What’s New in - agilent.com 400 pg/mL Agilent Confidential . 7890B and OpenLab CDS - More...

What’s New in

Agilent GC

Joy Jennison

October 2013

Agilent Technologies

Introducing the 7890B Gas Chromatograph Re-defining Premium Gas Chromatography

New & Expanded Accessories & Options

New Inert Flowpath option

Improved FPD-Plus detector

ECD as 3rd detector option

Dual MMI inlets

Improved Performance Specifications

Best-in-class package of performance specifications

Integrated Intelligence Functions – OpenLab CDS

GC-MSD communication

Integrated GC calculators

3D Interactive Graphical Parts Finder

Barcode Scanning with Auto-Input

Early Maintenance Feedback

Sleep-wake function – Helium Conservation

October 4, 2013 2

Inert From Injection to Detection Agilent Ultra Inert and UltiMetal-Plus

October 4, 2013 3

UltiMetal – TCD,

FPD, NPD/FID Jets

UltiMetal Capillary Flow Technology

Devices, Ultimate Union

UltiMetal Inlet Weldment, Shell

and Transfer Lines

Ultra Inert GC Column

Ultra Inert Gold Seal

Ultra Inert Inlet

Liner

New UltiMetal

FlexiMetal Ferrules

http://www.chem.agilent.com/en-US/products-services/Columns-Sample-Preparation/GC-GC-MS-Columns/Capillary

Agilent Inert Flowpath SSL Inlet Option Proprietary UltiMetal-Plus Treatment

October 4, 2013 4

Enhanced performance for trace GCMS and

GC-ECD analysis of pesticides and drugs of

abuse

Protects active analytes contacting injector

metal structure during high volume injections

Available as 7890B Inert Flowpath option #114

or upgrade G3453B for 7890A/B

Agilent Confidential

Agilent UI Gold Seal: Deactivated Gold Surface

• Soft gold plating is essential for proper sealing

• Ultra Inert chemistry blocks active sites

(gold is NOT inert)

• Smooth surface doesn't leak

October 4, 2013 5

Agilent Metal

Injection Moulding

for seal

Competitor’s

machined seal

Reliable ppb and ppt

measurements require

attention to the little things!


Response Comparison for Sensitive Pesticides

Ultra Inert Gold Seal


Siltite Ferrules

Stiff, can cause damage

to column or fitting

Smaller compression

area (40 to 60um) –

leaks more likely

Tolerances less tightly

controlled

Agilent Flexi-Metal Ferrules

Computer aided Design

More flexible - Less column

damage

Larger compression area

(100 to 120um) – less

leaks

Agilent design alleviates

current quality issues

Previous Ferrule Versus New Agilent Flexi-Metal Ferrule


Agilent Confidential October 4, 2013

Enlarged chromatograms for sensitive pesticides

UltiMetal Plus on Flexible Metal Ferrule

Is deactivation needed for such small surface?

8

4 x10

0

1

2

4 x10

0

1

2

Counts vs. Acquisition Time (min)

4.5 5 5.5 6 6.5 7 7.5

Untreated FMF

Post column Std 500ppb

FMF + UltiMetal Plus

Post column Std 500ppb

Acephate

Omethoate

Demeton-S

Acephate

Omethoate Demeton-S

New FPD Plus Higher temperature and better sensitivity

October 4, 2013 9

250C 400C

Higher Response

Lower Noise

S

P

Max Temp

MDL pg/s

7890A FPD 7890B FPD Plus

3.6 2.5

45 60

Higher Tmax

Design Improvements

Two heated zones – hot

transfer line, cooler

emission block

UltiMetal Deactivation

FPD Plus


4, 6 -DMDBT

C3-DBT’s

4MDBT

2,3 DMDBT

Dibenzothiophenes in Light Crude

Requires operating

temperature above 300C

New FPD Plus Higher Operating Temperature

October 4, 2013 10


Expanded Laboratory Capability More flexibility

October 4, 2013 11

Design Improvements

Two heated zones – hot

transfer line, cooler

emission block

UltiMetal Deactivation

FPD Plus

Allows Cl-containing

pesticides in

environmental and food

samples to be detected

along with an FPD and

FID installed

ECD 3rd Detector

Used commonly in

Europe for high

throughput Total

Petroleum Hydrocarbon

(TPH) environmental

analysis

Dual MMI


Improved Performance Deliver better results

October 4, 2013 12

Detector Performance

MSD Scan 1500:1 S/N; SIM 10 fg IDL OFN

FID <1.4 pg C/sec

ECD <4.4 fg/sec

FPD <2.5 pg S/sec; <45 fg P/sec

SCD <0.5 pg S/sec

NPD <0.01 pg P/sec, 0.08 pg N/sec (Blos bead)

