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Agilent Technologies GPSD Analyzer Solutions

Agilent Science and Technology Symposium

May 2014

May 2014

1

What is an Analyzer

An Analyzer is a factory-configured GC or GC/MSD system configured, tuned and tested for the application prior to

delivery to the customer’s laboratory.Capillary

Flow Technology

Retention Time

Locking

RTL Database

Deconvolution Reporting Software MRM

Database

App. Specific Supplies

Synchronous SIM/SCAN

Sample Prep WorkBench

Capillary Flow

Technology

Retention Time

Locking

Specialized Columns

and Accessories

MultichannelCustomized

Configurations

Valves

Sample Prep WorkBench

May 2014

Agilent Science and Technology Symposium 20142

Intrinsic Value for Analyzer Solutions

Configured with Market Leading Hardware, and Leveraging Technology

Innovation

Databases and Libraries developed and maintained

by Agilent Technologies

Methods Developed by Agilent’s Top Application

Experts and Collaborators

Receive systems optimized for a particular analysis

Obtain accurate and reliable results

Save time and reduce cost for system configuration and method development

Chromatography guarantee Quicker start to system calibration

and validation

…Faster Application Startup with a Guaranteed Method

Sample Ready

Order Fulfillment

Standard Installation &

FamiliarizationCustomer Method Development

and Verification

Agilent Method

DevelopmentApplication checkout

Analyzer Installation &

Familiarization

Customer Method

VerificationOrder

Fulfillment Agilent Analyzers

End User Configured

Order Placement

Sample Ready

Time Savings

May 2014


App. optimized consumables

GPD AnalyzersThe Solution Approach

Individual Components

produced

Individual Components Tested (OFN)

System assembled

App. method developed on cust. system

System checkout on App. mix

Run 1st customer sample

customization or optimization

method

On-going maintains/service

Factory FSE

Factory

Analyzer Delivery Point

FSS

Report follows Standard Method

System withapplication setup

w/o Analyzer

FSS (specialist)I&F

Std. HW, SW

Data CD

Box Delivery Point

Configured for a specific analysis with factory setup, chemical test, I&F, and field verified

performance

May 2014


Intrinsic Value for Analyzer Solutions

Configured with Market Leading Hardware, and Leveraging Technology

Innovation

Databases and Libraries developed and maintained

by Agilent Technologies

Methods Developed by Agilent’s Top Application

Experts and Collaborators

Receive systems optimized for your particular analysis

Obtain accurate and reliable results

Save time and reduce cost for system configuration and method development

Chromatography Guarantee Quicker start to system calibration

and validation

May 2014


Typical Analyst RequirementsAgilent Analyzer Solutions

Sample Prep

Sample Introduction Separation Detection Validated

Reports

Agilent’s Analyzers Provide

Customer’s Responsibility

Customer’s Responsibility

May 2014


Selected Agilent GPSD AnalyzersApplication based Solutions

Food Safety• Pesticides - Sensitivity (TQ)• Pesticides – Sens., Op. Ease (TQ)• Pesticides – Economical (SQ)• Enhanced PAHs – Sensitivity (TQ)*• Enhanced PAHs – Economic. (SQ)*

Environmental• Pesticides - Sensitivity (TQ)• Pesticides – Sens., Op. Ease (TQ)• Pesticides – Economical (SQ)• Enhanced PAHs – Sensitivity (TQ)*• Enhanced PAHs – Economic. (SQ)*• Semi-Volatiles – Economical (SQ)• Greenhouse Gases (GC)

* - New for 2014 * - New for 2014

May 2014



Energy and Chemical• LVO High Capacity RGA* • LVO Fast RGA* • LVO Fuels (D4815, D5580, D3606)*• Fast RGA with He or H2 Carrier• Extended Natural Gas Analyzer• Natural Gas Analyzer• Transformer Oil Gas Analyzer

(TOGA)

Forensics and Toxicology• Controlled Substances – He (SQ)*• Controlled Substances – H2 (SQ) *• Blood Alcohol (GC)• Blood Alcohol – MS Confirmation (SQ)*• Toxicology Screening (SQ)

* - New for 2014 * - New for 2014

May 2014



Pharmaceutical (USP 467) • Residual Solvents (GC)• Residual Solvents (MS)

February 19, 2014

9May 2014



Select GC/MSD Analyzers

May 2014

May 2014

10

P&EP 3.0GC/MS/MS Pesticides Analyzer

Get Customers on the Analytical FAST TRACK

May 2014

11

Feature Elements for P&EP 3.0 AnalyzerGC/MS/MS Pesticides and Environmental Pollutants Analyzer• MRM database with ~1100 compounds and

~8500 optimized transitions including 710+ pesticides and breakdown products

• GUI that facilitates building MRM acquisition and quantitation methods based on customer’s compound list

• Retention Time Locked separation for reliable peak identification and quantitation for CF and CP BF methods

• Multimode inlet for large volume injection helps optimize detection limit performance

• Opt 114 UI S/SL for when there is no requirement for optimal LOD performance

• Capillary Flow Technology Backflush for faster cycle time and reduced system maintenance Pesticide & Environmental Pollutant Analyzer 3.0

May 2014


Note: In this example, the acquisition is in full-scan mode.

Acquire RTLock Calibration Data…

Now available for both CP & CF methods!

May 2014


Home Screen of the MRM DatabaseSure it’s an Excel file, but…

No More vLookup!

New GUI thanks to the efforts of Pascal Vattaire and Laurent Pascaud!

