Firma:              Hewlett Packard

Modell:            GC/MS System

Kommentar:   Dokumente engl. (für IDNR 11139)

HP GC 5890 II

HP 5890 Series II and HP 5890 Series II Plus Gaschromatographs

(Note: The HP 5890 II Plus is a version of the HP Series II configured specifically for the use of EPC).

Technische Daten

Instrument Dimensions and Weight

Height:                  18-3/8 inches (465 mm)

Width:                   25-7/8 inches (655 mm

Depth:                   20-1/8 inches (511 mm)

Weight:                 90 pounds (41 kg)

Power Requirements:

Voltages:              120/200/220/240

Range:                  +5, -10% each

Frequency:           47.5-66 Hz

Consumption:       2200 VA max

Output:                 7500 Btu/hr max

Environmental

Operating range is: 0-55°C ambient (20-27°C optimum)

5-95% humidity (50-60% optimum)

Heated Devices

Five heated zones standard: Two detectors

                                               Two inlets

                                               One auxiliary

Methods stored:                      Two

Flow Sensor (not available with EPC or Series II Plus)

Range.-                0-35 sccm [sccm = standard cc/minute]

Accuracy:             ± 3 sccm für He and H ₂

                            ± 5 sccm for N ₂ and ArCH ₄

Extended range:   100-150 sccm

Accuracy:             ±15 sccm

Detector Signal

For external processing by a recorder, integrator, or computer:

Signal Path	Signal Bandwidth	Minimum Peak Width*
INET digital	4 Hz	0.32 sec
0-1 mV analog	~ 4 Hz**	**
0-1.1 V analog	2.6 Hz	0.50 sec

* That can be calculated accuratey by an external measuring device (e.g., integrator) operating at ≥ 4-Hz bandwidth frequency.

**Actual bandwidth depends on the input impedance of the measuing device.

Standard Inlets on the HP 5890 Series II

Split/Splitless Capillary

Paked witb Septum Purge

Temperature-Programmable

Cool On-Column Capillary

Detectors

Thermal Conductivity Detector

Electron Capture Detector

Flame Ionization Detector

Nitrogen Phosphorus Detector

Flame Photometric Detector

Column Oven

• Usable volume:      11 in. x 12 in. x 6.5 in. (h x w x d)

                                279 mm x 305 mm x 165 mm (h x w x d)

• Column span:        228.5 mm, 9 in. (coil size)

  •                                                  Automatic cooling under processor control

  •                                                  Operatmg range:   4°C above ambient to 450°C:

- 80 to 450°C with cryogenic cooling

                                • Setpoint entry: 1°C for temperatures

                                                    0.1°C for programm rates

• Programming:        Rates 0.1 to 70°C per min

                                650 min maximum run time

Three ramps with initial/final holds

*Achievable rates depend on zone temperature, voltage and columns.

Technical Performance

Accuracy (true temperature relative to setpoint)

Specification:   ±1% (°K) from 4°C above ambient to 450°C

Stability (effect of ambient change on actual temperature)

Specification:       <0.01°C for 1°C ambient change

Calibration (setting true temperature at a setpoint)

Oven can be recalibrated to ± 0.01°C with appropriate instrumentation

Gradients (temperature variations within a column)

Specification: less than 2°C within a 9-in. coil anywhere within the operating range

HP MSD 5971 A

General Description

The HP 5971A Mass Selective Detector (MSD) is a stand-alone capillary GC detector designed for use with the HP 5890A gas chromatograph. It is compact and portable (mainframe weighs 21 kg), requires no cooling water or compressed air, and operates on 110/120 volts or 220/240 volts power. The MSD mainframe includes the GC interface, electron irnpact ion source, monolithic quartz hyperbolic quadrupole mass filter, electron multiplier detector, power supply, drive electronics, and analyzer vacuum system. The MSD is configured for a right-side sample inlet.

General Specifications

The MSD is controlled from an HP 59970C ChemStation (Pascal Series) which includes a computer, disc drive and printer. Operating software provides a complete set of MSD and GC/MS applications including programs for Tuning, Data Acquisition, Data Retrieval, Reporting and Library Searches.

Installation and 90-day warranty are provided. Operator training is highly recommended and a good understanding of capillary chromatography is useful.

Mass Selection: Scanning mode-Scan any mass range between 10 and 650 amu in 0.1 amu steps. Up to three mass ranges may be selected using time programming.

Resolution: Unit resolution throughout mass range established automatically under computer control.

Scan Speed: Instrument provides for scan rates up to 2000 amu/sec with 0.1 amu mass resolution.

