气相色谱质谱联用仪
操作流程:operate flow :
1、装置的准备(更换柱,进样口隔垫 ,玻璃衬管)installation preparation (galss insert preparation :玻璃衬管:确保正确的安装,没有脱落的迹象; 进样口隔垫:在每100次进样后,换隔垫;
更换柱:保证正确的安装。)
在安装完上述的步骤后,打开GC 。
1)接通GC的前处理装置的电源开关:
2)接通GC主机的电源开关:
3)接通MS主机的电源开关;
4)接通PC的打印机、显示器的开关;
5)接通PC部的电源开关;
6)双击“GCMS实时分析”图标;
2.装置的启动(真空系统的启动)
1)点击“GCMS实时分析“窗的分析辅助栏的”真空控制“图标。
2)点击自动启动。
3)显示完毕,点击关闭,关闭窗
4)等待10分钟,
5)进行泄漏检验
3.调谐(检漏,自动调谐等)
1)点击实时分析辅助栏的调谐,打开调谐界面。
2)点击调谐辅助栏的“峰监视”
3)改变监视组为“水,空气”
4)检测器电压为0.7KV
5)点亮灯丝
6)检测器的电压每变化0.1KV,直到最强峰的高度达到显示窗的一半高度
7)确认峰强度
自动调谐:装置启动后或离子源变更后,等温度稳定后进行自动调谐。
点击辅助栏的调谐,打开调谐界面
点击“自动调谐文件”显示“调谐信息”窗,进行自动调谐。
点击OK,电机自动调协开始,结束后输出调谐报告并保存文件。
4.条件设定(GC参数:升温程序,流量控制等
MS参数:质量数的测定范围,分析时间等)
Notes :数据获得SCAN 方式
5、数据处理:(TIC,MC,MS和谱库检索)
在GCMS后处理程序中进行。点击qualitative,从菜单栏“file ”中选择文件,进行相应的处理,(如TIC,MIC的放大,质谱的显示和背景扣除,质量色谱图的显示,谱库检索,登记目标化合物)进行相似性检索,保存数据。
6、定性结果(登入质谱处理表)
7、条件设定(GC参数:升温程序,流量控制等
MS参数:监测的质量数,分析时间等
定量参数:峰处理,校正曲线参数等)
8、建立化合物表(create compound table /wizard (new))
9、数据采集(标准式样的SIM测定)
设置方法
1) 根据SCAN 方式定性分析的结果作成表格。(化合物名称,保留时间,特征离
子,组等)
2) 启动“GMCS“图标。
3) 点击“数据采集辅助栏“的”方法详细显示/不显示“。
4) SCAN 的方法文件未打开时选择菜单的“文件F“中的”打开方法文件“
5) 选择SCAN 用的方法文件,点击“打开“
GC和MS参数的设定
样品分析
10、校准曲线生成、确认和修正(由数据管理器读取数据)
1)目标成分的登记、
2)定量参数的设定
3)汇集的输入
4)化合物表的编辑和保存
5)校准曲线的计算
11、数据采集(未知试样的SIM测定)
使用GC/MS分析上的校准线作成的方法文件,进行未知样品分析。
1) 点击后运行辅助栏的定量处理
2) 从菜单中的文件F中选择打开数据文件
3) 选择欲定理的数据文件,点击打开
4) 点击定量处理辅助栏的峰积分
5) 点击化合物表的结果登记,显示定量结果
6) 色谱图上的峰检测标志基线,确认结果。
使用GC/MS分析上校准线作成的方法文件,进行未知样品分析。
12、定量计算
13.报告
英文的:对应的6节
1.Preparation
1)Glass insert preparation :confirm that the silica wool has not moved ,and that the galss insert O-ring has not deteriorated .
2)Septum preparaion : after approximately 100 injections ,replace the septum .
3)Column preparation : attach the column to the hanger ,install the hanger ,and verify the proper position of the graphite ferrules .tighten the injection port and detector collumn nuts.
When the above preparations are complete ,turn on the GC.
