hao de wenz好的文章多来些撒

我觉得70-80度的温度太高啦，不够合理！

我们实验室icp突然显示标样中Pb,Cu的实际浓度与设定浓度不在一个数量级，故无法确定校正值，也即无法得到标准曲线，重配标样后，结果依然，不知哪位同仁有此遭遇？

1.    Purpose
To ensure the operators are able to operate ICAP PE-3300XL Spectrometer in accordance with a standard procedure.

2. Scope
This procedure is used as a guideline in the operation of ICAP PE-3300XL Spectrometer for metal contents analysis.

3.    Procedure

3.1 Start up (Cold start up mode)

3.1.1 Turn on the gases (purified argon gas, compressed air as shear gas) and the water re-circulating unit.
3.1.2    Turn on the main instrument switch and the RF generator standby switch.
3.1.3    With both the main instrument and RF generator standby switches on, the blue system power light goes on.
3.1.4    Switch on the computer, monitor and printer.
3.1.5    Click on the “Start” icon, click on “Programs”, select “ICP WinLab Optima
3000”, click on “Optima”.
3.1.6    The ICP WinLab software starts.
3.1.7    The software will communicate with the spectrometer and the accessories
configured (such as autosampler) and check the start up status of the
instrument/accessories, there is a 73 minutes wait before you can use the
instrument.

3.2    Start up checklist (Hot start up mode):

3.2.1    Chiller is on at 18 C.
3.2.2    Argon gas supply at 80-100 psi.
3.2.3    Fan of exhaust vent is on.
3.2.4    Compressor should drain daily.

3.3    Plasma ignition

3.3.1    Turn on the computer and enter the ICP WinLab-Optima.
3.3.2    Replace the rubbing and close the clamps.
3.3.3    Click on the “Plasma” icon to show the plasma control panel.
3.3.4    If “OK” appear, click on the button to “ON” position.
3.3.5    Wait about 90 seconds for the plasma to ignite.
3.3.6    After plasma ignition, screw the cam levers on the pump to apply tension on the sample tubing until smooth flow is obtained.

3.3.7    Wait for 30 to 60 minutes for plasma to be stable.
3.4    Manual analysis

3.4.1    Click on “File” icon and choose the file “DEMO, WSP”.
3.4.2    Click on “Method” icon and open a desired method.
3.4.3    In the “manual analysis control window”, choose information file by clicking on “Open” and then select “w&v.SIF”.
3.4.4    Click on “OPEN” of the “Result Data Set” and typing the required file name. (e.g. 031230-EN).
3.4.5    Standardization

3.4.5.1 Aspirate standard-blank and click on “analyze blank” icon.
3.4.5.2 Aspirate standards and click on analyze standards respective to element and concentration.
3.4.5.3 Click on “Calibration” icon to show the calibration curves of the element.
3.4.5.4 Do the QC check by aspirate QC standard, and click on “analyze sample”.
3.4.5.5 If all the results are within ±10% of the nominal value, proceed the following steps. If not, repeat 3.3.5 or perform maintenance procedure.

3.4.6    Sample analysis

3.4.6.1 In the “sample information editor” window, type the sample No. in the “Sample ID column”; sample weight in the “Initial sample wt.” Column; final volume in the “Sample Pre Vol” column and Dilution factor in the “Diluted to Vol” column, if any.
3.4.6.2 Aspirate the sample and click on “Analyze Sample”.
3.4.6.3 Repeat 3.4.6.1 to 3.4.6.2 for other samples.
3.4.6.4 QC checking should be done at least every 40 samples.
Re-calibrate and re-analyze samples whenever QC check fails.
3.4.6.5 Collect the results from the printer.

3.5    Automatic analysis

3.5.1 Click on “File” icon and choose “AUTO.WSP”.
3.5.2    In the “Automated Analysis Control” window, click “OPEN” on the results data, set name and type the required file name (e.g.040101-EN AUTO).

3.5.3    In the “Sample Information Editor” window, repeat 3.4.6.1 for all the samples. Save the Sample Information Editor and type “1” at the end of “Analyze QC, before” column.
3.5.4    Click the analyze page of the “Automated Analysis Control” window.
3.5.5    In the menu tool bar, click on “analysis” and then “analytical sequence”.
3.5.6    Check the sample ID and autosampler location in the “Analytical sequence” window.
3.5.7    Place the standard and sample into the autosampler according to the analytical sequence.
3.5.8    In the “Automated Analysis Control” window, click on “Analyze All” icon and pay attention to the analysis until the first QC is done and the result is within the acceptable range.
3.5.9    In the menu tool bar, click on system and then auto startup/ shut down, click on the square of the end of automated analysis in case of overnight analysis.
3.5.10    Collect the results from the printer.

3.6    Shutting down the instrument manually

3.6.1 Flush the sample introduction system for five minutes with the plasma on.
3.6.2 Extinguish the plasma by clicking on the “Plasma Off” icon in the plasma
control window.
3.6.3 When the plasma is extinguished, the plasma off / on switch in the plasma
control window changes from blue to white and the peristaltic pump stops
pumping solution to the plasma.
3.6.4 In the plasma control window, click on pump button to activate the peristaltic pump. This is to pump dry the liquid in the peristaltic pump tubings.
3.6.5 Release the pump tubings.
3.6.6 Normally, set the instrument in the standby mode. DO NOT SWITCH OFF THE MAIN INSTRUMENT AND RF GENERATOR.
3.6.7 Turn off the computer and printer.
3.6.8 Turn off the RF generator standby switch and the main instrument switch and turn off the gases and the water recirculating unit if there is no need to put the instrument in the standard mode.

4.    Examine Spectra

4.1 Click on the “Examine spectra” icon to show the “Examine Spectra Window”
4.2 Click on “Data” and then “Data Set” icon.
4.3    Choose the data set name required.

4.4    In the “Create Sample List”, choose the “Sample”, “Std” and “Blk” by pressing “Ctrl” Key and click the mouse button.
4.5    Choose the element by clicking “Element” icon.
4.6    In the style column, click to move the rectangle to the target sample. and then “Style”.
4.7    In the style column, choose different style for different sample.
4.8    Click the “Control” icon and then “Print”.

Note : - Always keep the cursor on the center of the peak. if not, perform the following steps:
a) Click on the “← → ” icon at the bottom of the screen, and move the “∆ ” point to the cursor.
b) Click on “Method” icon, and then “Params” and click on “Update”
c) Exit and save the method.

- Besides, the background point should be at the base of the peak and
free of any interference.
d) Click on the green spot and more to a desirable position.
e) Repeat step b) and step c).

说的还有道理