uv-visible systems operational qualification · this document describes the hardware test...

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OQ Tests Specifications for Agilent UV-Visible Systems This document describes the hardware test specifications for UV-Visible systems performed in the Operational Qualification service – as applicable to the Agilent Cary systems and the Agilent 8453 / 8454 Systems. For each test, a short rationale and test description are included, together with the test setpoints and acceptance limits used in the Agilent Recommended test programs. Where applicable, variance information is also shown to indicate the allowed range for configurability. Note that both the core standard tests and the optional tests are described. The definition of Optional vs. Standard test is system dependent: optional tests are noted as such in the individual descriptions in the following pages. You can also refer to the table below for a mapping of core tests included for each of the different UV-Vis system types. You can complement the standard test program for your system by adding optional tests – ordered as Extra cost Tests. Selecting the optional tests check boxes in the table below as appropriate provides a record of your qualification scope. System test mapping. Operational Qualification (OQ) 8453 / 8454 Cary 50/60 Cary 100/300 Cary 4000/5000/ 6000i Wavelength Accuracy – Source Line Wavelength Accuracy – Holmium Oxide in Perchloric Acid Wavelength Accuracy – Mercury Line Wavelength Reproducibility Maximum Resolution Toluene/Hexane Resolution Stray Light – Potassium Chloride Stray Light – Sodium Iodide Stray Light – Sodium Nitrite Photometric Accuracy – Potassium Dichromate Photometric Accuracy – NIST Glass Filters Photometric Reproducibility – Potassium Dichromate Photometric Reproducibility – NIST Glass Filters Photometric Noise Baseline Flatness Photometric Stability Key: Standard Core Tests Optional Tests UV-VISIBLE SYSTEMS OPERATIONAL QUALIFICATION Agilent Enterprise Edition Compliance Services Page 1 of 15

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Page 1: UV-VISIBLE SYSTEMS OPERATIONAL QUALIFICATION · This document describes the hardware test specifications for UV-Visible systems performed in the Operational Qualification service

OQ Tests Specifications for Agilent UV-Visible Systems

This document describes the hardware test specifications for UV-Visible systems performed in the Operational Qualification service – as applicable to the Agilent Cary systems and the Agilent 8453 / 8454 Systems.

For each test, a short rationale and test description are included, together with the test setpoints and acceptance limits used in the Agilent Recommended test programs. Where applicable, variance information is also shown to indicate the allowed range for configurability.

Note that both the core standard tests and the optional tests are described. The definition of Optional vs. Standard test is system dependent: optional tests are noted as such in the individual descriptions in the following pages. You can also refer to the table below for a mapping of core tests included for each of the different UV-Vis system types.

You can complement the standard test program for your system by adding optional tests – ordered as Extra cost Tests. Selecting the optional tests check boxes in the table below as appropriate provides a record of your qualification scope.

System test mapping. Operational Qualification (OQ) 8453 / 8454 Cary 50/60 Cary 100/300 Cary 4000/5000/

6000iWavelength Accuracy – Source Line ● ● ● ●Wavelength Accuracy – Holmium Oxide in Perchloric Acid ● ● ● ●Wavelength Accuracy – Mercury Line — — —Wavelength Reproducibility ●Maximum Resolution — — —Toluene/Hexane Resolution ● ● ● ●Stray Light – Potassium Chloride ● ● ● ●Stray Light – Sodium Iodide ●Stray Light – Sodium Nitrite ●Photometric Accuracy – Potassium Dichromate ● ● ● ●Photometric Accuracy – NIST Glass FiltersPhotometric Reproducibility – Potassium DichromatePhotometric Reproducibility – NIST Glass Filters —Photometric Noise ●Baseline Flatness ●Photometric Stability ●

Key:Standard Core Tests Optional Tests

UV-VISIBLE SYSTEMS OPERATIONAL QUALIFICATION

Agilent Enterprise Edition Compliance Services

Page 1 of 15

Page 2: UV-VISIBLE SYSTEMS OPERATIONAL QUALIFICATION · This document describes the hardware test specifications for UV-Visible systems performed in the Operational Qualification service

Page 2 of 15

Agilent_Recommended_EQP

© Agilent Technologies, Inc. 2014

Document Released: May 2014 Enterprise Edition Compliance Services

No reproduction, translation, or use without permission

Individual OQ Test Design and Rationale for UV-Vis Systems

Test 1: Standard on all Systems

Test Name: Wavelength Accuracy – Source Line

Rationale: Wavelength Accuracy is performed as a verification of the installed source lamp (either Xenon or Deuterium) performance. The source lamp produces peak maxima at various wavelengths. In this test, Wavelength Accuracy is verified by scanning a spectrum a number of nanometers above and below the theoretical maxima for the installed source lamp. The test passes if the reported wavelength maxima do not differ from the expected values by more than the accuracy limit. This test is applied to all UV-Vis spectrophotometers and meets all major pharmacopoeia and ASTM requirements.