May 2014


View of “Target Compound List”

May 2014


Build MRM TableStep 1 – Select Method of ChoiceStep 2 – Select Quant & Qualifier ions

May 2014


Two Methods Can be developed:1) MRM Acquisition Method (qqqacqmethod.xml) via the Compound List Assistant (CLA )2) Quant Method (quantmethod.xml) via the MRM database

May 2014


C.-K. Meng, Agilent Application Brief 5989-6018EN

• Elimination of long “baked out” at a high temperature to remove less volatile, late eluting matrix components

• Reduced analysis time• Increased column life time• Prevention of the MS source contamination• Less frequent MS source maintenance

Increased sample

throughput

Column Backflush - Benefits

May 2014


Column Backflush - Benefits

M. Mezcua, M.A. Martinez-Uroz, P.L. Wylie, A.R. Fernandez-Alba,J. AOAC Int. 92 (2009) 1790-1806.

Improved Ruggedness

Reduced Maintenance

May 2014


Overlays of GC-MS/MS chromatograms for selected analytes (at 50 ng/g ) obtained within a 2.5-day sequence of 125 dietary supplement sample injections

Deltamethrinm/z 253>174

GinsengRootPowder

Saw Palmetto Berry Powder

ScutellariaPowderedExtract

2x10

0

0.5

1

1.5

2

2.5

3

3.5

4

4.5

Counts vs. Acquisition Time (min)18.1 18.2 18.3 18.4 18.5 18.6

3x10

0

0.5

1

1.5

2

2.5

3

3.5

Counts vs. Acquisition Time (min)4 4.05 4.1 4.15 4.2

3x10

0

0.5

1

1.5

2

2.5

3

3.5

4


Dichlorvosm/z 185>93

3x10

0

1

2

3

4

5


Malathionm/z 173>99

Ethionm/z 231>129

3x10

0

0.5

1

1.5

2

2.5

Counts vs. Acquisition Time (min)9.9 10 10.1 10.2 10.3 10.4

3x10

0

0.5

1

1.5

2

2.5

3


3x10

0.5

1

1.5

2

2.5


2x10

0

1

2

3

4

5

6

7

Counts vs. Acquisition Time (min)15.3 15.4 15.5 15.6 15.7

Phosalonem/z 367>182

3x10

0

0.5

1

1.5

2

2.5

3

3.5


3x10

0.5

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2x10

0

0.5

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3.5

4


Deltamethrinm/z 253>174

GinsengRootPowder

Saw Palmetto Berry Powder

ScutellariaPowderedExtract

2x10

0

0.5

1

1.5

2

2.5

3

3.5

4

4.5


3x10

0

0.5

1

1.5

2

2.5

3

3.5


3x10

0

0.5

1

1.5

2

2.5

3

3.5

4


Dichlorvosm/z 185>93

3x10

0

1

2

3

4

5


Malathionm/z 173>99

Ethionm/z 231>129

3x10

0

0.5

1

1.5

2

2.5


3x10

0

0.5

1

1.5

2

2.5

3


3x10

0.5

1

1.5

2

2.5


2x10

0

1

2

3

4

5

6

7


Phosalonem/z 367>182

3x10

0

0.5

1

1.5

2

2.5

3

3.5


3x10

0.5

1

1.5

2

2.5

3

3.5

4


3x10

0.5

1

1.5

2

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3


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0

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0

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3.5


2x10

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0.5

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2.5

3

3.5

4


Column Backflushing - Benefits

K. Mastovska and P.L. Wylie,J. Chromatogr. A 1265 (2012) 155-164

Accurate DB Match

May 2014


• MRM Spectrum Unchanged

• Troubleshooting

• Repeatability- Run-to-run- Operator-to-operator- Instrument-to-instrument

Retention Time Locking (RTL)Improve Confidence with Retention Time Locking

Initial run4.72 psi

Trim 1 meter4.72 psi

Relock4.42 psi

0

50

100

0

50

100

0

50

100

4.296 min.

4.064 min.

4.297 min.

Accurate DB Match

May 2014


Importance of MRM TransitionsMalathion Identification

Confident Identification

May 2014


Why are MRM Transitions Important?Endosulfan Sulfate (?) in Tea Extract – Two (2) Transitions

3.3 ppb, Equiv : 0.016 mg/Kg in TeaTea EU MRL :Sum Endo a+b+sulfate = 30 mg/kg

Std 5 ppb Reagent BlankOrganic Tea A

• Single Qualifier Transition• Ion Ratio outside 80-120%

confidence band• Unconfirmed

• Rerun of data • Ion Ratio within 80-120%

confidence band• CONFIRMED!!

• Demonstrates the value of multiple optimized transitions in the MRM Database.

• Not just to avoid matrix interferences but also for additional confirmation!

Organic Tea A

Accurate Confirmation

May 2014


Powerful MRM Database

• The Most Comprehensive and Flexible MRM database!

• New User Interface that streamlines the creation of custom MRM acquisition and quant methods.

MultiMode Inlet (MMI)

• Large volume injection helps optimize LOD performance

• Opt 114 UI S/SL for customers that do not require for optimal LOD performance

Includes New Analytical Methods

• Expands analysis options:• Constant Pressure

methods: #411 & #415• Constant Flow methods:

#412 & #414

Auto RTL for CFT BF Methods

• Auto RTL for CF and CP BF method• Facilitates relocking

methods• In Situ Source Cleaning

• Keeps source clean continuously

• Improves quantitative performance for many analyses

GC/MS/MS Pesticide AnalyzerValue Overview

Accurately confirm target pesticides while reducing the time required from start-up to results

Industry Leading

Technology

May 2014


Enhanced PAH Analyzers


May 2014

25

PAH Analysis Using GC/MS and GC/MS/MS

1. GC/MSD in SIM mode

2. GC/MS/MS in MRM mode

3. Typical calibration range from 1-1000 pg

4. Typical method acceptable linearity, R2 > 0.99

5. Typical method ISTD reproducibilitya) +/- 20% with calibrationb) +/- 30% to 50% with samples

May 2014


PAH Properties and Issues with PAH Analysis 1. Properties

a) Span wide molecular weight and BP rangesb) They are sticky, not activec) Subject to desublimation (deposition)

2. Analysis Issuesa) Difficult to vaporize and keep from depositingb) High temperatures are importantc) Minimize surface contactd) Tailing peaks need manual integration e) ISTD inconsistent response across cal rangef) ESTD linearity

May 2014


Optimized PAH Analyzer

1. Inlet temperature of 310-330 oC

2. Inlet liner, 4mm, with glass wool, Agilent p/n 5190-2293

3. Pulsed injection of 50 psi, Purge time of 0.5 - 1.0 min

4. PAH specific column, Agilent p/n 122-9632

5. Post-column backflushing

6. Constant column flow between 1 and 2 mL/min

7. Source temp 320-350 oC, Quad temp >= 180 oC

8. 9mm drawout or extractor lens

9. Self-Cleaning Ion Source

May 2014


Add Hydrogen Through Transfer Line

Hydrogen In

Use CI transfer line on EI MSD. Hydrogen flows concentrically around end of column into ion volume, the same path used for CI reagent addition

