6890 Standard Operating Procedures G1530-90380

Standard Operating Procedures

The HP 6890 SeriesGas Chromatograph

Little Falls SiteHewlett-Packard Company2850 Centerville RoadWilmington, DE 19808-1610

Hewlett-Packard Company1995

All Rights Reserved.Reproduction, adaptation,or translation withoutpermission is prohibitedexcept as allowed undercopyright laws.

HP part numberG1530-90380

First Edition:November 1995

Printed in USA

Warranty

The information contained in thisdocument is subject to changewithout notice.

Hewlett-Packard makes nowarranty of any kind withregard to this material,including, but not limited to,the implied warranties ormerchantability and fitnessfor a particular purpose.Hewlett-Packard shall not beliable for errors contained hereinor for incidental or consequen-tial damages in connection withthe furnishing, performance, oruse of this material

Safety Information

This manual contains safetyinformation that should befollowed by the user to ensuresafe operation.

WARNING

A warning calls attention to acondition or possible situationthat could cause injury to theuser.

CAUTION

A caution calls attention to acondition or possible situationthat could damage or destroy theproduct or the user’s work.

The HP 6890 Series GasChromatograph OperatingManual supplied with theHewlett-Packard 6890 gaschromatograph (HP GC) con-tains WARNING and CAUTIONmessages that inform the userabout potential hazards thataccompany working on and/oroperating the instrument. Referto them for complete safetyinformation.

Table of Contents

Overview...................................................................................................................................... 1

Using This Handbook.................................................................................................................. 2

BASIC MAINTENANCEColumn Adapter/Makeup Gas Fitting, Installation.................................................................... 3

Column Installation..................................................................................................................... 9

Liner/Insert, Installation ............................................................................................................. 17

Inlet Septum, Installation............................................................................................................ 23

FID CHECKOUTSFID (Flame Ionization Detector) Checkout Using a Packed or Purged Packed .....................Column Inlet

27

FID (Flame Ionization Detector) Checkout Using a Split-Only or Split/Splitless ...................(in Split Mode) Capillary Column Inlet

41

FID (Flame Ionization Detector) Checkout Using a Cool On-Column Capillary ....................Column Inlet

55

TCD CHECKOUTSTCD (Thermal Conductivity Detector) Checkout Using a Packed or Purged Packed ...........Column Inlet

67

TCD (Thermal Conductivity Detector) Checkout Using a Split-Only or Split/Splitless .........(in Split Mode) Capillary Column Inlet

79

TCD (Thermal Conductivity Detector) Checkout Using a Cool On-Column Capillary ..........Column Inlet

91

ECD CHECKOUTSECD (Electron Capture Detector) Checkout Using a Packed or Purged Packed ..................Column Inlet

103

ECD (Electron Capture Detector) Checkout Using a Split-Only or Split/Splitless ................ (in Split Mode) Capillary Column Inlet

115

ECD (Electron Capture Detector) Checkout Using a Cool On-Column Capillary .................Column Inlet

127

Table of Contents

NPD CHECKOUTSNPD (Nitrogen Phosphorus Detector) Checkout Using a Packed or Purged Packed ............Column Inlet

139

NPD (Nitrogen Phosphorus Detector) Checkout Using a Split-Only or Split/Splitless .......... (in Split Mode) Capillary Column Inlet

153

NPD (Nitrogen Phosphorus Detector) Checkout Using a Cool On-Column Capillary ...........Column Inlet

167

1

Overview

The following procedures are protocols and criteria developed by Hewlett-Packard as part of thequality system used for the HP 6890 Series gas chromatograph (GC) manufacturing process. Theintent is to recommend a means for the user to review if a given HP 6890 Series GC continues toperform according to the original chemical checkout testing expectations.

In performing these protocols, please be aware that the following procedures were developed andtested on new instruments that were free from the effects of usage and time. Under normaloperating conditions, these instrument checkout testing expectations should serve as a usefulguideline or model for integrating performance operating procedures into individual laboratorystandard operating procedures (SOPs). However, these SOPs alone cannot determine completelyif an instrument is not performing to its intended capabilities.

This book is not intended to be used as a substitute for any regulatory requirements. They shouldbe addressed by the user in his/her perspective laboratory environment. It should, however, serveas a useful reference document when creating SOPs based on individual preventive maintenancepractices surrounding the HP 6890 Series GC instrument.

As a single-point measurement method, meeting acceptance criteria described in these SOPs doesnot necessarily assure performance capability required for any given analytical method the usermay wish to use. Performance capability for any given analytical method must be demonstratedseparately within the context of that method. Therefore, the SOPs given in this book are writtenas suggested guidelines that are independent of any method for performance checks.

For specific operating or maintenance questions, please refer to the HP 6890 Series GasChromatograph Operating Manual (HP part no. G1530-90310) or the HP 6890 Series GasChromatograph Maintenance and Troubleshooting Manual (HP part no. G1530-90320).

2

Using This Handbook

This handbook contains standard operating procedures (SOPs) for the HP 6890 Series gaschromatograph (GC). These SOPs include procedures and good laboratory practices (GLPs) thatapply to operation and maintenance of the HP 6890 Series GC.

The SOPs carry the following information on each page:

• Date of issue

• Page number

• Number of pages in the SOP

The SOPs have open fields for you to add information specific to your company. On each page ofthe SOPs, you can add a procedure number. On the first page of the SOPs you can add:

• Company name and official stamp

• Procedure number

• Revision number

• Replacement revision number

• Authorizing person

• Reviewing person

• Effective date

• Distribution list

Column Adapter/Makeup Gas Fitting, Installation

Revision Date 9-Jan-98 Procedure no.:________________ Hewlett-Packard Company

3

Standard Operating Procedure

Title: Column Adapter/Makeup Gas Fitting, InstallationProcedure Number: ___________________________________________________________________

Revision Number: ____________________________________________________________________

Replaces Revision: ___________________________________________________________________

Approved by: ________________________________________________________________________

Reviewed by: ________________________________________________________________________

Effective Date: _______________________________________________________________________

Company Stamp:

Distribution List:• __________________________________________________________________

• __________________________________________________________________

• __________________________________________________________________

• __________________________________________________________________

• __________________________________________________________________

• __________________________________________________________________

Page 1 of 6


4

Scope

Use the following procedure to install an appropriate column or makeup gas adapterproperly in various inlet and detector types.

Instrumentation

This SOP applies to all HP 6890 Series GCs and standard inlet and detector options.

General Overview

All the detectors are normally shipped with the hardware installed for capillary columnuse. With the capillary-only bases for the flame ionization detector (FID) and nitrogen-phosphorus detector (NPD), it is not possible to install packed columns. However, withthe thermal conductivity detector (TCD), electron capture detector (ECD), and thepacked FID and NPD detector bases, packed columns can be used by changing (orremoving) the adapter to accommodate a variety of column types. The following“Comments, General” section is for both general considerations and those associatedwith specific inlet and detector types.

Related SOPs

• Liner/insert, installation, SOP no. _____________

• Column, installation, SOP no. _____________

References

HP 6890 Series Gas Chromatograph Operating Manual, “Column Installation” section,HP part no. G1530-90310

Comments, General

With the exception of the TCD, all adapters have a 1/4-inch in outer diameter. Those forthe TCD have a 1/8-inch outer diameter. All adapters are inserted fully into the inlet ordetector in installation.

In all cases, installation of a nut and ferrule to obtain a gas tight seal is best done byfirst finger tightening to ensure no cross-threading occurs. If the nut does not turneasily by fingers, it is often evidence of distorted threads caused by overtighteningand/or by extended high-temperature exposure in prior installations.

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5

Overtightening the nut during installation may distort/damage the sealing ferrule to thepoint where a leak-free seal cannot be achieved no matter how tight. Follow vendorrecommendations for the particular ferrule.

Note that tightening recommendations are often different for installation of an adapterwith a new ferrule as opposed to those for reinstalling an adapter with an existingferrule from a previous installation. Generally, you do not tighten a preset ferrule to thesame degree as for a new ferrule.

A variety of types of ferrules exist to provide a gas-tight seal. Each type has its ownparticular set of advantages and disadvantages:

1. Stainless steel nut and ferrules are used in applications requiring extended exposureto very high temperatures. In selecting stainless steel, be aware of the following:

• The ferrules will form a permanent seal to the given adapter and, therefore,cannot be removed later. If leakage occurs despite reasonable tightening, a newadapter is the best solution.

• In cases of overtightening, a stainless steel nut and ferrules can harden enough todistort threads permanently on the inlet/detector body.

2. Brass nut and ferrules are used in applications requiring more moderate tempera-tures or less extended exposure to very high temperatures. In selecting brass, beaware of the following:

• The ferrules will form a permanent seal to the given adapter and, therefore,cannot be removed later. If leakage occurs despite reasonable tightening, a newadapter is the best solution.

• Over long periods of usage, brass can both oxidize and distort in shape leading toincreasing difficulty in installation or removal of an adapter. A new adapter is thebest solution.

3. Composite material ferrules (Vespel, graphitized Vespel, graphite, etc) are used inapplications requiring moderate temperatures or short-duration exposure to hightemperatures. They have an advantage over metal ferrules in that they are easilyremoved from the adapter when necessary. In selecting such ferrules, be aware ofthe following:

• Vespel-type ferrules may fail immediately if overtightened (by splitting, beingcrushed, etc.); soft graphite ferrules may extrude into the fitting if overtightened.In such failure cases, inspect both the nut and fitting for pieces of ferrule, andremove any found.

• In usage, Vespel-type ferrules can degrade thermally giving eventual failure byleakage and thereby leading to the need of replacement.

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• Vespel-type ferrules tend to shrink upon first exposure to typical gas chromato-graphic temperatures. One should plan to recheck tightness after initial usage ofa new ferrule or, alternatively, the ferrule may be preshrunk before installation byplacing it in an oven at 250°C for at least 4 hours.

When tightening or loosening the nut on the adapter while securing the adapter into theinlet/detector body, use of two wrenches in opposition to each other is stronglyrecommended.

NOTE: Depending upon the given HP 6890 instrument and its specific configuration, the particular inlet or detectormay have an insulating cup present that prevents access to the base of the inlet or detector body. In thesecases, access is achieved in final tightening of the nut and ferrule by removing the cup temporarily andallowing it to hang on the connected column.

d. If using metal ferrules (brass or stainless steel) where torque forces are relativelyhigh, one wrench should be placed on the nut portion of the inlet/detector body toprevent it from being twisted during tightening or loosening performed with thesecond wrench on the nut that secures the adapter and ferrules into theinlet/detector body.

e. If using a composite ferrule (Vespel-type, graphite, etc) where torque forces arerelatively mild, one wrench should be placed on the nut portion of the adapter bodyto prevent it from rotation during tightening or loosening performed by the secondwrench on the nut that secures the adapter and ferrule into the inlet/detector body.Rotation of the adapter within a composite ferrule system may damage the ferrule.

NOTE: If installing the capillary column makeup gas adapter in either the TCD or ECD, it is especially important touse a second wrench to prevent rotation of the adapter. Rotation of the makeup gas adapter may break thegas line where it is welded to the adapter.

Specific Comments, Purged Packed Column Inlet

1. The inlet body without any adapter is designed to accommodate a 1/4-inch glasspacked column where the column itself can be inserted fully to serve as a liner.

2. Some adapters provided for these inlets are designed to accommodate a drop-inglass insert. The insert should be present in these adapters to provide properexpansion volume at sample injection time. They are mostly used to trapnonvolatiles and should be replaced when they get dirty or as prescribed by localprocedures.

Specific Comments, FIDs and NPDs with Packed Column Bases

1. The detector makeup gas function is internal and, therefore, no separate makeup gasadapter is provided.

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2. The detector body without any adapter is designed to accommodate a 1/4-inch glasspacked column where the column itself can be inserted fully to serve as a liner.

3. Some adapters provided for these detectors may require a jet exchange to optimizedetector performance for the particular column type being installed.

Specific Comments, TCD

1. The detector makeup gas function is internal and, therefore, no separate makeup gasadapter is provided.

2. The detector body without any adapter is designed to accommodate a 1/8-inch metalpacked column.

Specific Comments, ECD

1. The detector makeup gas function is externally provided by a separate makeup gasadapter located inside the oven next to the detector and designed to accommodatecapillary columns only. No makeup gas is used in packed column applications.

2. The detector body without any adapter is designed to accommodate a 1/4-inch glasspacked column where the column itself can be inserted fully to serve as a liner.

Page 5 of 6


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Page 6 of 6


9


Title: Column, InstallationProcedure Number: ___________________________________________________________________

Revision Number: ____________________________________________________________________


Approved by: ________________________________________________________________________

Reviewed by: ________________________________________________________________________

Effective Date: _______________________________________________________________________

Company Stamp:


• __________________________________________________________________

• __________________________________________________________________

• __________________________________________________________________

• __________________________________________________________________

• __________________________________________________________________

Page 1 of 8

Column, Installation


10

Scope

Use the following procedure to install a column properly in various inlet and detectortypes, and/or to condition or bakeout a column.

Instrumentation

This SOP applies to all HP 6890 Series GCs and standard inlet and detector options.

General Overview

The split/splitless and cool on-column capillary inlets are designed for use withcapillary columns. The purged-packed inlet is adaptable for use with packed orcapillary columns.

The flame ionization detector (FID), nitrogen-phosphorus detector (NPD), thermalconductivity detector (TCD), and electron capture detector (ECD) are available withadaptable bases that can be used with packed or capillary columns. The FID and NPDare also available with a capillary-optimized base that accepts capillary columns only.

When an adapter is required, the type is determined by the type and size of the column.The following comments assume you have already selected the correct adapters foryour inlet/column/detector combination. If you are unsure about which adapter to use,consult your user documentation section on column installation.

Related SOPs

• Column adapter/makeup gas fitting, installation, SOP no. ____________

References

• HP 6890 Series Gas Chromatograph Operating Manual, HP part no. G1530-90310

Comments, General

Adaptable inlets and detectors, with the exception of the TCD, are designed to accept1/4-inch or 6-mm od glass packed columns without use of any adapter. Other columntypes require an adapter for installation. The TCD accepts 1/8-inch columns with noadapter but requires adapters for all others. Instruments are normally shipped with theappropriate adapters for capillary columns.

The column connection at each end is made with a nut and ferrule to obtain a gas tightPage 2 of 8



11

seal.

In all cases, installation of nuts and ferrules to obtain a gas tight seal is best done byfirst tightening by fingers to ensure no cross-threading occurs. If the nut does not turneasily by fingers, it is often evidence of distorted threads caused by over-tighteningand/or by extended high-temperature exposure in prior installations.

Over-tightening the nut during installation may distort or damage the sealing ferrule tothe extent that a leak-free seal cannot be achieved no matter how tight. In the case ofglass or fused silica column types, the column itself can be broken if the fitting is over-tightened. Follow vendor recommendations for the chosen sealing ferrules.

Note that tightening recommendations are often different for installation of a columnwith new ferrules as opposed to those for reinstallation with existing ferrules.Generally, you do not tighten preset ferrules to the same degree as for new ferrules.

A variety of types of ferrules exist to provide a gas-tight seal. Each type has its ownparticular set of advantages and disadvantages in usage:

1. Stainless steel nuts and ferrules are used in metal packed column applicationsrequiring extended exposure to very high temperatures. In selecting stainless steel,be aware of the following:

• The ferrules will form a permanent seal to the given column and, therefore,cannot be removed later. If leakage occurs despite reasonable tightening, a newcolumn or cutting off the bad section of an existing column is the best solution.