Procedure: Power on and warm up the spectrophotometer for the appropriate time prior to testing. If a cell changer is present disable the cell changer for testing. Verify there are no samples in the reference and sample cell holders. Using the spectrophotometer’s controlling data software (CDS) setup the Wavelength Accuracy test for the Source Lamp Emission Line. Perform the test by following the software prompts. When the test is complete record the values to the test record.

Models Set points Allowable range Limits Allowable range

84538454

486.0 nmN/A ≤ 0.20 nm 0.20 – 3.0 nm

656.1 nm

Cary 50Cary 60 541.92 nm

N/A

≤ 0.50 nm 0.50 – 3.0 nm

Cary 100Cary 300

Zero Order ≤ 0.70 nm 0.70 – 1.0 nm

486.0 nm ≤ 0.20 nm 0.20 – 3.0 nm

656.1 nm ≤ 0.20 nm 0.20 – 3.0 nm

Cary 4000Cary 5000Cary 6000i

Zero Order

≤ 0.08 nm

0.08 – 1.0 nm

486.0 nm 0.08 – 3.0 nm

656.1 nm 0.08 – 3.0 nm

Cary 5000Cary 6000i

Zero Order

≤ 0.08 nm

0.08 – 1.0 nm

486.0 nm 0.08 – 3.0 nm

656.1 nm 0.08 – 3.0 nm

1312.2 nm ≤ 0.40 nm 0.04 – 3.0 nm

1968.3 nm ≤ 0.40 nm 0.04 – 3.0 nm

Generic*

541.92 nm

≤ 3.0 nm 0.1 – 3.0 nm486.0 nm

656.1 nm

* Generic test descriptions can be used for non-specified UV-Systems, other than the Agilent Cary and 8453/8454. Please consult your Agilent representative for compatibility questions.

Page 3: UV-VISIBLE SYSTEMS OPERATIONAL QUALIFICATION · This document describes the hardware test specifications for UV-Visible systems performed in the Operational Qualification service

Page 3 of 15

Agilent_Recommended_EQP

© Agilent Technologies, Inc. 2014

Document Released: May 2014 Enterprise Edition Compliance Services

No reproduction, translation, or use without permission

Individual OQ Test Design and Rationale for UV-Vis Systems (continued)

Test 2: Standard on all Systems

Test Name: Wavelength Accuracy – Holmium Oxide in Perchloric Acid

Rationale: Wavelength Accuracy is calculated by comparing the reported wavelength values against the expected wavelength values of a Holmium Oxide in Perchloric Acid test solution (Holmium Perchlorate). The test passes if the reported wavelength values do not differ from the expected values by more than the accuracy limit. This test is applied to all UV-Vis spectrophotometers and meets all major pharmacopoeia and ASTM requirements.

Procedure: Power on and warm up the spectrophotometer for the appropriate time prior to testing. If a cell changer is present disable the cell changer for testing. Using the spectrophotometer’s CDS setup the Wavelength Accuracy test for the Holmium Oxide in Perchloric Acid (Holmium Perchlorate). Perform the test by following the software prompts. When the test is complete record the values to the test record.

Models Set points Allowable range Limits Allowable range

84538454

241.13 nm249.98 nm278.11 nm287.40 nm333.49 nm345.38 nm361.18 nm385.70 nm N/A

≤ 0.6 nm 0.6 – 1.0 nm

416.42 nm451.33 nm467.86 nm485.26 nm536.71 nm640.62 nm

≤ 0.6 nm 0.6 – 3.0 nm

Cary 50Cary 60Cary 100Cary 300Cary 4000Cary 5000Cary 6000iGeneric*

241.15 nm287.15 nm361.5 nm

N/A

≤ 1.0 nm≤ 1.0 nm≤ 1.0 nm

0.1 – 1.0 nm

536.3 nm ≤ 3.0 nm 0.1 – 3.0 nm

* Generic test descriptions can be used for non-specified UV-Systems, other than the Agilent Cary and 8453/8454. Please consult your Agilent representative for compatibility questions.

