HAPSITEER高級操作培訓(xùn)PPT學(xué)習(xí)課件

1、Course Outline 課程大綱課程大綱 Overview 綜述 Instrument Setup 儀器設(shè)置 Tune 調(diào)諧 Troubleshooting 故障查找 Advanced Data Review 高級數(shù)據(jù)處理 Creating AMDIS Libraries 創(chuàng)建 AMDIS 庫 Recognizing Co-Elution 識別共淘析 Chromatogram Overlay 色譜圖迭加 Accessing Quantitation Reports 查訪定量報(bào)告 Basic Method Writing 基本方法編寫 Method Editor Overview 方法編寫

2、器概述 SIM Methods SIM 方法 Method Sequencing 方法序列 Blank Subtraction 空樣扣除 Communications 通訊 Instrument Setup 儀器設(shè)置儀器設(shè)置 Insert Gas Canisters 插入氣瓶 Turn on the Analytical Module or take the Analytical Module out of Extended Standby 將分析模件電源 on 或?qū)?分析模件離開延伸的待機(jī)狀態(tài) System will heat, AutoTune and run a Concentrator

3、 cleanout 系統(tǒng)將加熱, 自動(dòng)調(diào)諧和運(yùn)行濃縮器清理 Turn on the Laptop 將計(jì)算機(jī)電源 on Double click the ER IQ/Plus IQ icon to open the software 雙擊 ER IQ/Plus IQ 圖標(biāo), 打開軟件 Tune 調(diào)諧調(diào)諧 Tune Overview 調(diào)諧概述 AutoTune 自動(dòng)調(diào)諧 Manual Tune 手動(dòng)調(diào)諧 Tune Overview 調(diào)諧概述調(diào)諧概述 Tune optimizes the performance of the MS 調(diào)諧使 MS 的性能最佳化 An improperly tuned

4、MS can result in: 未正確調(diào)諧的 MS 可導(dǎo)致: Low sensitivity 靈敏度低 Undetected compounds 未能檢測到化合物 Mass misalignment 質(zhì)量數(shù)未對準(zhǔn) Incorrect identifications 不正確的 ID 鑒別 Incorrect Mass Ratios 不正確的質(zhì)量比 Low Net Fit or SI numbers 低純 擬合或 SI 數(shù) Tune Overview 調(diào)諧概述調(diào)諧概述 Ten masses are used when tuning the MS 調(diào)諧 MS 使用 10 個(gè)質(zhì)量數(shù) Masses

5、are between 50-282 to encompass the full 41-300 range of mass fragments 質(zhì)量數(shù)在 50- 282 之間包含整個(gè) 41-300 質(zhì)量分裂物范圍 The Internal Standard gas contains the chemicals that provide these masses used for tuning 內(nèi)部標(biāo)準(zhǔn)氣體包含提供這 些用于調(diào)諧質(zhì)量數(shù)的化合物 AutoTune 自動(dòng)調(diào)諧自動(dòng)調(diào)諧 The HAPSITE will automatically AutoTune: HAPSITE 將自動(dòng)調(diào)諧: Upo

6、n Startup 當(dāng)啟動(dòng)時(shí) Upon exiting Extended Standby 當(dāng)退出延伸的待機(jī)狀態(tài)時(shí) After 12 hours of operation運(yùn)行 12 個(gè)小時(shí)后 AutoTune 自動(dòng)調(diào)諧自動(dòng)調(diào)諧 AutoTune can be initialized by: 自動(dòng)調(diào)諧可由下列動(dòng)作起始 : Clicking Tune AutoTune on the laptop 在計(jì)算 機(jī)上單擊 Tune AutoTune Touching RUN AUTOTUNE on the front panel 觸摸面板上的 RUN AUTOTUNE 按鈕 Rebooting the HA

7、PSITE 重新啟 動(dòng) HAPSITE Troubleshooting a Failed AutoTune 不成功自動(dòng)調(diào)不成功自動(dòng)調(diào) 諧的故障查找諧的故障查找 Internal Standard Canister 內(nèi)部標(biāo)準(zhǔn)氣瓶 Verify that the pressure is adequate 核實(shí)壓強(qiáng)是否適當(dāng) Verify the expiration date 核實(shí)是否已到使用期限 Insert new IS canister if necessary 必要時(shí)插入新的 IS 氣瓶 Carrier Gas (Smart Plus Only) 載氣 (僅 Smart Plus) Veri