• In cases of overtightening, a stainless steel nut and ferrules can harden enough todistort threads permanently on the inlet/detector body.

2. Brass nuts and ferrules are used in metal packed column applications requiring moremoderate temperatures or less extended exposure to very high temperatures. Inselecting brass, be aware of the following:

• The ferrules will form a permanent seal to the given column and, therefore,cannot be removed later. If leakage occurs despite reasonable tightening, a newcolumn or cutting off the bad section of an existing column is the best solution.

Over long periods of usage, brass can both oxidize and distort in shape leading toincreasing difficulty in installation or removal of a column. A new column or cuttingoff the bad section of an existing column are the best solutions.

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3. Composite material ferrules (Vespel, graphitized Vespel, graphite, etc.) that arecompatible with virtually any column type are used in applications where operatingtemperatures do not exceed the temperature limit of the ferrule material. They havean advantage over metal ferrules in that they are easily removed from the adapterwhen necessary. In selecting such ferrules, be aware of the following:

• Vespel-type ferrules may fail immediately if overtightened (by splitting, beingcrushed, etc); soft graphite ferrules may extrude into the fitting if overtightened.In such failure cases, inspect both the nut and fitting for pieces of ferrule, andremove any found.

• In usage, Vespel-type ferrules can degrade thermally giving eventual failure byleakage and thereby leading to the need of replacement.

• Vespel-type ferrules tend to shrink upon first exposure to typical gas chromato-graphic temperatures. You should plan to recheck tightness after initial usage ofa new ferrule, or alternatively, the ferrule may be preshrunk before installation byplacing it in an oven at 250°C for at least 4 hours.

When tightening or loosening the nut securing the column onto the column adapteror inlet/detector body, use of two wrenches in opposition to each other is stronglyrecommended.

NOTE: Depending upon the given HP 6890 instrument and its specific configuration, the particular inlet or detectormay have an insulating cup present that prevents access to the base of the inlet or detector body. In thesecases, access is achieved in final tightening of the nut and ferrule(s) by removing the cup temporarily andallowing it to hang on the connected column.

• If using metal ferrules (brass or stainless steel) where torque forces are relativelyhigh, one wrench should be placed on the nut portion of the column adapter orinlet/detector body to prevent rotation during tightening or loosening performedwith the second wrench on the nut that secures the column and ferrules onto thecolumn adapter or inlet/detector body.

• If using a composite ferrule (Vespel-type, graphite, etc) where torque forces arerelatively mild, one wrench should be placed on the nut portion of the columnadapter or inlet/detector body to prevent rotation during tightening or looseningperformed by the second wrench on the nut that secures the column and ferruleonto the column adapter or inlet/detector body. Rotation within a compositeferrule system may damage the ferrule.

NOTE: If installing a capillary column in the ECD, it is especially important to use a second wrench to preventrotation of the already installed makeup gas adapter. Rotation of the makeup gas adapter may break the gasline connected to it.

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Specific Comments, Installing Packed Columns

To minimize both dead volume and mechanical distortion of the column and ferrules ininstalling a metal column with new metal ferrules, the column should be pushed fullyinto the receiving fitting, then withdrawn by approximately 1 mm before the nut istightened to set the ferrules permanently to form the gas tight seal. A reference markmade on the column to aid in maintaining its position during tightening isrecommended.

For convenience, the column may be positioned properly and its new ferrules presetoutside the GC by the procedure described in the user documentation.

Specific Comments, Installing Capillary Columns

To assure a gas tight seal without undue tightening of the nut, the inner diameter of thechosen ferrule should match the outer diameter of the column to be installed as closelyas possible. In some installation situations, it is necessary to make a reference mark onthe column. For these cases, suitable marking fluid should be readily available.

In placing the column nut and new ferrule onto a capillary column, ferrule material mayenter the column. It is, therefore, recommended that 2–3 cm of the column end bebroken off at a scribe mark made by a suitable, sharp scribing tool. The freshly cut endshould be inspected for burrs and other irregularities and should be at right angles tothe column length.

The following are comments related to installation of a column with a new ferrule intospecific inlet and detector types:

1. Purged packed column inlet:

NOTE: Packed column and purged packed column inlets are not suitable for use with capillary columns with internaldiameters less than 0.32 mm. For use with capillary columns, the purged packed inlet should be used atcolumn flows ≥ 5 mL/min.

a. On a suitable work surface, adjust the column position so that 3 ± 1 mm (alength suitable for most applications) extends beyond the threaded portion ofthe column nut. The end of the column should be 1–2 mm above the ferrule.

b. Using a suitable marking fluid, mark the column at the opposite end of thecolumn nut as a reference aid during installation.

a. While maintaining the column position in reference to the nut, install thecolumn and nut into the inlet column fitting.

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b. Using fingers only, tighten the column nut just enough to feel resistance inmoving the column, then if necessary, position the column correctly inreference to the nut and previously made mark on the column.

c. Tighten the column nut further following vendor recommendations to avoidferrule damage from overtightening.

2. Split/splitless capillary column inlet:

a. On a suitable work surface, adjust the column position so that 9 ± 1 mm (alength suitable for most applications) extends beyond the threaded portion ofthe column nut. The end of the column should be 5–8 mm above the ferrule.(Check your local procedures, and use the recommendation in your proceduresif different from this.)


c. While maintaining the column position in reference to the nut, install thecolumn and nut into the inlet column fitting.

d. Using fingers only, tighten the column nut just enough to feel resistance inmoving the column, then, if necessary, position the column correctly inreference to the nut and previously made mark on the column.

e. Tighten the column nut further following vendor recommendations to avoidferrule damage through overtightening.

3. On-column capillary column inlets:

NOTE: The on-column inlet and the HP 7673 automatic injector require hardware changes for different internal andoutside diameter columns. Before you proceed, confirm that the correct hardware is installed. The inletrequires changes to the insert and septum nut, while the injector requires changes to the needle guide. It isalso necessary to use the correct syringe with the correct syringe needle. Check the HP 6890 Series GasChromatograph Operating Manual and the HP Automatic Liquid Sampler Operating Manual for further details.

a. Install the column by gently inserting the column fully into the detector fittinguntil you first feel resistance to further insertion.

a. Tighten the column nut following vendor recommendations to avoid ferruledamage from overtightening.

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4. FIDs, NPDs, and TCDs:

a. Install the column by gently inserting the column fully into the column fittinguntil it stops.

b. Using fingers only, tighten the column nut just enough to feel resistance inmoving the column.

c. Withdraw the column by 1 mm from its fully inserted position. A suitablereference mark made on the column is recommended as an aid in judging the1-mm withdrawal.

d. Tighten the column nut further following vendor recommendations to avoidferrule damage from overtightening.

5. ECDs:

NOTE: Some HP 6890 instruments use an ECD makeup gas adapter that provides a hard stop to column insertion.More recent instruments use a makeup gas adapter that is open-ended. The following process accommodateseither situation.

a. On a suitable work surface, adjust the column position so that 53 ± 1 mmextends beyond the threaded portion of the column nut.


c. While maintaining the column position in reference to the nut, install thecolumn and nut into the detector column fitting.

d. Using fingers only, tighten the column nut just enough to feel resistance inmoving the column, then gently attempt to insert the column further by anadditional 1 to 2 mm:

• If further insertion is possible, withdraw the column and position it correctlyin reference to the nut and previously made mark on the column.

• If a hard stop is encountered preventing further insertion, withdraw thecolumn by 1 mm from the fully inserted position. If necessary, an additionalreference mark can be made on the column as an aid in judging the 1-mmwithdrawal.

a. Tighten the column nut further following vendor recommendations to avoidferrule damage from overtightening.

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Column Conditioning/Bakeout

New columns often exhibit high levels of stationary phase bleed. Older columns mayexhibit bleed problems from slow-moving sample components accumulated in thecolumn over many injections. Either situation typically causes increasing drift and/orwander in the chromatographic baseline as column temperature increases duringtemperature-programmed analyses.

In either case, a simple procedure may be used to condition the column to improve itsbleed behavior when returned to normal service.

1. Install the column at the inlet only. In leaving the detector unconnected, materialexiting the column is prevented from contaminating the detector. The detectorcolumn connection fitting should be plugged to prevent entry of other foreignmaterial from the oven as well.

2. Provide carrier gas flow through the column. Any flow rate normal for the type ofcolumn in its intended application is acceptable.

WARNING: If hydrogen is the normal carrier gas choice, due to a possible explosion hazard within the oven,temporarily switch the inlet to a supply of helium or nitrogen.

NOTE: It is advisable to purge the column with carrier flow for 20–30 minutes at room temperature toremove oxygen. Some liquid phases are especially sensitive to oxidation and may be damaged byheating before complete equilibration with carrier gas.

3. Set the oven to a temperature at or somewhat greater than the highest temperatureto which the column is exposed in its analytical applications.

NOTE: Do not exceed the vendor-specified isothermal temperature limit for the specific column to beconditioned. Permanent damage to the column and/or its stationary phase may occur.

4. Shortest time of exposure to elevated temperature is obtained through experience,depending upon the type of column, type and thickness of stationary phase, usagein applications, etc. Usually several hours exposure is a sufficient starting point.The process may be repeated if needed.

5. To minimize thermal shock to the column, at the end of the conditioning time,allow the oven and column to cool gradually while maintaining carrier flow.Gradual cooling may be achieved simply by switching the oven off.

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Title: Liner/Insert, InstallationProcedure Number: ___________________________________________________________________

Revision Number: ____________________________________________________________________


Approved by: ________________________________________________________________________

Reviewed by: ________________________________________________________________________

Effective Date: _______________________________________________________________________

Company Stamp:


• __________________________________________________________________

• __________________________________________________________________

• __________________________________________________________________

• __________________________________________________________________

• __________________________________________________________________

Page 1 of 6

Liner/Insert, Installation


18

Scope

Use the following procedure to properly install an insert.

Frequency

Liner/insert replacement frequency is highly dependent upon working variables, such assample cleanliness, sample composition, temperature, etc. Therefore, frequency mustbe a local (user) decision based upon experience. As a general guideline, however, youshould be conservative, changing the glass insert/liner more frequently than might benecessary.

An alignment insert, used in cool on-column capillary column inlets, serves to align thecolumn and syringe needle. Therefore, it is replaced only if the present column is to bereplaced by a column of different outer diameter.

Instrumentation

This SOP applies to all HP 6890 Series GCs with standard inlet options.

General Overview

Section A describes glass insert replacement applicable to purged packed column inlets.Section B describes glass liner/insert replacement applicable to all split/splitless andsplit-only capillary column inlets. Section C describes alignment insert replacementapplicable to all cool on-column capillary column inlets.

In all three cases, exchange is performed at the top of the HP 6890 Series GC.

Related SOPs

1. Column adapter/makeup gas fitting, installation, SOP no. ____________

References

1. HP 6890 Series Gas Chromatograph Operating Manual, “Inlets” section (HP partno. G1530-90310)

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Section A: Purged Packed Column Inlet

WARNING: If the unit has been used recently, the inlet area may be hot enough to cause serious burns. Ifnecessary, switch off the appropriate heated zone, and allow sufficient cooling time.

WARNING: If hydrogen is used as the carrier gas, a possible fire or explosion hazard exists if it is allowed toflow during glass insert exchange. It is recommended that hydrogen carrier flow be switched offduring the procedure.

NOTE: As carrier gas flow through the column ceases during glass insert exchange, it is recommended that columnoven temperature be reduced to a conservative value during the procedure. If local procedures and/or themethod specifies, the oven temperature should be set near ambient (35–40°C).

Procedure

1. For the purged packed column inlet, remove the combined assembly of septumretainer nut, septum, and top insert weldment. Inspect the O-ring seal between thetop insert weldment and inlet body, and replace it if necessary.

2. Generally, the old glass insert may now be removed through the now-exposed topof the inlet body. A fibrous, cylindrical object of suitable outer diameter (such as amatch stick, large-diameter tooth pick, etc) can be inserted into the insert from thetop, then used to extract it from the inlet body.

If the old glass insert cannot be extracted through the top of the inlet body, thenfrom inside the oven, the column adapter containing the insert must be removedfrom the inlet body. This may require disconnecting the column first to preventpossible damage and/or loss of gas-tight sealing.

3. Install the glass insert simply by placing it gently into the column adapter orientedwith its unflared end entering the adapter first.

Note that if the column adapter was never removed from the inlet body in extract-ing the old glass insert, the new insert should disappear entirely from view at thetop of the inlet body. If its flared end is too large to pass through the top of theinlet body, try a different insert. If necessary, the column adapter must beremoved from the inlet body. This may require disconnecting the column first toprevent possible damage and/or loss of gas-tight sealing.

4. Replace items removed to exchange glass inserts. Restore inlet gas flow rate(s)and temperature setpoints. Check the flow rate through the injection port. If thecarrier flow rate is higher than expected, the adapter fitting in the oven will have to

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be tightened. Tighten if necessary.

Section B: Split/Splitless Capillary Column Inlets


WARNING: If hydrogen is used as the carrier gas, possible fire or explosion hazard exists if it is allowed toflow during glass liner exchange. It is recommended that hydrogen carrier flow be switched offduring the procedure.

NOTE: For split/splitless capillary column inlets, if either the old glass liner to be replaced or the new glass liner to beinstalled contains unsecured material (for example, glass wool), the material may become dislodged if carriergas is allowed to flow during exchange. In this case, it is recommended that carrier flow be switched off andallowed to drop to zero before starting the procedure.

NOTE: As carrier gas flow through the column ceases during glass liner exchange, it is recommended that columnoven temperature be reduced to a conservative value during the procedure.

Procedure

1. Remove the combined assembly of septum retainer nut, septum, and split/splitlessinsert weldment. Carefully bend the attached tubing just enough to gain access tothe top of the inlet body and to the liner to be replaced.

2. Carefully remove the old liner and its O-ring seal. If fragments of O-ring materialadhere to the metal surfaces (often a sign of lengthy service at high temperature),they must be removed.

NOTE: Avoid allowing fragments of either the O-ring seal or liner (if broken) from entering the inlet itself. Having avacuum cleaner available is also recommended in this situation.

3. Install the new liner with an appropriate seal; the inner diameter of the new sealshould closely match the outer diameter of the replacement liner. The new sealshould never be loose on the liner or have to be forced onto the liner. Leakage mayoccur if an inappropriately sized seal is used.

Also note that some liner styles may require a specific orientation in installation,especially those containing unsecured material (for example, glass wool). Followvendor recommendations, bearing in mind that gas flow through the liner is alwaysfrom the top of the inlet (septum location) to its bottom (column location).

Page 4 of 6



21

4. Carefully replace the inlet top assembly that was removed to exchange liners,tightening firmly the nut portion of the split/splitless insert weldment. Restoreinlet gas flow rate(s) and temperature setpoints, and check the pressure.

Section C: Cool On-Column Capillary Column Inlets

WARNING: If the unit has been used recently, the oven and inlet area may be hot enough to cause seriousburns. If necessary, switch off the oven (and inlet heated zone if applicable) and allow sufficientcooling time.

WARNING: If hydrogen is used as the carrier gas, a possible fire or explosion hazard exists if it is allowed toflow during alignment insert exchange. It is recommended that hydrogen carrier flow be switchedoff during the procedure.