Scanning Acquisition Process: Sample flows from GC into ion source where it is constantly bombarded by 70 eV electrons, causing molecules to fragment and ionize. Positive ions are focused into the quadrupole mass filter by the lens system. An AC 1.0 MHz voltage and a DC voltage are superimposed in an accurately controlled ratio on the quadrupole. The voltages are stepped to allow an ion with a specific m/z value to pass through the filter while all others are rejected. At each quadrupole filter voltage step, the amplified electron multiplier detector output is digitized and read by the Series 300 Computer through the GPIO interface.

Total Ion Mode: AC voltage-only mode, with adjustable low mass cut-off, allows the HP 5971A to operate as a non-spedfic, high sensitivity detector.

Sensitivity: Typical performance for 1 ng of methyl stearate yields a signal-to-noise ratio of better than 20:1 at m/z 298.3 when scanned at 380 amu/sec between m/z 290 and 310.

Selected Ion Monitoring Mode: Monitors up to 20 individually selected masses at one time. Up to 200 groups of 20 masses may be selected for each nm using time programming.

Dwell Time: User selectable from a minimum of 10 milliseconds per m/z value up to a maximum of 32,767 milliseconds.

Selected Ion Monitoring Acquisition Process: Rather than dividing the mass range into 0.1 m/z increments and recording information at each m/z, a different acquisition process is used for selected ion monitoring. The quadrupole mass filter is programmed to select a few specific m/z values rather than scanning large areas with no signal present. Since only a few areas of the total m/z range need to be measured, the GC peak is sampled more often, resulting in more accurate quantitation.

Sample flows from the GC into the ion source, and is constantly bombarded by 70 eV electrons, causing the molecules to fragment and ionize. Positive ions are focused into the quadrupole mass Elter by the lens system. An AC 1.0 MHz voltalte and the DC voltage are superimposed to the correct ratio for the first user-specified m/z value. The amplified electron multiplier detector output is digitized and accumu­lated for the duration of the user-specified dwell time. At the end of all m/z settings, the pro cess is repeated again beginning from highest m/z value to lowest until the end of the run is reached.

Sensitivity: Typical performance in selected ion monitoring: 10 pg of methyl stearate when monitoring m/z 298.3 for a dwell time of. 50 milliseconds, with a 10:1 signal-to-noise.

Detector: Continuous dynode electron multiplier. Power supply to the multiplier is computer contralled. Maximum voltage is 3000 volts, settable in 12.5 volt increments.

Ion Source: Electron impact source with electron energy of 70 eV. Two filaments are selectable under computer control to allow continued operation in the event of filament failure. Complete source is remov­able as an assembly for convenient cleaning.

Dynamic Range: An FET logarithmic preamplifier provides morethan six decades of dynamic range.

Mass Axis Stability: ±0.15 amu in 12 hours assuming normal operating temperature, adequate ion statistics, and thermal equilibration of electronics.

Vacuum System: Analyzer vacuum is maintained by an aircooled diffusion pump backed by a two-stage direct drive mechanical pump. Overall system pumping speed is approximately 60 liters per second for helium. Vacuum system can accommodate a capillary flow rate of 1.0 atm cc per minute of helium. Pump-down from (or venting to) atmosphere requires approximately 10 minutes. Time to reach operating temperature (or cool down for venting) is approximately one hour. Pump down/vent cycle is completely automated via computer control.

Optional ion gauge controller monitors pressure in the high vacuum chamber up to 1 X 10-3 tonr. Typical chamber pressure is 5 X 10-5 torr at 0.5 cc/min. of helium.

Safety Features: Automatic interrupt system provides protection against damage due to excess signal level or 1-IV failure, as well as filament or RFPA failure.

In addition, system operating voltages are interlocked with the vacuum pump to prevent instrument damage due to operation at excess pressure (low vacuum).

Temperature Control: Interface temperature is controlled by the gas chromatograph through the B Detector zone Controller. Other exter­nal temperature controI is also possible.

The analyzer and ion source are heated by the MSD interface. Ion source temperature is sensed by a thermocouple and reported to the data system.

Recommended interface operating temperature is from 250 to 300°C.

Two Interfaces:       GC Capillary Direct       -            9" (229 mm)

                                 Infrared Detector           -            19" (457 mm)

Temperature Environment: The MSD will operate within specifications in a temperature environment of 15 to 35°C.

Carrier Gas: A regulated supply of high purity GC Cartier gas is required. Minimum purity of 99.9995% is recommended. Molecular sieve trap is also recommended.

Calibration Valve: Computer-controlled solenoid valve provides automated calibration with reference compound.

Utilities

Power: Detector mainframe operates an 99-127 volts or 198-254 volts, single-phase, 700VA. Line frequency is 48-66 Hz.

