New 1100 Series DAD SL and MWD SL 80Hz Data Acquisition for Ultra-fast LC.

New 1100 Series DAD SL and MWD SL

80Hz Data Acquisition for Ultra-fast LC

2

1100 Series DAD SL and MWD SL

Agilent 1100 Series Diode-array Detector SL Agilent 1100 Series Multi-wavelength Detector SL

The 1st Diode-array Detector designed for Ultra-fast LC

3

1100 Series DAD SL and MWD SLOverview

Next Generation Electronics and Firmware provides

80Hz Data Acquisition of up to 8 Signals Up to 100% resolution gain in ultra-fast,

quantitative LC 80Hz Full Spectral Data Acquisition (DAD SL only)

for ultra-fast peak purity analysis and spectral conformation even for trace level compounds

Improved Diode-Array Front-end Electronics for minimized noise (typical < +/- 6μAU

ASTM) New Build-in Data Recovery Card

for a „data never lost insurance“ New RFID Tags for all Flow Cells and UV Lamp

for unambiguous data traceability LAN on Board

eliminates need for additional LAN interface Future proof design

Build-in web-server, USB, PCMCIA (WLAN, Bluetooth)

4

1100 Series DAD SL and MWD SLOverview (cont’d)

New Electronic Temperature Control (ETC) For maximum practical sensitivity by

minimized baseline wander, especially under harsh and fluctuating ambient temperature and humidity conditions

New standard flow cell for maximum practical sensitivity by

minimized RI-sensitivity and dispersion

Builds upon 1100 DAD Optical Design preserves features like programmable slit

and dual lamp design for highest sensitivity from 190 to 950nm

Up to 20x Sensitivity from 400 – 950nm

+ 40% (+ 80%) Sensitivity by 8 and 16nm slit

Re-use spectral libraries of 1100 DAD „A“ and „B“

Confidence and robustness of a diode-array detector with more than 25,000 installations.

5

What is Ultra-fast LC?

What is the Objective of Ultra-fast LC?

1.Significant gains in productivity, while maintaining or increasing data quality

• Ultra-fast LC provides up to 10x gains in analysis speed while preserving or increasing Resolution, Sensitivity, Linearity, Precision and Robustness.

• Thereby, Ultra-fast LC ensures compliance with strictest (regulatory) performance requirements.

2. Uncompromised compatibility with existing methods.

• Run conventional LC methods without compromising performance

• Comply with today’s and future requirements

3. Improved Data Security.

• Ultra-fast LC systems provide a new level of data security and traceability that prevents data losses and minimizes the risk of false data interpretation.

6

• Conventional LC: Analysis Times = 5.0 – 120 min

• Fast LC: Analysis Times = 2.0 – 5.0 min

• Ultra-fast LC: Analysis Times = 0.2– 2.0 min

Gradient Time = 0.2 – 1.5 min

Cycle Times = 0.5 – 2.5 min

50% Peak Width = 0.1– 1.0 sec

PW = 0.3 sec

min0.1 0.2 0.3 0.4 0.50

How fast is Ultra-fast?


7

Which 1100 Configuration do I need for Ultra-fast LC?

1100 Series Ultra-fast LC System

• 1100 Series Binary Pump – for precise, high-pressure mixing gradient formation and low delay volume

• 1100 Series WPS – for precise, high-speed injection with lowest delay volume and carry over

• 1100 Series TCC – for precise, peltier-controlled high-temperature LC up to 80C

• 1100 Series DAD/MWD SL – for highest chromatographic resolution by 80Hz data rate

• Zorbax RRHT 1.8um Columns – for highest efficiency at high linear flows


8

min0.1 0.2 0.3 0.4 0.50

80Hz

PW=0.30sec

40Hz

PW=0.33sec

20Hz

PW=0.42sec

10Hz

PW=0.67sec

5HzPW=1.24sec

• Sample: Phenone Test Mix• Column: Zorbax SB-C18, 4.6x30,

1.8um• Gradient: 50-100% ACN in 0.3min• Flow cell: 5ul

80Hz versus 20Hz– 30% Peak Width+ 30% Resolution + 40% Peak Capacity+ 70% Apparent Column Efficiency

80Hz versus 10Hz– 55% Peak Width+ 90% Resolution+ 120% Peak Capacity+ 260% Apparent Column

Efficiency

What’s the Benefit of 80Hz Data Acquisition Rate?