May 2014


Add Hydrogen to the Source (top view)Use CI transfer line on EI MSD. Hydrogen flows concentrically around end of column into ion volume, the same path used for CI reagent addition

Hydrogen in via CI transfer line

Repeller

Drawout (or extractor) lens

May 2014


PAHs on 2 different 7000B MS/MS systems, MRM

Dibenzo(a,l)pyrene, a late eluter

stock configuration

Optimized PAH Analyzer

Cou

nts

Cou

nts

May 2014


PAH 1000 pg Standard With ISTDs

4.00 6.00 8.00 10.00 12.00 14.00 16.00 18.00 20.00

20000

40000

60000

80000

100000

120000

140000

160000

180000

200000

220000

Time-->

Abundance

TIC: 1000_34_2.D\data.ms

May 2014


500 fg Dibenzo(a,l)pyrene : 3 Runs EachEach Run Separated By 6 Injections

75 uL/min H2 added

No H2 added

May 2014


0.750

0.800

0.850

0.900

0.950

1.000

1.050

1.100

1.150

norm

aliz

ed re

spon

se

pg inj

30 Mix PAH ISTDs, 9 mm DO With 75 uL/min H2 on SQ

Naphthalene D8Acenaphthene-d10Phenanthrene D10Chrysene-D12Perylene-d12

Continuous H2 addition

No H2addition

GC/MS PAH AnalysisPAH ISTDs, Cal Range 0.5-500 pg

May 2014


GC/MS/MS PAH AnalysisPAH ISTDs, Cal Range 1-1000 pg

Initial data

CCM Day 1

CCM Day 3

CCM Day 12

May 2014


Calibration Issues – Standard PAHsDibenzo(a,l)pyrene (1-1000 pg, R2 = 0.9785)

Rel

ativ

e R

espo

nses

Trying to fit the data to a straight line

Rel

ativ

e R

espo

nses

May 2014


Calibration in Continuous Clean ModeDibenzo(a,l)pyrene (1-1000pg, R2=0.99998)

Rel

ativ

e R

espo

nses Std PAH

Enhanced PAH

May 2014


GC/MS/MS PAH AnalysisR2 values for calibration 1-1000 pg, Cont. Cleaning Mode

R2 values for 5977A SIM with Continuous Cleaning are nearly identical to 7000B, across the same 1-1000 pg calibration range

Continuous ContinuousInitial Data Clean Initial Data Clean

R2 R2 R2 R2

Naphthalene 0.9982 0.9999 2,3-Dimethyl anthracene 0.9648 0.99991-Methyl naphthalene 0.9981 1.0000 Fluoranthene 0.9978 0.99992-Methyl naphthalene 0.9977 1.0000 9,10 Dimethyl anthracene 0.9726 1.00001,2-Dimethyl naphthalene 0.9974 1.0000 Pyrene 0.9846 1.00001,6-Dimethyl naphthalene 0.9976 1.0000 1-Methyl pyrene 0.9927 0.9997Acenaphthylene 0.9975 0.9999 Benz (a) anthracene 0.9976 0.9998Acenaphthene 0.9983 1.0000 Chrysene 0.9976 0.9999Fluorene 0.9976 1.0000 6-Methyl chrysene 0.9690 0.9998Phenanthrene 0.9972 0.9999 Benzo (k) fluoranthene 0.9954 1.0000Anthracene 0.9959 0.9999 Benzo (a) pyrene 0.9576 1.00002-Methyl phenanthrene 0.9846 0.9999 Dibenz (a,h) anthracene 0.9581 0.99992-Methyl anthracene 0.9846 0.9999 Indeno (1,2,3-c,d) pyrene 0.9642 0.99991-Methyl phenanthrene 0.9969 1.0000 Benzo (ghi) perylene 0.9965 1.00003,6-Dimethyl phenanthrene 0.9851 1.0000 Dibenzo (a,l) pyrene 0.9788 1.0000

May 2014


Optimized PAH Analyzer Summary Overview1. System and Method Improvements:

a) Linerb) Appropriate Temperaturesc) Backflushingd) 9mm drawout or extractor lense) Self Cleaning Ion Source

2. Analyzer Performance Results:a) Improved peak shapes, less tailingb) Consistent ISTD responsesc) Linearity improved to 0.999 - 1.000d) Sensitivity maintainede) Source stays clean indefinitely

May 2014


Controlled Substances Analyzers


May 2014

40

Analysis of Controlled Substances: ChallengesRoutine Seized Drug Analysis

Multiple sample types:• Pharmaceuticals: oxycodone, alprazolam, acetaminophen• Traditional drugs of abuse: heroin, cocaine, PCP• Botanical materials: marijuana, mushrooms • Syringe residues: heroin, morphine, fentanyl• Charred pipe residues: crack cocaine, hashish, methamphetamine

Analyte list constantly growing including novel psychoactive substances:• Synthetic cannabinoids: JWH-018, PB-22, AB-FUBINACA, XLR-11• Designer stimulants: MDPV, BZP, NBOMe compounds

May 2014


Analysis of Controlled Substances: ChallengesRoutine Seized Drug Analysis

Laboratory Needs:• Analyze complex mixtures by GC/MS• Efficiency of testing• Speed of analysis• High quality results• Time efficient data processing• Simple sample prepAnalytical Challenges• Samples of varying nature• Identify closely related analytes: isomers, analogs, etc.• Variable concentrations: column overload to trace concentrations• Complex matrix: botanicals, cutting agents, adulterants, non-volatile

compounds

May 2014


Current SituationRoutine Seized Drug Analysis

Expanding list of new drug targetsLong Cycle Times (23.0 Min)Carry-over interferences between samplesPBM Based SearchingSubjective Manual Data Review

• Manual Baseline Review and Spectral Subtraction• Variability of Results Through Different Reviewers (Data Bias)

Methods vary from lab-to-lab• Limited standardization of method

Inconsistent spectral libraries and retention timesCost of Analysis with Helium Carrier

May 2014


Need for New MethodRapid Identification of Seized Drug Samples

• Reduce Operating Expense

• Improve Sample Throughput

• Reliable and Robust Analytical Performance

• Consistent Identification Operator-to-Operator and System-to-System

• Up-to-Date Target List including Novel Psychoactive Substances

May 2014


Objective: Create a New Configuration Rapid Identification of Seized Drug Samples