NOTE: The cool on-column capillary column inlet has a small coil spring located in the inlet body just below theseptum location. The spring is removed in this procedure and can be easily lost. It is an integral part of theinlet assembly, helping to maintain correct column and syringe needle alignment. Proceed with vigilance.

NOTE: As carrier gas flow through the column ceases during alignment insert exchange, it is recommended that thecolumn oven temperature be reduced to a conservative value during the procedure.

Procedure

1. If not already done, remove the column. If the diameter is different on the columnto be installed, the insert will have to be replaced.

2. Depending upon the inlet configuration, remove the cooling tower or septum nutbase assembly located at the top of the inlet.

3. Carefully remove the small coil spring now visible, extending just above the top ofthe inlet body. Place the spring in a safe place.

4. Remove the old alignment insert by pushing it out at the top of the inlet body fromthe inlet column fitting inside the oven. A piece of straight wire of suitablediameter, such as a syringe plunger, can be used. Place the removed insert in asafe place to be used again if needed.

Page 5 of 6



22

5. Select the replacement alignment insert according to the diameter of the column tobe installed, and simply drop it into the inlet body from the top. Orientation doesnot matter.

Consult your user documentation for information about selecting an alignmentinsert appropriate for the outer diameter of the column to be installed.

6. Replace the coil spring and cooling tower or septum nut base assembly, andtighten the nut fully using your fingers only.

7. Install the new column, restore the inlet gas flow, and check the pressure andtemperature setpoints.

Page 6 of 6


23


Title: Inlet Septum, InstallationProcedure Number: ___________________________________________________________________

Revision Number: ____________________________________________________________________


Approved by: ________________________________________________________________________

Reviewed by: ________________________________________________________________________

Effective Date: _______________________________________________________________________

Company Stamp:


• __________________________________________________________________

• __________________________________________________________________

• __________________________________________________________________

• __________________________________________________________________

• __________________________________________________________________

Page 1 of 4

Inlet Septum, Installation


24

Scope

Use the following procedure to install a septum into an inlet properly.

Frequency

Septum replacement frequency is highly dependent upon working variables, such asseptum temperature, septum material, syringe needle quality, injection methodologyand/or technique, etc. Therefore, frequency must be a local (user) decision based uponexperience. As a general guideline, however, you should be conservative, changing theseptum more frequently than might be necessary.

Instrumentation

This SOP applies to all HP 6890 Series GCs and standard inlet options.

General Overview

Septum replacement is described in two separate sections: Section A is applicable toall purged packed and split/splitless capillary column inlets. Section B is applicable toall cool on-column capillary column inlets.

Parts/Equipment Referenced

The following tools and parts are used for replacement of the septum in the inlets.

• Septum nut wrench (HP part no. 19251-00100)

• 11-mm septum (HP part no. 5181-1263)

• 5-mm septum (HP part no. 5181-1261)

• A nonmetallic (plastic or wood) tool with a sharp tip to remove septum from the inlet

• Forceps or tweezers

References

HP 6890 Series Gas Chromatograph Maintenance and Troubleshooting Manual(HP part no. G1530-90320)

Page 2 of 4



25

Section A: Purged Packed Column and Split/Splitless CapillaryColumn Inlets


WARNING: If hydrogen is used as the carrier gas, a possible fire or explosion hazard exists if it is allowed toflow during septum exchange. It is recommended that hydrogen carrier flow be switched off duringthe procedure.

NOTE: For split/splitless capillary column inlets, if a liner is present containing unsecured material (for example, glasswool), the material may become dislodged if carrier gas is allowed to flow during septum exchange. In thiscase, it is recommended that carrier flow be switched off and allowed to drop to zero before starting theprocedure.

NOTE: As carrier gas flow through the column ceases during septum exchange, it is recommended that column oventemperature be reduced to a conservative value during the procedure. If local procedures and/or the methodspecifies, the oven temperature should be set near ambient (35–40°C)

Procedure

1. Remove the septum retainer nut located at the top of the inlet.

2. Remove the old septum. If fragments of septum material adhere to the metalsurfaces (often a sign of lengthy service at high temperature), they must beremoved.

NOTE: Do not let septum material fragments enter the inlet. If necessary, temporarily block the inlet opening with apiece of aluminum foil. Having a vacuum cleaner available is also recommended in this situation.

3. Install the new septum.

a. For an 11-mm diameter septum, the septum must be pressed evenly into place,working around its edges.

b. Replace the septum retainer nut and tighten it using your fingers only until youfirst begin to feel resistance. Then tighten further by 1/4- to 1/2-turn.

Note that fully tightening the nut with an 11-mm diameter septum may compressthe septum material to an extent that it is not easily pierced by a syringe needle.This could cause a bent needle or septum "coring" whereby the needle carries

Page 3 of 4



26

small pieces of septum material into the inlet.

4. Restore the inlet gas flow rate(s), and allow the carrier gas to purge the inlet andcolumn thoroughly.

5. Restore temperature setpoints.

Section B: Cool On-Column Capillary Column Inlets

WARNING: If hydrogen is used as the carrier gas, a possible fire or explosion hazard exists if it is allowed toflow during septum exchange. It is recommended that hydrogen carrier flow be switched off duringthe procedure.

NOTE: The cool on-column capillary column inlet has a small coil spring located in the inlet body just below theseptum location. Although the spring is not removed in this procedure, it can be easily lost. It is an integralpart of the inlet assembly, helping to maintain correct column and syringe needle alignment. Proceed withvigilance.

NOTE: As carrier gas flow through the column ceases during septum exchange, it is recommended that the columnoven temperature be reduced to a conservative value during the procedure.

Procedure

1. Depending upon the inlet configuration, remove the cooling tower or septum nutbase assembly located at the top of the inlet.

2. Remove the old septum from the underside of the removed cooling tower orseptum base assembly. A pointed tool, such as a bamboo skewer, may be neededto pry out the old septum. Any remaining fragments of septum material must beremoved.

3. Insert the replacement septum into the cooling tower or septum nut baseassembly. Note that if a "duck bill" septum is being installed (for manual injectionuse only), the septum "bill" must be oriented to point into the inlet body (towardthe column).

4. Replace the cooling tower or septum nut base assembly containing the newseptum, and tighten the nut fully using fingers only.

5. Restore the inlet gas flow rate(s) and temperature setpoints.

Page 4 of 4


27


Title: FID (Flame Ionization Detector) Checkout Using a Purged PackedColumn Inlet

Procedure Number: ___________________________________________________________________

Revision Number: ____________________________________________________________________


Approved by: ________________________________________________________________________

Reviewed by: ________________________________________________________________________

Effective Date: _______________________________________________________________________

Company Stamp:


• __________________________________________________________________

• __________________________________________________________________

• __________________________________________________________________

• __________________________________________________________________

• __________________________________________________________________

FID (Flame Ionization Detector), Purged Packed


28

Scope

Use the following procedure to verify proper FID operation with the purged packedinlet.


• HP 6890 evaluation column, 30 m x 0.320 mm x 0.25 µm HP-5, HP part no. 19091J-413

• FID/TCD performance evaluation ("checkout") sample, HP part no. 18710-60170

• 10-µl syringe, HP part no. 9301-0810 or equivalent

• Disposable glass inserts, HP part no. 5080-8732

• Septum, HP part no. 5181-1263

• Liner for wide-bore capillary columns, HP part no. 19244-80540

• Viton O-ring, HP part no. 5080-8898

• Soap film flowmeter (500-mL volume, multirange), HP part no. 9301-0981 orequivalent

• FID flow measurement adapter, HP part no. 19301-60660

• Chromatographic-grade purity gases: helium as carrier, nitrogen as makeup, air, andhydrogen

Analog Input

• HP 3395B, HP 3396 Series II (HP 3396B), HP 3396 Series III (HP 3396C), or HP 6890Series (HP 3397A) integrator

• HP 6890A-to-HP 3396B/C or HP 3397A analog signal cable, HP part no. G1530-60570(2-meter, 6-pin)

• HP 6890A-to-HP 3396B remote start cable, HP part no. G1530-61020 (9-pin/15-pin)

• HP 6890A-to-HP 3396C or HP 3397A remote start cable, HP part no. 3396-61010(9-pin/15-pin)

INET Input

• HP 3396 Series II (HP 3396B), HP 3396 Series III (HP 3396C), or HP 6890 Series(HP 3397A) integrator

• INET communication card, HP 6890 Option 510 (accessory HP G1553A)



29

• HP 3396B/C or HP 3397A INET cable, HP part no. 82167-60003 (5-meter, tworequired)

ChemStation Input

• HP GC ChemStation software loaded as part of the HP multitechnique ChemStationon an IBM-compatible personal computer with an HP-IB interface and the properamount of memory for applications to be run. (See the HP Multitechnique Chem-Station Manual for requirements.)

• HP-IB cable, HP part no. 8120-3445 (1 meter)

Related SOPs

• Inlet septum, installation, SOP no. _____________


• Column adapter/makeup gas fitting, installation, SOP no. _____________


Procedure

WARNING: If the unit has been previously in operation, areas may be hot enough to cause serious burns.Switch off the heated zones and the oven, and allow the unit sufficient time to cool.

1. Following the SOPs cited above in the “Related SOPs” section, do the following:

a. At the packed column inlet, install a new septum, a capillary column adapter,new liner, and the HP 6890 evaluation column.

b. At the FID, install a 0.28-mm (0.011-in.) jet and/or the capillary column adapter,if needed, and the remaining end of the HP 6890 evaluation column.

2. At the HP 6890, verify that the FID to be evaluated has its Gas Type set to nitrogenby pressing the [Configure] [Front Detector] {or [Back Detector]}. If necessary,change the gas type to nitrogen by pressing the [Mode/Type] key and choosingnitrogen from the menu.

3. After choosing one data handling device for the test, set up the data path betweenthe HP 6890 and the data handling device by choosing the appropriatecombination:



30

a. HP 6890 analog output to the integrator

• Install the analog signal cable from the Signal 1 output receptacle on theHP 6890 and the integrator.

• Install the remote start cable from the Remote receptacle on the HP 6890 andthe integrator.

• At the HP 6890, assign Signal 1 to the FID to be evaluated:[Signal 1] [Front Detector] {or [Back Detector]}

• Switch on the integrator.

b. HP 6890 INET output to the integrator

• Install the INET signal cables between the INET I/O connectors on theHP 6890 and the integrator.



c. HP 6890 HP-IB output to the HP Multitechnique ChemStation

• This procedure assumes that the ChemStation is properly installed on thecomputer and connected to the HP 6890. If it is necessary to install andconfigure the ChemStation, please refer to the HP Multitechnique Chem-Station Manual set, especially “Installing Your GC ChemStation” (HP part no.G2070-90001).

• Once the ChemStation is properly installed and configured, bring up theproper on-line instrument for the HP 6890 to be tested. Then at the Chem-Station under the View menu, choose Run Method and Control View. On theRun Method and Control View, choose Instrument. From the Instrumentmenu, choose Edit Parameters. On the Edit Parameters screen, click onOptions. On the Options screen, choose the radio button labeled “No” for thequestion “Keep instrument keyboard locked after method is loaded?” Clickon [OK] to leave the screen. This will allow you to enter setpoints from thekey-board. You may remain in the Edit Parameters screen, and enter thesetpoints directly from the ChemStation.

• Assign Signal 1 to the appropriate detector. On the ChemStation EditParameters screen, this is under Signals. Also choose Save Data All and aData Rate of 20 Hz.



31

4. To ensure carrier flow through the column during oven and zone heat-up, thefollowing flow rates should be established:

a. For an instrument with electronic pressure and flow control, enter the followingvalues :

Column pressure = 25 psi

Verify that the column is operating in constant flow mode by pressing the[Column 1] or [Column 2] key. Toggle down to the Mode line to check the mode.If necessary, change to constant flow by pressing the [Mode/Type] key andselecting Constant Flow.

b. For an instrument with manual pressure and flow control for the inlet:

Set the pressure to 25 psi, insert the flow measurement adapter onto the FID,connect the flowmeter, and measure the carrier flow rate. It should be between7.5 and 7.9 mL/min at an oven temperature of 40°C.

5. Using the appropriate Inlet and Detector Control Tables on the HP 6890, set thefollowing heated zone and oven setpoint values:

Inlet Temperature: 250°CDetector Temperature: 300°C

Oven Program :Temperature: 40°CInitial time: 0 minRate 1: 25°C/minFinal temperature: 90°CFinal time: 0 minRate 2: 15°C/minFinal temperature: 170°CFinal time: 2 min

Allow the unit at least 30 minutes to stabilize thermally.

6. After thermal stabilization, set the following values according to the appropriateinstrument.

a. For an electronic pressure and flow controlled FID, input the following valuesby pressing the appropriate detector key to open the control screen and thenentering the following flow setpoint values:

Hydrogen flow = 30 mL/minAir flow = 400 mL/minMakeup flow (nitrogen) = 25 mL/min



32

Check that the detector is in constant makeup mode. If it is not, scroll to Mode,press the [Mode/Type] key, and select Constant Makeup Flow. If the detectorflow rates are checked, the values should be within the limits set in step 6b for amanual flow controlled FID.

b. For a manual flow controlled FID, establish the following flow rates by insertingthe flow measurement adapter fully onto the FID collector and connecting theflowmeter:

Hydrogen flow = 30 mL/min + 2 mL/minAir flow = 400 mL/min + 30 mL/minMakeup flow (nitrogen) = 25 mL/min + 2 mL/min

After setting the flows above, remove the flowmeter and FID flow measurementadapter.

7. At the HP 6890, turn on the FID electrometer by pressing [Configure] [FrontDetector] {or [Back Detector]}. Turn the electrometer on by scrolling to theelectrometer line and pressing [ON]. Press [Signal 1] to display its flame-offbackground offset. A stable value, <2.0 display units, is acceptable criteria tocontinue. If not met, stop here, and consult your HP 6890 service and userdocumentation for additional information. If necessary, contact your localHewlett-Packard service representative.

8. Ignite the FID flame by going to the appropriate Detector Control Table, scrollingdown to Flame, and pressing [ON].

a. Observe the FID flame signal at the display. Successful flame ignition typicallyresults in a permanent increase in signal output. If no appreciable increase isobserved, perform the next check; otherwise, continue to step 9.

b. Hold a cool, shiny, metal object, such as a chrome-plated wrench, just above theFID chimney. Any observed water condensation signifies the flame is indeedignited.

c. If the flame has not ignited, recheck all flow rates, and attempt ignition again. Ifthe flame cannot be lit even though flow rates are correct, consult your HP 6890service and user documentation for additional information. If necessary,contact your Hewlett-Packard service representative.

9. With the flame lit, observe the FID signal at the display. This is the flame-onbackground offset. A stable value between 5 and 20 display units is acceptablecriteria to continue to step 10. If an air cleaning system is being used, it is possiblethat the value will stabilize to a value below 5.