8、fy pressure that the pressure is adequate 核實(shí)壓強(qiáng)是否適當(dāng) Reservoir pressure ( 400 kPa) 貯存器壓強(qiáng) ( 400 仟帕) ER does not have a reservoir ER 無貯存器 Insert new Carrier Gas canister if necessary 必要時(shí)插入 新的載氣瓶 Repeat AutoTune 重新執(zhí)行自動(dòng)調(diào)諧 Tune Requires Advanced Mode 調(diào)諧要求高級模式調(diào)諧要求高級模式 The Access Level must be set to Advance

9、d to manually tune the instrument 必須將 Access Level 設(shè)定于高級, 手動(dòng)調(diào) 諧儀器 Set Access Level is used to change the ER IQ/Plus IQ user mode Set Access Level 用于更改 ER IQ / Plus IQ 的用戶模式 Normal Mode: Allows access to default methods and data analysis 常規(guī)模式: 允許進(jìn) 入默認(rèn)方法和數(shù)據(jù)分析 Advanced Mode: Allows access to method edi

10、ting, manual tuning, file transfer and file deletion 高級模式:允許進(jìn)入方法 編寫, 手動(dòng)調(diào)諧, 文件傳送和文件刪除 ER IQ/Plus IQ Set Access Level ER IQ/Plus IQ 設(shè)定查訪層次設(shè)定查訪層次 Select Set Access Level 選 Set Access Level Select Advanced from the drop down menu 從下拉菜單 上選 Advanced Neither access level is password protected under the def

11、ault settings 默認(rèn)設(shè)定查訪層次 無口令保護(hù) Advanced mode can be password protected if desired 必要時(shí)可用口令保護(hù)高級模式 Click OK 單擊 OK Set Access Level 設(shè)定查訪層次設(shè)定查訪層次 Manual Tune 手動(dòng)調(diào)諧手動(dòng)調(diào)諧 Double click the Tune icon 雙擊 調(diào)諧圖標(biāo) Select 選 default.tun Click OK 單擊 OK Note: The NEG is being consumed while Manual Tune is open 注: 在打開手動(dòng)調(diào)諧的

12、同時(shí), 消耗 NEG Base Peak Gain (BPG) 基峰增益基峰增益 (BPG) BPG is related to the intensity of mass 117 BPG 與 M 117 的強(qiáng)度有關(guān) BPG influences sensitivity BPG 影響靈敏度 ER ideal setting is 0.5 ER 理想的設(shè)定值為 0.5 Range is 0.4 to 0.6 范圍為 0.4 至 0.6 Smart Plus ideal setting is 1.0 Smart Plus理想的設(shè)定值為 0.1 Range is 0.8 to 2.0 范圍為 0.8

13、 至 2.0 Adjusting Base Peak Gain 調(diào)整基峰增益調(diào)整基峰增益 The BPG is adjusted using EM (Electron Multiplier) voltage 用 EM (電子倍增 器) 電壓調(diào)整 BPG Adjust using increments of 25 V 用增量 25 伏調(diào)整 The normal operating range is 1000 to 2000 volts 常規(guī)工作范圍為 1000 至 2000 伏 Adjusting Base Peak Gain (BPG) 調(diào)整基峰增益調(diào)整基峰增益 (BPG) Adjusted

14、Base Peak Gain for an ER 為 ER 調(diào)整基峰增益 Real Time Mass Calibration Table 實(shí)時(shí)質(zhì)量校準(zhǔn)表實(shí)時(shí)質(zhì)量校準(zhǔn)表 Red boxes may be present in the Real Time Mass Calibration Area 在 實(shí)時(shí)質(zhì)量校準(zhǔn)區(qū)可出現(xiàn)紅色框 This indicates that resolution and/or intensity of the mass is out of range 這表明質(zhì)量數(shù)的分辨率和/或強(qiáng)度已超出范圍 Status Column 狀態(tài)欄狀態(tài)欄 Status Column wil