Page 4: UV-VISIBLE SYSTEMS OPERATIONAL QUALIFICATION · This document describes the hardware test specifications for UV-Visible systems performed in the Operational Qualification service

Page 4 of 15

Agilent_Recommended_EQP

© Agilent Technologies, Inc. 2014

Document Released: May 2014 Enterprise Edition Compliance Services

No reproduction, translation, or use without permission

Individual OQ Test Design and Rationale for UV-Vis Systems (continued)

Test 3: Standard on all Systems

Test Name: Toluene/Hexane Resolution

Rationale: Decreased spectral resolution can impact the photometric sensitivity and selectivity. Toluene /Hexane Resolution is determined by calculating the peak-to-trough ratio between the reported absorbance maximum and minimum from a scan of 0.02 %v/v Toluene in Hexane. The absorbance maximum should occur at approximately 269 and the minimum at approximately 266nm. The test passes if the calculated spectral resolution ratio is greater than or equal to the test limit. This test is applied to all UV-Vis spectrophotometers and meets European Pharmacopoeia requirements.

Procedure: Power on and warm up the spectrophotometer for the appropriate time prior to testing. If a cell changer is present disable the cell changer for testing. Using the spectrophotometer’s CDS setup the Resolution Toluene / Hexane test. Perform the test by following the software prompts. When the test is complete record the values to the test record.

Models Set points Allowable range Limits Allowable range

84538454

N/A N/A

≥ 1.5 1.5 – 2.5

Cary 50Cary 60Cary 100Cary 300Cary 4000Cary 5000Cary 6000iGeneric*

> 1.6 1.6 – 2.5

* Generic test descriptions can be used for non-specified UV-Systems, other than the Agilent Cary and 8453/8454. Please consult your Agilent representative for compatibility questions.

Test 4: Standard on all systems

Test Name: Stray Light – Potassium Chloride

Rationale: The Stray Light Test measures the presence of light outside the bandwidth of a selected wavelength that reaches the detector. The presence of stray light can decrease the photometric selectivity, increase the photometric response and create non-linear response of the instrument causing problems with quantitative analysis. Potassium Chloride will completely absorb light below 200nm, however is transparent above 200nm. The test will pass if the Percent Transmittance is less than 1.0% at 198nm. This test is applied to all UV-Vis spectrophotometers and meets all major pharmacopoeia and ASTM requirements.

Procedure: Power on and warm up the spectrophotometer for the appropriate time prior to testing. If a cell changer is present disable the cell changer for testing. Using the spectrophotometer’s CDS setup the Stray Light – Potassium Chloride test. Perform the test by following the software prompts. When the test is complete record the values to the test record.

Models Set points Allowable range Limits Allowable range

All 198 nm 190 – 200 nm ≥ 0.0 – < 1.0%T N/A

Page 5: UV-VISIBLE SYSTEMS OPERATIONAL QUALIFICATION · This document describes the hardware test specifications for UV-Visible systems performed in the Operational Qualification service

Page 5 of 15

Agilent_Recommended_EQP

© Agilent Technologies, Inc. 2014

Document Released: May 2014 Enterprise Edition Compliance Services

No reproduction, translation, or use without permission

Individual OQ Test Design and Rationale for UV-Vis Systems (continued)

Test 5: Standard on all systems

Test Name: Photometric Accuracy – Potassium Dichromate

Rationale: The Photometric Accuracy - Potassium Dichromate Test uses two strengths of the Potassium Dichromate standard

Firstly the 60mg/L Potassium Dichromate standard is used to measure the difference between the expected absorbance values (listed on the Certificate of Analysis) and the actual absorbance values reported by the instrument at four wavelengths: 235nm, 257nm, 313nm, and 350nm. The test passes if the expected absorbance values are within +/- 0.010 AU of the actual absorbance values at the four wavelengths.

Then the 600mg/L Potassium Dichromate standard is used to measure the difference between the expected absorbance value (listed on the Certificate of Analysis) and the actual absorbance value reported by the instrument at 430nm. The test passes if the expected absorbance value is within +/- 0.012 AU of the actual absorbance value at 430nm. This test is applied to all UV-Vis spectrophotometers and meets all major pharmacopoeia, ASTM, and NIST requirements.

Procedure: Power on and warm up the spectrophotometer for the appropriate time prior to testing. If a cell changer is present disable the cell changer for testing. Using the spectrophotometer’s CDS setup the Photometric Accuracy – Potassium Dichromate test for both the 60mg/L and 600mg/L standard concentrations. Perform the test by following the software prompts. When the test is complete record the values to the test record.

Models Set points Allowable range Limits Allowable range

All

235 nm

N/A

≤ 0.010 Abs

N/A

257 nm ≤ 0.010 Abs

313 nm ≤ 0.010 Abs

350 nm ≤ 0.010 Abs

430 nm ≤ 0.012 Abs

Page 6: UV-VISIBLE SYSTEMS OPERATIONAL QUALIFICATION · This document describes the hardware test specifications for UV-Visible systems performed in the Operational Qualification service

Page 6 of 15

Agilent_Recommended_EQP

© Agilent Technologies, Inc. 2014

Document Released: May 2014 Enterprise Edition Compliance Services

No reproduction, translation, or use without permission

Individual OQ Test Design and Rationale for UV-Vis Systems (continued)

Test 6: Standard for 8453/8454; Optional for Cary / Generic systems

Test Name: Stray Light – Sodium Iodide

Rationale: The Stray Light test measures the presence of light outside the bandwidth of a selected wavelength that reaches the detector. The presence of stray light can decrease the photometric selectivity, increase the photometric response and create non-linear response of the instrument causing problems with quantitative analysis.