33

Typically, the value may be >20 display units indicating system bakeout isnecessary:

a. Turn the detector off, remove the column from the detector, and cap thedetector fitting.

b. Reset the oven and heated zone temperature to the following values:Front detector (or back detector) temperature: 400°COven temperature: 250°C

c. Reignite the detector, and monitor the displayed detector signal; it should risequickly to some higher value as the FID heats to the higher temperature. Then,over a longer time, the signal should decrease to some reasonably constantvalue.

d. Reinstall the column in the detector.

e. Restore the original setpoint temperatures specified in step 4, and allow the unitat least 2 hours to stabilize thermally. Observe the displayed detector signal todetermine it is now within the acceptable range of between 5 and 20 displayunits, verify all gas flow rates, then continue to step 10.

f. If the displayed detector signal is still too great to continue, repeat the bakeoutprocess. If repeated bakeout cycles fail to give the acceptable signal level, itmay be an indication that the gases and/or traps may be necessary. If cleaningthe gases fails to give an acceptable signal level, consult your HP 6890 serviceand user documentation for additional information. If necessary, contact yourlocal Hewlett-Packard service representative.

10. To check signal noise, wander, and drift, perform one of the following stepsaccording to the data handling device connected to the HP 6890:

a. For HP 6890 analog output to the integrator

• At the HP 6890, enter a range value of 0 (zero) for Signal 1 (or Signal 2) bypressing [Signal 1] and scrolling down the control table to Range.

• At the HP integrator, enter the following setpoint values: [ATT 2^] [-] [2] [ENTER][ZERO] [5] [0] [ENTER][CHT SP] [1] [ENTER]

• Press [PLOT] to begin plotting the FID signal.

• At an elapsed time of 1 minute, enter the following key sequence at theintegrator, and allow plotting to continue for another 10 minutes:

[ATT 2^] [0] [ENTER]



34

• Using the method shown, measure the plot to check for the following:

− Noise in the first 1-minute portion of the plot should be <24 mm in width.

− Wander over any given 2-minute period in the 10-minute portion of the plotshould be <14 mm in width.

− Drift over any given 5-minute period in the 10-minute portion of the plotshould be <30 mm in width.

• If these criteria are not met, repeat the test. If after repeated testing thecriteria cannot be met, stop here, and consult your HP 6890 service and userdocumentation for additional information. If necessary, contact your localHewlett-Packard service representative.

b. For HP 6890 INET output to the integrator

• At the HP 6890, enter a range value of 0 (zero) for Signal 1 (or Signal 2) bypressing [Signal 1] and scaling down the control table to Range.

NOTE: For the HP 3396 Series II (HP 3396B), HP 3396 Series III (HP 3396C),or HP 6890 Series (HP 3397A) integrator, the range value can be determinedby entering:

[LIST] [OP#] [6]

This will give the HP 6890 method listing. At the bottom of the listing is therange value for signal 1 and 2. This is the range set at the MIO (INET) card.Normally this value is set to 5. The noise can be plotted with the integratorrange value (this range is designated as SIG1RANGE) set to 5. The nextbulleted step is to be used with a SIG1RANGE = 5. The attenuation valueshave been adjusted to give the same amplitude plot as the analog. It ispermissible for the user to change the SIG1RANGE value to 0 (zero) and usethe same integrator settings as in step 10a. The user is referred to the HP 3396manual for further details in how to change the SIG1RANGE value.

• At the integrator, enter the following setpoint values: [ATT 2^] [-] [7] [ENTER][ZERO] [5] [0] [ENTER][CHT SP] [1] [ENTER]


• At an elapsed time of 1 minute, enter the following key sequence at theHP 3396B/C or HP 3397A, and allow plotting to continue for another10 minutes:

[ATT 2^] [-] [5] [ENTER]




35

− When plotted at [ATT 2^] [-] [7], noise in the first 1-minute portion of theplot should be <30 mm in width.

− Wander over any given 5-minute portion of the plot should be <17.5 mm inwidth.

− Drift over the full 30-minute plot should be <37.5 mm in width.

c. For HP 6890 HP-IB output to the HP GC ChemStation

• At the ChemStation under the View menu, choose Full Menu then DataAnalysis.

• On the Data Analysis View, choose Report.

• From the Report menu, choose Specify Report.

• On the Specify Report window, choose the “performance + noise” ReportStyle for the report format. Close the window by clicking OK.

• From the Report menu, choose System Suitability, which will bring up asecond menu. On the second menu, choose Edit Noise Ranges. (If SystemSuitability does not appear under the Report menu, go to the View menu, andchoose Full Menu.) Once Edit Noise Ranges has been chosen, a window willappear that allows time ranges to be entered. The ChemStation calculatesseveral different noise calculations. The ASTM noise will be used in the MDLcalculation later. The ASTM noise measurement requires that the noise rangebe ≥1.01 minutes. Enter several time ranges that are ≥1.01 minutes. A timerange of 2.0 minutes and 5.0 minutes should also be entered. These rangescan overlap with the other ranges. Close the window by choosing OK.

• Under View, choose Method and Run Control. Under the Method menu,choose Save Method As, which will allow a unique method name to be chosenfor the noise measurement. Once a method name has been assigned, go tothe Instrument menu, and choose Edit Parameters. On the Edit Parametersscreen, select the oven icon, and check that the oven temperature is 40°C.Set the initial time to 12 minutes and rate 1 to 0°C/min. (This sets up a12-minute isothermal run.) Check the other parameters in steps 4 through 6by choosing the appropriate icon. Then click on OK to close the EditParameters screen.

• Under Run Control, choose Sample Information. Enter a directory name and,if you choose, a file name. (This will allow you to have the file as a uniquefile and not as the default.) Once this is completed, close the window. Pressstart at the HP 6890 keyboard. This will start the noise measurement oncethe run is completed. (If the method has not been set up to print the report,go to Data Analysis View.) See the ChemStation manual for moreinstructions on Data Analysis.



36

• Under View, choose Data Analysis. Load the data file for the blank run justcompleted. Under Report, choose Specify Report. Choose printer andscreen. Under Integration, choose Integrate. After integration is completed,print the report by choosing Print Report under Report. The report will listmeasure-ments for noise (peak to peak, 6 * sd, and ASTM) and for drift andwander.

− ASTM noise should be <0.0382 pA.

− Wander (for a 2-minute time window) should be <0.0892 pA.

− Drift (for a 5-minute time window) should be <0.1911 pA.

11. To perform chemical checkout, choose the appropriate data handling device:


• At the HP 6890, enter a range value of 8 for Signal 1 (or Signal 2) by pressing[Signal 1] and scrolling down the control table to Range.

• At the integrator, enter the following setpoint values:[ZERO] [1] [0] [ENTER][ATT 2^] [4] [ENTER][CHT SP] [1] [ENTER][PK WD] [.] [0] [4] [ENTER][THRSH] [3] [ENTER][TIME] [8] [.] [7] [5] [STOP]

• Inject 1 µl of the checkout sample, and press [START] at the HP 6890 to beginthe checkout run.

min0 2 4 6 8 10 12 14

pA

2.75

3

3.25

3.5

3.75

4

4.25

4.5

FID1 B, of FIDNOISE\NOISE001.D



37

• The resulting chromatogram should appear similar to that shown in thechromatogram figure. The following criteria indicate successful completionof FID chemical checkout:

− Area counts for components labeled C14, C15, and C16 should each be>125,000.

− The area counts ratio calculated as C14/C16 should be 1.00 + 0.1.

− MDL(C) = (86,800 x (Noise))/(Area C16) <= 4 pg/s with the area measuredwith the range 2^8 and the noise in mm at attn 2^0 (noise measured peakto peak).

• If these criteria are not met, repeat the test. If after repeated testing thecriteria cannot be met, consult your HP 6890 service and user documentationfor additional information. If necessary, contact your local Hewlett-Packardservice representative.


• At the HP 6890, enter a range value of 5 for Signal 1 or (Signal 2) by pressing[Signal 1] and scaling down the control table to Range.

NOTE: For the HP 3396C or HP 3397A integrator, ensure that the range value isfive by pressing:

[LIST] [OPTION] [8]

which displays the integrator range value.

• At the integrator, enter the following setpoint values:[ZERO] [1] [0] [ENTER][ATT 2^] [4] [ENTER][CHT SP] [1] [ENTER][PK WD] [.] [0] [4] [ENTER][THRSH] [3] [ENTER][AR REJ] [0] [ENTER][TIME] [8] [.] [7] [5] [STOP]



− Area counts for components labeled C14, C15, and C16 should each be>1,250,000.




38

− MDL(C) = (694,000 x (Noise))/(Area C16) <= 4 pg/s with the noisemeasured in mm at attn 2^-6 (noise measured peak to peak).


c. HP 6890 HP-IB output to HP GC ChemStation





− MDL(C) = (436,000 x Noise)/(Area C16) <= 4 pg/s (noise measured peakto peak).




39

2 4 6 8

0

200

400

600

800

1000

1200

1400

1600

1800

2000

Time (min.)

C14 C15

C16


Revision Date 9-Jan-98 Procedure no. :________________ Hewlett-Packard Company

40


41


Title: FID (Flame Ionization Detector) Checkout Using a Split/SplitlessCapillary Column Inlet


Revision Number: ____________________________________________________________________


Approved by: ________________________________________________________________________

Reviewed by: ________________________________________________________________________

Effective Date: _______________________________________________________________________

Company Stamp:


• __________________________________________________________________

• __________________________________________________________________

• __________________________________________________________________

• __________________________________________________________________

• __________________________________________________________________

Page 1 of 14

FID (Flame Ionization Detector), Split/Splitless


42

Scope

Use the following procedure to verify proper FID operation with the split/splitless inlet.






• O-ring, HP part no. 5180-4182



• Chromatographic-grade purity gases: hydrogen, helium, nitrogen, and air

Data Handling Devices, Parts and Equipment

Analog Input





INET Input




Page 2 of 14



43

ChemStation Input



Related SOPs





• Calculation of chromatographic performance factors for the HP 6890 with differentdata systems

Procedure



a. At the capillary column inlet, install a new septum, a new split liner,O-ring seal, and the HP 6890 evaluation column.

b. At the FID, install a 0.28-mm (0.011-in.) jet and/or the capillary column adapter,if needed, and the remaining end of the HP 6890 evaluation column.



Page 3 of 14



44







• Install the INET signal cables between the INET I/O connectors on the HP6890 and the integrators.







Page 4 of 14



45

4. Verify the inlet is operating in splitless mode by pressing the [Front Inlet] or [BackInlet] key. If not, change to the splitless mode by pressing the [Mode/Type] key andselecting Splitless.


a. For an instrument with electronic pressure and flow control, enter the followingvalues:

Column pressure = 25 psi heliumPurge flow = 60.0 mL/minPurge time = 0.75 min

Verify that the column is operating in constant pressure mode by pressing the[Column 1] or [Column 2] key. Toggle down to the Mode line to check the mode.If necessary, change to constant pressure by pressing the [Mode/Type] key andselecting Constant Pressure.



Connect the flowmeter to the inlet split flow vent, and adjust the flow rate to50–70 mL/min. Record this value

As measured at the inlet vent using the flowmeter, set the septum purge flowrate at 5 ± 1 mL/min.


Inlet Temperature: 250°CDetector Temperature: 300°COven Program:Temperature: 40°CInitial time: 0 minRate 1: 25°C/min.Final temperature: 90°CFinal time: 0 minRate 2: 15°C/minFinal temperature: 170°CFinal time: 2 min


Page 5 of 14



46

7. After thermal stabilization, set the following values according to the appropriateinstrument:

a. For an electronic pressure and flow controlled FID, input the following valuesby pressing the appropriate detector key to open the control screen and thenentering the following flow values:

Hydrogen at 30Air at 400Makeup (nitrogen) at 25

Check that the detector is in constant makeup mode. If it is not, scroll to Mode,press the [Mode/Type] key, and select Constant Makeup Flow. If detector flowrates are checked, the values should be within the limits set in step 7b for amanual flow controlled FID.

b. For a manual flow controlled FID, establish the following flow rates by insertingthe flow measurement adapter fully onto the FID collector and connecting theflowmeter.

Hydrogen at 30 + 2 mL/minAir at 400 + 30 mL/minMakeup (nitrogen) at 25 + 2 mL/min

After setting the flows above, remove the flowmeter and flow measurementadapter.

8. At the HP 6890, turn on the FID electrometer by pressing [Configure] [FrontDetector] {or [Back Detector]}. Turn the electrometer on by scrolling to theelectrometer line and pressing [ON]. Press [Signal 1] to display its flame-offbackground offset. A stable value, <2.0 display units, is acceptable criteria tocontinue. If not met, stop here, and consult your HP 6890 service and userdocumentation for additional information. If necessary, contact your localHewlett-Packard service representative.




a. If the flame has not ignited, recheck all flow rates, and attempt ignition again.If the flame cannot be lit even though the flow rates are correct, consult your

Page 6 of 14



47

HP 6890 service and user documentation for additional information. If neces-sary, contact your Hewlett-Packard service representative.





c. Reignite the detector, and monitor the displayed detector signal; it should risequickly to some higher value as the FID heats to the higher temperature. Then,over a longer time, the signal should decrease to some reasonably constantvalue.


e. Restore the original setpoint temperatures specified in step 5, and allow the unitat least 2 hours to stabilize thermally. Observe the displayed detector signal todetermine it is now within the acceptable range of between 5 and 20 displayunits, verify all gas flow rates, then continue to step 11.

f. If the displayed detector signal is still too great to continue, repeat the bakeoutprocess. If repeated bakeout cycles fail to give the acceptable signal level, itmay be an indication that the gases are impure. Higher purity gases and/or trapsmay be necessary. If cleaning the gases fails to give an acceptable signal level,consult your HP 6890 service and user documentation for additionalinformation. If necessary, contact your local Hewlett-Packard servicerepresentative.




• At the integrator, enter the following setpoint values:

Page 7 of 14



48

[ATT 2^] [-] [2] [ENTER][ZERO] [5] [0] [ENTER][CHT SP] [1] [ENTER]


• At an elapsed time of 1 minute, enter the following key sequence at theintegrator, and allow plotting to continue for another 10 minutes:




− Wander over any given 2-minute period in the 10-minute portion of the plotshould be <14 mm in width.






[LIST] [OP#] [6]


• At the integrator, enter the following setpoint values:[ATT 2^] [-] [7] [ENTER][ZERO] [5] [0] [ENTER][CHT SP] [1] [ENTER]


Page 8 of 14



49


[ATT 2^] [-] [5] [ENTER]


− When plotted at [ATT 2^] [-] [7], noise in the first 1-minute portion of theplot should be <30 mm in width.

− Wander over any given 5-minute portion of the plot should be <17.5 mmin width.






• On the Specify Report window, choose the “performance + noise” ReportStyle for the report format. Close the window by clicking on OK.



Page 9 of 14



50






12. To perform a chemical checkout, choose the appropriate data handling device:




min0 2 4 6 8 10 12 14

pA

2.75

3

3.25

3.5

3.75

4

4.25

4.5


Page 10 of 14



51

[ZERO] [1] [0] [ENTER][ATT 2^] [4] [ENTER][CHT SP] [1] [ENTER][PK WD] [.] [0] [4] [ENTER][THRSH] [3] [ENTER][TIME] [8] [.] [7] [5] [STOP]

• Press [Prep Run] to prepare the inlet for splitless injection. Press [Status]and wait for the message “Ready for Injection.” Then inject 1 µL of thecheckout sample, and press [Start].

• The resulting chromatogram should appear similar to that shown in the chro-matogram figure. The following criteria indicate successful completion ofFID chemical checkout:



− MDL(C) = (86,800 x (Noise))/(Area C16) <= 4 pg/s with the area measuredwith the range 2^8 and the noise in mm at attn 2^0 (noise measured peakto peak).