15、l read OK, OK Low, OK High, Low or High 狀態(tài)欄將出現(xiàn) OK, OK 低, OK 高, 低 或 高等讀值 High and Low are not acceptable 高和低是不可接受的 Mass Alignment 質(zhì)量對準(zhǔn)質(zhì)量對準(zhǔn) Perform a Mass Alignment by pressing F5 按 F5 執(zhí)行質(zhì)量對準(zhǔn) Updates the Status column readings 更新狀態(tài)欄讀值 Perform a Mass Alignment prior to and after making adjustments to t

16、he tune parameters 調(diào)整調(diào)諧參數(shù)前和后執(zhí)行質(zhì)量對 準(zhǔn) Target Resolution 靶分辨率靶分辨率 Resolution refers to the width of the mass 分辨率與質(zhì) 量數(shù)的寬度有關(guān) The mass width should be 1 AMU 質(zhì)量數(shù)寬度應(yīng)為 1 AMU The range for the Target Resolution is 0.85 and 1.10 靶分辨率的 范圍在 0.85 至 1.10 之間 Adjusting Target Resolution 調(diào)整靶分辨率調(diào)整靶分辨率 Adjust in increm

17、ents of 0.05 調(diào)整的增量為 0.05 The number in the Actual Percentage column is affected by the target resolution adjustments 實(shí)際百分?jǐn)?shù)欄的數(shù)受 靶分辨率調(diào)整的影響 It should fall between the Max. and Min. Targets 它應(yīng)落入 最大和最小靶之間 If the masses cannot be brought into range by adjusting the Target Resolution, adjust the Ion Energi

18、es 如調(diào)整靶分辨率不 能使質(zhì)量數(shù)進(jìn)入范圍, 調(diào)整離子能量 Ion Energies 離子能量離子能量 Adjusting the Ion Energy adjusts the intensity (height) of the mass 調(diào)整離子能量調(diào)整質(zhì)量的強(qiáng)度(高度) Adjust the Ion Energies if the target resolution is at 0.85 and the red box continues to indicate that the mass is above the maximum target resolution 如靶分辨率在 0.85

19、 和紅框 繼續(xù)表示質(zhì)量在最大靶分辨率以上, 調(diào)整離子能量 Adjust the Ion Energies if the target resolution is at 1.10 and the red box continues to indicate that the mass is below the minimum target resolution 如靶分辨率在 1.10 和紅 框繼續(xù)表示質(zhì)量在最小靶分辨率以下, 調(diào)整離子能量 Ion Energies 離子能量離子能量 Adjust the Ion Energy 調(diào)整離子能量 Ion Energies should generally

20、 be in ascending order from Low to High 一般離子能量應(yīng)從低至高地 向上升 Perform a Mass Alignment (F5) after each change until OK is reported in the Status column 每次更改后執(zhí)行質(zhì)量對準(zhǔn) (F5), 直到狀 態(tài)欄內(nèi)顯示 OK Save Tune 保存調(diào)諧保存調(diào)諧 Verify that OK is displayed in the Status Column 核實(shí)在狀態(tài)欄內(nèi)顯示 OK Readjustment of the BPG, Target Resolutio

21、n and Ion Energies may be necessary to attain acceptable tune parameters 重新 調(diào)整 BPG, 靶分辨率和離子能量 可能必須達(dá)到可接受的調(diào)諧參數(shù) Click Save Tune 單擊 保存調(diào)諧 Close Manual Tune 關(guān)閉手 動(dòng)調(diào)諧 How to Manual Tune 如何手動(dòng)調(diào)諧如何手動(dòng)調(diào)諧 Verify Mass 117 is in range 核實(shí) M 117 在范圍內(nèi) Target Resolution (0.85-1.10) 靶分辨率 (0.85-1.10) Ion Energy (140-170)

22、 離子能量 (140-170) Adjust Base Peak Gain (BPG) sensitivity, if needed 如需要, 調(diào)整 基峰增益 (BPG)靈敏度 Adjust using EM voltage 用 EM 電壓調(diào)整 Range 范圍 0.6-0.8 for ER with 0.5 as optimal setting 對 ER 0.6-0.8, 0.5為最佳設(shè)定值 0.8-2.0 for Smart Plus with 1.0 as optimal setting 對 Smart Plus 0.8-2.0, 1.0為最佳設(shè)定值 Adjust peak width