This Stray Light test uses Sodium Iodide as the filter to measure the stray light. Sodium Iodide will begin to absorb light below 260nm, however is transparent above 260nm. The test will pass if the Percent Transmittance is less than the test limit.

This test is applied as a standard test for the 8453 and 8454 UV-Vis spectrophotometers and meets ASTM requirements.

This test can be added to the protocol for Cary and Generic UV-Vis spectrophotometers models and meets ASTM requirements.

Procedure: Power on and warm up the spectrophotometer for the appropriate time prior to testing. If a cell changer is present disable the cell changer for testing. Using the spectrophotometer’s CDS setup the Stray Light – NaI (Sodium Iodide) at 220nm test. Perform the test by following the software prompts. When the test is complete record the values to the test record.

Models Set points Allowable range Limits Allowable range

84538454 220 nm 200 – 230 nm ≥ 0.0 – < 0.05 %T 0.0 – 0.50 %T

Cary 50Cary 60

220 nm 200 – 230 nm

≥ 0.0 – < 0.05 %T 0.0 – 0.50 %T

Cary 100 ≥ 0.0 – < 0.02 %T 0.0 – 0.20 %T

Cary 300 ≥ 0.0 – < 0.0005 %T 0.0 – 0.0050 %T

Cary 4000Cary 5000Cary 6000i

≥ 0.0 – < 0.00007 %T 0.0 – 0.00070 %T

Generic* ≥ 0.0 – < 0.05 %T 0.0 – 0.50 %T

* Generic test descriptions can be used for non-specified UV-Systems, other than the Agilent Cary and 8453/8454. Please consult your Agilent representative for compatibility questions.

Page 7: UV-VISIBLE SYSTEMS OPERATIONAL QUALIFICATION · This document describes the hardware test specifications for UV-Visible systems performed in the Operational Qualification service

Page 7 of 15

Agilent_Recommended_EQP

© Agilent Technologies, Inc. 2014

Document Released: May 2014 Enterprise Edition Compliance Services

No reproduction, translation, or use without permission

Individual OQ Test Design and Rationale for UV-Vis Systems (continued)

Test 7: Standard for 8453/8454; Optional for Cary / Generic systems

Test Name: Stray Light – Sodium Nitrite

Rationale: The Stray Light test measures the presence of light outside the bandwidth of a selected wavelength that reaches the detector. The presence of stray light can decrease the photometric selectivity, increase the photometric response and create non-linear response of the instrument causing problems with quantitative analysis.

This Stray Light test uses Sodium Nitrite as the filter to measure the stray light. Sodium Nitrite will begin to absorb light below 385 nm, however is transparent above 385 nm. The test will pass if the Percent Transmittance is less than the test limit.

This test is applied as a standard test for the 8453 and 8454 UV-Vis spectrophotometers and meets ASTM requirements.

This test can be added to the protocol for Cary or Generic UV-Vis spectrophotometers models and meets ASTM requirements.

Procedure: Power on and warm up the spectrophotometer for the appropriate time prior to testing. If a cell changer is present disable the cell changer for testing. Using the spectrophotometer’s CDS setup the Stray Light – NaNO2 (Sodium Nitrite) at 340 nm test. Perform the test by following the software prompts. When the test is complete record the values to the test record.

Models Set points Allowable range Limits Allowable range

84538454 340 nm 340 – 390 nm ≥ 0.0 – < 0.03 %T 0.0 – 0.30 %T

Cary 50Cary 60

340 nm 340 – 390 nm

≥ 0.0 – < 0.05 %T 0.0 – 0.50 %T

Cary 100 ≥ 0.0 – < 0.005 %T 0.0 – 0.050 %T

Cary 300 ≥ 0.0 – < 0.0002 %T 0.0 – 0.0020 %T

Cary 4000Cary 5000Cary 6000i

≥ 0.0 – < 0.00007 %T 0.0 – 0.00070 %T

Generic* ≥ 0.0 – < 0.05 %T 0.0 – 0.50 %T

* Generic test descriptions can be used for non-specified UV-Systems, other than the Agilent Cary and 8453/8454. Please consult your Agilent representative for compatibility questions.