NOTE: For the HP 3396C or HP 3397A integrator, ensure that the range valueis five by pressing:

[LIST] [OPTION] [8]




Page 11 of 14



52




− MDL(C) = (694,000 x (Noise*2^-6))/(Area C16) <= 4 pg/s with the noisemeasured in mm at attn 2^-6 (noise measured peak to peak).


c. HP 6890 HP-IB output to the HP GC ChemStation







Page 12 of 14



53

2 4 6 8

0

200

400

600

800

1000

1200

1400

1600

1800

2000

Time (min.)

C14 C15C16

Page 13 of 14



54

Page 14 of 14

FID (Flame Ionization Detector), Cool On-Column


55


Title: FID (Flame Ionization Detector) Checkout Using a CoolOn-Column Capillary Column Inlet


Revision Number: ____________________________________________________________________


Approved by: ________________________________________________________________________

Reviewed by: ________________________________________________________________________

Effective Date: _______________________________________________________________________

Company Stamp:


• __________________________________________________________________

• __________________________________________________________________

• __________________________________________________________________

• __________________________________________________________________

• __________________________________________________________________

Page 1 of 12



56

Scope

Use the following procedure to verify proper FID operation with the Cool On-Columninlet.




• 5-µl syringe (without needle), HP part no. 5182-0836

• Needles for 0.32-mm columns (3/pk), HP part no. 5182-0831

• Plunger button (10/pk) that converts HP 7673 syringes for manual use, HP part no.5181-8866



• Chromatographic-grade purity gases: air and hydrogen to support the FID, helium ascarrier, and nitrogen or helium as makeup

• 320-µm capillary column on-column insert, HP part no. 19245-20525



Analog Input







57

INET Input




ChemStation Input



Related SOPs






Procedure



a. At the cool on-column capillary column inlet, install a new septum, a 320-µmcapillary column on-column insert, and the HP 6890 evaluation column.

b. At the FID, install a 0.28-mm (0.011 in.) jet and/or the capillary column adapter,if needed, and the remaining end of the checkout column.

Page 2 of 12



58



Page 3 of 12



59










c. HP 6890 HP-IB Output to the HP Multitechnique ChemStation





Page 4 of 12



60

a. For an instrument with electronic pressure and flow control, enter the followingvalue:


Verify that the column is operating in constant pressure mode by pressing the[Column 1] or [Column 2] key. Toggle down to the Mode line to check themode. If necessary, change to constant pressure by pressing the [Mode/Type]key and selecting Constant Pressure.




Inlet Temperature: Oven TrackDetector Temperature: 300°C

Oven Program:Temperature: 40°CInitial time: 0 minRate 1: 25°C/minFinal temperature: 90°CFinal time: 0 minRate 2: 15°C/minFinal temperature: 170°CFinal time: 2 min


6. After thermal stabilization, set the following values according to the appropriateinstrument.

a. For an electronic pressure and flow controlled FID, input the values below bypressing the appropriate detector key to open the control screen and thenentering the following flow values:

Hydrogen at 30Air at 400Makeup (nitrogen) at 25

Check that the detector is in constant makeup mode. If it is not, scroll to Mode,press the [Mode/Type] key, and select Constant Makeup Flow. If the detectorflow rates are checked, the values should be within the limits set in step 6b for amanual flow controlled FID.

b. For a manual flow controlled FID, establish the following flow rates by inserting

Page 5 of 12



61

the flow measurement adapter fully onto the FID collector and connecting theflowmeter:

Hydrogen at 30 ± 2 mL/minAir at 400 ± 30 mL/minMakeup (nitrogen) at 25 ± 2 mL/min

After setting the flows above, remove the flowmeter and flow measurementadapter.

7. At the HP 6890, turn on the FID electrometer by pressing [Configure] [FrontDetector] {or [Back Detector]}. Turn the electrometer on by scrolling to theelectrometer line and pressing [ON]. Press [Signal 1] to display its flame-offbackground offset. A stable value, <2.0 display units, is acceptable criteria tocontinue. If not met, stop here, and consult your HP 6890 service and user docu-mentation for additional information. If necessary, contact your local Hewlett-Packard service representative.




c. If the flame has not ignited, recheck all flow rates, and attempt ignition again.If the flame cannot be lit even though the flow rates are correct, consult yourHP 6890 service and user documentation for additional information.If necessary, contact your Hewlett-Packard service representative.



a. Remove the column from the detector, and replace the cap detector fitting.


Page 6 of 12



62

c. Monitor the displayed detector signal; it should rise quickly to some highervalue as the FID heats to the higher temperature. Then, over a longer time, thesignal should decrease to some reasonably constant value.


e. Restore the original setpoint temperatures specified in step 4, and allow the unitat least 2 hours to stabilize thermally. Observe the displayed detector signal todetermine if it is now within the acceptable range of between 5 and 20 displayunits, verify all gas flow rates, then continue to step 10.

f. If the displayed detector signal is still too great to continue, repeat the bakeoutprocess. If repeated bakeout cycles fail to give the acceptable signal level, itmay be an indication that the gases are impure. Higher purity gases and/or trapsmay be necessary. If cleaning the gases fails to give an acceptable signal level,consult your HP 6890 service and user documentation for additionalinformation. If necessary, contact your local Hewlett-Packard servicerepresentative.




• At the HP 3396B/C or HP 3397A integrator, enter the following setpointvalues:

[ATT 2^] [-] [2] [ENTER][ZERO] [5] [0] [ENTER][CHT SP] [1] [ENTER]






− Wander over any given 2-minute portion of the plot should be <14 mmin width.

Page 7 of 12



63






[LIST] [OP#] [6]





[ATT 2^] [-] [5] [ENTER]


− When plotted at [ATT 2^] [-] [7] noise in the first 1-minute portion of theplot should be <30 mm in width.



Page 8 of 12



64





• On the Specify Report window, choose the “performance + noise” ReportStyle for the report format. Close the window by clicking on OK.





− ASTM noise should be <0.0382 pA.Page 9 of 12



65











− MDL(C) = (86,800 x (Noise))/(Area C16) <= 4 pg/s with the area measured

min0 2 4 6 8 10 12 14

pA

2.75

3

3.25

3.5

3.75

4

4.25

4.5


Page 10 of 12



66

with the range 2^8 and the noise in mm at attn 2^0 (noise measured peakto peak).




NOTE: For the HP 3396C or HP 3397A integrator, ensure that the range value isfive by pressing:

[LIST] [OPTION] [8]


• At the integrator, enter the following setpoint values:[ZERO] [1] [0] [ENTER][ATT 2^] [7] [ENTER][CHT SP] [1] [ENTER][PK WD] [.] [0] [4] [ENTER][THRSH] [3] [ENTER][AR REJ] [0] [ENTER][TIME] [8] [.] [7] [5] [STOP]





− MDL(C) = (694,000 x (Noise*2^-6))/(Area C16) <= 4 pg/s with the noisemeasured in mm at attn 2^-6 (noise measured peak to peak).


Page 11 of 12



67








2 4 6 8

0

200

400

600

800

1000

1200

1400

1600

1800

2000

Time (min.)

C14 C15C16

Page 12 of 12


67


Title: TCD (Thermal Conductivity Detector) Checkout Using a PurgedPacked Column Inlet


Revision Number: ____________________________________________________________________


Approved by: ________________________________________________________________________

Reviewed by: ________________________________________________________________________

Effective Date: _______________________________________________________________________

Company Stamp:


• __________________________________________________________________

• __________________________________________________________________

• __________________________________________________________________

• __________________________________________________________________

• __________________________________________________________________

Page 1 of 12

TCD (Thermal Conductivity Detector), Purged Packed


68

Scope

Use the following procedure to verify proper TCD operation with the purged packedinlet.






• TCD flow measurement adapter, HP part no. 19301-60660

• Chromatographic-grade purity gas: helium as carrier, reference, and makeup




Analog Input





INET Input



Page 2 of 12



69


ChemStation Input



Related SOPs





Procedure



a. At the purged packed column inlet, install a new septum, a new O-ring (ifneeded), a capillary column adapter, a new insert, and the HP 6890 evaluationcolumn.

b. At the TCD, install the capillary column fitting, if necessary, and the remainingend of the checkout column.

2. At the HP 6890, verify that the TCD to be evaluated has its Gas Type set to heliumby pressing the [Configure] [Front Detector] {or [Back Detector]}. If necessary,change the gas type to helium by pressing the [Mode/Type] key and choosinghelium from the menu.


Page 3 of 12



70



• Install the remote start cable from the Remote receptacle on the HP 6890and the integrator.

• At the HP 6890, assign Signal 1 to the TCD to be evaluated:[Signal 1] [Front Detector] {or [Back Detector]}






c. HP 6890 HP-IB Output to the HP Multitechnique ChemStation

• This procedure assumes that the ChemStation is properly installed on thecomputer and connected to the HP 6890. If it is necessary to install andconfigure the ChemStation, please refer to the HP Multitechnique Chem-Station Manual set, especially “Installing Your GC ChemStation” (HP partno. G2070-90001).

• Once the ChemStation is properly installed and configured, bring up theproper on-line instrument for the HP 6890 to be tested. Then at the Chem-Station under the View menu, choose Run Method and Control View. On theRun Method and Control View, choose Instrument. From the Instrumentmenu, choose Edit Parameters. On the Edit Parameters screen, click onOptions. On the Options screen, choose the radio button labeled “No” forthe question “Keep instrument keyboard locked after method is loaded?”Click on [OK] to leave the screen. This will allow you to enter setpointsfrom the key-board. You may remain in the Edit Parameters screen, andenter the setpoints directly from the ChemStation.


Page 4 of 12



71

4. If present, remove the protective cap found installed on the TCD exhaust vent atthe top of the detector.


a. For an instrument with electronic pressure and flow control enter the followingvalues:


Verify that the column is operating in constant pressure mode by pressing the[Column 1] or [Column 2] key. Toggle down to the Mode line to check themode. If necessary, change to constant flow by pressing the [Mode/Type] keyand selecting Constant Flow.


Set the pressure to 25 psi, insert the flow measurement adapter onto the TCD,connect the flowmeter, and measure the carrier flow rate. It should bebetween 7.5 and 7.9 mL/min at an oven temperature of 40°C.

6. Insert the flow measurement adapter fully onto the TCD exhaust vent, and connectthe flowmeter:

a. For an electronic pressure and flow controlled TCD, establish the followingflow rates:

Carrier (helium) at 7.7 (+ 0.5) mL/minTCD reference (helium) at 20 (+ 1) mL/minTCD makeup (helium) at 2 (+ 0.5) mL/min

Input the above values by pressing the appropriate detector key to open thecontrol screen and then entering the flow values given above.

Check that the detector is in constant makeup mode. If it is not, scroll toMode, press the [Mode/Type] key, and select Constant Makeup Flow.

b. For a manual flow controlled TCD, establish the following flow rates:Carrier (helium) at 7.7 (+ 0.5) mL/minTCD reference (helium) at 20 (+ 1) mL/minTCD makeup (helium) at 2 (+ 0.5) mL/min

Then remove the flowmeter and flow measurement adapter.


Page 5 of 12



72




8. After thermal stabilization, at the HP 6890, turn on the TCD electrically bypressing the appropriate detector key to open the control screen. Turn thefilament on by toggling down to the filament line in the screen and pressing [ON].Allow about 3 minutes for stabilization.

Display the signal output to determine background offset by pressing [Signal 1]. Ifthe detector is not assigned properly, move the cursor to the signal line. Changethe signal by pressing the [Mode/Type] key, and then select the proper detectorfrom the signal list.

a. A stable offset at any value between 0.5 and 30 display units (inclusive) isacceptable. Continue to step 10.

b. If offset is <0.5 display unit, stop here, and consult your HP 6890 service anduser documentation for additional information. If necessary, contact your localHewlett-Packard service representative.

c. If offset is >30 display units, there may be chemical contamination contributingto the signal. Continue to step 9.

9. Perform a bakeout of the TCD in the following manner:

a. Remove the column from the detector, and cap the detector fitting.

b. Reset the TCD temperature to 400ºC, and allow at least 30 minutes for thermalstabilization.

c. Monitor the displayed detector signal; for chemical contamination, it shouldrise quickly to some higher value as the TCD heats to the higher temperature.Then, over a longer time, the signal should decrease to some reasonablyconstant value.

Page 6 of 12



73

a. Restore the original setpoint temperature of 300ºC, and allow at least 30minutes for thermal stabilization.

b. Observe the displayed detector signal to determine if it is now within theacceptable range of between 0.5 and 30 display units, verify all gas flow rates,then continue to step 10.

• If the displayed detector signal is still too great to continue, repeat thebakeout process. If repeated bakeout cycles fail to give the acceptablesignal level, consult your HP 6890 service and user documentation foradditional information. If necessary, contact your local Hewlett-Packardservice representative.

10. To check signal noise, wander, and drift, perform the following steps according tothe data handling device connected to the HP 6890:



• At the integrator, enter the following setpoint values:[ATT 2^] [0] [ENTER][ZERO] [5] [0] [ENTER][CHT SP] [1] [ENTER]

• Press [PLOT] to begin plotting the TCD signal.

• Allow plotting to continue for at least 15 minutes.

• Measure the plot to check for the following:

− Noise over any given 1-minute portion of the plot should be <9.0 mm inwidth. Up to four spikes (not exceeding 18 mm) are allowed in any givenportion provided they do not exceed limits.

− Drift or wander over any given 5-minute portion of the plot should be<22 mm in width.


Page 7 of 12



74



NOTE: For the HP 3396 Series II (HP 3396B), HP 3396 Series III (HP3396C), or HP 6890 Series (HP 3397A) integrator, the range value can bedetermined by entering:[LIST] [OP#] [6]

This will give the HP 6890 method listing. At the bottom of the listing is therange value for signal 1 and 2. This is the range set at the MIO (INET) card.Normally this value is set to 5. The noise can be plotted with the integratorrange value (this range is designated as SIG1RANGE) set to 5. The nextbulleted step is to be used with a SIG1RANGE = 5. The attenuation valueshave been adjusted to give the same amplitude plot as the analog. It ispermissible for the user to change the SIG1RANGE value to 0 (zero) and usethe same integrator settings as in step 10a. The user is referred to theHP 3396 manual for further details in how to change the SIG1RANGE value.



(Allow plotting to continue for at least 15 minutes.)


− Noise over any given 1-minute portion of the plot should be <11.25 mm inwidth. Up to four spikes (not exceeding 27.5 mm) are allowed in anygiven portion provided they do not exceed the limits.

− Drift or wander over any given 5-minute portion of the plot should be<27.5 mm in width.


Page 8 of 12



75

c. For HP 6890 HP-IB output to the HP ChemStation





• From the Report menu, choose System Suitability, which will bring up asecond menu. On the second menu, choose Edit Noise Ranges. (If SystemSuitability does not appear under the Report menu, go to the View menu,and choose Full Menu.) Once Edit Noise Ranges has been chosen, awindow will appear that allows time ranges to be entered. The ChemStationcalculates several different noise calculations. The ASTM noise will be usedin the MDL calculation later. The ASTM noise measurement requires thatthe noise range be ≥1.01 minutes. Enter several time ranges that are ≥1.01minutes. A time range of 5.0 minutes should also be entered. These rangescan overlap with the other ranges. Close the window by choosing OK.

