Factory and Field Installation System Integration Test Procedures

The following procedures are followed in the initial factory testing of the NMR system before shipping to site, and are then repeated upon installation at site. The tests check the basic functionality of the magnet and RF components of the NMR instrument and allow the system to be brought up to the optimum operating conditions for on-line operation

Test Bench

• System under Test, i.e. complete assembly of NEMA enclosed NMR system with the appropriate ‘Process probe’ installed inside the Magnet and connected to the sample system  pipes.

• All units connected after insuring that all the internal boards (in the PC and the Shim box) are plugged in well and software is installed properly.

• Remote computer configured to run the NMR software as a client of the NMR system under test.

Initial Steps

•     Check wiring and power - trace wiring per schematics.

•      Power up system – electric and air.

•      Check power distribution to system – Barber-Coleman temperature control setup (including alarm relay), LED’s on all the NMR components and fans on all components.

•      Check system safety features – purge system, gas detector (requires butane gas source), and alarms.

•      Check that all system documentation is present and that serial numbers of all components (NMR and enclosure) are correct.

•      Attach sample system (1/4” loop with peristaltic).

•      Check A/C and heaters on enclosure. Make sure that the left A/C is configured to run non-stop.

•      Allow system to equilibrate for 24 hours – running ‘Heater diagnostics’ as system settles.

•      Determine that system is stable and ready for steady state operation.

•      Insert water into the probe through the sample system pipes.

System Software and Configuration

2) NMR System Computer Settings:

Users and Password – Make sure that the same user is logged on the System Computer and the Remote Computer.

dcomcnfg setup-

                 Run dcomcnfg (Start->run->dcomcnfg)

                 Find the name "NMRServer" in the applications' list.

In the properties menu verify that the Program location is on this computer, and the identity is set to "Interactive User"

PcAnyWhere configuration under NT- Make sure that the Computer is set as Network NetBios host, with the right Username and Password. Verify that PcAnyWhere is set to run automatically as an NT Service. Reboot the computer and check if it is running automatically.

NMR software components – Run each of the following software and verify that it functions properly:

• Shim Test – Verify that the Shim box is connected to COM5. Run ShimBoxTest read data from all coils, run quick test, accurate test and address test.

• Heater Test – Verify that the Heater is connected to COM1. Run Heater diagnostic Program and make sure you can read data from the heater.

• Diagnostic – Run the Diagnostic program with Magnet test configuration and verify that it is running properly.

• Lab NMR – Run the Lab NMR program and check the lock, the shimming routines.

• Process NMR – Run the Process NMR program and verify that the ‘Software plug’ is installed and detected by the software.

Serial COM setting and communication -

Modem – Connect a phone cable, set pcAnywhere to run temporarily as a modem host, and dial from another computer. After communication is established, disconnect and set pcAnywhere back as a network host.

FieldPoint – Verify that the Power Supply is connected to COM6. Make sure that in the SampleControl.INI the device is set to FieldPoint. Run LabNMR, add valves commands to the ‘Event Table’, and make sure that every valve can be operated from the software.

Modbus – Verify that the Power Supply is connected to COM7. Make sure in ProcessNMR.INI that the DCS type is set to Modbus. Run ProcessNMR. From the Modbus Configuration Dialog Box – Write data to the PLC and read it back to verify it was written OK.

3) Remote computer Settings:

Users and Password - Make sure that the same user is logged on the System Computer and the Remote Computer.                   

dcomcnfg setup-

Run dcomcnfg (Start->run->dcomcnfg)

Find the name "NMRServer" in the Applications' list.

In the properties menu verify that the Program Location is On this computer, and the identity is set to "Interactive User"

PcAnyWhere configuration - Make sure that the Computer is set as a modem host, with the right User Name and Password. Verify that PcAnyWhere is set to run automatically as an NT Service. Reboot the computer and check if it is running automatically.

NMR software components – Run each of the following software and verify that it function properly:

• Shim Test – Run ShimBoxTest read data from all coils, run quick test, accurate test and address test.

•   Heater Test – Run Heater diagnostic Program and make sure you can read data from the heater.

•   Diagnostic – Run the Diagnostic program with Magnet test configuration and verify that it is running properly.

•   Lab NMR – Run the Lab NMR program and check the lock, the shimming routines.