2.Setting parameter
1) Set the column information and the flow rates
From the “flow”key screen,set the column inlet pressure,the injection mode ,the split ratio,the sampling time ,etc.from the”column “inner diameter ,the column length and the film thickness ,from the “purge “(Pfmenu),set the purge flow rate .
Changing the column temperature after the flow rate has been set may change the flow rate .
2)set the temperature of the detector and the injection port
From the screens of the “INJ”and “DET”keys ,set the temperatures .if the detector is set to “OFF”,trn it “ON”,from “DET GAS”(PF menu),set hydrogen ,air ,makeup gad ,etc.
3)set the COL temperature and the temperature program
From the screen of the :COL”key ,set the column intial temperature and the
temperature program .temperature settings muat be within and allowable column and detecor ranges .
4) start GC control
Press the “SYSTEM “key to display the main screen
Press “start GC”(PF menu) to start GC control
Press the “MONIT”key ,and ensure that the temperature of each zone ,the gas flow rate ,the gas pressure,etc.are correct.
5) set the detector
From the screem of the “DET”key ,set the range and the time filter constant.
Ensure that the temperature of the detector is rising ,then ignite the FID or set the TCD current value.
When all parameters reach their respective setup valus ,the STATUS indicator light becomes green and the system is ready for analysis .
The default zero parameter,”zero at ready “zeroes the detector signal when the GC is ready .
6)set the data processing unit
Perform the required settings for the data processing unit,such as specifying the processing parameters.
7) check the baseline
Press the “MONIT”key ,and ensure that the baselines is stable .
Press “ZERO ADJ”(PF menu) to zero the detector output ,when the basiling is stable ,you can start analysis .
8)inject the sample
Aspirate the sample in the suringe,inject it into the Gcinjection port .and press “START”to analyze it .
For capillary column analysis ,normally inject 1~2ūL
Glass insert (liner)
Select the splitless type based on the sample injection method .
2.alytical column
Verify that carrier gas is flowing hrough the column before increasing the column oven temperature.
Press the “SYSTEM”key ,and set the start time.
Slection of the analysis column is very important in GC analysis .
3.installing the analysis column
Install the column ,use box nut on the injection port side .use a column nut on the detector side .
4.sample injection modes
This method is effective for analying a low concention sample .
5.setting the heated zone temperatures
The temperature of th einjection port ,tne column oven and the detector are set individually.
6.column temperature program
Ues a temperature program to analyze samples with a wide boiling point range
7.injection counter
Every 100,replace the glass insert .
8.starting up the GC
Turn on the power and/or press the “SYSTEM”key to display the Gcstarup screen. Press “start GC”(PF menu)to start temperature cintrol of each heated turned on.set the start up method to “auto”to start the file as soon as the power on.
9.setting startup (startup the vacuum system )
1)Click the “vacuum control “in the GCMS real analysis ,
2)click auto startup
3) after display over ,click shutdoff ,shutoff the window
4)wait until 10mintes
5) goto leakage test
10.tuning (Test leakage ,auto tuning ,etc.)
1)Click tuning in the real time analysis ,open tuning interphase.
2)click peak mointor view in the assistant column ,open the interphase.
3)change the monitor group :H2O,N2,O2
4)the voltage of the detector is 0.7KV
5) lighten filament
6)every time the voltage of the detector change 0.1KV,until the the maximum of the height achives the half of the display window.
7) affirm the intensity of the peak .
Auto tuning :after startup the devise or change the temperature of the ion sourse ,wait 2 hours untill the temperature stabilization ,must be go to the auto tuning .
11.data acquisition
GC parameter: temperature rise program ,the control of the flow rate,etc
MS parameter:the range of the determine about mass number,analysis time ,etc. Notes :data gain method :scan
12.qualitative (TIC ,MC,MS and table searches )
Despose in the GCMS postrun analysis program,click qualitative ,select specifically file and open it ,dispose it as required ,eg:blow up TIC,MC and MS ,display mass spectrum ,deduct background,display chromatogram chart,