TCD 400 pg/mL


7890B and OpenLab CDS - More

Efficient Operation

October 4, 2013 13

Integrated Intelligence Benefit

Parts Finder Find parts faster & order easier

Barcode Scanning with Auto-Input Easier configuration

Integrated early-maintenance feedback Manage assets more efficiently

GC:MSD communication including MSD fast vent Protect system better

Integrated GC Calculators Develop methods easier

Easier sleep-wake functionality, He conservation Lower cost of ownership


7890A Enhancements Kit

October 4, 2013

Confidentiality Label

18

7890A Logic Board Enhancements Kit (G3444A)

- Makes 7890A GC ready for most (but not all) 7890B GC enhancements. For

example:

• “Integrated Intelligence” features:

- Early Maintenance Feedback (EMF), Sleep/Wake modes

- Method Translation Calculator (via CDS)

- Enable 2-way communication – 7890A/5977A

• Serial Port for:

- 2nd communication port for Remote Advisor

- Optional Bar Code Reader connects directly to GC

• FPD Plus

Logic Board Upgrade does not support

• 2nd Multimode Inlet (MMI)

• 3rd detector as uECD

Helium Market Situation

He supply is not reliable, prices are increasing and customers are

seeking alternative carrier gases or ways to conserve

October 4, 2013 19


What Are Your Choices?

Reducing Dependence on Helium by

Helium Conservation – switch to nitrogen when GC is idle

• Smarter helium use with new hardware/software tools

• No need to revalidate existing GC methods

Or….

Migrating Existing Helium GC Methods to H2 or N2 *

• Best practices for obtaining the same results and minimizing method revalidation

*Courtesy: James D. McCurry, Ph. D. Senior Scientist, Agilent Technologies

October 4, 2013


20

Reducing Helium Use With Conservation

New 7890B Helium Conservation Module • Automatically switches carrier gas supply to N2 Standby

during idle time

• Integrates into the new 7890B Sleep and Wake function

• Better alternative to just “shutting off the GC”

– Automated

– No system contamination with ambient air exposure

– Faster re-start of heated zones

• Combine with Gas Saver for even less helium

consumption

October 4, 2013 21


Helium Conservation Module Seamlessly integrated onto 7890 GC hardware and software

To Inlet EPCs Purge

He in

N2 in

Flow channel inside

the bridge block

Std. Aux EPC

22

• Built on 5th generation EPC

• Fully controlled by Agilent

data systems

• Purge channel prevents

cross contamination of gases

• Precise pressure control

between tank and GC

• Switch between gases within

15-30 min for most detectors

GC/FID Wake Method: 15-30 Min

GC/MS Wake Method: 15-30 Min

Some other detectors may need longer

23 Agilent Restricted

How Does It Work? Normal Operation Mode (Helium Carrier or Wake Mode)

To GC Inlet

EPC

AUX EPC 1

Nitrogen

0 psig

AUX EPC 3

Purge

10 psig

AUX EPC 2

Helium

80 psig

24.2 mL/min He

(< 0.2 mL/min) N2 25.2 mL/min He

1 mL/min (out)

Bridge Block

Helium ON at 80 psig, Nitrogen OFF

How Does It Work? Helium Savings Mode (Nitrogen Carrier, or Sleep Mode)


Bridge Block

To GC Inlet

EPC

AUX EPC 1

Nitrogen

70 psig

AUX EPC 3

Purge Vent

10 psig

AUX EPC 2

Helium

0 psig

24.2 mL/min N2

(< 0.2 mL/min)

He 25.2 mL/min N2

1.0 mL/min (out)

Helium OFF, Nitrogen ON at 70 psig

How It Works: Configuring Sleep/Wake Operation Simple, Straight Forward Setup

25 Agilent Solutions

Performance: No Change in Chromatography After

N2 Carrier Sleep Method. GC/FID Analysis

26

Day 1 - Original He carrier gas run

Day 2 – First He carrier gas run after overnight N2 Sleep.M method

Day 3 – First He carrier gas run after overnight N2 Sleep.M method

14 16 18 20 22 24 Min.