Peak Width, Resolution and Peak Capacity in Ultra-Fast LC

9

80Hz versus 20Hz Data Rate:– 30% Peak Width=> +40% Peak Capacity+30% Resolution => + 70% Apparent

Column Efficiency

80Hz versus 10Hz Data Rate:– 55% Peak Width => +120% Peak Capacity+90% Resolution => +260%

Apparent Column Efficiency

Data Rate

Peak Width

Resolution

Peak Capacity

80 Hz

0.300 2.25 61

40 Hz

0.329 2.05 56

20 Hz

0.416 1.71 44

10 Hz

0.666 1.17 28

5 Hz 1.236 0.67 16

0.2

0.4

0.6

0.8

1

1.2

1.4

0 20 40 60 80 100

Data Rate [Hz]

Peak

Wid

ths

/ se

c

0

10

20

30

40

50

60

70

Peak

Cap

acity

Peak Width [s]

Peak Capacity

0.2

0.4

0.6

0.8

1

1.2

1.4

0 20 40 60 80 100

Data Rate [Hz]

Peak

Wid

ths

/ se

c

0

0.5

1

1.5

2

2.5

Reso

lutio

n

Peak Width [s]

Resolution (4,5)

What’s the Benefit of 80Hz Data Acquisition Rate?

Peak Width, Resolution and Peak Capacity in Ultra-Fast LC

10

Performance Requirements of Ultra-Fast LC

Ultra-fast LC using the 1100 DAD SL provides Resolution and Peak Capacity gains of up to 100%.

But – Can I still fulfill my (regulatory) performance requirements under ultra-fast LC conditions?

• Quantification of Side Products at 0.05% level ?

• RT Precision < 0.5% ?

• Area Precision < 1% ?

• Peak Purity Analysis at Trace Levels ?

• Spectral Conformation at Trace Levels ?

11

Sensitivity and Linearity in Ultra-Fast LC Can I Simultaneously Quantity Main Compounds and Side

Products at 0.05% Level?

min0.5 1 1.5 2 2.5

mAU

0

500

1000

1500

2000

Main Compound = 2000mAU

Impurities = 1mAU

DMSO

Impurities

Is the detectors Dynamic Range large enough to accurately and precisely quantify Main

Compound and Impurities simultaneously?

12

Sensitivity and Linearity in Ultra-Fast LC

Is the Noise Low Enough for my Quantitative Analysis?

ASTM Noise Specification:20 µAU Peak-to-Peak (+/- 10 µAU)

4nm Slit

8nm Slit

16nm Slit

80 Hz

42 31 23

40 Hz

30 22 16

20 Hz

21 16 11

10 Hz

15 11 8.0

2.5 Hz

7.4 5.4 4.0

• Temperature: 20C• DAD: 254nm,16nm, Ref 360,

80nm • PW: > 0.1min (2.5Hz, 2sec RT)

min5 10 15 20

mAU

-0.04-0.03-0.02-0.01

0

min5 10 15 20

mAU

-0.1-0.08-0.06-0.04-0.02

Conditions• Eluent: Water/ACN = 70/30• Flow rate: 1ml/min• Column: 4.6x30mm SB C18,

1.8um

min5 10 15 20

mAU

-0.06

-0.04

-0.02

0 4nm Slit widthNoise < +/– 3.7 µAU

8nm Slit widthNoise < +/– 2.7 µAU

16nm Slit widthNoise < +/– 2.0 µAU

Peak-to-Peak Noise on 13ul Flow Cell

– 27% – 26%

Note: 50µAU Noise gives S/N = 20 at 1mAU (0.05% level)

13


Is the Linear Range Large Enough for my Quantitative Analysis?

Linearity (Caffeine Sample):

Deviation at 2.0AU:

• 2.0% (Vis Lamp off)

• 2.5% (Vis Lamp on)

5% Deviation:

• 2.5 AU (Vis Lamp off)

• 2.4 AU (Vis Lamp off)

Specification:

• 5% Deviation at 2.0 AU

80.0%

85.0%

90.0%

95.0%

100.0%

105.0%

0 500 1000 1500 2000 2500 3000

Absorbance / mAU

% D

evia

tion

from

Lin

ear V

alue

Vis Lamp off

Vis Lamp on

14

•Gradient: 50–70% B in 0.85min

•Column: 4.6 x 50, 1.8um•Injection: 5ul of

550 µg/ml Nimodipin•Flow Rate: 4 ml/min•Flow cell: 13ul•Data Rate: 80Hz•Slit: 8nm

mAU

1800

1850

1900

1950

2000

0.6

28

0.6

27

0.6

27

0.6

27

0.6

27

0.6

27

0.6

27

0.6

28

0.6

27

0.6

27

min0.6250.6250.6260.6260.6270.6270.6280.6280.6291750

Overlay of 10 analyses at 245nm

• RT Precision: 0.067% RSD

• Area Precision: 0.13% RSD


Reproducibility of Main Compounds at 2000mAU (100% Level)

min0.61 0.62 0.63 0.64 0.65 0.66 0.67

mAU

0

250

500

750

1000

1250

1500

1750

2000

Peak Width

0.70 sec

15

min0.2 0.25 0.3 0.35 0.4 0.45 0.5 0.55

mAU

0

1

2

3

4

5

6


Reproducibility of Impurities and Side Products at Trace Level

Overlay of 10 analyses at 245 nm:

Nifedipin • A = 2.5mAU (0.1%

level)• RT Precision =

0.092% RSDNifedipin degradation

product • A = 0.5mAU (0.03%

level)• RT Precision =

0.123% RSD

•Column: 4.6 x 50, 1.8um

•Gradient: 50–70% B in 0.85 min

•Injection: 5ul•Flow Rate: 4 ml/min•Flow cell: 13ul•Data Rate: 80Hz•Slit: 8nm

16

Nifedipin at trace levelsPeak Width = 0.63 sec

min0.3 0.31 0.32 0.33

mAU

0

0.5

1

1.5

22mAU = 0.1%

levelS/N = 50

1mAU = 0.05% level

S/N = 25

0.5mAU = 0.025% level

S/N = 12

Conditions:•Column: 4.6 x 50, 1.8um• Gradient: 50–70% B in 0.85 min• Injection: 5ul• Flow Rate: 4 ml/min• Flow cell: 13ul • Data Rate: 80Hz• Slit: 8nm

Result:Under ultra-fast LC conditions the DAD SL allows accurate quantitation of impurities and side products at levels smaller than 0.05% of the main compound(s).


Can I quantity Impurities and Side Products at 0.05% Level?

Noise 40 µAU

17

Apex Spectrum of Nifedipin at 0.1% (1.8 mAU) measured at 80 Hz:

nm300 400 500 600 700 800

mAU

0

0.5

1.0

1.5

nm300 400 500 600 700 800

mAU

0

400

800

1200

Reference Spectrum of Nifedipin at 100% level (1800 mAU) measured at 80 Hz:

Spectral Analysis in Ultra-Fast LCCan I do Peak Purity and Spectral Conformation at

Trace Levels?

Is the spectral quality obtained at trace level under ultra-fast LC conditions and 80Hz spectral sampling rate good enough for peak purity analysis and spectral conformation?

18

UV Spectrum of Nifedipin at higher concentration (ca. x180):

Spectral Analysis in Ultra-Fast LCCan I do 80Hz Peak Purity Analysis at Trace Levels?

min1.6 1.7 1.8 1.9 2

Norm.

6

8

10

12

14

DAD1 A, Sig=245,10 Ref=500,80 (N:\BACKUP_MSD\DATA_MRZ\MF_180305_STD_A_ALL\NIMIX_1_2000_1_G_05.D)

1.6

29

2.0

26

nm300 400 500 600 700 800 900

Fl

-0.25

0

0.25

0.5

0.75

1

1.25

1.5

1.75

mAU

Overlay of extracted Nifedipin spectra at trace level

Result: Nifedipin peak at 0.1% level (1.8mAU) measured with 80Hz spectral rate is pure

– no other compounds are co-eluting with Nifedipin

19

nm300 400 500 600 700 800 900

Norm

0

0.25

0.5

0.75

1

1.25

1.5

1.75

2

nm300 400 500 600 700 800 900

Norm

0

0.25

0.5

0.75

1

1.25

1.5

1.75

2Overlay of 80Hz Reference and Apex Spectrum

•Nifedipin Ref: 1800mAU (100% level)

•Nifedipin Apex: 1.8mAU (0.1% level)

Spectral Analysis in Ultra-Fast LCCan I do 80Hz Spectral Conformation at Trace Levels?