Page 8: UV-VISIBLE SYSTEMS OPERATIONAL QUALIFICATION · This document describes the hardware test specifications for UV-Visible systems performed in the Operational Qualification service

Page 8 of 15

Agilent_Recommended_EQP

© Agilent Technologies, Inc. 2014

Document Released: May 2014 Enterprise Edition Compliance Services

No reproduction, translation, or use without permission

Individual OQ Test Design and Rationale for UV-Vis Systems (continued)

Test 8: Standard for 8453/8454; Optional for Cary / Generic systems

Test Name: Wavelength Reproducibility – Holmium Oxide in Perchloric Acid

Rationale: The Wavelength Reproducibility test measures the instrument’s reproducibility when making repeated readings of the same wavelength. The reproducibility is defined as the deviation of 10 consecutive wavelength maximum readings taken using the peak(s) of the reference – either the deuterium lamp or the Holmium Oxide in Perchloric Acid standard. The test passes if the maximum deviation of the 10 wavelength maxima values is less than the test limit.

This test is applied as a standard test for the 8453 and 8454 UV-Vis spectrophotometers and meets the requirements of NIST and ASTM. For the 8453 and 8454 spectrophotometer models, this test is completed together with the Wavelength Accuracy tests.

This test can be added to the protocol for Cary or Generic UV-Vis spectrophotometers and meets the requirements of NIST and ASTM.

Procedure: Power on and warm up the spectrophotometer for the appropriate time prior to testing. If a cell changer is present disable the cell changer for testing. Using the spectrophotometer’s CDS setup the Wavelength Accuracy test for the Holmium Oxide in Perchloric Acid (Holmium Perchlorate). Perform the test by following the software prompts. When the test is complete record the values to the test record.

Models Set points Allowable range Limits Allowable range

84538454

8454

N/A –0.02 – 0.02 nm –0.04 – 0.04 nm

656.10 nm

241.13 nm

249.98 nm

278.11 nm

287.40 nm

333.49 nm

345.38 nm

361.18 nm

385.70 nm

416.42 nm

451.33 nm

467.86 nm

485.26 nm

536.71 nm

640.62 nm

Cary 50Cary 60 536.50 nm

N/A

–0.1 – 0.1 nm –0.2 – 0.2 nm

Cary 100Cary 300Generic*

656.10 nm –0.08 – 0.08 nm –0.16 – 0.16 nm

Cary 4000Cary 5000Cary 6000i

656.10 nm –0.025 – 0.025 nm –0.050 – 0.050 nm

* Generic test descriptions can be used for non-specified UV-Systems, other than the Agilent Cary and 8453/8454. Please consult your Agilent representative for compatibility questions.

Page 9: UV-VISIBLE SYSTEMS OPERATIONAL QUALIFICATION · This document describes the hardware test specifications for UV-Visible systems performed in the Operational Qualification service

Page 9 of 15

Agilent_Recommended_EQP

© Agilent Technologies, Inc. 2014

Document Released: May 2014 Enterprise Edition Compliance Services

No reproduction, translation, or use without permission

Individual OQ Test Design and Rationale for UV-Vis Systems (continued)

Test 9: Standard for 8453/8454; Optional for Cary / Generic systems

Test Name: Photometric Noise

Rationale: Photometric noise measures short-term fluctuations in the detector signal caused by inherent optical and electronic noise. The amount of photometric noise will define the precision and minimum detection limit of the spectrophotometer. The test passes if the measured photometric noise is within the test limits.

This test is applied as a standard test for the 8453 and 8454 UV-Vis spectrophotometers with limits that conform to manufacturer requirements.

This test can be added to the protocol for Cary and Generic UV-Vis spectrophotometers with limits that conform to manufacturer requirements.

Procedure: Power on and warm up the spectrophotometer for the appropriate time prior to testing. If a cell changer is present disable the cell changer for testing. Verify there are no samples in the cell holders. Using the spectrophotometer’s CDS setup the Photometric Noise test. Perform the test by following the software prompts. When the test is complete record the values to the test record.

Models Set points Allowable range Limits Allowable range

84538454 0 Abs at 500 nm N/A < 0.00020 Abs, rms 0.000020 – 0.00200 Abs, rms

Cary 50Cary 60

0 Abs at 500 nm

N/A

< 0.00010 Abs, rms 0.00010 – 0.00100 Abs, rms

Generic* < 0.00010 Abs, rms 0.00010 – 0.00100 Abs, rms

Cary 100 < 0.000085 Abs, rms 0.000085 – 0.000850 Abs, rms

Cary 300 < 0.00006 Abs, rms 0.00006 – 0.00060 Abs, rms

Cary 4000Cary 5000Cary 6000i

< 0.00003 Abs, rms 0.00003 – 0.00030 Abs, rms

Cary 5000 0 Abs at 1500 nm < 0.00003 Abs, rms 0.00003 – 0.00030 Abs, rms

Cary 6000i 0 Abs at 1500 nm < 0.00002 Abs, rms 0.00002 – 0.00020 Abs, rms

* Generic test descriptions can be used for non-specified UV-Systems, other than the Agilent Cary and 8453/8454. Please consult your Agilent representative for compatibility questions.