• Under View, choose Method and Run Control. Under the Method menu,choose Save Method As, which will allow a unique method name to bechosen for the noise measurement. Once a method name has been assigned,go to the Instrument menu, and choose Edit Parameters. On the EditParameters screen, select the oven icon, and check that the oven tempera-ture is 40°C. Set the initial time to 12 minutes and rate 1 to 0°C/min. (Thissets up a 12-minute isothermal run.) Check the other parameters in steps 4through 6 by choosing the appropriate icon. Then click on OK to close theEdit Parameters screen.

• Under Run Control, choose Sample Information. Enter a directory nameand, if you choose, a file name. (This will allow you to have the file as aunique file and not as the default.) Once this is completed, close thewindow. Press start at the HP 6890 keyboard. This will start the noisemeasurement once the run is completed. (If the method has not been set upto print the report, go to Data Analysis View.) See the ChemStation manualfor more instructions on Data Analysis.

• Under View, choose Data Analysis. Load the data file for the blank run justcompleted. Under Report, choose Specify Report. Choose printer andscreen. Under Integration, choose Integrate. After integration is completed,print the report by choosing Print Report under Report. The report will listmeasurements for noise (peak to peak, 6 * sd, and ASTM) and for drift and

Page 9 of 12



76

wander.

− ASTM noise should be <0.05733 display units (25 µV/display unit forTCD).

− Wander or drift (for a 5-minute time window) should be <0.14 displayunits.





• Inject 1 µl of the checkout sample, and press [START] at the HP 6890 tobegin the checkout run.

• The resulting chromatogram should appear similar to that shown in thechromatogram figure. The following criteria indicate successful completionof the TCD chemical checkout:

− Area counts for components labeled C14, C15, and C16 should each be

min0 2 4 6 8 10 12 14

25 uV

11.5

11.75

12

12.25

12.5

12.75

13

13.25

TCD1 A, of TCDNOISE\NOISE002.D

Page 10 of 12



77

>515,000.


− MDL(C16 pg/mL) = (57,300,000 x Noise)/(Area C16) <= 1,000 pg/mL.




• Inject 1 µL of the checkout sample, and press [START] at the HP 6890 tobegin the checkout run.





• If these criteria are not met, repeat the test. If after repeated testing thecriteria cannot be met, consult your HP 6890 service and userdocumentation for additional information. If necessary, contact your localHewlett-Packard service representative.


• Inject 1 µl of the checkout sample, and press [START] at the HP 6890 tobegin the checkout run.

• The resulting chromatogram should appear similar to that shown in thechromatogram figure. The following criteria indicate successful completionof TCD chemical checkout:

− Area counts for components labeled C14, C15, and C16 should each be>65.

Page 11 of 12



78


− MDL (C16, pg/mL) = (1,125,000 x Noise)/(Area C16) <= 1,000 pg/mL.


2 4 6 80

10

20

30

40

50

60

Time (min.)

C14 C15

C16

Page 12 of 12


79


Title: TCD (Thermal Conductivity Detector) Checkout Using aSplit/Splitless Capillary Column Inlet


Revision Number: ____________________________________________________________________


Approved by: ________________________________________________________________________

Reviewed by: ________________________________________________________________________

Effective Date: _______________________________________________________________________

Company Stamp:


• __________________________________________________________________

• __________________________________________________________________

• __________________________________________________________________

• __________________________________________________________________

• __________________________________________________________________

Page 1 of 12

TCD (Thermal Conductivity Detector), Split/Splitless


80

Scope

Use the following procedure to verify proper TCD operation with the split/splitless inlet.







• Chromatographic-grade purity gases: helium as carrier, makeup, and reference


Analog Input





INET Input




ChemStation Input

• HP GC ChemStation software loaded as part of the HP multitechnique ChemStationPage 2 of 12



81

on an IBM-compatible personal computer with an HP-IB interface and the properamount of memory for applications to be run. (See the HP Multitechnique Chem-Station Manual for requirements.)


Related SOPs


• Liner/insert installation, SOP no. _____________



Procedure



a. At the capillary column inlet, install a new septum, a new split liner, an O-ringseal, and the HP 6890 evaluation column.

b. At the TCD, install the capillary column, if necessary, and the remaining end ofthe HP 6890 evaluation column.

2. At the HP 6890, verify that the TCD to be evaluated has its Gas Type set to heliumby pressing the [Configure] [Front Detector] {or [Back Detector]}. If necessary,change the gas type to helium by pressing the [Mode/Type] key and choosinghelium from the menu.




• Install the remote start cable from the Remote receptacle on the HP 6890and the integrator.



Page 3 of 12



82


• Install the INET signal cables between the INET I/O connectors on theHP 6890 and the integrator

• At the HP 6890, assign Signal 1 to the TCD to be evaluated: [Signal 1] [Front Detector] {or [Back Detector]}


c. HP 6890 HP-IB output to the HP multitechnique ChemStation

• This procedure assumes that the ChemStation is properly installed on thecomputer and connected to the HP 6890. If it is necessary to install andconfigure the ChemStation, please refer to the HP Multitechnique Chem-Station Manual set, especially “Installing Your GC ChemStation” (HP partno. G2070-90001).

• Once the ChemStation is properly installed and configured, bring up theproper on-line instrument for the HP 6890 to be tested. Then at the Chem-Station under the View menu, choose Run Method and Control View. On theRun Method and Control View, choose Instrument. From the Instrumentmenu, choose Edit Parameters. On the Edit Parameters screen, click onOptions. On the Options screen, choose the radio button labeled “No” forthe question “Keep instrument keyboard locked after method is loaded?”Click on [OK] to leave the screen. This will allow you to enter setpointsfrom the key-board. You may remain in the Edit Parameters screen, andenter the setpoints directly from the ChemStation.



5. Verify the inlet is operating in splitless mode by pressing the [Front Inlet] or [BackInlet] key. If not, change to the splitless mode by pressing the [Mode/Type] keyand selecting Splitless.


a. For an instrument with electronic pressure and flow control, enter thefollowing values:

Page 4 of 12



83

Column pressure = 25 psiPurge flow = 60Purge time = 0.75 min

Verify that the column is operating in constant pressure mode by pressing the[Column 1] or [Column 2] key. Toggle down to the Mode line to check themode. If necessary, change to constant pressure by pressing the [Mode/Type]key and selecting Constant Pressure.


Set the pressure to 25 psi, insert the flow measurement adapter onto the TCD,connect the flowmeter, and measure the carrier flow rate. It should bebetween 7.5 and 7.9 mL/min at an oven temperature of 40°C.

Connect the flowmeter to the inlet split flow vent, and adjust the flow rate to50− 70 mL/min. Record this value.

As measured at the inlet vents using the flowmeter, set the septum purge flowrate at 5 ± 1 mL/min.


For an electronic pressure and flow controlled TCD, input the values bypressing the appropriate detector key to open the control screen and thenentering the flow values given:

Carrier (helium) at 7.7 (± 0.5) mL/minTCD reference (helium) at 20 (± 1) mL/minTCD makeup (helium) at 2 (± 0.5) mL/min

Check that the detector is in constant makeup mode. If it is not, scroll toMode, press the [Mode/Type] key, and select Constant Makeup Flow.

b. For a manual flow controlled TCD, establish the following flow rates:Carrier (helium) at 7.7 (± 0.5) mL/minTCD reference (helium) at 20 (± 1) mL/minTCD makeup (helium) at 2 (± 0.5) mL/min




Page 5 of 12



84


9. After thermal stabilization, at the HP 6890, turn on the TCD electrically bypressing the appropriate detector key to open the control screen. Turn thefilament on by toggling down to the filament line in the screen and pressing [ON].Allow about 3 minutes for stabilization.

Display the signal output to determine background offset by pressing [Signal 1]. Ifthe detector is not assigned properly, move the cursor to the signal line. Changethe signal by pressing [Mode/Type], and then select the proper detector from thesignal list.


b. If offset is <0.5 display units, stop here, and consult your HP 6890 service anduser documentation for additional information. If necessary, contact your localHewlett-Packard service representative.




b. Reset the TCD temperature to 400ºC, and allow at least 30 minutes for thermalstabilization.

c. Monitor the displayed detector signal; for chemical contamination, it shouldrise quickly to some higher value as the TCD heats to the higher temperature.Then, over a longer time, the signal should decrease to some reasonablyconstant value.

a. Restore the original setpoint temperature of 300ºC, and allow at least 30minutes for thermal stabilization.

b. Observe the displayed detector signal to determine if it is now within theacceptable range of between 0.5 and 30 display units, verify all gas flow rates,then continue to step 11.

Page 6 of 12



85

c. If the displayed detector signal is still too great to continue, repeat the bakeoutprocess. If repeated bakeout cycles fail to give the acceptable signal level, itmay be an indication that the gases are impure. Higher purity gases and/ortraps may be necessary. If cleaning the gases fails to give an acceptable signallevel, consult your HP 6890 service and user documentation for additionalinformation. If necessary, contact your local Hewlett-Packard servicerepresentative.



• At the HP 6890, enter a Range value of 0 (zero) for Signal 1 (or Signal 2) bypressing [Signal 1] and scrolling down the control table to Range.





− Noise over any given 1 minute portion of the plot should be <9.0 mm inwidth. Up to four spikes (not exceeding 18 mm) are allowed in any givenportion provided they do not exceed limits.

− Drift or wander over any given 5-minute portion of the plot should be<22 mm in width.

• If these criteria are not met, repeat the test. If after repeated testing thecriteria cannot be met, stop here, and consult your HP 6890 service and userdocumentation for additional information. If necessary, contact your localHewlett-Packard Service representative.


• At the HP 6890, enter a range vale of 0 (zero) for Signal 1 (or Signal 2) bypressing [Signal 1] and scrolling down the control table to Range.

NOTE: For the HP 3396 Series II (HP 3396B), HP 3396 Series III (HP3396C), or HP 6890 Series (HP 3397A) integrator, the range value can bedetermined by entering:[LIST] [OP#] [6]

This will give the HP 6890 method listing. At the bottom of the listing is thePage 7 of 12



86

range value for signal 1 and 2. This is the range set at the MIO (INET) card.Normally this value is set to 5. The noise can be plotted with the integratorrange value (this range is designated as SIG1RANGE) set to 5. The nextbulleted step is to be used with a SIG1RANGE = 5. The attenuation valueshave been adjusted to give the same amplitude plot as the analog. It ispermissible for the user to change the SIG1RANGE value to 0 (zero) and usethe same integrator settings as in step 10a. The user is referred to the HP3396 manual for further details in how to change the SIG1RANGE value.

• At the integrator, enter the following setpoint values:[ATT 2^] [-] [5][ZERO] [5] [0][CHT SP] [1]



− Noise in the first 1-minute portion of the plot should be <11.25 mmin width. Up to 4 spikes (not exceeding 27.5 mm) are allowed in anygiven portion provided they do not exceed limits.



• If these criteria are not met, repeat the test. If after repeated testing thecriteria cannot be met, stop here, and consult your HP 6890 service and userdocumentation for additional information. If necessary, contact your localHewlett-Packard Service representative.






Page 8 of 12



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• From the Report menu, choose System Suitability, which will bring up asecond menu. On the second menu, choose Edit Noise Ranges. (If SystemSuitability does not appear under the Report menu, go to the View menu,and choose Full Menu.) Once Edit Noise Ranges has been chosen, awindow will appear that allows time ranges to be entered. The ChemStationcalculates several different noise calculations. The ASTM noise will be usedin the MDL calculation later. The ASTM noise measurement requires thatthe noise range be ≥1.01 minutes. Enter several time ranges that are ≥1.01minutes. A time range of 5.0 minutes should also be entered. These rangescan overlap with the other ranges. Close the window by choosing OK.

• Under View, choose Method and Run Control. Under the Method menu,choose Save Method As, which will allow a unique method name to bechosen for the noise measurement. Once a method name has been assigned,go to the Instrument menu, and choose Edit Parameters. On the EditParameters screen, select the oven icon, and check that the oven tempera-ture is 40°C. Set the initial time to 12 minutes and rate 1 to 0°C/min. (Thissets up a 12-minute isothermal run.) Check the other parameters in steps 4through 6 by choosing the appropriate icon. Then click on OK to close theEdit Parameters screen.

• Under Run Control, choose Sample Information. Enter a directory nameand, if you choose, a file name. (This will allow you to have the file as aunique file and not as the default.) Once this is completed, close thewindow. Press start at the HP 6890 keyboard. This will start the noisemeasurement once the run is completed. (If the method has not been set upto print the report, go to Data Analysis View.) See the ChemStation manualfor more instructions on Data Analysis.


− ASTM noise should be <0.05733 display units (25 µV/display unit forTCD).


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• Press [Prep Run] at the HP 6890 to prepare the inlet for splitless injection.Press [Status], and wait for the message “Ready for Injection.” Then inject1 µL of the checkout sample, and press [Start] at the HP 6890 to begin thecheckout run.





• If these criteria are not met, repeat the test. If after repeated testing the

min0 2 4 6 8 10 12 14

25 uV

11.5

11.75

12

12.25

12.5

12.75

13

13.25


Page 10 of 12



89

criteria cannot be met, consult your HP 6890 service and userdocumentation for additional information. If necessary, contact your localHewlett-Packard service representative.


• At the HP 6890, enter a range value of 8 for Signal 1 (or Signal 2) by pressing[Signal 1] and scrolling down the control table to Range.[Signal 1] [Range ^ ( )] [0] [ENTER]











− Area counts for components labeled C14, C15, and C16 should each bePage 11 of 12



90

>73.


− MDL(C16,pg/mL) = (1,272,000 x Noise)/(Area C16) <= 1,000 pg/mL.


2 4 6 8

20

30

40

50

60

70

Time (min.)

C14 C15 C16

Page 12 of 12


91


Title: TCD (Thermal Conductivity Detector) Checkout Using a CoolOn-Column Capillary Column Inlet


Revision Number: ____________________________________________________________________


Approved by: ________________________________________________________________________

Reviewed by: ________________________________________________________________________

Effective Date: _______________________________________________________________________

Company Stamp:


• __________________________________________________________________

• __________________________________________________________________

• __________________________________________________________________

• __________________________________________________________________

• __________________________________________________________________

Page 1 of 12

TCD (Thermal Conductivity Detector), Cool On-Column

Revision Date 9-Jan-98 Procedure no.:__________ Hewlett-Packard Company

92

Scope

Use the following procedure to verify proper TCD operation with the cool on-columninlet.






• Plunger button (10/pk) that converts HP 7673 syringes for manual use, HP part no.5181-8866



• Chromatographic-grade purity gases: helium as carrier, reference, and makeup



Analog Input





INET Input



Revision Date 9-Jan-98 Procedure no.:_________ Hewlett-Packard Company

93



ChemStation Input



Related SOPs





Procedure




b. At the TCD, install the capillary column fitting, if necessary, and the remainingend of the checkout column.

2. At the HP 6890, verify that the TCD to be evaluated has its Gas Type set to H2/Heand its Sensitivity set to HIGH:

a. Locate the Gas Type switch at the top of the HP 6890, adjacent to the TCD to beevaluated. If needed, set the switch to its H2/He position.

b. Depending upon the particular HP 6890, do one of the following to setSensitivity:

• On some HP 6890s, TCD sensitivity is set by a switch adjacent to the GasType switch. If a sensitivity switch is present, set it to the HIGH position.