• Reduce operating expense: Use hydrogen carrier gas• High speed analysis: Reduce cycle time• Ultra Inert Flow Path: Minimizes sample decomposition • Backflushing: Minimize column trimming and eliminate sample carry-over• Retention Time Locking (RTL): Precise RT matching column-to-column,

instrument-to-instrument, and lab-to-lab• Deconvolution Reporting Software: Rapid reliable compound

identification • Expand compound database: Comprehensive list of controlled

substances including new psycho active substances (synthetic cannabinoid, and “Bath Salt” compounds)

May 2014


Test Mix using Helium and Hydrogen SystemsAnalyzer Checkout Sample1 Amphetamine2 Phentermine3 Methamphetamine4 N-Propylamphetamine5 Pentobarbital6 10,11-Dihydrodibenz(b,f)(1,4)oxazepin-11-one

7 Cocaine8 Oxycodone9 Alprazolam10 Strychnine

2 3 4 5 6 7 8 9

12

3

4

5

6

7

89

10Original Helium Method

TIC: [BSB2]SAK10.D\data.ms

TIC: BCP45.D\data.ms

3 4 5 6 7 8 9

1

2 3

4

5

6 7

89 10 New Analyzer

Method

May 2014


Deconvolution Training StandardDeconvolution Reporting Software (DRS) Familiarization

3 4 5 6 7 8 9

What is this peak?First, use conventional approach of average spectrum and PBM search to identify it

5.2 5.3 5.4

May 2014


Probability Based Matching Identifies THCConventional Approach

• First hit is THC with 96 PBM match. • Second hit is hydrocodone with only

35 match

40 50 60 70 80 90 100 110 120 130 140 150 160 170 180 190 200 210 220 230 240 250 260 270 280 290 300 310 320 330 340 350 360

41 59 70 77 9196

107

115

121

128141147 155 165

174185

193199214

228

231

243

258

271

284

299

314

Average Spectrum

55 67 8191

107 115 128 147 165174 193 201 217

231

243

258

271

285

299

314

40 50 60 70 80 90 100 110 120 130 140 150 160 170 180 190 200 210 220 230 240 250 260 270 280 290 300 310 320 330 340 350 360

THC, 96 Match

May 2014


Peak Is THC, Right?How confident are you?

55 67 8191

107 115 128 147 165174 193 201 217

231

243

258

271

285

299

314

40 50 60 70 80 90 100 110 120 130 140 150 160 170 180 190 200 210 220 230 240 250 260 270 280 290 300 310 320 330 340 350 360

Hit 1:THC, 96 Match PBM

4244 5155

596870 7782

84 91

96

103

115

121

128

141 155162 171

185

188 199

214228

242

256 270 284

299

40 50 60 70 80 90 100 110 120 130 140 150 160 170 180 190 200 210 220 230 240 250 260 270 280 290 300 310 320 330 340 350 360

Hit 2: Hydrocodone, 35 Match PBM

40 50 60 70 80 90 100 110 120 130 140 150 160 170 180 190 200 210 220 230 240 250 260 270 280 290 300 310 320 330 340 350 360

41 59 70 77 9196107

115

121128

141147 155 165174

185

193199214 228

231

243

258

271

284

299

314

Average Spectrum

May 2014


Overlap of THC and HydrocodoneAs viewed in AMDIS

THC 5.281 min Hydrocodone 5.283 min

THC 314THC 271

Hydrocodone 185Hydrocodone 96

• Deconvolution finds 2 compounds closely merged together.• Peaks are separated by only 0.002 min. (Less than 1 scan)

May 2014


First Peak Found By AMDISTHC

Deconvoluted Spectrum at 5.281 min

THC, 95 Net Match

40 50 60 70 80 90 100 110 120 130 140 150 160 170 180 190 200 210 220 230 240 250 260 270 280 290 300 310 320 330 340 350 360

4153 60

69 8185

9195 107 121 129 141 153 165

174 187193 201211

215

231

239

243

258

271

285

299

314

55 67 8191

107 115 128 147 165174 193

201 217

231

243

258

271

285

299

314

40 50 60 70 80 90 100 110 120 130 140 150 160 170 180 190 200 210 220 230 240 250 260 270 280 290 300 310 320 330 340 350 360

AMDIS deconvolution confirms that the first peak is THC

May 2014


Second Peak Found By AMDISHydrocodone

40 50 60 70 80 90 100 110 120 130 140 150 160 170 180 190 200 210 220 230 240 250 260 270 280 290 300 310 320 330 340 350 360

42 5559 70 7782 89

9194

96

103

115

124

128141 155161 173

185

188 199214

228

243

256 270273

284

295

299

316

Deconvoluted Spectrum at 5.283 min

Hydrocodone, 95 Net Match

4244 51

5559

68

707782

8491

96

103

115

121

128

141 155162 171

185

188 199

214228

242

256 270 284

299

40 50 60 70 80 90 100 110 120 130 140 150 160 170 180 190 200 210 220 230 240 250 260 270 280 290 300 310 320 330 340 350 360

This peak would probably have been missed without AMDIS deconvolution

May 2014


DRS Report For Training SampleAutomated Deconvolution and Reporting

MSD Deconvolution ReportSample Name: THC/HCData File: D:\MassHunter\GCMS\1\data\HCOD_THC.DDate/Time: 17:18 Wednesday, Oct 2 2013

Adjacent Peak Subtraction = 1Resolution = HighSensitivity = MediumShape Requirements = Medium

The NIST library was searched for the components that were found in the AMDIS target library.

Retention Time (R.T.) Cas # Compound Name Chemstation AMDIS Match R.T.

DiffReverse Match

Hit Number

3.2702 51799327 N-Propylamphetamine 99 -1.3 91 1

4.6881 3158858 10,11-Dihydrodibenz(b,f)(1,4)oxazepin-11-one 97 -0.7 90 1

5.2479 521379 Cannabidiol 68 5.6 64 3

5.281 1972083 Delta-9-tetrahydrocannabinol (THC) 95 0.5 85 1

5.283 125291 Hydrocodone 95 0.2 88 1

5.3145 466999 Hydromorphone 78 -0.1 67 2

5.3637 521357 Cannabinol 67 0.8 55 4

Amount (ng) AMDIS NIST

Automated report generation takes about ~ 60 sec!

