505889_MSPMform_NOAA_12NOV2015.doc

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PREVENTATIVE MAINTENANCE FOR AB SCIEX SPECTROMETER Federal contract opportunity
Solicitation number
EA-133C-16-RQ-0419
Issued by
Department of Commerce National Oceanic and Atmospheric Administration

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PM Calibration Form

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API 4000™ MS/MS Detector

Preventive Maintenance & Calibration Form - MSF1004-D

API 4000™ MS/MS Detector

Preventive Maintenance & Calibration Form

MSF1004-D 01-Jul-2012

Record of Document Revisions

Date
Revision Level
Description of Revision
04-Dec-2006
A
First issue of document.
01-Sep-2008
B
Format changes. Moved High Res & High Mass Tests to Appendix.
09-Jul-2009
C
Text and format changes. Removed High Res & High Mass Tests to a separate form. Restored content removed from Rev A. Added CAD valve function test. Adjusted Lens voltage tolerances to match those of the OEM.
01-Jul-2012
D
Updated references to OEM to reflect company name change and improved trademark recognition. Added Slope Variation Guideline to “Unit Resolution Calibration & Performance Tests”. Removed Appendix A. Multiple text changes. Updated document template with new colors/graphics.

Table of Contents

1.0 Foreword…………………………………………………………………………………

2.0 Pre-PM Performance Evaluation……………………………………………………………….4-5

3.0 Workstation Maintenance…...…………………….………………………………………………5

4.0 Instrument Maintenance…………….……………………………………………………………..5

5.0 Ion Source Maintenance…………………………………………………………………………...5

6.0 Instrument Checks…….……………………………………………………………………………6

7.0 Unit Resolution Calibration & Performance Tests..…………….………………………….7-8 8.0 Cleanup & Review…………………………………………………………………………………..9

9.0 Customer Information……………………………………………………………………………...9

10.0 PM Acceptance Sign-off…………………………………………………………………………...9

1.0

FOREWORD

Preventive Maintenance & Calibration is typically performed every six months. It is designed to help maintain system performance and to help diagnose any system deficiencies. The mSPEC Product Specialist (PS) may perform more testing than is outlined in this document to help diagnose any system deficiencies. The PM & Calibration will not correct on-going performance problems caused by improper maintenance, dirty samples, electronic failures or incorrect usage. mSPEC uses OEM Performance Standards, Specs, and Test Conditions. Refer to ‘Unit Resolution Calibration & Performance Tests’ in this document for test parameters, specifications, & results. For detailed instructions on how to complete this procedure, please refer to the current revision of MSI1004 – mSPEC Service Instruction for API 4000™ Preventive Maintenance & Calibration.

Portions of this document make reference to software, instruments, components, or other accessories which are registered as trademarks by AB SCIEX™ and other companies. These include API 4000™, Curtain Gas™, TurboV®, and Analyst®. Any such reference to these products in this document is intended only to designate those products as supported by mSPEC Group and does not imply any right and/or license to use or permit others to use such product names as trademarks. Software described in this document (such as Analyst®) is furnished under a license agreement between AB SCIEX™ and the instrument owner. It is against the law to copy, modify, or distribute the software on any medium, except as specifically allowed in the license agreement.

mSPEC makes no representations of the fitness of any products mentioned in this document for any particular purpose and assumes no liability, including indirect or consequential damages, for any use for which the instrument owner may put the products described herein, or for any adverse circumstances arising therefrom. The products described in this document have not been approved by their manufacturers for diagnostic use, and are intended for use in research only.

2.0

PRE-PM PERFORMANCE EVALUATION:

N/A

Ask customer about system performance and review instrument’s maintenance records.

Backup the API Instrument Project before beginning testing.

Record base vacuum reading: 0.7 x 10-5 Torr.

Record customer’s optimal Pre-PM TIS position: Horiz: 5, Vert: 0

Record the Current CEM voltage: Current CEM Pos/Neg = 2400 / 2400 VDC. Optimal CEM = 2600 VDC

Replace while performing PM if CEM optimizes > 2800VDC.