Page 10: UV-VISIBLE SYSTEMS OPERATIONAL QUALIFICATION · This document describes the hardware test specifications for UV-Visible systems performed in the Operational Qualification service

Page 10 of 15

Agilent_Recommended_EQP

© Agilent Technologies, Inc. 2014

Document Released: May 2014 Enterprise Edition Compliance Services

No reproduction, translation, or use without permission

Individual OQ Test Design and Rationale for UV-Vis Systems (continued)

Test 10: Standard for 8453/8454; Optional for Cary / Generic systems

Test Name: Baseline Flatness

Rationale: Baseline Flatness measures the instrument’s ability to compensate for inherent optical and electronic noise across the entire wavelength range. A baseline correction and test scan are performed across the entire wavelength range of the instrument. The corrected signal is evaluated for peak-to-peak fluctuations. The test passes if the measured baseline stability is within test limits.

This test is applied as a standard test for the 8453 and 8454 UV-Vis spectrophotometers with limits that conform to manufacturer requirements.

This test can be added to the protocol for Cary or Generic UV-Vis spectrophotometers with limits that conform to manufacturer requirements.

Procedure: Power on and warm up the spectrophotometer for the appropriate time prior to testing. If a cell changer is present disable the cell changer for testing. Verify there are no samples in the cell holders. Using the spectrophotometer’s CDS setup the Baseline Flatness test. Perform the test by following the software prompts. When the test is complete record the values to the test record.

Models Set points Allowable range Limits Allowable range

84538454

0 Abs(190 – 1100nm) N/A –0.00100 – 0.00100 Abs –0.01000 – 0.01000 Abs

Cary 50Cary 60Cary 100Cary 300Generic*

0 Abs(200 – 850 nm)

N/A

–0.001 – 0.001 Abs –0.010 – 0.010 Abs

Cary 4000 0 Abs (200 – 850 nm) –0.0012 – 0.0012 Abs –0.0120 – 0.0120 Abs

Cary 5000 0 Abs (200 – 3000 nm) –0.0012 – 0.0012 Abs –0.0120 – 0.0120 Abs

Cary 6000i 0 Abs (200 – 1700 nm) –0.0012 – 0.0012 Abs –0.0120 – 0.0120 Abs

* Generic test descriptions can be used for non-specified UV-Systems, other than the Agilent Cary and 8453/8454. Please consult your Agilent representative for compatibility questions.

Page 11: UV-VISIBLE SYSTEMS OPERATIONAL QUALIFICATION · This document describes the hardware test specifications for UV-Visible systems performed in the Operational Qualification service

Page 11 of 15

Agilent_Recommended_EQP

© Agilent Technologies, Inc. 2014

Document Released: May 2014 Enterprise Edition Compliance Services

No reproduction, translation, or use without permission

Individual OQ Test Design and Rationale for UV-Vis Systems (continued)

Test 11: Standard for 8453/8454; Optional for Cary / Generic systems

Test Name: Photometric Stability

Rationale: Photometric Stability measures the photometric drift of the spectrophotometer when monitoring the Zero Absorbance signal at a single wavelength for an hour. Photometric Stability is an indicator of how stable photometric results will be over an extended period of time. The test passes if the measured drift of the photometric stability is within test limits.

This test is applied as a standard test for the 8453 and 8454 UV-Vis with limits that conform to manufacturer requirements.

This test can be added to the protocol for Cary or Generic UV-Vis spectrophotometers if Photometric Stability is a local requirement.

Procedure: Power on and warm up the spectrophotometer for the appropriate time prior to testing. If a cell changer is present disable the cell changer for testing. Verify there are no samples in the cell holders. Using the spectrophotometer’s CDS setup the Photometric Stability test. Perform the test by following the software prompts. When the test is complete record the values to the test record.

Models Set points Allowable range Limits Allowable range

84538454 0 Abs at 340 nm N/A –0.00100 – 0.00100 Abs/hr –0.01000 – 0.01000 Abs/hr

Cary 50Cary 60 0 Abs at 500 nm

N/A

–0.0004 – 0.0004 Abs/hr –0.0040 – 0.00400 Abs/hr

Cary 100Cary 300 0 Abs at 500 nm –0.0003 – 0.0003 Abs/hr –0.0030 – 0.00300 Abs/hr

Cary 4000Cary 5000Cary 6000i

0 Abs at 500 nm –0.00018 – 0.00018 Abs/hr –0.00180 – 0.00180 Abs/hr

Generic* 0 Abs at 340 nm –0.00100 – 0.00100 Abs/hr –0.01000 – 0.01000 Abs/hr

* Generic test descriptions can be used for non-specified UV-Systems, other than the Agilent Cary and 8453/8454. Please consult your Agilent representative for compatibility questions.