Overlay of 80Hz Reference and Apex Spectrum

•Nimodipin Ref: 1800mAU (100% level)

•Nifedipin Apex: 1.8mAU (0.1% level)

Result:

Identification of Nifedipin at 0.1% trace level under fast LC conditions and 80Hz spectral sampling rate

Match Factor = 963

Match Factor = 929

20

min0 0.05 0.1 0.15 0.2 0.25 0.3 0.350

20

40

60

80

100

120

Performance• Average 50% Peakwidth =

0.34 sec• Resolution (4,5) = 1.5• Analysis Time = 24 sec • Cycle time = 50 sec• RT Precision = 0.7 – 0.22%

RSD• Area Precision = 1.5 – 0.3%

RSD

Conditions – An extreme Example• Sample: Phenone Test Mix• Column: 4.6 x 30mm, 3.5µm SB-C18• Gradient: 50-100% ACN in 0.3min• Flow rate: 5ml/min• Temperature: 40°C• Data Rate: 40Hz

Speed and Precision in Ultra-Fast LCPushing the Limits for highest Throughput

Peak RSD RT (%) RSD Area (%)

1 0.70 1.3

2 0.58 0.7

3 0.43 0.9

4 0.34 0.3

5 0.32 0.9

6 0.29 0.9

7 0.26 1.5

8 0.24 0.7

9 0.22 1.0

Overlay of 6 Runs

Application Areas• Screening

Experiments• HT LC/MS/UV• Early Formulation

Studies• Process Analytical

Techn.

21

Speed and Precision in Ultra-Fast LCModerate Gradients for highest-quality Quantitative Data

Peak RSD RT (%) RSD Area (%)

1 0.47 0.472 0.44 0.193 0.31 0.304 0.27 0.275 0.25 0.486 0.23 0.427 0.20 0.338 0.17 0.359 0.15 0.27

min0.1 0.2 0.3 0.4 0.5 0.6 0.7

mAU

0

200

400

600

800

1000 Overlay of 6 Runs

• 2x slower gradient

• 2 – 5x better Precision

• Still very fast

Performance• Peakwidth = 0.38 sec FWHM• Resolution (4,5) = 1.6• Analysis Time = 40 sec • Cycle time = 70 sec• RT Precision = 0.1 – 0.5%

RSD• Area Precision = 0.2 – 0.5%

RSD

Conditions – Less extreme Condtions

• Sample: Phenone Test Mix• Column: 4.6 x 30mm, 3.5µm

SB-C18• Gradient: 50-100% ACN in

0.6min• Flow rate: 5ml/min• Temperature: 40°C• Data Rate: 40Hz

Application Areas• Formulation Studies• Analytical

Development• Process Control• QA/QC

22

min0.2 0.4 0.6 0.8 1

injection 1

injection 4000

Column 2

Column 1injection 4000

injection 2000

injection 2000

injection 1

min0.2 0.4 0.6 0.8 1

Robustness in Ultra-Fast LCAre Methods and Instrumentation Robust Enough for

24x7 Operation?

Stability study on system configuration with automated column regeneration:

• Stable system and column performance for 8000 injection (4000 injections per column)

• System suitable for unattended and automated 24x7 operation and reliable over-weekend runs

Injection Number

0.4

0.5

0.6

0.7

0.8

0.4

0.5

0.6

0.7

0.8

0 500 1000150020002500300035004000

Column 1

Column 2

RT/min

W1/2 /sec

0 500 1000150020002500300035004000

RT/min

W1/2 /sec

P=300bar

23

New Data Recovery Card*The first LC Detector with “Data Never Lost”

Insurance

*Patent Filed

Data Recovery Card* - DRC

• All signals, spectra and meta data are buffered on high-capacity, embedded 256MB Compact Flash Card compliant with 21 CFR Part 11.

• Prevents any data loss in case of communication breakdowns between instrument and PC.

• Automatic Run Recovery in case of temporary communication failures

• Manual Run Recovery in case of permanent communication failures” after software, PC, and/or instrument re-boot.

24

New Data Recovery CardThe first LC Detector with “Data Never Lost”

Insurance

Automated Run Recovery in case of temporary communication failuresA) Time Elapsed = 0.3 min Run in Progress

B) Time Elapsed = 0.6 minCommunication Failure Occurs

C) Time Elapsed = 1.9 min • Communication is re-

established• Automatic data transfer from

DRC to PC• No user interaction necessary

25

New Data Recovery CardThe first LC Detector with “Data Never Lost”

Insurance

Manual Run Recovery in case of permanent communication failures

• Run Recovery dialog pops-up automatically after system re-boot.