Not Required

Perform each of the following tests. Optimize ion source position only. The Pre-PM Performance tests are an Evaluation only. Meeting the Guidelines is not required.

Check for charging and clean Ion Path (extra charge may be applicable) while vented if necessary:

Charging Observed None

Q1 PPG Positive Unit Resolution Evaluation No Data *

Standard: PPG Pos 2x10-6 M, SP Flow: 5-10uL/min, Scans: 10 MCA
Data Attached (sample of file):
Mass (Da)
Intensity (cps)
Peak Width (Da)
( Mass (Da)
Value
Guideline
Value
Guideline
Guideline
906.673
1.58e7
≥ 2.0e7
0.654
0.6-0.8 @ 50% (Masses < 2000)
< 0.1
2242.637
9.83e5
≥ 1.0e6
0.850
0.6-0.85 @ 50% (Masses > 2000)

Q3 PPG Positive Unit Resolution Evaluation No Data *

Standard: PPG Pos 2x10-6 M, SP Flow: 5-10uL/min, Scans: 10 MCA
Data Attached (sample of file):
Mass (Da)
Intensity (cps)
Peak Width (Da)
( Mass (Da)
Value
Guideline
Value
Guideline
Guideline
906.673
3.46e6
≥ 2.0e7
0.925
0.6-0.8 @ 50% (Masses < 2000)
< 0.1
2242.637
9.66e5
≥ 8.0e5
0.601
0.6-0.85 @ 50% (Masses > 2000)

Q1 PPG Negative Unit Resolution Evaluation No Data *

Standard: PPG Neg 3x10-4 M, SP Flow: 5-10uL/min, Scans: 10 MCA
Data Attached (sample of file):
Mass (Da)
Intensity (cps)
Peak Width (Da)
( Mass (Da)
Value
Guideline
Value
Guideline
Guideline
933.636
6.78e6
≥ 2.0e7
0.843
0.6-0.8 @ 50% (Masses < 2000)
< 0.1
2037.431
9.75e5
≥ 3.0e6
0.634
0.6-0.85 @ 50% (Masses > 2000)

Q3 PPG Negative Unit Resolution Evaluation No Data *

Standard: PPG Neg 3x10-4 M, SP Flow: 5-10uL/min, Scans: 10 MCA
Data Attached (sample of file):
Mass (Da)
Intensity (cps)
Peak Width (Da)
( Mass (Da)
Value
Guideline
Value
Guideline
Guideline
933.636
4.85e6
≥ 1.0e7
0.750
0.6-0.8 @ 50% (Masses < 2000)

0.6-0.85 @ 50% (Masses > 2000) < 0.1

* Some data may be unattainable due to required remedial maintenance or time constraints.

3.0

WORKSTATION MAINTENANCE:

Software platform used: Analyst® Version: 1.5.2 Hotfixes to: Feb 2011

At customer request, update Analyst® software/hotfixes, drivers, or firmware as needed.

Run disk cleanup/maintenance utilities or advise customer to do so.

4.0

INSTRUMENT MAINTENANCE:

Clean instrument surfaces including: covers, turbo fans, bench, & vacuum pump(s).

Replace the card cage air filter.

If using roughing pump(s):

Replace roughing pump oil mist filter(s) if necessary ( N/A).

Replace roughing pump oil. Check and replace pump seals as necessary.

If using a scroll pump:

Clean the inlet strainer, gas ballast control, and fan cover.

Replace the tip seals (clean grooves) ( N/A) /exhaust valve ( N/A) and silencer/HEPA filter (if installed) ( N/A) annually or as needed.

Check vacuum pump line(s) & o-rings and replace if damaged or discolored.

Check gas regulator lines and replace if crimped or damaged.

Disassemble the interface:

Clean curtain plate, orifice, & skimmer.