23、resolutions, if needed如需要, 調(diào)整峰寬分辨率 Adjust using Target Resolution 用靶分辨率調(diào)整 Range 0.85-1.10 范圍 0.85-1.10 Adjust mass ratio intensity, if needed如需要, 調(diào)整質(zhì)量比強(qiáng)度 Adjust using Ion Energy 用離子能量調(diào)整 Refer to Ion Energy range chart 參閱離子能量范圍圖表 Save tune as default.tun 保存調(diào)諧為 default.tun Tune Worksheet 調(diào)諧工作表 Advance

24、d Manual Tune Worksheet 高級的手動(dòng)調(diào)諧工作表 Troubleshooting 故障查找故障查找 Common Problems 常見問題 High Pressure Troubleshooting 高壓強(qiáng)故障查找 Common Problems: High Internal Standard TIC常見問題常見問題: 內(nèi)部內(nèi)部 標(biāo)準(zhǔn)標(biāo)準(zhǔn) TIC 高高 Possible causes 可能原因 Blocked air flow in probe 探頭中空氣流堵塞 Sample bag closed 樣品袋關(guān)閉 Plugged exhaust 排氣阻塞 Note: The

25、air peak is not present in the chromatogram 注: 色譜圖中未出現(xiàn)空氣峰 Common Problems: Shifted Retention Time常見問題常見問題: 移位移位 的滯留時(shí)間的滯留時(shí)間 A blank may show that the Retention time has shifted 空樣可表示滯留時(shí)間已移位 Smart Plus BPFB range is 8:00 (+/- 10 seconds) Smart Plus BPFB 的范圍 為 8:00 (+/- 10 秒) ER BPFB range is 3:45 (+/-

26、 5 seconds) ER BPFB 的范圍為 3:45 (+/- 5 秒) Adjusting the GC column pressure will adjust the Retention time 調(diào)整 GC 柱壓強(qiáng)將調(diào)整滯留時(shí)間 GC Column Pressure settings are unique to each HAPSITE 每臺 HAPSITE 的 GC 柱 壓強(qiáng)是獨(dú)特的 Common Problems: Shifted Retention Time 常見問題常見問題: 移位的移位的 滯留時(shí)間滯留時(shí)間 Double click on the Status icon 雙

27、 擊狀態(tài)圖標(biāo) Click 單擊 Pressure Flow and Offsets Increase kPa to decrease RT 增大仟 帕來減小RT 1 kPa change 3 second RT change 更 改1 仟帕 RT更改3 秒 Re-run the blank to verify that RT for BPFB is corrected 重新運(yùn)行空樣, 證實(shí)BPFB的RT已改正 Common Problems: Multiple Internal Standard Peaks 常見問常見問 題題: 多個(gè)內(nèi)部標(biāo)準(zhǔn)峰多個(gè)內(nèi)部標(biāo)準(zhǔn)峰 Occurs when the p

28、revious run is aborted 當(dāng)先前的運(yùn)行被中止時(shí)發(fā)生 The Internal Standards were unable to elute內(nèi)部標(biāo)準(zhǔn)不能淘析 Continue running blanks until the extra peaks are no longer present 繼續(xù)運(yùn)行空樣直到額外的峰不再出現(xiàn) Common Problems: GC Column Hardware Error 常見問題常見問題: GC 柱硬件誤差柱硬件誤差 Possible causes include:可能的原因包括: Empty or low nitrogen canist

29、er 氮瓶空或壓力低 Insert a new, full can of nitrogen 插入新的, 滿的氮瓶 A cracked or chipped Concentrator 濃縮器破裂或碎裂 Uninstall the Concentrator to verify its condition 卸下濃縮 器, 核實(shí)它的情況 Incorrect ferrule orientation 套圈方向不正確 Orient ferrules as shown in picture 套圈方向如圖所示 Ferrules are old or warped 套圈老化或彎曲 Verify the condi