• Data are stored on the PC under a pre-configured location.

26

The Next Level of Data Traceability Proprietary RFID Technology for Flow Cells and

UV Lamp

Radio Frequency Identification Tags

• RFID tags records all relevant data necessary to recall instrument conditions under which a run has been executed.

• Minimizes the risk of false data interpretation, because measurement conditions are documented.

• Meta data stored on RFID tags are saved with each raw data file for unambiguous answers to (auditor-) questions like

“Which type of flow cell was used to generate this chromatogram - what was the path length and volume?”

“Did the accumulated burn-time of the lamp exceed pre-defined limit?”

Flow Cell • Path length• Volume• Max pressure• Date last test passed• Product number• Serial number• Production date

UV Lamp • Accumulated on-time• Actual on-time• Number of ignitions• Date last test passed• Product number• Serial number• Production date

27


UV Lamp

ChemStation Report

RFID-tag information documents run conditions.

28


UV Lamp

10

10 1010 RFID Tag Info for Diagnostics

29

The next Level of Baseline StabilityNew Electronic Temperature Control – ETC

Electronic Temperature Control - ETC

Advantages of ETC

Compensation of changes of ambient conditions (temperature and humidity)

Reduced baseline wander for improved practical sensitivity and reproducibility under harsh environmental conditions

Optical Unit

Main Board

Optical Temp. Sensor

Ambient Temp. Sensor

Air Flow

Fan

Heater

1100 Series DAD SL / MWD SL

Front

30

Conditions: Relative humidity = 60%RH = const;

Temp = 25°C +/-2°C; 4 x 1h CyclesNote: By keeping RH=const, the absolute humidity is strongly modulated due to temperature variations (worst case condition).

TempCntrl ON 254,4 No Ref 750,4 No Ref

TempCntrl OFF 254,4 No Ref 750,4 No Ref

2.6mAU / 4°C = 0.7mAU/°C


Ambient Rejection at

60% RH:

ETC off: ~

700µAU/°C

ETC on: < 30µAU/°C

Temp. C

RH %

AH g/kg

AH Dev. %

23 60 10.5 - 12

25 60 11.9 0

27 60 13.4 13

31

TempCntrl ON 254,4 No Ref 750,4 No Ref

TempCntrl OFF 254,4 No Ref 750,4 No Ref

~0.5mAU/°C

~0.7mAU/°C

Conditions: Relative humidity = 95% RH = const;



Ambient Rejection at

95% RH:

ETC off: ~

700µAU/°C

ETC on: < 30µAU/°C Temp. C

RH %

AH g/kg

AH Dev. %

23 95 16.9 - 12

25 95 19.1 0

27 95 21.5 13

32

1100 DAD SL: 254,4 / No REF 1100 DAD SL: 254,4 /

360,100

1100 DAD B: 254,4 No REF

1100 DAD B: 254,4 / 360,100

~100µAU/°C

Comparison between 1100 DAD SL and 1100 DAD (“B”-model)

Conditions: Relative humidity = 60%RH = const;



Ambient Rejection ETC

on:

DAD “B”: ~

100µAU/°C

DAD SL: < 30µAU/°C Temp. C

RH %

AH g/kg

AH Dev. %

23 60 10.5 - 12

25 60 11.9 0

27 60 13.4 13

33

- Insert- Body- Ring

New 13ul Standard Flow Cell Design*

Ceramic Ring for thermal de-coupling

*Patent Filed

“Drill” Design of Inlet and Outlet for faster flush-out

Advantages

Reduced RI-sensitivity

Improved peak dispersion

Minimized noise in in high-flow, high-temperature applications

34

New 13ul Standard Flow Cell Reduced RI Sensitivity

New Standard Flow Cell provides

3-4x lower RI-Sensitivity1100 DAD/MWD with old Standard Cell

1100 DAD SL/MWD SL with new Standard Cell

12 mAU

4 mAU

36 mAU

9 mAU

Demanding RI Test Gradient

35

ColumnSample

TempFlow

WLEluent

Injection

SB-C18 1.0x50 Iso Std +H2NCSNH2

250.1 ml/min254,4; -/-80/20 H2O/ACN1 ul

New 13ul Standard Flow CellMinimized Dispersion for Maximum Resolution

and Sensitivity

Improved flush-out behavior of the new standard flow cell minimizes peak tailing thereby increasing peak heights and resolution.