Clean the Q0 Ion Guide.

Clean or replace any worn or damaged components or o-rings and reassemble.

5.0

ION SOURCE MAINTENANCE:

Record the TurboV® source S/N: 500020815

Disassemble and clean the TurboV® source housing:

Remove and clean exhaust chimney/nut.

Clean and inspect the ceramic tube and ionizer needle.

Replace the PEEK™ line and fittings (ensure new line is >30cm). Clean the grounding union.

Inspect TIS heaters. Replace if beads are falling out (extra charge may be applicable) ( Replaced N/A).

Replace any other parts as required and reassemble source housing.

Disassemble and clean the TIS Probe. Replace the electrode.

Disassemble and clean the APCI Probe. Replace the electrode.

If customer owns any optional sources document their maintenance using appropriate service form. N/A 6.0

INSTRUMENT CHECKS:

Record meter info: Model: Fluke 87 V S/N: 94880453 Cal. Exp. Date: 25JUN2016

If the line adjust transformers are installed, measure output voltage and adjust taps for 230VAC if required. Record tap setting: 208 (188, 200, 208, 220, 230, 240, 250)

Record voltage to instrument/vacuum pump: 208 VAC (207-242VAC)

Tune the Q1 QPS. Measure voltage at park mass: 291 mVDC

Tune the Q3 QPS. Measure voltage at park mass: 393 mVDC

Check Ion Optics voltages in Q1± (adjust expected values to match instrument defaults as required):

TP
Positive
Negative
Reading
Expected
Reading
Expected
DF
-199.2V
-200.0V ((10V)
+399.0V
+400.0V ((10V)
DP
+120.5V
+120.0V ((5V)
-120.6V
-120.0V ((5V)
IQ2
-18.0V
-18.0V ((1V)
+18.0V
+18.0V ((1V)
ST
-14.9V
-15.0V ((1V)
+14.9V
+15.0V ((1V)
RO2
-60.8V
-60.0V ((5V)
+61.1V
+60.0V ((5V)
ST3
-78.2V
-80.0V ((5V)
+078.7V
+80.0V ((5V)
IQ1
-10.9V
-11.0V ((0.2V)
+11.0V
+11.0V ((0.2V)
Q0
-9.9V
-10.0V ((0.2V)
+9.9V
+10.0V ((0.2V)

Check Multiplier HV board voltages for accuracy and polarity (with CEM at 2000VDC):

TP
Name
Positive
Negative
Reading
Expected
Reading
Expected
1
CEM Float
-61.6mV
-60.0mV ((10mV)
+38.8mV
+40.0mV ((10mV)
2
CEM Bias
-38.5mV
-40.0mV ((10mV)
+67.5mV
+60.0mV ((10mV)
3
Discriminator
-119.7mV
~ -120.0mV ((40mV) (Do not adjust – optimized at factory).

Vacuum pump interlock(s) trip when roughing pump vacuum lost.

Exhaust interlock trips when source exhaust pressure fails or is blocked.

Curtain Gas™ interlock trips when pressure falls <20PSI (bleed line to test).

Electronics interlock trips when ion source removed.

Adjust & Record Instrument Gas Regulator Settings:

Input Gas
Pressure (psi)
Pressure Spec (psi)
Gas Type
Gas Type Spec
Maximum

Flow Rate

Gas 1/2
100
100-105
Nitrogen
Nitrogen (UHP or Approved*) or Zero Air
17.0 L/min
Curtain Gas™
60
60
Nitrogen
Nitrogen (UHP or Approved*)
5.0 L/min
Exhaust Gas
60
55-60
Nitrogen
Clean Air or Nitrogen
6.0 L/min

* Note: Approved Nitrogen Generators or Purities with impurities known not to negatively impact performance may also be used.

Record base pressure when pumpdown is complete: 0.9 x10-5 Torr (<1.5x10-5 Torr).