May 2014


Confirming Presence of Drugs of AbuseGC/MS DRS Controlled Substances Analyzer

• Retention Time Locked method ensuring reliable database matching

• Video training tutorials for easy learning about DRS and other advanced Analyzer features

• Quick-start guide and Application Note that guide you through operation of the screening method

• CD-ROM with analysis methods, data files, and reports

Toxicology DRS Screening GC/MS Analyzer

May 2014


Confirming Presence of Drugs of AbuseGC/MS DRS Controlled Substances Analyzer

Order an Agilent 5977A Series GC/MSD along with the following system option:• G3445B#472 Controlled Substances

Analyzer Helium Carrier Gas • G3445B#476 Controlled Substances

Analyzer Hydrogen Carrier Gas

Marijuana Sample with Synthetic Cannabinoids from Real World Forensics Lab Sample

AMDISRetention Time (R.T.) Cas # Compound Name Chemstation AMDIS Match R.T. Diff (sec) Reverse Match Hit Num.

3.2713 51799327 N‐Propylamphetamine 100 ‐1.2 89 14.6926 3158858 10,11‐Dihydrodibenz(b,f)(1,4)oxazepin‐11‐one 98 ‐0.4 93 15.2699 1972083 Delta‐9‐tetrahydrocannabinol (THC) 100 ‐0.1 95 15.3508 521357 Cannabinol 100 0 93 15.8397 864445432 JWH‐250 99 ‐0.8 89 16.2516 209414073 JWH‐018 96 ‐1 89 1

Amount (ng) NIST

Synthetic Cannabinoids

May 2014


Controlled Substances AnalyzerValue Overview for Customers

Retention Time Locking (RTL)• RT stability column-to-

column, instrument-to-instrument and lab-to-lab

Helium or Hydrogen Carrier Gas• Quantitation and

confirmation from three signals Scan, SIM, and NPD collected in a single run

CFT Post Column Backflush• Improved throughput

through shorter reduced cycle times, cleaner baselines and reduced system maintenance

Deconvolution Reporting Software (DRS)• Improved data quality

using fewer QA resources

New 460 compound data base including new Psychoactive Substances incl. Synthetic Cannabinoids and Bath Salts

May 2014


Blood Alcohol Analysis


May 2014

57

Blood Alcohol AnalyzerSystem OverviewHeadspace Sampler coupled to S/SL inlet

• Reproducible sampling across a wide calibration range

Dual Column-Dual FID configuration or Single Column GC/FID/MS• Provides differentiation of ethanol peak from potential contaminants

• Provides confirmation of ethanol presence with a single injection- MSD provide spectral confirmation

Retention gap with deactivated fused silica• Serves as guard column to protect analytical columns

• Easily replaced to facilitate maintenance

Un-purged splitter for dual column analysis• Replaces problematic two hole ferrules or “Y” splitters

- Eliminates leaks common to Y splitter- Overcomes uncertainty of two hole ferrules

• Precise reproducible split of sample between columns• Provides reliable split of flow between columns

May 2014


Model 7697A Vial Sampling PneumaticsDesigned to minimize carryover

May 2014


7890B GC

HSTrsfrLine

DB-ALC1

FID

Restrictor

5977 MSD

S/Sl

GC/FID/MS Configuration for Blood AlcoholHelium carrier gas

AuxEPC

May 2014


Capillary Flow Technology (CFT) 2-Way SplitterReproducible flow to both detectors

Effluent Splitter (2 Way)

Aux EPC in

DB-ALC1 Column in

MSD out

FID out

Competitive Advantage

May 2014


Split/Splitless ConnectionsReproducible transfer from the headspace sampler

Split/Splitless

Fused silica inserted through septum

Deactivated fused silica transfer line (0.53 mm ID)

Uses G3521A Weldment

Liner (1 mm): Ultra Inert #5190-4047

Transfer line (0.53 mm): Inert, #G3440-60015

Competitive Advantage

May 2014


TIC and FID Retention Time Alignment

n-propanolEthanolMethanol

2-propanolAcetone

MS

FID

May 2014


Ethanol LinearityFID and MS Performance

Real world data from Domestic Toxicology Laboratory (USA)• FID R2 0.9991• MS R2 0.9989

May 2014


Carry Over TestingPotential for Cross Contamination between Samples?

Multicomponent mix at 0.4% w/v ISTD Blank after 0.4% Multicomponent mix

No carry over following challenge with a high concentration!

TIC

FID

May 2014


Blood Alcohol AnalysisGC/FID/MS Blood Alcohol Analyzer Benefits

Blood Alcohol AnalyzerGC/FID/MS

• Rapid Cycle time to maximize sample throughput: less than three (<3) minute run time• Agilent proven EPC and CFTprovides reproducible split between FID and MSD• Defensible data through MS confirmation of ethanol presence with spectral comparison reporting • No carry over following challenge of the system with a 0.50% EtOH concentration sample

May 2014


Blood Alcohol AnalysisDual Channel Blood Alcohol Analyzer (GC/FID/MS)

Order an Agilent G3440B GC system with 5977A MS and the following SP1 Option:• 7890-0634 GC/MS/FID Blood Alcohol Analyzer

Calibration Curve for GC/FID/MSReal World Toxicology Laboratory

Collected Spectra

FID for Quantitation

NIST SpectralConfirmation

Link to Solution Portal Information

Custom Report: FID Quant, MS Confirmation

May 2014


Headspace Sampler Coupled to S/SL Inlet• Reproducible

sampling across a wide calibration range

CFT Purged Dual Column Splitter• Single column

analysis• Precise reproducible

split of flow between FID and MS

Detection with FID and Single Quad MS• Quantitation of

Alcohol content with the FID

• Simultaneous Spectral confirmation of ethanol presence

Custom Reporting with MS Spectra Comparison

GC/FID/MS Blood Alcohol AnalyzerValue Overview (7890-0634)

Less than three minute run time. Spectral confirmation of ethanol presence.