Page 2 of 12Page 3 of 12



94

• For other HP 6890s, there is no TCD Sensitivity switch; the function is setthrough the keyboard. If no switch is present, enter the following keysequence to set the TCD to be evaluated to high sensitivity:[gold] [DET] [A] {or [B]} [ON]











c. HP 6890 HP-IB Output to HP GC ChemStation


• Once the ChemStation is properly installed and configured, bring up theproper on-line instrument for the HP 6890 to be tested. Then at the Chem-Station under the View menu, choose Run Method and Control View. On theRun Method and Control View, choose Instrument. From the Instrumentmenu, choose Edit Parameters. On the Edit Parameters screen, click onOptions. On the Options screen, choose the radio button labeled “No” for thequestion “Keep instrument keyboard locked after method is loaded?” Clickon [OK] to leave the screen. This will allow you to enter setpoints from thekey-board. You may remain in the Edit Parameters screen, and enter the

Page 4 of 12



95

setpoints directly from the ChemStation.





Column Pressure = 25 psi

Verify that the column is operating in constant pressure mode by pressing the[Column 1] or [Column 2] key. Toggle down to the Mode line to check the mode.If necessary, change to constant pressure using the [Mode/Type] key andselecting Constant Pressure.


Set the pressure to 25 psi. Insert the flow measurement adapter onto the TCD,connect the flowmeter and measure the carrier flow rate. It should be between7.5 and 7.9 mL/min (at an oven temperature of 40°C).


a. For an electron pressure and flow controlled TCD, establish the following flowrates:

Carrier (helium) at 7.7 (+ 0.5) mL/minTCD reference (helium) at 20 (+ 1) mL/minTCD makeup (helium) at 2 (+ 0.5) mL/min

Input the above values by pressing the appropriate detector key to open thecontrol screen and then entering the flow values given above.

Check that the detector is in constant makeup mode. If it is not, scroll to Mode,press the [Mode/Type] key, and select Constant Makeup Flow.

b. For a manual flow controlled TCD, establish the following flow rates:Carrier (helium) at 7.7 (+ 0.5) mL/minTCD reference (helium) at 20 (+ 1) mL/minTCD makeup (helium) at 2 (+ 0.5) mL/min

Page 5 of 12



96


7. Using the appropriate Inlet and Detector Control Tables on the HP 6890, set thefollowing heated zone and oven setpoint values.

Inlet Temperature: Oven TrackDetector Temperature: 300°C

Oven Program:Temperature: 40°CInitial time: 0 minRate 1: 25°C/minFinal Temperature: 90°CFinal Time: 0 minRate 2: 15°C/minFinal temperature: 170°CFinal Time: 2 min


8. After thermal stabilization, at the HP 6890, turn on the TCD electrically by pressingthe appropriate detector key to open the control screen. Turn the filament on bytoggling down to the filament line in the screen and pressing [ON]. Allow about3 minutes for stabilization.

Display the signal output to determine background offset by pressing [Signal 1]. Ifthe detector is not assigned properly, move the cursor to the signal line. Changethe signal by pressing the [Mode/Type] key, and then select the proper detectorfrom the signal list.


b. If offset is <0.5 display unit, stop here, and consult your HP 6890 service anduser documentation for additional information. If necessary, contact your localHewlett-Packard service representative.




a. Reset the TCD temperature to 400ºC, and allow at least 30 minutes for thermalstabilization.

b. Monitor the displayed detector signal; it should rise quickly to some higherPage 6 of 12



97

value as the TCD heats to the higher temperature. Then, over a longer time, thesignal should decrease to some reasonably constant value.

c. Restore the original setpoint temperature of 300ºC, and allow at least 30 minutesfor thermal stabilization.

d. Observe the displayed detector signal to determine if it is now within theacceptable range of between 0.5 and 30 display units, verify all gas flow rates,then continue to step 10.

e. If the displayed detector signal is still too great to continue, repeat the bakeoutprocess. If repeated bakeout cycles fail to give the acceptable signal level, itmay be an indication that the gases are impure. Higher purity gases and/or trapsmay be necessary. If cleaning the gases fails to give an acceptable signal level,consult your HP 6890 service and user documentation for additionalinformation. If necessary, contact your local Hewlett-Packard servicerepresentative.



• At the HP 6890, enter a range value of 0 (zero) for Signal 1 (or Signal 2) bypressing [Signal 1] by scrolling down the control table to Range:





− Noise over any given 1-minute portion of the plot should be <9.0 mm inwidth. Up to four spikes (not exceeding 18 mm) are allowed in any givenportion provided they do not exceed limits.

− Wander over any given 5-minute portion of the plot should be <22 mmin width.


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98



NOTE: For the HP 3396 Series II (HP 3396B), HP 3396 Series III (HP 3396C),or HP 6890 Series (HP 3397A) integrator, the range value can be determinedby entering:[LIST] [OP#] [6]

This will give the HP 6890 method listing. At the bottom of the listing is therange value for signal 1 and 2. This is the range set at the MIO (INET) card.Normally this value is set to 5. The noise can be plotted with the integratorrange value (this range is designated as SIG1RANGE) set to 5. The nextbulleted step is to be used with a SIG1RANGE = 5. The attenuation valueshave been adjusted to give the same amplitude plot as the analog. It ispermissible for the user to change the SIG1RANGE value to 0 (zero) and usethe same integrator settings as in step 10a. The user is referred to the HP3396 manual for further details in how to change the SIG1RANGE value.

• At the integrator, enter the following setpoint values:[ZERO] [5] [0] [ENTER][ATT 2^] [-] [5] [ENTER][CHT SP] [1] [ENTER]



− Noise in the first 1-minute portion of the plot should be <11.25 mm inwidth. Up to four spikes (not exceeding 27.5) are allowed in any givenportion provided they do not exceed the limits.







• From the Report menu, choose Specify Report.Page 8 of 12



99


• From the Report menu, choose System Suitability, which will bring up asecond menu. On the second menu, choose Edit Noise Ranges. (If SystemSuitability does not appear under the Report menu, go to the View menu, andchoose Full Menu.) Once Edit Noise Ranges has been chosen, a window willappear that allows time ranges to be entered. The ChemStation calculatesseveral different noise calculations. The ASTM noise will be used in the MDLcalculation later. The ASTM noise measurement requires that the noise rangebe ≥1.01 minutes. Enter several time ranges that are ≥1.01 minutes. A timerange of 5.0 minutes should also be entered. These ranges can overlap withthe other ranges. Close the window by choosing OK.

• Under View, choose Method and Run Control. Under the Method menu,choose Save Method As, which will allow a unique method name to bechosen for the noise measurement. Once a method name has been assigned,go to the Instrument menu, and choose Edit Parameters. On the EditParameters screen, select the oven icon, and check that the oven temperatureis 40°C. Set the initial time to 12 minutes and rate 1 to 0°C/min. (This sets upa12-minute isothermal run.) Check the other parameters in steps 4 through 6by choosing the appropriate icon. Then click on OK to close the EditParameters screen.



− ASTM noise should be <0.05733 display units (25 µV/display unit for TCD).


Page 9 of 12



100



• At the HP 6890, enter a range value of 0 for Signal 1 (or Signal 2] by pressing[Signal 1] and scrolling down the control table to Range.






− MDL(C) = (64,800,000 x (Noise*2^0))/(Area C16) <= 1,000 pg/mL with thearea measured with the range 2^0 and the noise in mm at attn 2^0.

• If these criteria are not met, repeat the test. If after repeated testing the

min0 2 4 6 8 10 12 14

25 uV

11.5

11.75

12

12.25

12.5

12.75

13

13.25


Page 10 of 12



101

criteria cannot be met, consult your HP 6890 service and user documentationfor additional information. If necessary, contact your local Hewlett-Packardservice representative.


• At the HP 6890, enter a range value of 0 for Signal 1 (or Signal 2] by pressing[Signal 1] and scrolling down the control table to Range.






− MDL(C) = (2,025,000 x (Noise*2^0))/(Area C16) <= 1,000 pg/mL with thearea measured with the range 2^0 and the noise in mm at attn 2^0.





− Area counts for components labeled C14, C15, and C16 should each be>73.


− MDL (C16, pg/mL) = (1,272,000 x Noise)/(Area C16)<= 1,000 pg/mL.Page 11 of 12



102


2 4 6 820

30

40

50

60

70

Time (min.)

C14 C15 C16

Page 12 of 12


103


Title: ECD (Electron Capture Detector) Checkout Using a PurgedPacked Column Inlet


Revision Number: ____________________________________________________________________


Approved by: ________________________________________________________________________

Reviewed by: ________________________________________________________________________

Effective Date: _______________________________________________________________________

Company Stamp:


• __________________________________________________________________

• __________________________________________________________________

• __________________________________________________________________

• __________________________________________________________________

• __________________________________________________________________

Page 1 of 12

ECD (Electron Capture Detector), Purged Packed


104

Scope

Use the following procedure to verify proper ECD operation with the purged packedinlet.



• ECD performance evaluation ("checkout") sample, HP part no. 18713-60040



• ECD flow measurement adapter, HP part no. 5020-8231

• Chromatographic-grade purity gas: helium as carrier and nitrogen as makeup

• Deactivated glass insert, HP part no. 5181-3382




Analog Input





INET Input

• HP 3396 Series II (HP 3396B), HP 3396 Series III (HP 3396C), or HP 6890 Seriesintegrator




105


ChemStation Input



Related SOPs





Procedure



a. At the purged packed column inlet, install a new septum, a new O-ring (ifneeded), a capillary column adapter, a new glass insert, and the HP 6890evaluation column.

b. At the ECD, install the makeup gas fitting and remaining end of the HP 6890evaluation column.

2. At the HP 6890, verify that the ECD to be evaluated has its Gas Type set to nitrogenby pressing the [Configure] [Front Detector] {or [Back Detector]}. If necessary,change the gas type to nitrogen by pressing the [Mode/Type] key and choosingnitrogen from the menu.





106




• At the HP 6890, assign Signal 1 to the ECD to be evaluated:[Signal 1] [Front Detector] {or [Back Detector]}









• Assign Signal 1 to the appropriate detector. On the ChemStation EditParameters screen, this is under Signals. Also choose Save Data All and aData Rate of 20 Hz

Page 4 of 12



107




Verify that the column is operating in constant flow mode by pressing the[Column 1] or [Column 2] key. Toggle down to the Mode line to check themode. If necessary, change to constant flow by pressing the [Mode/Type] keyand selecting Constant Flow. Verify that the correct gas type (helium) is chosenfor the inlet. Change to helium following the steps outlined in item 2.


Set the pressure to 25 psi, insert the flow measurement adapter onto the ECD,connect the flowmeter, and measure the carrier flow rate. It should be between7.5 and 7.9 mL/min at an oven temperature of 40°C.

5. If present, remove the vent line found installed on the ECD exhaust vent at the topof the detector, then insert the flow measurement adapter fully onto the ECDexhaust vent, and connect the flowmeter.

a. For an electron pressure and flow controlled ECD, input the values by pressingthe appropriate detector key to open the control screen and then entering theflow values:

ECD makeup (nitrogen) at 60 (± 3) mL/minECD anode purge (nitrogen) at 6 (± 1) mL/min


b. For a manual flow controlled ECD establish the following flow rates byinserting the flow measurement adapter fully onto the ECD collector andconnecting the flowmeter:


After setting the values above, remove the flowmeter and flow measurementadapter, and reconnect the vent line.

Error! Not a valid link..

Page 5 of 12



108



Oven Program:Temperature: 80°CInitial time: 0 minRate 1: 15°C/minFinal temperature: 180°CFinal time: 10 min


7. At the HP 6890, turn on the ECD by:

[Configure] [Front Detector] {or [Back Detector]}

a. Then under the configuration screen:Electrometer [ON]

b. Check the reference current value by [Front Detector] {or [Back Detector]}.Scroll to Reference Current, and set the value to 1.0.

c. A stable value, <100 display units, is acceptable criteria to continue to step 9.The value may be much higher indicating system bakeout is necessary; continueto step 8.

8. Perform a bakeout of the ECD in the following manner:


b. Reset the detector, oven, and inlet temperatures to the following values usingthe appropriate Inlet and Detector Control Tables on the HP 6890:

Inlet Temperature: 250°COven Temperature: 250°CDetector Temperature: 375°C

c. Monitor the displayed detector signal; for chemical contamination, it should risequickly to some higher value as the ECD heats to the higher temperature. Then,over a longer time, the signal should decrease to some reasonably constantvalue.

a. Restore the original setpoint temperatures specified in step 6, and allow the unitat least 30 minutes stabilize thermally.

Page 6 of 12



109

b. Observe the displayed detector signal to determine if it is now less than 100display units; if so, reinstall the column and allow at least 30 minutes forthermal stabilization.

c. If the displayed signal remains below 100 display units, verify all gas flow rates,then continue to step 9.

d. If the displayed detector signal is still too great to continue, repeat the bakeoutprocess. If repeated bakeout cycles fail to give the acceptable signal level, itmay be an indication that the gases are impure. Higher purity gases and/or trapsmay be necessary. If cleaning the gases fails to give an acceptable level, consultyour HP 6890 service and user documentation for additional information. Ifnecessary, contact your local Hewlett-Packard service representative.





• Press [PLOT] to begin plotting the ECD signal and continue for at least10 minutes.


− Noise over any given 1-minute portion of the plot should be <9 mmin width.

− Wander or drift over any given 10-minute portion of the plot should be<90 mm in width.


Page 7 of 12



110




[LIST] [OP#] [6]





− Noise over any given 1-minute portion of the plot should be <11.25 mmin width.

− Wander or drift over any given 10-minute portion of the plot should be<112.5 mm in width.





Page 8 of 12



111




• Under View, choose Method and Run Control. Under the Method menu,choose Save Method As, which will allow a unique method name to be chosenfor the noise measurement. Once a method name has been assigned, go tothe Instrument menu, and choose Edit Parameters. On the Edit Parametersscreen, select the oven icon, and check that the oven temperature is 80°C.Set the initial time to 12 minutes and rate 1 to 0°C/min. (This sets up a 12-minute isothermal run.) Check the other parameters in steps 4 through 6 bychoosing the appropriate icon. Then click on OK to close the Edit Parametersscreen.



− ASTM noise should be <0.05733.

− Wander or drift (for a 10-minute time window) should be <0.5733.




112



• At the integrator, enter the following setpoint values:[ZERO] [1] [0] [ENTER][ATT 2^] [7] [ENTER][CHT SP] [1] [ENTER][PK WD] [.] [0] [4] [ENTER][THRSH] [7] [ENTER][TIME] [1] [1] [STOP]


• The resulting chromatogram should appear similar to that shown in thechromatogram figure. The following criteria indicates successful completionof the ECD chemical checkout.

− MDL (lindane, pg/s) = (3366 x Noise)/(Area Lindane)

− MDL (lindane) < = 0.04 pg/s


• At the HP 6890, enter a range value of 0 for Signal 1 [or Signal 2] by pressing[Signal 1] and scrolling down the control table to Range.