Agilent Restricted

Performance: Pass MS Tune Within 15min After

Switching from N2 to He as Carrier. GC/MSD

5000

50000

500000

5000000

0 5 10 15 20

Co

un

ts

Time (min)

Nitrogen Background

5 mL/min He

2 mL/min He

Counts of Nitrogen Ion

Time (min) 5 mL/min He

Relative to

Saturation 2 mL/min He

Relative to

Saturation

3 1735168 20.69% 8388096 100.00%

4 1033280 12.32% 4959232 59.12%

5 590080 7.03% 1618944 19.30%

6 354112 4.22% 722944 8.62%

7 228480 2.72% 333696 3.98%

10 56984 0.68% 102576 1.22%

15 9052 0.11% 17080 0.20%


Helium Savings Calculator – Single GC Channel Extend helium supply and lower cost using conservation techniques

October 4, 2013


28

Method:

Column:

GC Flow Conditions

He Carrier Flow (mL/min): 8

He Split flow (mL/min): 70

Gas Saver Flow (mL/min): 20

Gas Saver On (min): 3

Run Time(min.): 20

Gas Volume in Cylinder (L): 8000

Runs per Day: 30

He Cylinder Cost ($): 300

N2 Cylinder Cost ($): 60

ParameterNo

ConservationHelium Conservation

Daily He Usage (L) 112 21

He Cylinder Life (days) 71 376

Daily N2 Usage (L) 0 24

N2 Cylinder Life (days) 0 340

Yearly He Cost ($) $1,537 $292

Yearly N2 Cost ($) $0 $64

Yearly Total Gas Cost ($) $1,537 $356

ASTM D4815 - Ethanol in Gasoline

PDMS 30m x 0.53mm x 2.65um

Example

• ASTM Method D4815

– Widely used to measure ethanol in

gasoline

– Helium cylinder last 2 months

under normal operation

• Helium Conservation

– Helium cylinder life extended to 12

months

– 4x less gas costs per year

Carrier Gas Decision Tree Migrating GC methods to nitrogen or hydrogen

Consider migration to H2 Consider migration to N2 He Conservation

GC/MS specific H2

considerations

Are you willing to convert

to alternative gases?

Is the Application based on

GC or GC/MS?

Does the current GC method

have more than enough resolution?

No

No

Yes

Yes

GC/MS GC

29 Agilent Solutions

The Tyranny of Van Deemter

Why Nitrogen Gets a Bad Rap for Capillary GC

• N2 provides the best efficiency, but at a slower speed

• H2 provides the best efficiency at higher speeds

• Some helium methods have more resolution than is needed and, as long

as peaks are fully separated, N2 will be a good alternative

October 4, 2013 30

Average Linear Velocity (cm/sec)

HETP (mm)

1.2

1.0

.8

.6

.4

.2

10 20 30 40 50 60 70 80 90

C17 at 175º C

k' = 4.95

OV-101

25m x 0.25 mm x 0.4m

N2

He

H2

Helium

58 cm/s

2.5 mL/min

R = 1.17

Nitrogen

58 cm/s

2.4 mL/min

Hydrogen

58 cm/s

1.7 mL/min

R = 1.37

Similar efficiency at 20 cm/s

Using N2 as carrier gas

Many helium GC methods are suited to nitrogen conversion

• Readily available and less expensive gas

• No safety concerns

• Suitable for simple routine analysis (with sufficient resolution)

• Inert like helium, no reactivity concerns

Potential issues

• Reduced chromatographic resolution at higher flows

• Not suitable for GC/MSD and certain GC detector applications

October 4, 2013 31

Changing to N2 Carrier Gas - Let’s Make This Easy!