30、tion of the ferrules 核實(shí)套圈的情況 The Concentrator is improperly seated 濃 縮器就位不正確 Reinstall the Concentrator 重新安裝濃縮器 The Concentrator nuts are not fully tightened 濃縮器螺 帽未完全擰緊 Pump Failure: High Pressure Warning 泵損壞泵損壞: 高壓強(qiáng)警告高壓強(qiáng)警告 A high pressure warning appears when the total MS pressure is higher than a

31、cceptable 當(dāng) MS 的總壓強(qiáng)高于可接受的壓強(qiáng)時(shí)出現(xiàn)高壓強(qiáng)警告 Acceptable pressure is less than 6 E- 3 Pa可接受的壓強(qiáng)低于6 E- 3 帕 The HAPSITE will no longer run methods HAPSITE不再運(yùn)行方法 The source of the high pressure can be isolated using the Service Module 可用服務(wù)模件隔離高壓強(qiáng)源 Attach and pump down for a couple of hours連接和抽空數(shù)小時(shí) If the HAPSITE

32、runs a method, the cause is the NEG Pump 如 HAPSITE 運(yùn)行方法, 原因在于 NEG 泵 If the HAPSITE does not run a method, the cause is the Ion Pump 如 HAPSITE 不運(yùn)行方法, 原因在于離子泵 Pump Overview 泵概述泵概述 Ion Pump離子泵 Works in conjunction with the NEG to maintain vacuum in the Mass Spectrometer 與 NEG 一起工作維持質(zhì)譜儀 的真空 Removes the

33、noble gases 清除惰 性氣體 Average lifetime of an Ion Pump is 2000 to 4000 hours離子泵的平均壽 命為 2000 至 4000 小時(shí) To view the Ion Pump hours:查看離 子泵的小時(shí)數(shù) Double click the Status icon雙擊狀 態(tài)圖標(biāo) Select Maintenance 選維護(hù) Pump Overview 泵概述泵概述 NEG Pump NEG 泵 Maintains vacuum 維護(hù)真空 NEG can last over 200 hours when stored in Ext

34、ended Standby 當(dāng)貯存于延伸的待機(jī)模式時(shí), NEG 可 在 200 小時(shí)以上 Storing in Extended Standby improves NEG life 貯存于延伸的待機(jī)模式可延長 NEG壽命 To view the NEG hours 查看 NEG 的小時(shí)數(shù) Double click Status icon 雙 擊狀態(tài)圖標(biāo) Click on the NEG Status Tab High Pressure Troubleshooting 高壓強(qiáng)故障查找高壓強(qiáng)故障查找 NEG bakeout NEG 烘烤 NEG bakeout can be used if a N

35、EG has less than 100 hours of “On Time” 如 NEG 的 “On Time” 時(shí)間少于 100 小時(shí), 可使用 NEG 烘烤 The NEG is heated to 700C for 2 hours 將 NEG 加熱至 700C, 保持 2 個(gè)小時(shí) A bakeout may prolong NEG life, but is not a guarantee 烘烤可 延長 NEG 的壽命, 但不保證 NEG Bakeout NEG 烘烤烘烤 Double click the Status Icon 雙擊狀態(tài)圖標(biāo) Click on Service 單擊服務(wù)

36、Click on Bakeout NEG 單擊烘烤 NEG High Pressure in the HAPSITE Attach to Service Module and pump down for 2 hours Run a method. Does the method run? High pressure was caused by ion pump failure High pressure is caused by NEG pump failure Are there a lot of hours on the NEG pump? Replace the NEG pump Bak

37、eout the NEG pump YES NO NO YES Flowchart for High Pressure Troubleshooting 高壓強(qiáng)在 HAPSITE 中 連接至 服務(wù)模 件 抽空 2 個(gè)小時(shí) 運(yùn)行方法. 方法是 否 運(yùn)行? 高壓強(qiáng)的原因 是由于 離子泵故障 高壓強(qiáng)的原因是由于 NEG 泵故障 NEG 泵是否還有 許多 小時(shí)數(shù)? 更換更換 NEG 泵 烘烤烘烤 NEG 泵 是是 否否 否否 是是 高壓強(qiáng)故障查找流程圖高壓強(qiáng)故障查找流程圖 Advanced Data Review 高級數(shù)據(jù)處理高級數(shù)據(jù)處理 Creating AMDIS Libraries 創(chuàng)建 AMDI