new Standard Cellold Standard Cell

36

- Insert- Body- Ring

Flow Cell Portfolio of the 1100 DAD/MWD SL For Uncompromised Compatibility from Nano to Prep

Advantages – From Nano to Prep

Compatibility with Conventional LC, Ultra-fast LC, Capillary LC, Nano LC and Prep LC

Support of Analytical LC on Columns from 75 µm to 4.6mm ID

Support of Preparative LC on Columns from 4.6 to 50mm ID

RFID tags for Data Traceability and Diagnostics

Flow Cell Portfolio Standard: 13ul, 10mm path length,

120bar Semi-Micro: 5ul, 6mm path length,

120bar Micro: 1.7ul, 6mm path length,

400bar Semi-Nano: 500nl, 10mm path

length, 50bar Nano: 80nl, 6mm path length,

50bar Preparative: 3mm, 120bar Preparative: 0.3mm, 20bar Preparative: 0.06mm, 20bar

37

Which Flow Cell to use for Ultra-fast LC?

13µl Standard Flow Cell: For highest sensitivity and linearity High-demanding quantitative work,

e.g. analytical method development, QA/QC

4.6 – 3 mm ID Columns

1.7µl Micro Flow Cell: For highest selectivity Ultra-fast semi-quantitative work,

e.g. Screening Experiments, HT LC/MS/UV

2.1 – 1mm ID Columns

5µl Micro Flow Cell: Best compromise of sensitivity and

selectivity For good quantitative and qualitative

results, e.g. Screening, HT LC/MS/UV, Early Formulation Studies

4.6 – 1mm ID Columns

Flow Cell Volume/Pathle

ngth

Sensitivity &

Linearity

Resolution

13 µl / 10mm 100 % ~ 90 – 95% *

5 µl / 6mm ~ 75 – 85% *

~ 93 – 98% *

1.7 µl / 6mm ~ 65 – 75% *

100 %

* Depends on analytical conditions and column dimension

38

min5 10 15 20

mAU

-0.04

-0.03

-0.02

-0.01

0

Which Flow Cell to use for Ultra-fast LC? Noise Comparison

13ul Standard Flow CellNoise < +/- 2.1 uAU

5ul Semi-Micro Flow CellNoise < +/- 2.4 uAU

Conditions• Column: 4.6x30mm SB C18,

1.8um• Flow rate: 1ml/min• Mobile phase: Water• Temperature: 20C• DAD: 254nm, 16nm, Ref 360,

80nm• PW: > 0.1min (2.5Hz, 2sec

RT)• Slit = 16

min5 10 15 20

mAU

-0.04

-0.03

-0.02

-0.01

0

Specification:ASTM noise < +/- 10 uAU

Note:5ul cell shows similar noise as 13ul cell. However, the linear range is reduced due to the reduced path length of 6mm.

39

SensitivityLimit of Detection for Anthracene under Ultra-fast LC

Conditions

10pg Anthracene injected in 1ul 4nm slit

40Hz: LOD = 1.48pg

20Hz, LOD = 1.03pg

10Hz, LOD = 0.67pg

80Hz: LOD = 2.30pg

0 0.1 0.2 0.3 0.4

mAU

0

0.5

1

1.5

2

2.5

3

3.5

4

min

Performance: LOD/pg in Ultra-fast LCRetention Time = 12 sec, Peakwidth = 0.9

sec4nm Slit

8nm Slit

16nm Slit

80 Hz 2.30 1.68 1.24

40 Hz 1.48 1.08 0.80

20 Hz 1.03 0,75 0.56

10 Hz 0.67 0.49 0.36

5 Hz 0.48 0.35 0.26

– 27% – 26%

4nm Slit

8nm Slit

16nm Slit

2.5 Hz

1 0.73 0.53

Compare: Conventional LC on 1100 DAD/MWD „B“ Retention Time = 2 min, Peak width = 6 sec

40

1100 Series DAD SL and MWD SL – Builds upon 1100 DAD

Optical Design - Optimized for Best Sensitivity

Tungsten lamp Long-life

Deuterium Lamp

Holmium Oxide Filter

Flow Cell

Programmable slit Grating

1024 element

diode array

190 nm950 nm

Minimized Noise in

Visible WL-Range

Automated wavelength verification

Fast optimization of sensitivity and

resolution

Excellent wavelength resolution

More uptime > 2000h

1100 DAD – 25,000 Installations Worldwide

41

Tungsten Lamp Off:Noise: > 400 µAU

700nm

min0 1 2 3 4 5 6 7 8 9

mAU

-0.2

-0.1

0

0.1254nm

ACN/Water 20/800.2 ml/min1 nm

Eluent:Flow rate:Slit:


Dual Lamp Design for Highest Sensitivity from 190 to 950nm

Tungsten Lamp OnNoise: < 20 µAU

Tungsten Lamp Off:Noise: < 20 µAU

mAU

-0.20

0.20.40.6

min0 1 2 3 4 5 6 7 8 9

Tungsten Lamp OnNoise: < 20 µAU

Advantages Approx. constant Noise from

190 to 950nm

Up to 20x lower Limits of Detection for compounds absorbing in the visible range at λ > 400nm

Significantly higher confidence in qualitative, spectral analysis results

More accurate Peak Purity results, especially at trace levels.

More accurate Library Analysis and Spectral Confirmation results

42


Programmable Slit – Micromechanics

Motor Slit

1 Programmable Slit for 1, 2, 4, 8 and 16 nm

Advantages No need for manual slit changes

Fast optimization of sensitivity and resolution

Maximized Sensitivity by 16nm slit (+ 80% versus 4nm slit)

Maximized Spectral Resolution by 1nm slit (for optimized spectral analysis)

Documents slit width (GLP, data traceability)

43

nm230 240 250 260 270 280

ResolutionBenzene Spectrum at Trace Level0.7 mAU1 nm slit2 nm wavelength bunching

1 nm

2 nm

4 nm

8 nm

Absorbance

00.10.20.30.40.50.6

(mAU)

16 nm


Programmable Slit for fast Optimization of Sensitivity and Resolution

Noise level

44

Rapid Resolution HT 1100 Series Modification Kits

Converting an 1100 Binary System to Ultra-fast LC

3 Modification Kits

• 1100 – VWD: 4.6mm RRHT-1100 Series Ultra-fast LC Kit P/N 5188-5323

• 1100 – DAD: 4.6mm RRHT-1100 Series Ultra-fast LC Kit P/N 5188-5324

• 1100 – DAD/MS:2.1mm RRHT-1100 Series Ultra-fast LC Kit P/N 5188-5328

Content

• Filter

• Capillaries

• Fittings, Union

• UV Flow cell

• RRHT Columns

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Rapid Resolution HT 1100 Series Modification Kits

Converting an 1100 Binary System to Ultra-fast LC

Fast LC Modifications for 1110 Binary LC System with DAD/MWD Detector and 4.6mm ID RRHT Columns

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Summary1100 Series DAD SL and MWD SL

Faster resultswe

Higher Resolution

Higher Data Security

Higher Peak Capacity

80Hz Data Acquisition for up to 100% resolution gain in ultra-fast LC

High Precision, Linearity and Sensitivity to maintain data quality under ultra-fast LC conditions to comply with regulatory requirements to allow for spectral analysis at trace levels (DAD SL only)

High Instrument, Column and Method Stabilityenables robust 24x7 operation

Uncompromised Compatibility with Existing MethodsRun conventional methods without compromising data

quality Build-in Data Recovery Card

provides „data never lost insurance“ RFID Tags for Cells and UV Lamp

for unambiguous data traceability New Low Noise Electronics, New ETC, New Standard Flow

Cell for decreased short-term noise and increased practical

sensitivity

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Appendix

48

Overview – Features and Specifications

Feature/Spec 1100 DAD 1100 DAD SL

1100 MWD 1100 MWD SL

Spectral DA Rate

10 Hz 80 Hz N/A N/A

Signal DA Rate

20 Hz 80 Hz 20 Hz 80 Hz

Data Recov. Card

No Yes No Yes

RFID tags No Yes No Yes

LAN on-board

No Yes No Yes

Noise 254nm +/- 10uAU +/- 10uAU +/- 10uAU +/- 10uAU

Noise 750nm +/- 10uAU +/- 10uAU +/- 10uAU +/- 10uAU

Noise dual WL

+/- 10uAU +/- 10uAU +/- 10uAU +/- 10uAU

Linearity > 2 AU > 2 AU > 2 AU > 2 AU

WL-Range 190-950nm 190-950nm 190-950nm 190-950nm

WL Accuracy +/- 1nm +/- 1nm +/- 1nm +/- 1nm

Dual –Lamp Yes Yes Yes Yes

Slit/nm 1,2,4,8,16 progr.

1,2,4,8,16 progr.

1,2,4,8,16 progr.