May 2014


Dual Channel GC/FID/FID Blood Alcohol AnalyzerValue Overview Analyzer, G3445B #683

Headspace Sampler Coupled to S/SL Inlet• Reproducible

sampling across a wide calibration range

Retention Gap• Serves as guard

column to protect analytical columns

• Easily replaced to facilitate maintenance

CFT Splitter• Replaces

problematic two hole ferrules or “Y” splitters

• Precise reproducible split of sample between columns

Dual Column-Dual FID ConfigurationServes as guard column to protect analytical columns• Easily replaced to

facilitate maintenance

Four minute runtime and no carry over with a 0.50% EtOH sample challenge

May 2014



Select GC Analyzers

May 2014

May 2014

70

Refinery Gas Analyzers with External Valve Oven


May 2014

71

Importance of Refinery Gases and RGAProcess Characterization Quickly and Reliably

• Produced from hydrocarbon cracking and distillation

• Typically contains saturated and unsaturated HCs (C1-C5)

– H2, O2, N2, CO, and CO2. – C1 - C6 or higher hydrocarbons – Sulfur contaminants, e.g., H2S

• Challenging analysis due to variable source and composition

• Producers require quick accurate analysis to monitor process

– Typically complex mixtures from a broad range of samples

May 2014


Introducing the 7890B Large Valve Oven Isothermal Zone for Valves and Columns

• Temperature control: - Independent control of LVO and GC

oven zones • Temperature Limit:

- Max 330˚C (valve and column dependent)• Valve configurations:

- Accommodates 4/6/10/14 port valves including Hastelloy valves

• Column Compatibility: - Large Mandrel: Accommodates 15 feet of

1/8 inch OD metal column - Small Mandrel: Accommodates 7 Ft of 1/8”

OD metal column

May 2014


6-port Valve

Variable Restrictor

Column Mandrel

12-port Valves

Valve or Mandrel Position

Introducing the 7890B Large Valve OvenIsothermal Zone for Valves and Columns

6 Internal Positions: Valves or Columns

- Up to six (6) heated valve positions

- Four (4) needle valve positions

- Uses 1 heated zone

May 2014


Large Valve Oven Features/BenefitsFeature6 position isothermal valve oven for actuated valves, microgasifiers, needle valves, and columns (including 1/8 in packed columns) with access to valves connections without removing actuators

BenefitOpen configuration that allows for easy maintenance; maximizing up-time. Also allows for multiple configurations for method development as well as set SP1 and configured

FeatureUse only one 7890B heated zone

BenefitCurrent multi-valve configurations may quickly consume 6 heated zones, LVO uses 5 leaving 1 for future applications

FeatureDual thermal zones allow for thermal isolation between column oven and LVO

BenefitAbility to configure analyses that require multiple thermal zones. Can run isothermal temperatures in the LVO while temperature ramping the GC oven

7809B with Large Valve Oven

May 2014


Fast RGA with Micropacked ColumnsGC/FID/TCD/TCD

Micropack System Flow DiagramMicropack LVO Plumbing

May 2014


Performance FeaturesLVO RGA Analyzers

Fast RGA Analyzer • Total run time is 8 minutes

- LVO at 70 °C• Hydrocarbons to C5 (C6+ backflush)• Permanent Gases• O2 and H2S

Compounds LimitHydrocarbons 0.01 Mol%Hydrogen Sulfide 500 ppmCarbonyl Sulfide 300 ppmHydrogen 0.01 Mol%O2, N2, CO, CO2 0.01 Mol%

Fast RGA with Large Valve Oven G3445B #532

May 2014


Fast RGA with Micropacked ColumnsAnalytical Performance – Hydrocarbon Channel (FID), LVO 70 °C

May 2014


Fast RGA with Micropacked ColumnsAnalytical Performance – Perm. Gas Channel (TCD), LVO 70 °C

1 2 3 4 5 6

May 2014


Fast RGA with Micropacked Columns – Helium CarrierAnalytical Performance

Compound Concentration RT AreaC6+ 0.06 0.027 0.28Methane (FID) 4.99 0.006 0.14Ethane (FID) 4 0.011 0.15n‐butane 0.3 0.045 0.15t‐2‐butane 0.3 0.059 0.171‐butene 0.3 0.059 0.21n‐pentane 0.1 0.038 0.20Hydrogen 12.1 0.036 0.15Oxygen 2.98 0.026 0.64Nitrogen balance 0.022 0.18Carbon Monoxide 1.52 0.035 0.15Carbon Dioxide 2.01 0.086 0.15Methane (TCD) 4.99 0.031 0.16Ethane (TCD) 4 0.09 0.16Hydrogen Sulfide 0.5 0.215 4.80

Repeatability of Select Refinery Gas Components(% RSD’s for retention times and areas with the large valve oven at 70 °C)

May 2014


High Capacity RGA with Micropacked ColumnsApplication Note

Packed Column Refinery Gas Analysis System Based on the Agilent 7890B GC System and G3507A Large Valve Oven

Publication Number: 5991-3534EN

May 2014


Fast RGA LVO AnalyzerValue Overview Analyzer, G3445B #532

Large Valve Oven• External Thermal

Zone• Isothermal

Operation• Up to 6 valves or

columns• Expands capability

of 7890

Micropacked Columns• Built for speed• Rapid 8 minute cycle

time

Isothermal Zone• Protect temperature

sensitive columns• Simultaneous

analysis of hydrogen disulfide (H2S) and oxygen (O2)

• Stable response for oxygen (O2)

Three Channel Analytical Method• Simultaneous

analysis of hydrogen hydrocarbons and permanent gases

Simultaneous analysis of O2 and H2S <8 Minutes

May 2014


Performance FeaturesLVO High Capacity RGA Analyzer

High Capacity RGA Analyzer• Total run time is 16 minutes.• Hydrocarbons to C5 (C6+ backflush)• Permanent Gases• O2 and H2S

Compounds LimitHydrocarbons 0.01 Mol%Hydrogen Sulfide 500 ppmCarbonyl Sulfide 300 ppmHydrogen 0.01 Mol%O2, N2, CO, CO2 0.01 Mol%

High Capacity RGA with Large Valve Oven G3445B #531

May 2014


High Capacity Refinery Gas Analysis with Std ColumnsGC/FID/TCD/TCD

Std Column LVO Flow DiagramStandard Column LVO Plumbing

May 2014


High Capacity RGA with Standard ColumnsAnalytical Performance - LVO at 70 °C

Hydrocarbon Channel

Permanent Gas Channel

Hydrogen Channel

May 2014


High Capacity RGA with Standard ColumnsApplication Note

Packed Column Refinery Gas Analysis System Based on the Agilent 7890B GC System and G3507A Large Valve Oven

Publication Number: 5991-3535EN

May 2014


High Capacity RGA LVO AnalyzerValue Overview Analyzer, G3445B #531


Zone• Isothermal



of 7890

Standard 1/8” Packed Columns• High capacity• Rapid 17 minute

cycle time

Isothermal Zone• Protect temperature

sensitive columns• Simultaneous

analysis of hydrogen disulfide (H2S) and oxygen (O2)


Three Channel Analytical Method• Simultaneous

analysis of hydrogen hydrocarbons and permanent gases

Simultaneous analysis of O2 and H2S. Capacity for higher concentration samples.