38、S 庫 Using New AMDIS Library 使用新的 AMDIS 庫 Recognizing Co-Elution 識別共淘析 Chromatogram Overlay 色譜圖迭加 Chromatogram Subtract 色譜圖扣除 Creating AMDIS Libraries 創(chuàng)建創(chuàng)建 AMDIS 庫庫 To create an AMDIS library 為創(chuàng)建 AMDIS 庫 Select a spectrum from the NIST library 從 NIST 庫選譜圖 Export the spectrum to a new folder 輸出譜圖至新文件夾

39、 Create library file 創(chuàng)建庫文件 Add library to AMDIS 添加庫至 AMDIS Creating AMDIS Libraries 創(chuàng)建創(chuàng)建 AMDIS 庫庫 In this example, we will create a library that will include only CWAs 本例中, 我們將創(chuàng)建僅包含 CWAs 的庫 We will add the following compounds: 將添加下列化合物: Ethylmethylphosphonofluoridate (VX) 乙基甲基膦?；?(VX) Isobutylmet

40、hylphosphonofluoridate (R-33) 異丁基甲 基膦?；?(R-33) Sarin 沙林 Soman 束曼 Tabun 塔崩 Mustard Gas (Sulfur Mustard) 芥子氣 (硫芥子氣) Cyclohexylmethylphosphonofluoridate (Cyclosarin) 環(huán)己基甲基膦?；?(環(huán)沙林) Creating AMDIS Libraries 創(chuàng)建創(chuàng)建 AMDIS 庫庫 Open NIST 打開 NIST Enter the desired compound 鍵入所需的化合物 EnterEthylmethylphospho

41、nofluoridate (as much as will fit) 鍵入乙基甲基膦酰基氟化物 (盡管多將擬合) Right-click on the highlighted name 右擊點(diǎn)亮的名稱 Click Export Selected 單擊輸出已選 Creating AMDIS Libraries 創(chuàng)建創(chuàng)建 AMDIS 庫庫 Enter VX as the file name 在文件名中鍵入 VX This is the file that will be entered into the new library 這是 將輸入新庫的文件 Click Save 單擊 保存 Creati

42、ng AMDIS Libraries 創(chuàng)建創(chuàng)建 AMDIS 庫庫 Type Isobutylmethylphosphonofluoridate 鍵入異丁基甲基膦?；?Right-click on the name, and select Export Selected 右擊名稱, 并選輸出已選 Creating AMDIS Libraries 創(chuàng)建創(chuàng)建 AMDIS 庫庫 Click on VX 單擊VX Click on Save 單擊保存 Creating AMDIS Libraries 創(chuàng)建創(chuàng)建 AMDIS 庫庫 Click Append 單擊 添加 This will save t

43、he selected compound to the same library that VX is saved to 這將保存所選的化合物至與保存 VX 相同的庫 Repeat the previous steps until all desired compounds have been added 重復(fù)先前的步驟直到全部所需的化合物已經(jīng)被添加 Make sure to click on VX each time 務(wù)必每次單擊 VX Creating AMDIS Libraries 創(chuàng)建創(chuàng)建 AMDIS 庫庫 Open the data file to be analyzed 打開要分析

44、的數(shù)據(jù)文件 In the Basic Training Chromatograms- ER folder, open the data file labeled Agents 在基本培訓(xùn)色譜圖 - ER 文件夾中, 打開標(biāo)簽為 Agents 的數(shù)據(jù)文件 Creating AMDIS Libraries 創(chuàng)建創(chuàng)建 AMDIS 庫庫 Open AMDIS 打開 AMDIS Right-click in the chromatogram 在色譜圖上右擊 Highlight Peaks 點(diǎn)亮峰 Highlight Switch to AMDIS 點(diǎn)亮 切換至 AMDIS Creating AMDIS

