstrengthꎬ30g/LNaCl.c.extractionsolventꎬCCl4ꎬ40μLꎻdis ̄persionsolventꎬACNꎬ1 0mLꎻionicstrengthꎬ30g/LNaCl.d.extractionsolventꎬCCl4ꎬ40μLꎻdispersionsolventꎬACNꎬ1 0mLꎻultrasonictimeꎬ5min.2.1.4㊀分散剂的用量㊀㊀在固定萃取剂CCl4用量为40μL的情况下ꎬ考察了不同分散剂用量对PAEs萃取效率的影响ꎬ分散剂体积选择为0 25~1 75mLꎬ获得的不同分散剂用量之下的EF值如图2b所示ꎮ当乙腈的体积小于1 00mL时ꎬ4种PAEs的EF值随着乙腈体积的增加而增大ꎬ这是因为在小体积分散剂作用下ꎬ萃取剂相不能完全被分散ꎬ难以形成乳浊液ꎮ而当乙腈的体积大于1 00mL时ꎬEF值反而随着乙腈体积的增加而减小ꎬ这是由于在大体积分散剂作用下ꎬPAEs在水中的溶解量增大ꎮ所以ꎬ1 00mL乙腈为最佳分散剂用量ꎮ2.1.5㊀超声时间的影响㊀㊀利用超声对DLLME进行辅助ꎬ能够加速不互溶两相之间的质量传递ꎬ使得萃取效率在最小的溶剂使用量和最短的时间内得到快速的提高ꎮ本实验中选取超声时间为0~15minꎬ获得不同超声时间下的EF值ꎬ如图2c所示ꎮ当超声时间较短时(3min内)ꎬPAEs未能很好地萃取ꎬEF较小ꎻ随着超声时间的增加ꎬEF显著增大ꎬ说明超声加快了萃取过程中的传质作用ꎬ从而提高了萃取效率ꎻ但当超声时间高于5min时(8min内)ꎬEF值反而随着超声时间的增加而减小ꎬ这可能是因为超声过程中产生的热量使得PAEs重新溶解回水相ꎬ导致萃取量下降ꎮ继续延长超声时间可能导致萃取剂挥发严重ꎮ因此ꎬ超声时间选择为5minꎮ2.1.6㊀离子强度的影响㊀㊀为了考察离子强度对DLLME效率的影响ꎬ在其他实验条件不变的情况下ꎬ分别加入不同质量浓度的NaCl(0~50g/L)ꎬ得到不同NaCl加入量下的EF值ꎬ如图2d所示ꎮ在加入的NaCl质量浓度为30g/L时ꎬ除DMP获得的EF稍低于40g/L和50g/L时的值ꎬDEP㊁DBP和DnOP均获得明显高于其他加入量下的EF值ꎮ综合考虑ꎬ选择加入30g/LNaClꎮ851第2期马燕玲ꎬ等:超声辅助分散液液微萃取 ̄高效液相色谱测定水样中的4种邻苯二甲酸酯类增塑剂2.1.7㊀萃取时间的影响㊀㊀在DLLME过程中ꎬ萃取时间是指在体系中注入分散剂和萃取剂到开始离心之间的时间ꎮ在其他萃取条件不变的情况下ꎬ考察了0~60min内萃取效率的变化情况ꎮ结果表明ꎬ萃取效率随萃取时间的变化无明显改变ꎮ体系中加入分散剂和萃取剂ꎬ超声5min后ꎬ离心即可ꎮ萃取时间非常短ꎬ这也是DLLME的主要优势之一ꎮ2.1.8㊀pH值的影响㊀㊀实验比较了溶液pH值对萃取效率的影响ꎬ结果表明ꎬ萃取效率受pH值的影响不大ꎮ2.2㊀方法评价2.2.1㊀HPLC条件的优化㊀㊀在1 3节色谱条件下ꎬ4种PAEs混合标准溶液的分离效果如图3所示ꎬ可以看出ꎬ4种PAEs在18 5min内完成基线分离ꎮ图3㊀4种邻苯二甲酸酯混合标准溶液的色谱图Fig.3㊀ChromatogramofamixedstandardsolutionofthefourPAEs㊀Mobilephases:A:methanolꎻB:water.Gradientelution:0-3minꎬ85%Aꎻ3-10minꎬ85%Ato100%Aꎻ10-20minꎬ100%A.Flowrate:1 0mL/min.Injectedvolume:10μL.Wavelength:225nm.㊀Peaks:1:DMPꎻ2:DEPꎻ3:DBPꎻ4:DnOP.表1㊀4种PAEs的线性方程㊁线性相关系数㊁线性范围㊁线性方程斜率的RSD㊁LOD㊁LOQ和富集因子Table1㊀Linearequationsꎬcorrelationcoefficientsꎬlinearrangesꎬrelativestandarddeviation(RSD)ofslopeꎬlimitsofdetection(LOD)ꎬlimitsofquantitation(LOQ)andenrichmentfactorsofthefourPAEsPAE㊀LinearequationCorrelationcoefficientLinearrange/(μg/L)RSDa)/%LOD/(μg/L)LOQ/(μg/L)EnrichmentfactorDMPAb)=63056Cc)+155290.995350-100003.713.7812.6071DEPA=142272C+111430.99355-100006.981.775.90144DBPA=210451C-922.210.999820-100005.493.0710.23169DnOPA=127169C+698.380.998620-100007.523.3011.00159㊀a)relativestandarddeviationꎬn=3.b)peakarea.c)massconcentrationꎬmg/L.2.2.2㊀标准曲线㊀㊀按1 