May 2014


3-in-1 Reformulated Fuels AnalyzersASTM D5580, D4815 and D3606


Analysis of Oxygenates and Aromatics in GasolineASTM D3606 – Benzene and Toluene in Gasoline

- official EPA method for benzene (0.1 - 5.0 vol%) and toluene (2 to 20 vol%) in gasoline

ASTM Method D4815 – Oxygenated Additives- 14 different ethers and alcohols from 0.1 to 15 wt%- usually only one or two oxygenates found in a sample

ASTM Method D5580 –Aromatics in Gasoline- measures benzene (0.1 to 5%), toluene (1 to 15%), C8 aromatics

(0.5 to 10%) C9 plus aromatics (5 to 30%), and total aromatics (10 to 80%)

- requires two injections per sample for complete analysis

May 2014


3-in-1 Gasoline Solution 7890B GC with Large Valve Oven (LVO)

• Larger capacity for valves, packed columns and micro-packed columns

• Flexibility for method using complex valve/column configurations

• Enables multiple methods to reside on a single GC- reduce instrument costs- run more samples in less lab space- 3-in-1 Gasoline Solution

• D3606• D4815• D5580

LVO

May 2014


3-in-1 Gasoline Solution – Detailed LVO Configuration

D3606 6-port Valve

Variable Restrictor

TCEP Micro-packed Column on Heated Mandrel

D4815 & D5580 12-port Valves

May 2014


GC Configuration for D4815 and D5580Similarities between each method• Same GC hardware requirements

- Inlets, detectors, plumbing and valve configuration• Same separation scheme

• 2-D separation using polar TCEP micro-packed primary column• 20% TCEP on 80/100 Chromosorb PAW, 22“ x 1/16“ stainless

Only one difference in instrument requirements • Non-polar capillary column

- D4815 – 2.65 m methyl silicone, 30m x 0.53mm- D5580 – 5 m methyl silicone, 30m x 0.53mm

May 2014


3-in-1 Gasoline Solution – Main Column OvenD3606 Packed Columns D4815 and D5580

Capillary Columns

• PDMS packed pre-column• Polar packed analytical column

• D4815 HP-1 (30 m x 0.53 mm x 2.65 m)

• D5580 HP-1 (30 m x 0.53 mm x 5.0 m

May 2014


7890 Instrument Conditions for D3606carrier gas heliumInlet Purge Packed @ 59.4 psiInlet temperature 200 Deg CInlet total flow 23 mL/min Septum purge flow 3 mL/minColumn flow 20 mL/min Aux pressure 35.5 psiTCD temperature 250 deg CLVO Temperature 60 deg CMain oven temperature 135 deg C isothermalBackflush time 2.5 min

LVO temperature remains stable with high main oven temperature

May 2014


LVO Fuels AnalyzerSummary Overview

New Large Valve Oven for the 7890B GC: • Provides greater capacity and flexibility for GC methods using complex valve configurations• Allows multiple ASTM methods to be configured on a single GC reduces costs and saves lab space

May 2014


D3606 – Precision and Accuracy for Work Bench Prepared Samples

Run Benzene Toluene1 0.98 5.002 0.98 4.983 0.97 4.984 0.98 5.00

*benzene = 1.00 vol% (+/- 0.02)*toluene = 5.00 vol% (+/- 0.08)

vol%*D3606 Check Sample

Meets ASTM repeatability specifications

Analysis results match known quantities in sample

Commercial Gasoline SampleVolume %

run benzene toluene1 0.337 5.5272 0.344 5.5233 0.344 5.5194 0.348 5.5245 0.347 5.4756 0.346 5.4837 0.344 5.5458 0.346 5.5069 0.348 5.55610 0.343 5.604avg 0.345 5.526

stddev 0.00323 0.03690RSD 0.938% 0.668%

r (exp) 0.005 0.129r (ASTM Spec) 0.020 0.186

May 2014


D5580 - Precision for WorkBench SamplesMeets ASTM Repeatability (r) Specifications

benzene toluene ethylbenzene m,p-xylene o-xylene C9 plus TotalRun 1 0.96 8.93 2.97 3.00 3.00 6.12 24.98Run 2 0.96 8.91 2.96 3.00 3.00 6.11 24.94 r (calc) 0.00 0.02 0.01 0.00 0.00 0.01 0.04 r (ASTM spec) 0.03 0.09 0.03 0.07 0.05 0.16 0.45



wt% Found in Gasoline Sample 1



May 2014


D4815 – Comparison of Manual and WorkBenchSample PrepManual Sample Prep• Add 0.5 mL DME to 10 mL volumetric flask• Record DME weight to 0.1 mg• Add sample to 10 mL mark• Record sample weight to 0.1 mg• Mix

Work Bench Sample Prep• Add 0.95 mL sample to an empty 2 mL vial• Record sample weight to 0.01 mg• Add 0.05 mL DME to sample in the 2 mL vial• Record DME weight to 0.01 mg• Mix

Gas1 wt% MTBE Gas2 wt% Ethanol Gas3 wt% EthanolManual Prep WorkBench Manual Prep WorkBench Manual Prep WorkBench

run1 13.15 13.18 6.01 6.08 10.47 10.55run2 13.13 13.12 5.98 6.13 10.58 10.66Avg 13.14 13.15 6.00 6.10 10.52 10.61

r (calc) 0.02 0.07 0.02 0.05 0.11 0.11r (spec) 0.21 0.21 0.18 0.18 0.25 0.25

May 2014


High Capacity Reformulated Fuel AnalyzerAnalyzer Overview, G3445B #621


Zone• Isothermal



of 7890

Multiple ASTM Methods on a Single GC• D 4815, D5580 and

D3606• Rapid change over

between methods

Thermal Isolation from Main Oven• Protect temperature

sensitive columns• Higher main oven

temperature (135 deg C) has no effect on lower LVO temperature (60 degC)


7696A Sample Prep Workbench• Automates sample

preparation (ISTD addition)

• Provides reproducibility that meets or beats ASTM method requirements


May 2014


Ultrafast Simulated DistillationApplication of the Low Thermal Mass (LTM) Module


May 2014

100

Fast Simulated DistillationDesigned for ASTM D7798

• For the determination of boiling range distribution of petroleum products and biodiesel (B5,B10,B20)

• Applicable to petroleum distillates having a final boiling point not greater than 538 C

• Difference between initial BP and final BP must be greater than 55 C

• Not applicable to naphthas, reformates, gasolines or full range crude oils

• Tested in the factory. LTM Column and LTM Transferline will ship pre-assembled as 1 module.