Page 12: UV-VISIBLE SYSTEMS OPERATIONAL QUALIFICATION · This document describes the hardware test specifications for UV-Visible systems performed in the Operational Qualification service

Page 12 of 15

Agilent_Recommended_EQP

© Agilent Technologies, Inc. 2014

Document Released: May 2014 Enterprise Edition Compliance Services

No reproduction, translation, or use without permission

Individual OQ Test Design and Rationale for UV-Vis Systems (continued)

Test 12: Optional for all systems

Test Name: Photometric Accuracy – NIST Glass Filters

Rationale: The Photometric Accuracy – NIST Glass Filters test uses certified glass filter standard reference materials to measure the difference between the expected absorbance value (listed on the Certificate of Analysis) and the actual absorbance value reported by the instrument at various wavelengths. The Test passes if the expected absorbance value is within the test limit of the expected absorbance value.

This test can be added to the protocol for all UV-Vis spectrophotometers and meets all major pharmacopoeia, ASTM, and NIST requirements.

Procedure: Power on and warm up the spectrophotometer for the appropriate time prior to testing. If a cell changer is present disable the cell changer for testing. Using the spectrophotometer’s CDS setup the Photometric Accuracy – NIST test using the glass filter standard reference material. Perform the test by following the software prompts. When the test is complete record the values to the test record.

Models Set points Allowable range Limits Allowable range

84538454Generic*

1 Abs at 440.0 nm1 Abs at 465.0 nm1 Abs at 546.1 nm1 Abs at 590.0 nm1 Abs at 635.0 nm

N/A ≤ 0.0050 Abs N/A

Cary 50Cary 60Cary 100Cary 300Cary 4000Cary 5000Cary 6000i

1 Abs at 440.0 nm1 Abs at 465.0 nm1 Abs at 546.1 nm1 Abs at 590.0 nm1 Abs at 635.0 nm

N/A ≤ 0.0050 Abs N/A

0.7 Abs at 440.0 nm0.7 Abs at 465.0 nm0.7 Abs at 546.1 nm0.7 Abs at 590.0 nm0.7 Abs at 635.0 nm

N/A ≤ 0.0040 Abs N/A

0.5 Abs at 440.0 nm0.5 Abs at 465.0 nm0.5 Abs at 546.1 nm0.5 Abs at 590.0 nm0.5 Abs at 635.0 nm

N/A ≤ 0.0030 Abs N/A

* Generic test descriptions can be used for non-specified UV-Systems, other than the Agilent Cary and 8453/8454. Please consult your Agilent representative for compatibility questions.

Page 13: UV-VISIBLE SYSTEMS OPERATIONAL QUALIFICATION · This document describes the hardware test specifications for UV-Visible systems performed in the Operational Qualification service

Page 13 of 15

Agilent_Recommended_EQP

© Agilent Technologies, Inc. 2014

Document Released: May 2014 Enterprise Edition Compliance Services

No reproduction, translation, or use without permission

Individual OQ Test Design and Rationale for UV-Vis Systems (continued)

Test 13 – Optional for Cary / Generic systems

Test Name: Wavelength Accuracy – Mercury Line

Rationale for Cary / Generic: Wavelength Accuracy is performed as a verification of the mercury lamp performance. The mercury lamp produces photometric peak maxima at various wavelengths. In this test, Wavelength Accuracy is verified by scanning a wavelength range for the mercury lamp. The test passes if the reported wavelength maxima do not differ from the expected values by more than the accuracy limit. This test can be added to the protocol for only to UV-Vis spectrophotometers that have a mercury lamp installed and meets all major pharmacopeia requirements.

Procedure for Cary / Generic: Power on and warm up the spectrophotometer for the appropriate time prior to testing. If a cell changer is present disable the cell changer for testing. Verify there are no samples in the reference and sample cell holders. Using the spectrophotometer’s controlling data software (CDS) setup the Wavelength Accuracy test for the Mercury Lamp. Perform the test by following the software prompts. When the test is complete record the values to the test record.

Models Set points Allowable range Limits Allowable range

Cary 4000Cary 5000Cary 6000i

253.65 nm312.57 nm313.16 nm334.15 nm365.48 nm

N/A ≤ 0.10 nm

0.10 – 1 nm

404.66 nm435.83 nm546.08 nm576.96 nm579.07 nm

0.10 – 3 nm

Generic*

253.65 nm312.57 nm313.16 nm334.15 nm365.48 nm

N/A

≤ 1 nm 0.10 – 1 nm

404.66 nm435.83 nm546.08 nm576.96 nm579.07 nm

≤ 3 nm 0.10 – 3 nm

* Generic test descriptions can be used for non-specified UV-Systems, other than the Agilent Cary and 8453/8454. Please consult your Agilent representative for compatibility questions.