•   Process NMR – Run the Process NMR program and verify that the Software plug is installed and detected by the software.

Serial COM setting and communication -

Modem – Connect a phone cable, set PcAnyWhere to run as a modem host, and dial from another computer

Modbus – Verify that the Modicon PLC to COM 2. Make sure in ProcessNMR.INI that the DCS type is set to Modbus. Run ProcessNMR.

From the Modbus Configuration Dialog Box – Write data to the PLC and read it back to verify it was written OK.

4)  Shimming the NMR System

Magnet Resolution Unshimmed:

Disconnect the DC power to the Shim Box.

Check the H2O signal of the unshimmed magnet, write down the results in the following table. Verify that it is less than the tolerance allowed and similar to the results of the shipment documents.

Test results:

(H₂ O, 2Kpts, 50kHz BW, Process probe with inner tube diameter of 7mm for ‘D’ type magnet and 4mm for ‘C’ type magnet)

5) Hardware Testing:

On the NMR computer verify that the file nmr.ini has the shim matrix of the correct magnet type (ver ‘C’ or ver ‘D’).

On the NMR computer verify that the file nmr.ini has the correct serial COM port number for the Shim Box (usually it is com5).

On the NMR computer run Shim Test software

Get in the ‘Dac Map’ menu

Select all and run ‘Quick Test’ verify that all O.K

Select all and run ‘Accurate Test’ verify that all O.K

Select all and run ‘Address Test’ verify that all O.K

Exit the program

6) Improving existing Shimming:

On the remote computer run LabNMR software

In the ‘Event Table’ menu load file: Shim 3.et

In the ‘ADC’ menu load file: Shim 3.adc

Under the ‘Automated Analysis’ menu in the ‘Post Processing Definition’ menu load file: Remove DC.pp

In the ‘Average’ menu load file: 1 scan.avg

Start Lock

Wait till you get the ‘Fine lock 1’ message and verify a good Lock performance using the tools in ‘Lock Menu’

Start acquisition.

In the ‘Frequency’ menu, change the frequency shift in such a way that the peak will be about 300 Hz from the zero frequency.

Stop acquisition

Get in the ‘Shim’ menu

In the ‘Gradients’ menu load the previous shim gradient from file D:\nmr\200-xxx.grd from the System PC .

In the ‘Set Methods’ menu choose:         

Method file:    d:\nmr\newadv.shm

Criteria:             RMS

Start:               Advanced 3_1

Stop:                Advanced 4_3          

Click on ‘Start Shimming’ and wait for the Autoshim routine to finish. Using the ‘Gradients’ menu save all shim value in a file that will indicate the magnet serial number and the date such as : 200-xxx ‘date’.grd

On the remote computer run NMR Diagnostic software

Under ‘File’ menu load Resolution Test.cfg

Start acquisition.

After collecting the 10 successive readings, stop the acquisition.

Analyzing the Results:      

• Resolution at half height - Examine the “1/2 Height” window and right down the results of the mean value in the following table. Verify that is less then the tolerance allowed and similar to the results of the shipment documents.

• Resolution at tenth height  - Examine the “1/10 Height” window and right down the results of the mean value in the following table. Verify that is less then the tolerance allowed and similar to the results of the shipment documents.

• Resolution at the base - Examine the “Base Height” window and right down the results of the mean value in the following table. Verify that is less then the tolerance allowed and similar to the results of the shipment documents.

Magnet Resolution Shimmed Results

(H₂ O, 2Kpts, 2kHz SW, Process probe)

7) Long Term Inside NEMA Enclosure

Test Bench:

The system under test inside the NEMA enclosure (all units connected properly).

An external container full with water.

A water pump hooked to the external input and output of the NEMA enclosure.

Remote computer configured to run the NMR software as a client of the system under test.

Preparation:

On the NMR computer run LabNMR software

In the ‘Event Table’ menu load file: 90 deg.et. After the ‘Reset’ row, add additional row to the event table that will open valve #1 for 20 second. After that row, add another row that will close valve #1 for 20 second. Save the new event table as Flow 90 deg.et

In the ‘ADC’ menu load file: 90 deg.adc

Under the ‘Automated Analysis’ menu in the ‘Post Processing Definition’ menu load file: Remove DC.pp

In the ‘Average’ menu load file: 1 scan.avg

Start Lock

Wait till you get the ‘Fine lock 1’ message and verify a good Lock performance using the tools in ‘Lock Menu’

Open the external manual valves on the NEMA enclosure

Turn on the water pump.