45、Libraries 創(chuàng)建創(chuàng)建 AMDIS 庫庫 Click Confirm 單擊 確認(rèn) This will open up the Confirmation page (see next slide) 這將開啟確認(rèn)頁面 (見下一個(gè)幻燈片) Creating AMDIS Libraries 創(chuàng)建創(chuàng)建 AMDIS 庫庫 Creating AMDIS Libraries 創(chuàng)建創(chuàng)建 AMDIS 庫庫 In the Menu bar select Library, then select Library Transfer 在菜單欄中選 庫, 然后選 庫傳送 Creating AMDIS Librarie

46、s 創(chuàng)建創(chuàng)建 AMDIS 庫庫 Click on Files 單擊 文件 Click on Load Library 單擊 加載庫 Creating AMDIS Libraries 創(chuàng)建創(chuàng)建 AMDIS 庫庫 Change the File Type to .msp 將文件類型更改為 .msp Creating AMDIS Libraries 創(chuàng)建創(chuàng)建 AMDIS 庫庫 Find the file saved earlier from NIST 從 NIST 尋找早期保存的文件 Click the Up One Level button to get to the main NIST fold

47、er 單擊 返回上一級文件夾 按鈕, 進(jìn)入主 NIST 文件夾 Creating AMDIS Libraries 創(chuàng)建創(chuàng)建 AMDIS 庫庫 Double-click the MSSEARCH folder 雙擊 MSSEARCH 文件夾 Highlight the compound to add to the library 點(diǎn)亮化合物, 將它添加至庫中 This example is VX 本例為 VX Click Open 單擊 打開 Creating AMDIS Libraries 創(chuàng)建創(chuàng)建 AMDIS 庫庫 Click Create New Library 單擊 創(chuàng)建新庫 Creat

48、ing AMDIS Libraries 創(chuàng)建創(chuàng)建 AMDIS 庫庫 In File Name, type CWA Library.msl 在文件名中, 鍵入 CWA Library.msl This is the name of the new library that is being created 這是創(chuàng)建的新庫名 Click OK 單擊 OK Click Close in the Files window 單擊 在文件窗口中關(guān)閉 Creating AMDIS Libraries 創(chuàng)建創(chuàng)建 AMDIS 庫庫 Hold Ctrl button on the keyboard and cli

49、ck each compound to highlight 按住鍵盤上的 Ctrl 按鈕, 單擊每個(gè)化合物, 點(diǎn)亮它們 Click Transfer to add to the new CWA Library 單擊 傳送, 添加至新的 CWA 庫中 Creating AMDIS Libraries 創(chuàng)建創(chuàng)建 AMDIS 庫庫 Click Exit 單擊 退出 This will save the spectra to the new library 這將保存譜線至新庫中 Change to New AMDIS Library 變換至新變換至新 AMDIS 庫庫 To change to the

50、 new AMDIS Library 為變換至新 AMDIS 庫 In the Menu bar click File, then Go to Results 在菜單欄中單擊文件, 接著單擊 前往結(jié)果 This will bring up the Results page 這將調(diào)出結(jié)果頁面 Change to New AMDIS Library 變換至新變換至新 AMDIS 庫庫 Click on Analyze 單擊 分析 Change to New AMDIS Library 變換至新變換至新 AMDIS 庫庫 Click on Target Library 單擊 靶庫 Change to

51、 New AMDIS Library 變換至新變換至新 AMDIS 庫庫 Click on Select New 單擊 選新的 Change to New AMDIS Library 變換至新變換至新 AMDIS 庫庫 Click on the Up One Level button until the C: directory appears 單擊返回上一級文件夾按鈕直到出現(xiàn) C: 目錄 Change to New AMDIS Library 變換至新變換至新 AMDIS 庫庫 Double-click on the NIST08 folder 雙擊 NIST08 文件夾 Double-cl

52、ick on the MSSEARCH folder 雙擊 MSSEARCH 文件夾 Change to New AMDIS Library 變換至新變換至新 AMDIS 庫庫 Click on Files of type, and select MS Library (*.MSL) 單擊文件類型, 并選 MS 庫 (*.MSL) Change to New AMDIS Library 變換至新變換至新 AMDIS 庫庫 Click on CWA Library.msl 單擊 CWA Library.msl Click Open 單擊 打開 Change to New AMDIS Librar