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Agilent_Recommended_EQP

© Agilent Technologies, Inc. 2014

Document Released: May 2014 Enterprise Edition Compliance Services

No reproduction, translation, or use without permission

Individual OQ Test Design and Rationale for UV-Vis Systems (continued)

Test 14: Optional for all systems

Photometric Reproducibility – Potassium Dichromate

Rationale: The Photometric Reproducibility - Potassium Dichromate test uses two strengths of the Potassium Dichromate standard to find the reproducibility of the photometric measurement.

The 60mg/L Potassium Dichromate standard is used to measure the absorbance at four wavelengths: 235nm, 257nm, 313nm, and 350nm. Ten measurements are taken at each respective wavelength. The standard deviation is then calculated for each respective wavelength. The test passes if the calculated standard deviation of each set of measurements is within the test limits.

The 600mg/L Potassium Dichromate standard is used to measure the absorbance at 430nm. Ten measurements are taken at each respective wavelength. The standard deviation is then calculated for each respective wavelength. The test passes if the calculated standard deviation of each set of measurements is within the test limits.

This test can be added to the protocol for all UV-Vis spectrophotometers.

Procedure: Power on and warm up the spectrophotometer for the appropriate time prior to testing. If a cell changer is present disable the cell changer for testing. Using the spectrophotometer’s CDS setup the Photometric Accuracy – Potassium Dichromate test for both the 60mg/L and 600mg/L standard concentrations. Follow the software prompts to complete the test. Perform the test 10 times to obtain values for reproducibility at each wavelength. When the test is complete record the values to the test record.

Models Set points Allowable range Limits Allowable range

All

235 nm257 nm313 nm350 nm430 nm

N/A 0.000 – 0.005 Abs 0.000 – 0.010 Abs

Test 15: Optional for Cary systems

Test Name: Maximum Resolution

Rationale for Cary systems: Maximum Resolution (often called the ‘limiting’ resolution) of the instrument is determined by calculating the width of the 656.1 nm peak at half height that the instrument can achieve. The test passes if the calculated maximum resolution is less than or equal to the test limit. This test can be added to the protocol for the Cary 4000, Cary 5000 and Cary 6000i UV-Vis spectrophotometers only.

Procedure: Power on and warm up the spectrophotometer for the appropriate time prior to testing. If a cell changer is present disable the cell changer for testing. Verify there are no samples in the cell holders. Using the spectrophotometer’s CDS setup the Maximum Resolution. Perform the test by following the software prompts. When the test is complete record the values to the test record.

Models Set points Allowable range Limits Allowable range

Cary 4000Cary 5000Cary 6000i

N/A N/A 0.000 – 0.048 0.000 – 0.096

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Page 15 of 15

Agilent_Recommended_EQP Enterprise Edition Compliance ServicesDocument Released: May 2014

Information, descriptions and specifications in thispublication are subject to change without notice.

© Agilent Technologies, Inc. 2014Published in USA, May 29, 2014

www.agilent.com/chem/enterprise

Individual OQ Test Design and Rationale for UV-Vis Systems (continued)

Test 16: Optional for Cary systems

Test Name: Photometric Reproducibility – NIST Glass Filters

Rationale for Cary systems: The Photometric Reproducibility – NIST Glass Filters test uses certified glass filter standard reference materials to find the reproducibility of the photometric measurement.

The 30 %T glass filter NIST standard is used to take ten measurements at the absorbance at the 546.1 nm wavelength. The standard deviation is then calculated. The test passes if the calculated standard deviation is within the test limits. This test can be added to the protocol for the Agilent Technologies Cary UV-Vis spectrophotometer models.

Procedure: Power on and warm up the spectrophotometer for the appropriate time prior to testing. If a cell changer is present disable the cell changer for testing. Using the spectrophotometer’s CDS setup the Photometric Accuracy – NIST test for the 30 %T standard. Follow the software prompts to complete the test. Perform the test 10 times to obtain values for reproducibility at the 546.1 nm wavelength. When the test is complete record the values to the test record.

Models Set points Allowable range Limits Allowable range

Cary 50Cary 60

0.5 Abs at 546.1 nm N/A

0.0000 – 0.0030 Abs 0.0000 – 0.0300 Abs

Cary 100Cary 300Cary 4000Cary 5000Cary 6000i

0.00000 – 0.00008 Abs 0.00000 – 0.00080 Abs

Protocol Revision: UV.01.04Document Released: May 2014