Heat Dissipation: 2400 BTU/hr.; 3000 BTU/hr, including transfer live.

Size and Weight Detector Mainframe

Height:        34 cm (13.5 in.)

Width:         17 cm (6.5 in.)

Depth:         65 cm (25.75 in.)

Weight:       21 kg (46 lb.) mainframe

                  32 kg (70 lb.) mainframe plus forepump.

HP HS 7694

Static headspace sampling is a versatile technique for determining the volatile content of heterogeneous samples. Headspace sampling is particularly useful when the sample matrix is solid or when direct injection into a gas chromatograph (GC) is difficult because the sample would normally require preparation before analysis.

To this point, analytical laboratories have analyzed volatile components in sample rnatrixes using traditional sample extraction techniques. These techniques are time­consuming, expensive, and require special handling of solvents.

But with new demands for greater productivity, cost savings, and environmental responsibility, analytical laboratories have placed increased emphasis on the value of static headspace sampling to:

•   Eliminate the need for lengthy, labor-intensive sample preparation tasks.

•   Prescreen samples quickly and efficiently.

•   Minimize the use of hazardous solvents that can require special handling and time-consuming, expensive disposal procedures.

Now, Hewlett-Packard brings the new technology of Electronic Pressure Control (EPC) to headspace sampling and the benefits of single-point control of the entire GC system. With the HP 7694 Headspace Sampler, Hewlett-Packard offers you:

•   Greater reproducibility from run to run and user to user.

•   Maximum performance and ease of use for any user skill level.

•   Easier compliance with Good Laboratory Practice (GLP) requirements.

The HP 7694 Headspace Sampler is available in two versions: electronic pressure control or manual flow control.

Electronic Pressure Control Enhances Reproducibility

The EPC version of the HP 7694 Headspace Sampler is for dedicated use on the HP 5890 Series II Plus GC which features electronic pressure control.

Pressures and flows are critical parameters affecting the precision of your headspace analysis. Combining the HP 7694 Headspace Sampler with EPC improves pressure and flow stability from run to run and user to user. EPC ensures precise control of analyte transfer to the GC inlet and column during sampling. This offers precise quantitative reproducibility for compounds of interest.

Single-Point Control Integrates the Entire GC System

Complete control of the HP 7694 Headspace Sampler and your HP 5890 Series II Plus GC can be achieved with the HP 3365 Series II ChemStation. The HP ChemStation provides PC control of instrument parameters, runs sequences, generates reports, and stores data - all from one PC.

The HP 3396 Series II

Integrator can also be used for single-point control of the entire GC system, including the HP 7694 Headspace Sampler.

Single-Point Control with EPC Provides Electronic Storage and Retrieval of All Critical Parameters

Combining the HP ChemStation single-point control with the EPC version of the HP 7694 Headspace Sampler provides a new dimension in Good Laboratory Practice. Now, pressure parameters and methods can be stored electronically to ensure exact reproducibility - from run to run and user to user. Printed chromatographic results can show the critical parameters to meet GLP requirements for analysis in environmental, drug testing, and other applications in regulated industries.

Manual Flow Control for Any Gas Chromatograph

The HP 7694 Headspace Sampler is also available as a self-eontained, transportable standalone unit for use an manual pressure control gas chromatographs. An easy-to-use keypad provides access to headspace parameters.

Inert Sample Pathway Reduces Sample Degradation

Both versions of the HP 7694 Headspace Sampler minimize sample degradation with a chemically inert pathway extending from the sample loop to the column head.

Standard nickel sample loops and transfer lins provide the high level of inertness needed by most standard headspace applications.

However, many applications are highly vulrierable to corrosive action or compound degradation from active sites in the sample pathway. For maximum protection, Hewlett-Packard offers an optional Silcosteel® treatment of sample loops, transfer line, and inlet.

GC Inlet Design Provides Flexibility

A flexible HP 5890 Series II GC inlet design provides direct headspace injection into capillary or packed columns. Moreover, small volume syringe injections of calibration standards are easy, with no removal of the headspace sampler's transfer line required.

HP 7694 Headspace Sampler

Specification Guide

Heated Zones

Oven temperature range                            40°C to 200°C, ± 0.2°C

Loop temperature range                             40°C to 200°C

Transfer line temperature range                 40°C to 220°C

Event Times

Sample heating time range                        0 to 999.9 min

GC cycle time                                             1 to 999.9 min

Vial equilibration time                                  0 to 999.9 min

Pressurization time, loop fill time,              0 to 99.99 min

loop equilibration time, injection time

Pressure Parameter

Maximum vial pressure                              100 psi for standalone and EPC-ready headspace

Transfer Line

Transfer line material                                  Nickel standard, Silcosteele optional

Transfer line length                                     80 cm standard, 100 cm optional

Transfer line diameter                                0.030 in.