• Goal: change carrier gas while keeping other method conditions the same

– use the same column

– use the same oven program

– adjust column flow (same linear velocity and holdup time to):

• maintain same peak elution order

• maintain same peak retention times (or as close as possible)

• Easier method revalidation using this approach

– minimal changes to timed integration events

– minimal changes to peak identification table

• Test resolution of key components

– adjust GC conditions (temp, flow) if needed

32 October 4, 2013


Configure Inlet for Carrier Gas in Chemstation

35 October 4, 2013

Select H2 or N2


Set the Control Mode: Flow or Holdup Time

October 4, 2013 36

Try the same holdup time or linear velocity of the original Helium method


Same Holdup Time (Tr) Gives Consistent Retention

Times Compared to Original Helium Method

37

18 19 20 21 22 23 24

Helium

Flow: 3.00 mL/min

P: 7.63 psi

Tr: 0.472 min.

m: 52.97 cm/s

Hydrogen

Flow: 2.64 mL/min

P: 3.43 psi

Tr: 0.472 min.

m: 52.97 cm/s

Nitrogen

Flow: 2.94 mL/min

P: 6.98 psi

Tr: 0.472 min.

m: 52.97 cm/s

23.818 min

23.862 min

23.776 min

October 4, 2013

Wider Retention Time Variation Using the Same

Flow as the Original Helium Method

38

18 19 20 21 22 23 24

Helium

Flow: 3.00 mL/min

P: 7.63 psi

Tr: 0.472 min.

m: 52.97 cm/s

Hydrogen

Flow: 3.00 mL/min

P: 3.85 psi

Tr: 0.420 min.

m: 59.50 cm/s

Nitrogen

Flow: 3.00 mL/min

P: 7.09 psi

Tr: 0.464 min.

m: 53.84 cm/s

23.818 min

23.469 min

23.705 min

October 4, 2013

Safety Considerations for Hydrogen Migration

GC, GC/MS: Both offer H2 enabled features

• Agilent H2 safety letter and safety manuals available

• GC safety design – 6890 and 7890

• Safety Shutdown – any hydrogen channel unable to maintain pressure will shut down the flow, turn off the column oven heater and fan, turn off other heated zones and sound an alarm

• Flow Limiting Frit to restrict flow in case of major leak or column break

• Oven ON/OFF Sequence – fan on to purge oven before heater is turned on

• Explosion Tests – GC and MS designed to contain parts in case of explosion

• Other Considerations

• Read and follow safety manual procedures

• Use chromatographic quality stainless steel tubing if possible

• Do not use old tubing (H2 is known as scrubbing agent)

• No copper tubing (brittleness is a safety concern)

• Use a hydrogen generator if possible

• Split line and septum purge line should be vented safely

October 4, 2013 39


Other Considerations for Hydrogen Migration

• Hydrogen is not as efficient as helium at lower flow rates but hydrogen can be run

at much faster flow rates and maintain good efficiency so can speed up your

analysis. Good choice at higher linear velocities (35cm/sec+)

• Hydrogen exerts lower head pressure than helium at the same flow rates –

beware of backflash - consider using a pressure pulse to match normal helium

head pressure

• Hydrogen is not an inert gas, it is reactive, so there are some solvents like DCM,

that can “corrode” the inlet (especially in the presence of water with HCl

formation). Some analytes (with O and N) and matrices might behave badly in the

presence of heat, hydrogen and/or water or other components in the sample

matrix.

• Hydrogen will “clean” surfaces in it’s pathway so expect some “settle down” time

after switching, particularly with MS detectors – high background (looks like

hydrocarbons), loss of sensitivity and peak tailing are typical and can take days to

weeks to improve.

October 4, 2013 40


Other Considerations for Hydrogen Migration

• If you are converting an MSD please ask for further information – you may need to

change magnet in 5975, change draw out lens, pumping capacity is less for H2

than He (add ion gauge?) etc.

• For method translation and more details on MSD helium to hydrogen conversion

(webinar) go to:

http://www.chem.agilent.com/en-US/promotions/Pages/alternate-carrier-gas.aspx

• For an FID, now that you have hydrogen coming through the GC column, reduce

the fuel hydrogen flow to the detector to maintain the desired 40mls/min to the FID

flame. If you are flow programming use constant carrier/fuel mode. Nitrogen

makeup will provide better sensitivity than H2 or He makeup

October 4, 2013 41









Summary – Migration To H2 and N2

If you need a helium alternative:

– For resolution critical methods, H2 offers the best alternative

– Agilent GC and GC/MS systems have many built-in safety features

– For many GC applications, N2 offers a cheap, easy alternative without

any safety worries

• Many existing helium methods have excess resolution

• N2 can be used without changing any of the existing GC conditions

– keep the linear velocity the same as the original method

– For more information on Helium Carrier Gas

www.agilent.com/chem/heliumupdate

October 4, 2013 42

http://www.agilent.com/chem/heliumupdate

7890B Solutions Portfolio - Why Analyzers?