Record pressure with CAD set to 12: 4.4 x10-5 Torr (<5.5x10-5 Torr).

Record vacuum pressure from PRE TP at each CAD value to test valves using Analyst®:

CAD = 0
CAD = 1
CAD = 2
CAD = 3
CAD = 4
CAD = 12
92 mV
260 mV
319 mV
346 mV
343 mV
436 mV

Verify functionality of interface & source heaters (APCI and TIS) when complete and check for gas leaks.

7.0

UNIT RESOLUTION CALIBRATION & PERFORMANCE TESTS:

Perform each of the following tests. Print/capture Spectra, & Calibration Report or File Info (at customer request) for each test after optimizing for intensity, peak shape, resolution, and updating the calibration.

At customer request, perform the High Resolution and/or High Mass Calibration Tests in mSPEC’s API 4000™ Optional Calibration Form following the Unit Resolution mode tests.

Use Standards from an unexpired AB SCIEX™ Test Kit (P/N 4406127) ( Customer or mSPEC-supplied) to perform the following tests (customer prepared standards may be used if preferred). Record the Part Number, Lot Number & Expiration Date of the Standards used:

Standard
Concentration
Part Number
Lot/Batch Number
Expiration Date
PPG Pos
2x10-6 M
4405231
A4128
15APR2015
PPG Neg
3x10-4 M
4405234
A4134
18MAR2015
Reserpine
0.16pmol/uL
4405237
A4133
02MAY2015

Optimize the source position and Source/Gas parameters.

Confirm instrument is not charging post-PM cleaning.

CEM Replaced during PM Maintenance?: Yes N/A.

Optimize the CEM & Deflector. Record optimal CEM voltage. CEM Pos/Neg = 2600 / 2600 VDC

Q1 PPG Positive Unit Resolution Test Test Passed

Standard: PPG Pos 2x10-6 M, SP Flow: 5-10uL/min, Scans: 10 MCA
Test Failed

Calibration Performed/Verified

Note: Specified masses must meet the intensity specs listed below.

All masses in raw data must meet peak width and ( mass specs listed below.

Data Attached (sample of file):

3of505889PM

Mass (Da)
Intensity (cps)
Peak Width (Da)
( Mass (Da)
Slope Variation
Value
Spec
Value
Spec
Spec
Guideline
906.673
2.72e7
≥ 2.0e7
0.738
0.6-0.8 @ 50% (Masses < 2000)
< 0.1
≤ 0.003
2242.637
2.78e6
≥ 1.0e6
0.761
0.6-0.85 @ 50% (Masses > 2000)

Q3 PPG Positive Unit Resolution Test Test Passed

Standard: PPG Pos 2x10-6 M, SP Flow: 5-10uL/min, Scans: 10 MCA
Test Failed

Calibration Performed/Verified

Note: Specified masses must meet the intensity specs listed below.

All masses in raw data must meet peak width and ( mass specs listed below.

Data Attached (sample of file):

2of505889PM

Mass (Da)
Intensity (cps)
Peak Width (Da)
( Mass (Da)
Slope Variation
Value
Spec
Value
Spec
Spec
Guideline
906.673
2.53e7
≥ 2.0e7
0.716
0.6-0.8 @ 50% (Masses < 2000)
< 0.1
≤ 0.003
2242.637
3.53e6
≥ 8.0e5
0.777
0.6-0.85 @ 50% (Masses > 2000)

Q1 PPG Negative Unit Resolution Test Test Passed

Standard: PPG Neg 3x10-4 M, SP Flow: 5-10uL/min, Scans: 10 MCA
Test Failed

Calibration Performed/Verified

Note: Specified masses must meet the intensity specs listed below.

All masses in raw data must meet peak width and ( mass specs listed below.