May 2014


LTM ‐ Low Thermal Mass Technology

“Fast Temperature Ramps”“< 400oC/min Typical <400oC/min

Temperature Range 120 V Oven Fast Ramps Insert ** (°C) (°C/min) > 200 V, 15A > 200 V, 15A50 to 70 75 120 12070 to 115 45 95 120115 to 175 40 65 110175 to 300 30 45 80300 to 450 20 35 65

* * Requires G2646-60500

LTM Cooldown Times (Standard Size)

0

50

100

150

200

250

300

350

400

0 50 100 150 200 250

Time (sec)

Tem

p (o

C)

2m LTM5m LTM10m LTM7890 GC

“Fast Cool-Down”

May 2014


pA

0

1000

2000

3000

4000

5000

6000

min0.25 0.5 0.75 1 1.25 1.5 1.75 2 2.25

C5

C6 C

7C

8 C 9C

10

C11

C12

C14

C15

C16

C17

C18

C20

C24

C28 C

32

C36

C40

pA

min0.25 0.5 0.75 1 1.25 1.5 1.75 20

500

1000

1500

2000

Fast Simulated Distillation Under 3 Minutes Using LTM… 6x faster compared to conventional ASTM D2887 procedure

ASTM D2887 Reference Oil

LTM Module : 45ºC to 350ºC at 150ºC/min

Faster than conventional GC (75-120oC/min max)

Calibration sample C5-C44

LTM Module : 45ºC to 350ºC at 150ºC/min

May 2014


Repeatability: RGO with Split/Splitless @ 160 C/minTemperatures in °F

% OFF 1 2 3 4 5 6 7 8 9 10 AVG RSD %RSD ASTM DIFF °F0.5 238 239 238 238 239 238 238 239 239 239 239 0.53 0.0022 13.7 2405 302 302 302 302 302 301 302 302 303 302 302 0.47 0.0016 6.8 304

10 346 345 346 346 346 345 345 346 348 348 346 1.10 0.0032 7.4 34815 394 391 394 393 393 392 393 394 395 395 393 1.26 0.0032 8.1 39320 436 432 436 435 435 434 434 436 437 437 435 1.55 0.0036 8.7 43525 470 467 470 470 470 469 469 471 471 471 470 1.23 0.0026 47030 499 496 499 499 499 497 498 500 500 500 499 1.34 0.0027 8.4 49935 527 525 527 527 527 526 526 528 528 528 527 0.99 0.0019 52740 552 550 552 551 552 551 551 553 553 553 552 1.03 0.0019 7.7 55245 575 575 575 575 576 575 575 576 576 576 575 0.52 0.0009 57650 595 594 594 594 595 594 594 596 595 595 595 0.70 0.0012 7.7 59455 611 610 611 610 611 610 610 612 611 611 611 0.67 0.0011 7.7 61160 628 628 628 628 628 628 628 629 628 628 628 0.32 0.0005 7.7 62965 649 649 649 649 649 649 649 649 649 649 649 0.00 0.0000 7.7 64970 668 668 668 668 668 668 668 670 669 669 668 0.70 0.0010 7.7 66875 690 690 690 690 690 689 690 691 690 690 690 0.47 0.0007 7.7 69080 712 712 712 712 712 712 712 713 712 712 712 0.32 0.0004 7.7 71285 736 736 736 736 736 736 736 736 736 736 736 0.00 0.0000 7.7 73690 764 764 764 764 764 763 764 765 765 765 764 0.63 0.0008 7.7 76495 803 803 803 803 803 803 803 804 804 804 803 0.48 0.0006 9 803

99.5 881 881 881 881 882 881 881 882 882 882 881 0.52 0.0006 21.2 888

ASTM DIFF = Allowable difference (+ or -) from last column

May 2014


Examples of Calibration and %Off Reports

May 2014


Cracked Gas Oil Engineering Report

May 2014


LTM Simulated Distillation AnalyzerAnalyzer Overview, G3445B #658

Low Thermal Mass (LTM) Oven• Rapid temperature

programming, up to 1800 ºC/min

• Fast cooling allows for rapid cycle times

• Constant flow mode for very good retention time repeatability

Configured per Industry Standard• ASTM D2887• Round Robin review

underway

Available with Various Inlet Options• Multi-Mode Inlet• Split/Splitless Inlet• User defined within

Analyzer configuration

Simulated Distillation Software• Intuitive Graphic User

Interface (GUI)• Rapid analysis and

report generation• Interfaces with

ChemStation for report automation


May 2014


Analyzer Information

Product Flyers Solution Brochure 5991-1093EN

HPI Solution Guide5991-1561EN

GC Analyzer Webpagewww.chem.agilent.com/en-US/Products-

Services/Instruments-Systems/Gas-Chromatography/Pages/default.aspx

MS Analyzer Webpagewww.chem.agilent.com/en-US/Products-

Services/Instruments-Systems/Mass-Spectrometry/Pages/default.aspx

May 2014


The Value of Analyzer Solutions

Preconfigured and analytically tested

Consistent identification of drug targets operator-to-operator and lab-to-lab

No instrumentalmethod development.

May 2014


Analyzer Value to CustomersHelping customers enhance their competitive advantage

Alleviate Resource PressureAlleviate Resource Pressure

Guaranteed MethodGuaranteed Method

Optimized PerformanceOptimized Performance

Advanced TechnologiesAdvanced Technologies

Quicker Deployment and ReturnQuicker Deployment and Return

May 2014


Questions…Thank you for your attention

May 2014


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