5节操作得到的4种PAEs的标准曲线线性关系良好ꎬDMP㊁DEP㊁DBP和DnOP的线性相关系数r2分别为0 9995㊁0 9999㊁0 9996和0 9999ꎮ根据标准曲线建立过程中所能检测到的最低浓度和富集因子ꎬ来选定工作曲线的浓度起点ꎮ2.2.3㊀工作曲线㊁检出限㊁定量限和富集因子㊀㊀按1 5节所述方法制作工作曲线ꎮ检出限(LOD)和定量限(LOQ)采用向空白样品中逐级降低加标浓度的方法来确定ꎮ分别以3倍和10倍信噪比(S/N)对应的目标物浓度作为LOD和LOQꎮ所得到的线性方程㊁线性相关系数㊁线性范围㊁线性方程斜率的相对标准偏差(RSD)㊁LOD㊁LOQ和富集因子等结果见表1ꎮ从表1中数据可见ꎬ4种PAEs的线性相关系数为0 9935~0 9998ꎬ线性关系良好ꎮ富集因子EF是以标准溶液的直接进样色谱图与DLLME富集后进样的色谱图进行比较ꎬ以分析物经萃取后的浓度与样品溶液的初始浓度计算得到ꎬ获得DMP㊁DEP㊁DBP和DnOP的富集因子分别为71㊁144㊁169和159ꎬ说明此法对此4种PAEs有较大程度的富集ꎬ偏高或接近于文献报道的富集能力ꎬ即DMP的44㊁DEP的92和DBP的196[27]ꎮDMP㊁DEP㊁DBP和DnOP的LOD值分别为3 78㊁1 77㊁3 07和3 30μg/Lꎬ远低于采用胶束毛细管电泳技术获得的DBP检出限0 64mg/L[14]ꎮ近年来ꎬLi等[8]采用离子液体混合胶束作用的固相萃取(SPE)联用HPLC ̄UV(紫外)检测PAEsꎬ获得检出限为DEP0 17μg/L和DBP0 13μg/LꎻLiang等[27]采用DLLME结合HPLC ̄UVꎬ获得检出限为DMP1 8μg/L㊁DEP0 88μg/L和DBP0 64μg/LꎻMa等[13]利用分散的SPE结合HPLC ̄MSꎬ得到DMP的检出限为3 68μg/L和DEP0 43μg/Lꎮ虽然与之相比本法所得检出限相对稍高ꎬ但是该法仍具有明显的优越性ꎬ如更简便可行㊁成本更低等ꎬ成功地实现了对4种典型PAEs的同时富集㊁分离与测定ꎮ最近ꎬ林小葵等[28]采用超声辅助乳化液液微萃取结合HPLC ̄UVꎬ测定了水样中的DMP㊁DEP和DnOPꎬ检出限均为0 2μg/Lꎮ尽管方法类似且低于本法检出限ꎬ但是我们完成了4种PAEs的同时测定ꎬ并进行了除自来水外的矿泉水和湖水这两类更复杂水样的分析(见2 3节)ꎬ而且在实验操作上更省时省力ꎮ同时ꎬ该检出限远951色谱第31卷低于«生活饮用水卫生标准»国家标准规定限值的DEP的300μg/L和其他PAEs限定的8μg/Lꎮ因此ꎬ目前所发展的方法有望实现对实际水样的分析ꎬ进行PAEs的有效分析和监控ꎮ㊀㊀另外ꎬ对4种PAEs质量浓度均为2mg/L的混合标准溶液进行UA ̄DLLME前处理操作后ꎬ利用HPLC ̄UV检测ꎬ日内连续进样6次和日间累计进样6次所获得的迁移时间和峰面积值进行精密度计算ꎬ结果见表2ꎮ日内保留时间和峰面积的RSD值分别低于0 55%和4 71%ꎬ而日间保留时间和峰面积的RSD值分别低于1 12%和6 88%ꎬ它们均低于或者接近文献报道值[8ꎬ13ꎬ27ꎬ28]ꎮ可见该方法对于此4种PAEs的检测具有良好的精密度ꎮ表2㊀4种PAEs(2mg/L)的迁移时间和峰面积的精密度(RSDꎬn=6)Table2㊀PrecisionsofmigrationtimeandpeakareaofthefourPAEs(2mg/L)(RSDꎬn=6)%PAEIntra ̄dayMigrationtimePeakareaInter ̄dayMigrationtimePeakareaDMP0.284.711.126.53DEP0.262.680.412.97DBP0.553.840.853.97DnOP0.114.250.376.88表3㊀实际水样中4种PAEs的加标回收率及其精密度(n=3)Table3㊀Recoveriesandtheirprecisions(RSDs)ofthefourPAEsspikedinrealwatersamples(n=3)PAESpiked/(μg/L)TapwaterFound/(μg/L)Recovery(RSD)/%MineralwaterFound/(μg/L)Recovery(RSD)/%LakewaterFound/(μg/L)Recovery(RSD)/%DMP0ndndnd5049.0698.12(3.55)51.00102.00(3.61)46.1292.24(5.55)200186.0193.00(5.21)185.9092.95(7.09)200.86100.43(4.71)500450.5590.11(6.13)488.7997.76(8.31)499.0499.81(4.15)DEP0ndndnd5045.4890.97(6.09)47.9195.82(6.28)57.24114.47(2.85)200176.2888.14(2.96)201.61100.80(2.82)212.83106.42(3.15)500417.1783.43(7.12)463.7792.75(5.55)514.91102.98(3.78)DBP0ndndnd5055.78111.56(7.09)48.0696.12(6.27)47.2594.50(6.50)200201.78100.89(7.98)194.1797.08(6.67)202.25101.12(1.93)500428.0985.62(6.10)467.1493.43(1.95)512.43102.49(5.02)DnOP0ndndnd5055.83111.66(2.87)54.40108.80(2.68)50.97101.93(2.82)200165.9982.99(5.74)199.9799.99(4.25)199.4399.71(4.85)500447.3889.48(5.60)514.19102.84(4.07)493.0598.61(5.60)㊀nd:notdetected.2.3㊀实际水样测定㊀㊀利用该法对实验室自来水㊁某品牌矿泉水以及湖水进行了实际水样富集分析ꎮ对各实际水样分别加标50㊁200和500μg/Lꎬ所获得的加标回收率和RSD如表3所示ꎮ由表3中数据可见ꎬ加标回收率数值在82 99%至114 47%之间ꎬRSD在1 93%至8 31%之间ꎬ结果满意ꎮ另外ꎬ空白样品和加标样品在UA ̄DLLME处理前后的色谱图见图4ꎮ图4㊀(Ⅰ)实验室自来水㊁(Ⅱ)某品牌矿泉水和(Ⅲ)湖水样品的液相色谱图Fig.4㊀Chromatogramsof(Ⅰ)tapwaterfromlaboratoryꎬ(Ⅱ)mineralwaterand(Ⅲ)lakewatersamples㊀a.blanksamplewithoutpretreatmentꎻb.blanksampletrea ̄tedwithUA ̄DLLMEꎻc.blanksamplespikedwithstandardsat200 0μg/Lforeachwithoutpretreatmentꎻd.blanksamplespikedwithstandardsat200 0μg/LforeachtreatedwithUA ̄DLLME.㊀Mobilephases:A.methanolꎻB.water.Gradientelution:0-3minꎬ85%Aꎻ3-10minꎬ85%Ato100%Aꎻ10-20minꎬ100%A.Flowrate:1 0mL/min.Injectedvolume:10μL.Wavelength:225nm.㊀Peaks:1.DMPꎻ2.DEPꎻ3.DBPꎻ4.DnOP.061第2期马燕玲ꎬ等:超声辅助分散液液微萃取 ̄高效液相色谱测定水样中的4种邻苯二甲酸酯类增塑剂3 结论㊀㊀本文所建立的UA ̄DLLME ̄HPLC ̄UV可以测定实际水样中的PAEsꎬ有一定的实用参考价值ꎮ该法具有操作简便㊁萃取速度快㊁萃取效率和富集倍数高㊁试剂消耗量少㊁重现性好㊁环境友好等优点ꎮ参考文献:[1]㊀LiuXLꎬWuS.ChinaPlasticsIndustry(刘兴利ꎬ吴双.塑料工业)ꎬ2006ꎬ34(Suppl):230[2]㊀SwanSHꎬMainKMꎬLiuFꎬetal.EnvironHealthPer ̄spectꎬ2005ꎬ113(8):1056[3]㊀DeOrsiDꎬGagliardiLꎬPorraRꎬetal.AnalChimActaꎬ2006ꎬ555(2):238[4]㊀LinXTꎬWangXYꎬChenMꎬetal.ResearchofEnviron 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