Sample Loop

Sample loop material                                  Nickel standard, Silcosteel® optional

Sample loop capacities                              1-rnl and 3-mI loops

Vials

Vial size                                                      10 ml, 20 ml

Vial capacity at ambient temperature         44 ml

Vial capacity in headspace oven                6

Maximum fill volume

                                               10ml             8ml

                                               20 ml            17 ml

Vial Agitation

Constant shaking time, standard               Low, high, off

Communication Protocols

RS-232                                                       All Standard

BCD out

Remote output

Check GC ready

Instrument Control

25-key on-board user interface                  Standard

HP 3396 Series II integrator                        Optional

with APPack

HP 3365 Series II ChemStation                  Optional

Sampling

Sampling mechanics                                  Valve/loop/pressurized vial

Sampling Mode

CHT                                                            Standard

MHE                                                            Standard-up to ten extractions per vial; single-and      multi-puncture

Method Optimazation

Optimization of oven temperature              Standard-via parameter

Optimization of sample equilibration time increment function

Method Storage

Via keyboard                                               4

HP 3398 Series II integrator or                   Through method file

HP 3365 Series II ChemStation

Columns

Column size compatibility                          All calurans

Physical Specifications

Power requirements                                   600 VA maximum

Line voltage                                                 100/115 ± 10 %

                                                                   220/230/240 ±10 %

Dimension                                                  Height      19 in.

                                                                   Width       16.5 in.

                                                                   Depth      17.5 in.

                                                                   Weight     76 lbs

Safety

Certification                                                 CSA C22,2 No. 151-M1986,

                                                                   IEC 1010-1:1990+A1/EN 61010-1:1993

Environmental

Storage temperature                                  -40°C to 70°C

Operation temperature                               10°C to 45°C

Humidity                                                      0 to 95%

Gerstel LVI

The Large Volume Injector LVI was developed to permit the substances from large-volume, highly diluted samples to be concentrated an-line in conjunction with the CIS 3.

Important notes:

The Large Volume Injector LVI is only operable in conjunction with the CIS 3.

The injector LVI must be aligned with the septumless sampling head of the CIS 3.

Investigations in the trace

range necessitate a gas postcleaning system, e.g. the Megasorb System.

Gerstel CIS

Cooled Injection System CIS

For cold sample injection and subsequent vaporisation with freely programmable temperature paths and two freely selectable temperature plateaus.

Operating Instructions

The GERSTEL cooled injection system, abbreviated to CIS in the following, combines the advantages of various well-known injection methods and can be used for all tasks which previously required a split, on-column or cool-on­column injection system. The sample is injected into a special injector chamber which is not heated until injection has been completed; depending on the tasks involved, heat-up rates of between 2 and 12°C/sec. and two consecutive temperature plateaus can be pre-selected. The temperature of the injector chamber can be reduced by a built-in Peltier element, a CO ₂ cooling system (optional extra) down to -78°C or by an N ₂ liquid cooling System (optional extra) down to -150°C for the injection of low-boiling substances. The injection temperatures which can be achieved through the cooling capacity of the Peltier element depend on the insulation of the gas chromatograph; at an oven temperature of 70°C an injection temperature of 30°C can be attained. With well insulated gas chromatographs considerably greater temperature differences between the oven and the injector chamber can also be achieved.

Gerstel TDS

The Thermodesorption Unit TDS was developed to permit volatile and semi­volatile substances in gaseous and vaporous samples to be concentrated online and offline in conjunction with the CIS 3.

Important notes:

The Thermodesorption System TDS 1 can only be operated in conjunction with the CIS 3.

The Thermodesorption System must be aligned with the septum less sampling head of theCIS 3.

Analyses in the trace range necessitate a gas post-cleaning system, e.g. the Megasorb system.

Gerstel HSS/HSI

Der Headspacesampler HSS / HSI wur­de entwickelt, um flüchtige und semi­flüchtige Substanzen in wässrigen Pro­ben in Verbindung mit dem KAS 3 online anreichern zu können.

Wichtige Hinweise :

Der Headspacesampler HSS / HSI ist nur zusammen mit dem KAS 3 betriebsbereit.

Der Headspacesampler HSS / HSI muß mit dem septumfreien Auf­gabekopf des KAS 3 ausgerichtet sein.

Untersuchungen im Spurenbereich erfordern ein Gasnachreinungs­system z.B. das Megasorbsystem.