Reduce the time required for system deployment

October 4, 2013 43

…Faster Application Startup and a High Quality Method

Sample Ready

Order Fulfillment

Standard Installation &

Familiarization

Customer Method Development

and Validation

Agilent Method

Development

Application checkout

Analyzer Installation &

Familiarization

Customer Method

Validation

Order Fulfillment

Agilent Analyzers

End User Configured

Order Placement

Easy-to-Order New Analyzer Process: 50 Analyzer Configurations Available – G3445B

G3445A Opt. Analyzer Description

GC/MS/MS Analyzers

41x GC/MS/MS Pesticide Analyzers (2 versions)

42x GC/MS/MS PAH Analyzer

GC/MSD/DRS Analyzers

45x GC/MSD Pesticide DRS Screening Analyzers (2 versions)

46x GC/MSD Environmental DRS Analyzers (2 versions)

47x GC/MSD Toxicology DRS Analyzers (2 versions)

48x HSS GCMSDFID Residual Solvents Analyzer

GC Gas Analysis Analyzers

52x GC Refinery Gas Analyzers (6 versions)

54x GC Natural Gas Analyzers (7 versions)

56x GC Greenhouse Gas Analyzers (3 versions )

57x TOGA Analyzer for use with HSS

GC Gasoline, Fuel Analysis Analyzers

61x Gasoline Analyzer (inl. Oxygenates, Aromatics, 7 versions)

63x Biodiesel Analyzers (4 versions)

64x CO & CO2 Analyzer w Methanizer (2 versions)

65x Sim Dis Analyzers (4 versions)

66x S analysis with SCD Analyzer (2 versions)

68x Residual Solvents GC-HSS analyzers (2 versions)

January 2013

Analyzer Overview

44

Updated Solution Guide (Energy and Chemical) 5991-1561EN

Searchable by application or compliance method

Links to Analyzer Chapter

January 2013

Analyzer Overview

45

The Agilent 490 Micro GC - BioGas Analyser

Biogas Analysis

CH4 CO2 N2 O2 NH3 H2S H2 CO

Source (%) (%) (%) (%) mgr/m3 (%) (%)

Landfill 50 - 75 25 - 50 <10 <2 … <3% <1

Houshold waste 50 - 60 34 - 38 <5 <1 … 70 - 600 ppm

Wastewater treatment 60 - 75 19 - 33 <1 <0.5 0.2 - 0.3%

plants sludge

Agricultural waste 60 - 75 19 - 33 <1 <0.5 50 - 100 0.2 - 0.7%

Biogas is produced by anaerobic digestion or fermentation of

biodegradable materials such as biomass, manure, sewage, municipal

waste, green waste, plant material and energy crops.[1]

Reference [1]: http://en.wikipedia.org/wiki/Biogas

490-GC Micro-Machined Technology

CHIP INJECTOR

GC COLUMN

MICRO TCD MICRO EGC

Biogas: Molecular Sieve 5A for permanent

gases

0.4 0.8 1.2 1.6 2Min

H2

O2

N2

CH4

Column: MS5A ,10m

Temperature: 80°C

Carrier Gas: Argon, 150 kPa

Backflush of C2+, CO2, moisture

Biogas: PPU for C2, C3, H2S and CO2

0.3 1Min

CO2

H2S

Composite

Air Peak

Ethane

Propane

Column: PoraPLOT U

Temperature: 100°C

Carrier Gas: Helium, 100 kPa

Backflush of C4+

Biogas: CP-Sil 5 CB for C3+ Hydrocarbons

0.2 1.6Min

n-Hexane

iso-Pentane

n-Pentane

iso-Butane

n-Butane

Propane

H2S

Column: CP-Sil 5 CB

Temperature: 60°C

Carrier Gas: Helium, 150 kPa

THANK YOU!

52 ACUAPT 2013

What’s New in - agilent.com 400 pg/mL Agilent Confidential . 7890B and OpenLab CDS - More...

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