1,2,4,8,16 progr.

Note:

For uncompromised compatibility from nano-flow to preparative applications all detectors can be ordered with 5 different analytical flow cells (13ul, 5ul, 1.7ul, 500nl, 80nl) and 3 preparative flow cells (3mm, 0.3mm and 0.06mm)

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Future proof design

• State-of-the-Art Motorola PowerPC Processor

• LAN on board

• USB on board

• PCMCIA• Firewire• WLAN• Bluetooth

• Integrated Web-server

Module Independent Electronic Core

New Electronics platform

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Peak Width – Response Time – Data Rate and Sensitivity

Don‘t use for > 0.15 sec peak width.

> 0.15 sec

> 0.3 sec

> 0.6 sec

> 1.2 sec

> 3 sec

> 6 sec

> 12 sec

> 24 sec

> 51 secPeak Width = Peak Width at 50% Peak Height

Recommended settings in ultra-fast LC with 50% peak width between 0.15 and 0.6 sec For 50% peak width between 0.6 and 1.2 secNotes: •Noise level changes ~ proportional to the

square root of the change in data rate.•For optimum selectivity and sensitivity

the Peak Width should not be chosen smaller than necessary.

•For 50% peak width between 0.3 and 0.6 seconds Peak Width of > 0.005 min is recommended, which correspondes to 40Hz data rate.

•For peaks narrower than 0.3sec at half height, Peak Width of > 0.0025min (80Hz data rate) should be used.

•For highest sensitivity in ultra-fast LC the slit can be increased to 8 or 16nm.

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Linearity - OQ/PV Test on Caffeine Standards

min3 3.2 3.4 3.6 3.8

mAU

0

200

400

600

800

1000

Amount[ng/ul]0 200

Area

0

1000

2000

3000

4000

12

3

4

5

caffeine, DAD1 A

Correlation: 1.00000

Rel. Res%(1): 16.123

Area = 8.39574204*Amt +5.3180278

Correlation:

1.00000

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Agilent 1100 Series HT LC/MS SystemA Scalable and Flexible Solution for Ultra-fast

Analysis

1.

5.

2.

3.

4.

6.

1. HT LC System + 1.8um RRHT Columns

2. Capacity Extension

3. Valves

4. Mass-selective Detector

5. Integrated Controller

6. Services and Compliance Products

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-0.0005

0.0000

0.0005

0.0010

0.0015

0.0020

0.0025

0.0030

0.0035

0.0040

0.0045

0.0 0.2 0.4 0.6 0.8 1.0 1.2 1.4 1.6

Van Deemter Curves1.8um Rapid Resolution HT Columns on the

1100 HT System

ZORBAX Eclipse XDB-C18 4.6 x 50mm (30mm) 85:15 ACN:Water 1.0L Octanophenone 0.05 – 5.0 mL/min 20°C

5.0 m

3.5 m

1.8 m

260,740 N/m @ 2mL/min

5.0 mL/min

Efficiency gain of 1.8μm versus 5μm columns: 3.2x @ 2ml/min4.4x @ 5ml/min

HETP

(cm

/pla

te)

Interstitial linear velocity (ue- cm/sec)

Higher speed – Higher resolution – Higher sensitivity Particle H_min

5μm 9.3μm

3.5μm 6.0μm

1.8μm 3.8μm

Note: Efficiency of 1.8μm columns is virtually flow-rate independent.

Up to 2.1x Resolution Up to 4.4x Speed

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Ultra-fast Gradient Analysisof 9 Phenones

Performance Summary

9 Phenones baseline separated in 29 sec39 sec0.8 min (with column regeneration and run time = 0.7min)1.0 min (without column regeneration and run time = 0.7min)> 2.65 for all peaks0.50 sec (average)79 (0.65min gradient)< 0.2% RSD without column regeneration< 1.0% RSD with column regeneration< 0.003% (limit of detection)7.2 days or 8000 injections of continuous operation with stable

performance

Analysis speed

Analysis timeCycle time

Resolution 4 peakwidthPeak capacityRT precision

Carry over Robustness

min0 0.2 0.4 0.6 0.8 1

mAU

0

100

200

300

400

Possible cycle time with CR = 0.8 min

Analysis time = 0.65 min = 39 sec

Possible cycle time w/o CR = 1.0 min

60°C4.35ml/min390bar

New 1100 Series DAD SL and MWD SL 80Hz Data Acquisition for Ultra-fast LC.

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