Data Attached (sample of file):

4of505889PM

Mass (Da)
Intensity (cps)
Peak Width (Da)
( Mass (Da)
Slope Variation
Value
Spec
Value
Spec
Spec
Guideline
933.636
2.49e7
≥ 2.0e7
0.745
0.6-0.8 @ 50% (Masses < 2000)
< 0.1
≤ 0.003
2037.431
4.49e6
≥ 3.0e6
0.683
0.6-0.85 @ 50% (Masses > 2000)

Q3 PPG Negative Unit Resolution Test Test Passed

Standard: PPG Neg 3x10-4 M, SP Flow: 5-10uL/min, Scans: 10 MCA
Test Failed

Calibration Performed/Verified

Note: Specified masses must meet the intensity specs listed below.

All masses in raw data must meet peak width and ( mass specs listed below.

Data Attached (sample of file):

6of505889PM

Mass (Da)
Intensity (cps)
Peak Width (Da)
( Mass (Da)
Slope Variation
Value
Spec
Value
Spec
Spec
Guideline
933.636
1.90e7
≥ 1.0e7
0.775
0.6-0.8 @ 50% (Masses < 2000)

0.6-0.85 @ 50% (Masses > 2000)

< 0.1
≤ 0.003

Reserpine MSMS Positive Test Test Passed

Standard: Reserpine 0.16pmol/uL, SP Flow: 5-10uL/min, Products of: 609.x, Scans: 10 MCA
Test Failed

Note: Specified masses must meet the intensity specs listed below.

All masses in raw data must meet peak width specs listed below.

Data Attached (sample of file):

7,8of505889PM

Q1 609.x

Intensity (cps)

x Efficiency Factor
Fragment 195.1 Intensity (cps)
Fragment 195.1 Width (Da)
Spec
Value
Value
Spec
3.71e7
x 0.06 =
≥ 2.22e6
2.88e6
0.690
0.6-0.8 @ 50%

8.0

CLEANUP & REVIEW:

Reconnect the customer’s HPLC system to the ion source as well as any other connections removed for the PM. Ask the customer for assistance if required.

Return the source to its Pre-PM position recorded during Pre-PM Evaluation. Confirm desired position with customer to prevent potential Post-PM contamination problems.

In Manual Tune, set the source heat to 300°C and manually run the customer’s high organic mobile phase LC Pump into the source at 500uL/min for 30mins to clean any residual chemical background from the source region of the mass spec.

In Manual Tune, change scan type to MRM+/- and confirm no method resolution errors.

If any parameter setting access modes were changed during the PM, ensure they are returned to their normal access mode and that their offsets are adjusted to match optimized values from the Post-PM acquisition files.

If customer requested High Resolution and/or High Mass Calibration, attach the completed, signed mSPEC API 4000™ Optional Calibration Form along with raw data.

If High Resolution Calibration was not performed, copy the Post-PM unit resolution offsets and unit calibration values into high resolution and high calibration tables.

Backup the Post-PM API Instrument Project calibration files.

Review all work performed with customer and record any final comments on the CSR.

Leave the original copy of the Service Report, PM Form, and raw data for the customer’s records and take another copy with you. Ensure paperwork is signed & dated by both the customer and the mSPEC PS.

9.0

CUSTOMER INFORMATION:

Company:
Hollings Marine /NOAA
Address:
331 Fort Johnson Rd.

Charleston, SC 29412

USA

Start Date:
10NOV2015
Location:
B204
Finish Date:
12NOV2015
Serial Number:
S0660208
mSPEC WO:
505889
Customer System ID:
API4000
Customer WO:
505889
Customer Asset ID:
API4000

10.0

PM ACCEPTANCE SIGN-OFF:

By signing below you acknowledge that the PM was completely performed and that all acceptance criteria were met or exceeded by mSPEC.

mSPEC Service Representative:

Daniel Caruso

Signature & Date:
Name:

Authorized

Customer Representative:

Emily Pisarski

Signature & Date:
Name:

MSF1004-D-01JUL12-API4000-PM-FRM 1 of 9

MSF1004-D-01JUL12-API4000-PM-FRM 9 of 9

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