Run autoshim routines according to the “Improving existing Shimming” procedure using the new  Flow 90 deg.et

Run the Test:            

On the remote computer run NMR Diagnostic software

Under ‘File’ menu load NEMA Test.cfg

On the remote computer run Heater Diagnostic and start collecting data from the Heater.

Through the NMR Diagnostic start the acquisition.

Let the system run for at least 12 hour

Through the NMR Diagnostic stop the acquisition.

In the Heater Diagnostic stop the collecting data.

Analyzing the Results:

• Magnet heats control - Examine the “Spectrometer Frequency” window (in the NMR Diagnostic program) and verify that the total fluctuation of the frequency is less then the tolerance allowed. Write the result in the ‘Long Term Final Test Results.doc’.

• Performance of lock mechanism - Examine the “Lock Position” window (in the NMR Diagnostic program) and verify that the Standard Deviation of the relative lock frequency is less then the tolerance allowed. Write the result in the ‘Long Term Final Test Results.doc’.

• Resolution at half height - Examine the “1/2 Height” window (in the NMR Diagnostic program) and verify that the results are less then the tolerance allowed and neighboring to the results of the shipment documents. Write the result in the ‘Long Term Final Test Results.doc’.

• Resolution at tenth height  - Examine the “1/10 Height” window (in the NMR Diagnostic program) and verify that the results are less then the tolerance allowed and neighboring to the results of the shipment documents. Write the result in the ‘Long Term Final Test Results.doc’.

• Line shapes - Examine the “Base Height” window (in the NMR Diagnostic program) and verify that the results are less then the tolerance allowed and neighboring to the results of the shipment documents. Write the result in the ‘Long Term Final Test Results.doc’.

• Heater magnet sense - Examine the “Magnet Sense” (in the Heater Diagnostic program) and verify that the error (shown on the graph) is around zero and less ±50 units. Write the result in the ‘Long Term Final Test Results.doc’.

• Envelope Heater magnet sense - Examine the “Envelope Sense” (in the Heater Diagnostic program) and verify that the error (shown on the graph) is around zero and less ±50 units. Write the result in the ‘Long Term Final Test Results.doc’.

• Heater magnet heat output - Examine the “Magnet Heat” (in the Heater Diagnostic program) and verify that the mean value is in the reign of 20 to 200 units. Write the result in the ‘Long Term Final Test Results.doc’.

• Heater envelope heat output - Examine the “Envelope Heat” (in the Heater Diagnostic program) and verify that the mean value is in the reign of 20 to 200 units. Write the result in the ‘Long Term Final Test Results.doc’.

Long Term Final Test Results

(Continues test for 12 hours inside a nominal NEMA enclosure conditions. Other conditions are H₂ O, 2Kpts, 2173Hz SW, Calibrated Dewar Process Probe) 

NMR Calibration and  Background Check – Toluene Standard

Toluene is introduced into the NMR probe (in factory testing toluene is placed in probe in a sealed glass NMR tube). In field installation toluene is injected through the sample system with an appropriate flush cycle which includes a cooling flush cycle with water when system is operational at high temperature. NMR spectrum is obtained with a 4 kHz sweep width, 20 second recycle delay, and a 4 pulse average. Alpha resonance is referenced to 2.15 ppm.

This calibration check confirms NMR RF stability through quantitation of aromatic-H/Alpha-H ratio, which should integrate to a common ration of 5/3. Gain settings should be adjusted such that an RMS of around 1000 is obtained from the sample

Any significant deviation from this value indicates the presence of RF instability, and/or NMR probe contamination (wax on probe walls etc.).

Expected toluene spectrum is shown below:

At this point the NMR spectrometer is considered to be fully functional and ready for operation.

On-line sample can be placed in the NMR and the shimming procedure repeated to obtain optimum shim on the sample to be analysed. Calibration models can be loaded and the validation procedure begun.

[ Calibration/Validation Procedures  ]

For more information on this topic please contact:

John Edwards

Manager, Process and Analytical NMR Services

Process NMR Associates LLC, 87A Sand Pit Rd, Danbury, CT 06810, USA, Tel: (203) 744-5905