AB液质联用使用说明tune mass calibration and CEM

1.1 Introduction

This chapter is intended for the user to become familiar with manually tuning and calibrating the instrument.In this section, users will:

Open a PPG acquisition method

Acquire 10 MCA scans of PPG spectrum

Adjust Peak Widths to achieve Unit Resolution

Manually tune and calibrate the instrument using the Calibrate from Spectrum icon

Replace Mass Calibration

Review Calibration Results with instructorOptimize the CEM

1.2 Materials

Syringe PumpSyringe

PEEK tubing and union adapterAppropriate PPG calibrant solution

1.3 Procedure

Insert the syringe into the PEEK tubing and union adapterTighten fittings to ensure there will be no leaksPlace syringe on pump and lock in place

Slide push plate up against plunger of syringeSet flow rate and diameter of syringe

Plumb the loose end of the PEEK tubing to the inlet of the sourcePress start to begin infusion

1.4 Manual Tuning and Mass Calibration

1.4.1 Choosing Hardware Configuration

1.Choose the API Instrument Project folder from the drop down menu next

to the yellow folder icon on the task bar.2.Double-click the Hardware Configuration and activate the Mass Spec

Only Profile. After a green check appears for the selected profile, close the window.

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Manual Tune, Mass Calibration and CEM

1.4.2 Manual Tuning Set-up

1.Click on the Tune and Calibrate Mode on the Navigation Bar. You should

hear the gases turn on as the instrument becomes active for use. A green mass spec status icon also appears in the bottom right corner of the window. 2.Under the View menu, activate the Sample Queue or click on the View

Queue icon to open the Queue Manager window. Minimize the Queue Manager window.3.Double-click on Manual Tuning. Under File, select Open and choose an

acquisition method (*.dam) for calibration. Start with Q1 positive calibration. For positive Q1, select Q1PosPPG.dam, for negative Q3, select Q3NegPPG.dam and so on. The method then comes up in the Tune Method Editor window, shown in Figure1-1.

Figure 1-1Manual Tune Window with “Q1 PosPPG.dam” Method Open4.The settings on the Source/Gas, Compound, Resolution and Detector

settings found on the tabs on the left side of the window as well as the MS and Advanced MS settings on the right side are values established by the installation engineer. Consult the help files if you have any questions regarding the settings in this window.5.The API 2000 and API 3200 Systems have integrated syringe pumps,

be sure to create the hardware profile with it activated on the Mass Spec

Configuration tab. Click on the Mass Spec and click Set Up.

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Manual Tune, Mass Calibration and CEM

Figure 1-2Integrated Syringe Pump Set Up

1.4.3 PPG Dilution and Syringe Pump Set Up

Different calibration solutions must be used, depending on the specific instrument and the polarity being calibrated.

Table1-1PPG Solutions and Dilutions By InstrumentInstrument Type

API 2000 SystemAPI 3000 SystemAPI 3200 SystemAPI 4000 SystemAPI 5000 System

Negative Mode

PPG 3000 StandardPPG 3000 StandardPPG 3000 StandardPPG 3000 StandardPPG 3000 Standard, Diluted 1:10

Positive Mode

PPG Standard (10-4M)PPG Standard, Diluted 1:10 (10-5M)

PPG Standard, Diluted 1:10 (10-5M)

High Mass

NAPPG 3000 StandardPPG 3000 Standard

PPG Standard, Diluted PPG 3000

Standard1:50(2x10-6M)

PPG Standard, Diluted PPG 3000 Standard1:500(2x10-7M)

Note:The PPG Standard should be diluted with the appropriate diluent. DO

NOT use the vial marked “Diluent” in the Mass Spec Standards Kit. The appropriate dilution solution for the PPG Standard is: dissolve 15.4 mg of ammonium acetate in 49.9mL of water, then add 49.9 mL of methanol, 0.1 mL acetonitrile, and 0.1 mL formic acid. The appropriate dilution solution for the PPG 3000 standard is: dissolve 385 mg ammonium acetate in 49.9 mL of water, then add, 49.9 mL of methanol, 0.1 mL acetonitrile, and 0.1 mL formic acid.

1.Load a syringe with the appropriate PPG solution.

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Manual Tune, Mass Calibration and CEM

2.API 3000 , API 4000 , API 5000 Systems: Start the infusion pump at a

flow rate of 10 μL/min. Ensure that the appropriate syringe diameter is being used.

Table1-2Syringe Diameters

Syringe Volume (μ

L)

1000500250

Diameter (mm)

4.613.262.30

3.API 2000 and API 3200 Systems: Use the drop down menu to the

right of Edit Ramp to access the Syringe Pump Method dialog box. Input a rate of 10 μL/min and an appropriate diameter for the syringe being used. Click Set Flow Rate or Start Syringe Pump to start the infusion. Then go back to the MS Method Editor by selecting MS Method from the drop down menu to the right of Edit Ramp.

Figure 1-3API 2000 and API 3200 Systems Syringe Pump Method Set-up

4.Allow enough time for the infusion rate to equilibrate. 5.Verify that the sprayer is positioned properly.

API 2000 , API 3000 Systems: The edge of the spray should be at least 2 mm from the curtain plate hole. Momentarily increase flow rate to 100 μL/min to visibly see the spray for proper spray adjustment relative to the orifice.

API 3200 , API 4000 , & API 5000 Systems: Settings of 10 vertical and 4 to 6 horizontal are recommended.

1.4.4 Verify PPG Ion Intensities and Peak Shape

1.On the MS tab, enter 10 cycles and verify that MCA box is checked. Click

Start to acquire 10 scans in MCA mode.

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Manual Tune, Mass Calibration and CEM

Note:MCA is Multi-Channel Acquisition and when it is activated the successive scans will be summed in a running total of intensities starting from the first scan up to …… 此处隐藏：18882字，全部文档内容请下载后查看。喜欢就下载吧 ……