53、y 變換至新變換至新 AMDIS 庫庫 Click Save 單擊 保存 Change to New AMDIS Library 變換至新變換至新 AMDIS 庫庫 Click Run 單擊 運(yùn)行 Change to New AMDIS Library 變換至新變換至新 AMDIS 庫庫 The CWA Library is now the main AMDIS library 現(xiàn)在 CWA 庫是主 AMDIS 庫 Recognizing Co-Elution 識別共淘析識別共淘析 Co-elution occurs when two or more chemicals share the s

54、ame peak 當(dāng)兩個(gè)或更多化合物分享同一個(gè)峰時(shí), 發(fā)生共淘析 The Gas Chromatograph separates chemicals based on their boiling points 氣相色譜儀分離化合物基于它們的沸點(diǎn) Chemicals with the same or similar boiling points will co-elute 化合物 具有相同或相似的沸點(diǎn)將出現(xiàn)共淘析 Co-eluting chemicals will generally have a low purity 共淘析化合 物一般為低純度 Recognizing Co-Elution 識

55、別共淘析識別共淘析 AMDIS identified a mixture of 19 chemicals plus the two Internal Standards in the chromatogram below 在下面的色譜圖中 AMDIS 鑒別 19 個(gè)化合物加上 2 個(gè)內(nèi)部標(biāo)準(zhǔn)組成的混合物 Recognizing Co-Elution Using AMDIS 用用 AMDIS 識別共淘析識別共淘析 AMDIS is a powerful tool for detecting co-eluting chemicals AMDIS 是檢測共淘析化合物的強(qiáng)有力的 工具 For this

56、 example, the retention times for the co-eluting chemicals are 0.8810 and 0.9889 minutes 本例中, 共淘析化合物的滯留 時(shí)間為 0.8810 和 0.9889 分 Methylene Chloride二氯甲烷 1,1-Dichloroethene 二氯乙烯 Recognizing Co-Elution Using NIST Search/User 用用 NIST 搜索搜索/用戶識別共淘析用戶識別共淘析 Double click the peak at 00:53 雙擊 00:53 處的峰 The NIST

57、identification is Methylene Chloride NIST 識別的是二氯甲烷 Recognizing Co-Elution Using NIST/Search User 用用 NIST 搜索搜索/用戶用戶 識別共淘析識別共淘析 Notice the additional masses are present in Scan 48 注意 到附加的質(zhì)量數(shù)存在于掃描 48 Masses do not correlate with the library Spectrum of Methylene Chloride 質(zhì)量數(shù)與庫的譜線 二氯甲烷無關(guān)聯(lián) Recognizing Co

58、-Elution Using RIC Plots Further analyze the peak at 0:53 Use the NIST Library (Names tab) to locate the top three mass fragments for Methylene Chloride 49, 84, 86 Add these masses to the Control Panel Add the additional mass fragments found in Scan 48 61, 96, 98 Notice the RIC plot peaks do not ali

59、gn Two different chemicals are co- eluting at this peak 61 96 98 49 84 86 用用 RIC 圖識別共淘析圖識別共淘析 進(jìn)一步分析 0:53 處的峰 用 NIST 庫 (名稱標(biāo)簽條) 為 二氯甲 烷定位 頂上的三個(gè) 質(zhì)量分裂物 49, 84, 86 添加這些質(zhì)量數(shù)至控制屏 添加在掃描 48 中出現(xiàn)的 附加質(zhì) 量分裂物 61, 96, 98 注意到 RIC 圖的峰并未對齊 兩個(gè)不同的化合物共淘析于此峰 61 96 98 49 84 86 Recognizing Co-Elution Using NIST MS Search 用用

60、 NIST MS 搜索識別共淘析搜索識別共淘析 Each chemical in the co-eluted peak can be further isolated using the NIST MS Search 用 NIST MS 搜索可進(jìn)一步分離共洗 提峰中的每個(gè)化合物 Right click on the mass spectrum 在質(zhì) 譜圖上右擊 Select NIST Grab Spectrum for NIST 選 NIST Grab Spectrum for NIST Recognizing Co-Elution Using NIST MS Search 用用 NIST M