• At the integrator, enter the following setpoint values:[ZERO] [1] [0] [ENTER]

min0 2 4 6 8

5 Hz

50

55

60

65

70

75

Page 10 of 12



113

[ATT 2^] [7] [ENTER][CHT SP] [1] [ENTER][PK WD] [.] [0] [4] [ENTER][THRSH] [7] [ENTER][TIME] [1] [1] [STOP]



− MDL (lindane, pg/s) = (105.1 x Noise)/(Area Lindane)



• If you are not in the Method and Run Control view, choose Method and RunControl under View. Under method, choose Save Method As, and change thename of the method file. Under the Instrument menu, choose Edit Param-eters. Click on the oven icon, and input the oven program outlined in step 6.Check other parameters by choosing the appropriate icon. Exit the screen bychoosing OK. Under Run Control, choose Sample Information, and changethe file name.

• Inject 1 µl of sample. If using manual injection, press Start on the GCkeyboard. When the run is completed, print by going to Data Analysis view.


• The resulting chromatogram should appear similar to that shown in thechromatogram figure. The following criteria indicates successful completionof ECD chemical checkout



Page 11 of 12



114

min0 2 4 6 8 10

arbs

50

100

150

200

250

300

Lindane

Aldrin

Page 12 of 12


115


Title: ECD (Electron Capture Detector) Checkout Using a Split/SplitlessCapillary Column Inlet


Revision Number: ____________________________________________________________________


Approved by: ________________________________________________________________________

Reviewed by: ________________________________________________________________________

Effective Date: _______________________________________________________________________

Company Stamp:


• __________________________________________________________________

• __________________________________________________________________

• __________________________________________________________________

• __________________________________________________________________

• __________________________________________________________________

Page 1 of 12

ECD (Electron Capture Detector), Split/Splitless


116

Scope

Use the following procedure to verify proper ECD operation with the split/splitlessinlet.







• Chromatographic-grade purity gases: helium as carrier and nitrogen as makeup


Analog Input





INET Input

• HP 3396 Series II (HP 3396B), HP 3396 Series III (HP 3396C), or HP 6890 Seriesintegrator



Page 2 of 12



117

ChemStation Input



Related SOPs






Procedure



a. At the capillary column inlet, install a new septum, a new liner, an O-ring seal,and the HP 6890 evaluation column.



3. After choosing one data handling device for the test, setup the data path betweenthe HP 6890 and the data handling device by choosing the appropriatecombination:



118








• At the HP 6890, assign Signal 1 to the appropriate ECD to be evaluated:[Signal 1] [Front Detector] {or [Back Detector]}




• Once the ChemStation is properly installed and configured, bring up theproper on-line instrument for the HP 6890 to be tested. Then at the Chem-Station under the View menu, choose Run Method and Control View. On theRun Method and Control View, choose Instrument. From the Instrumentmenu, choose Edit Parameters. On the Edit Parameters screen, click onOptions. On the Options screen, choose the radio button labeled “No” for thequestion “Keep instrument keyboard locked after method is loaded?” Click on[OK] to leave the screen. This will allow you to enter setpoints from the key-board. You may remain in the Edit Parameters screen, and enter the setpointsdirectly from the ChemStation.





119

4. Verify the inlet is operating in splitless mode by pressing the [Front Inlet] or [BackInlet] key. If not, change to the splitless mode by pressing the [Mode/Type] keyand selecting Splitless.



Column pressure = 25 psiPurge flow = 60 mL/minPurge Time = 0.75 min

Verify that the column is operating in constant pressure mode by pressing the[Column 1] or [Column 2] key. Toggle down to the Mode line to check themode. If necessary, change to constant pressure by pressing the [Mode/Type]key and selecting Constant Pressure. Change to helium following the stepsoutlined in item 3.



Connect the flowmeter to the inlet split flow vent, and adjust the flow rate to50− 70 mL/min. Record this value. Then calculate the split ratio by dividing thesplit vent flow by the column flow.

As measured at the inlet vent using a flowmeter, set the septum purge flow rateat 5 + 1 mL/min.

6. If present, remove the vent line found installed on the ECD exhaust vent at the topof the detector, then insert the flow measurement adapter fully onto the ECDexhaust vent, and connect the flowmeter.

a. For an electronic pressure and flow controlled ECD, input the values bypressing the appropriate detector key to open the control screen and thenentering the flow values:





120

b. For a manual flow controlled ECD, establish the following flow rates byinserting the flow measurement adapter fully onto the ECD collector andconnecting the flowmeter.


After setting the flows above, remove the flowmeter and flow measurementadapter, and reconnect the vent line.

WARNING: Ensure the ECD is properly vented before beginning this procedure.





8. At the HP 6890, turn on the ECD by:[Configure] [Front Detector] {or [Back Detector]}

a. Then under the configuration screen:Electrometer [ON]

b. Check the reference current value by [Front Detector] {or [Back Detector]}.Scroll to Reference Current, and set the value to 1.0.

c. A stable value, <100 display units, is acceptable criteria to continue to step 10.The value may be much higher indicating a system bakeout is necessary;continue to step 9.



b. Reset oven and inlet temperatures to the following values using the appropriateInlet and Detector Control Tables on the HP 6890:




121


c. Monitor the displayed detector signal; it should rise quickly to some highervalue as the ECD heats to the higher temperature. Then, over a longer time, thesignal should decrease to some reasonably constant value.

d. Restore the original setpoint temperatures specified in step 7, and allow the unitat least 30 minutes to stabilize thermally.

e. Observe the displayed detector signal to determine if it is now less than 100display units; if so, reinstall the column and allow at least 30 minutes forstabilization.

f. If the displayed detector signal remains below 100 display units, verify all gasflow rates, then continue to step 10.

g. If the displayed detector signal is still too great to continue, repeat the bakeoutprocess. If repeated bakeout cycles fail to give the acceptable signal level, itmay be an indication that the gases are impure. Higher purity gases and/or trapsmay be necessary. If cleaning the gases fails to give an acceptable level, consultyour HP 6890 service and user documentation for additional information. Ifnecessary, contact your local Hewlett-Packard service representative.





• Press [PLOT] to begin plotting the ECD signal, and continue for at least10 minutes.



Page 7 of 12



122






[LIST] [OP#] [6]






− Wander or drift over any given 10-minute portion of the plot should be<112.5 mm in width.


Page 8 of 12



123






• From the Report menu, choose System Suitability, which will bring up asecond menu. On the second menu, choose Edit Noise Ranges. (If SystemSuitability does not appear under the Report menu, go to the View menu, andchoose Full Menu.) Once Edit Noise Ranges has been chosen, a window willappear that allows time ranges to be entered. The ChemStation calculatesseveral different noise calculations. The ASTM noise will be used in the MDLcalculation later. The ASTM noise measurement requires that the noise rangebe ≥1.01 minutes. Enter several time ranges that are ≥1.01 minutes. A timerange of 10 minutes should also be entered. These ranges can overlap withthe other ranges. Close the window by choosing OK.

• Under View, choose Method and Run Control. Under the Method menu,choose Save Method As, which will allow a unique method name to be chosenfor the noise measurement. Once a method name has been assigned, go tothe Instrument menu, and choose Edit Parameters. On the Edit Parametersscreen, select the oven icon, and check that the oven temperature is 80°C.Set the initial time to 12 minutes and rate 1 to 0°C/min. (This sets up a 12-minute isothermal run.) Check the other parameters in steps 4 through 6 bychoosing the appropriate icon. Then click on OK to close the Edit Parametersscreen.


Page 9 of 12



124

• Under View, choose Data Analysis. Load the data file for the blank run justcompleted. Under Report, choose Specify Report. Choose printer andscreen. Under Integration, choose Integrate. After integration is completed,

print the report by choosing Print Report under Report. The report will listmeasure-ments for noise (peak to peak, 6 * sd, and ASTM) and for drift andwander.





• At the HP 6890, enter a range value of 0 for Signal 1 [or Signal 2] by pressing[Signal 1] and scrolling down the control table to Range



Page 10 of 12

min0 2 4 6 8

5 Hz

50

55

60

65

70

75



125

• The resulting chromatogram should appear similar to that shown in thechromatogram figure. The following criteria indicates successful completionof the ECD checkout.













Page 11 of 12



126




• The resulting chromatogram should appear similar to that shown in thechromatogram figure. The following criteria indicates successful completionof ECD chemical checkout.

− MDL (lindane, pg/s)= (66 x Noise)/(Area Lindane)

− MDL (lindane) <= 0.04 pg/s


Page 12 of 12

min0 2 4 6 8 10

arbs

50

100

150

200

250

300

Lindane

Aldrin


127


Title: ECD (Electron Capture Detector) Checkout Using a CoolOn-Column Capillary Column Inlet


Revision Number: ____________________________________________________________________


Approved by: ________________________________________________________________________

Reviewed by: ________________________________________________________________________

Effective Date: _______________________________________________________________________

Company Stamp:


• __________________________________________________________________

• __________________________________________________________________

• __________________________________________________________________

• __________________________________________________________________

• __________________________________________________________________

Page 1 of 12

ECD (Electron Capture Detector), Cool On-Column


128

Scope

Use the following procedure to verify proper ECD operation with the cool on-columninlet.






• Plunger button (10/pk) converts HP 7673 syringes for manual use, HP part no.5181-8866



• Chromatographic-grade purity gas: helium as carrier and nitrogen as makeup



Analog Input





INET Input


• INET communication card, HP 6890 Option 510 (accessory HP G1553A)Page 2 of 12



129


ChemStation Input



Related SOPs





Procedure



a. At the cool on-column capillary inlet, install a new septum, a 320-µm capillarycolumn on-column insert, and the HP 6890 evaluation column.




Page 3 of 12



130




• At the HP 6890, assign Signal 1 to the ECD to be evaluated:

[Signal 1] [Front Detector] {or [Back Detector]}










Page 4 of 12



131

4. To ensure carrier flow through the column during oven and zone heat-up, thefollowing flow rates should be established.



Verify that the column is operating in constant pressure mode by pressing the[Column 1] or [Column 2] key. Toggle down to the Mode line to check the mode.If necessary change to constant pressure by pressing the [Mode/Type] key andselecting Constant Pressure. Verify that the correct gas type (helium) is chosenfor the inlet. Change to helium following the steps outlined in item 2.



5. If present, remove the vent line found installed on the ECD exhaust vent at the topof the detector, then insert the flow measurement adapter fully onto the ECDexhaust vent, and connect the flowmeter:

a. For an electronic pressure and flow controlled ECD input the values by pressingthe appropriate detector key to open the control screen and then entering theflow values:



b. For a manual flow controlled ECD establish the following flow rates byinserting the flow measurement adapter fully onto the ECD collector andconnecting the flowmeter:


After setting the flows above, remove the flowmeter and flow measurementadapter, and reconnect the vent line.

Error! Not a valid link..

Page 5 of 12



132

6. Using the appropriate Inlet and Detector Control Tables on the HP 6890 set thefollowing heated zone and oven setpoint values:

Inlet Temperature: Oven trackDetector Temperature: 300°C



7. At the HP 6890, turn on the ECD by:[Configure] [Front Detector] {or [Back Detector]}

a. Then under the configuration screenElectrometer [ON]

b. Check the reference current value by [Front Detector] {or [Back Detector]}.Scroll to Reference Current, and set the value to 1.0

c. A stable value, <100 display units, is acceptable criteria to continue to step 9.The value may be much higher indicating system bakeout is necessary; continueto step 8.



b. Reset the detector, oven, and inlet temperatures to the following values usingthe appropriate Inlet and Detector Control Tables on the HP 6890.

Inlet Temperature: Oven TrackOven Temperature: 250°CDetector Temperature: 375°C

c. Monitor the displayed detector signal; it should rise quickly to some highervalue as the ECD heats to the higher temperatures. Then, over a longer time,the signal should decrease to some reasonably constant value.

a. Restore the original setpoint temperatures specified in step 6, and allow the unitat least 30 minutes to stabilize thermally.

Page 6 of 12



133

b. Observe the displayed detector signal to determine if it is now less than 100display units; if so, reinstall the column, and allow at least 30 minutes forstabilization.

c. If the displayed detector signal remains below 100 display units, verify all gasflow rates, then continue to step 9.

d. If the displayed detector signal is still too great to continue, repeat the bakeoutprocess. If repeated bakeout cycles fail to give the acceptable signal level, itmay be an indication that the gases are impure. Higher purity gases and/or trapsmay be necessary. If cleaning the gases fails to give an acceptable level, consultyour HP 6890 service and user documentation for additional information. Ifnecessary, contact your local Hewlett-Packard service representative.





• Press [PLOT] to begin plotting the ECD signal, and continue for at least10 minutes.





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[LIST] [OP#] [6]




− Noise over any given 1-minute portion of the plot should be < 11.25 mmin width.

− Wander or drift over any given 10 minute portion of the plot should be<112.5 mm in width.

• If these criteria are not met, repeat the test. If after repeated testing thecriteria cannot be met, stop here, and consult your HP 6890 service and userdocumentation for additional information. If necessary, contact your localHewlett-Packard service representative




• From the Report menu, choose Specify Report.Page 8 of 12



135








Page 9 of 12



136











min0 2 4 6 8

5 Hz

50

55

60

65

70

75

Page 10 of 12



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[ZERO] [1] [0] [ENTER][ATT 2^] [7] [ENTER][CHT SP] [1] [ENTER][PK WD] [.] [0] [4] [ENTER][THRSH] [7] [ENTER][TIME] [1] [1] [STOP]









• The resulting chromatogram should appear similar to that shown in thechromatogram figure. The following criteria indicates successful completionof ECD chemical checkout.



Page 11 of 12



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min0 2 4 6 8 10

arbs

50

100

150

200

250

300

Lindane

Aldrin

Page 12 of 12

Revision Date 9-Jan-98 Procedure No.:________________ Hewlett-Packard Company

139


Title: NPD (Nitrogen Phosphorus Detector) Checkout Using a PurgedPacked Column Inlet


Revision Number: ____________________________________________________________________


Approved by: ________________________________________________________________________

Reviewed by: ________________________________________________________________________

Effective Date: _______________________________________________________________________

Company Stamp:


• __________________________________________________________________

• __________________________________________________________________

• __________________________________________________________________

• __________________________________________________________________

• _____________________________________________________________

Page 1 of 14

NPD (Nitrogen Phosphorus Detector), Purged Packed


140

Scope

Use the following procedure to verify proper NPD operation with the purged packedinlet.



• NPD performance evaluation ("checkout") sample, HP part no. 18789-60060

• O-ring, HP part no. 5080-8898

• HP Series 530 µm liner, HP part no. 19244-80540



• NPD bead/source, HP part no. G1534-60570



• NPD flow measurement adapter, HP part no. G1534-60640

• Chromatographic-grade purity gases: air and hydrogen to support the NPD, helium ascarrier and as makeup


Analog Input


• HP 6890A-to-HP 3396B/C or HP 3397A analog signal cable HP part no. G1530-60570(2-meter, 6-pin)


• HP 6890A-to-HP 3396C or HP 3397A remote start cable, HP part no. 03396-61010 (9-pin/15-pin)



141

INET Input




ChemStation Input



Related SOPs



• NPD flow measurement adapter, installation, SOP no. _____________



Procedure

WARNING: If the unit has been previously in operation, areas may be hot enough tocause serious burns. Switch off heated zones and the oven, and allow theunit sufficient time to cool.


a. At the purged packed inlet, install a new septum, a new glass insert, a newO-ring (if needed), and the HP 6890 evaluation column.

b. At the NPD, install an 0.011-inch jet and/or the capillary column adapter, ifneeded, and the remaining end of the HP 6890 evaluation column.

a. If needed, install a new NPD bead/source.




142

2. At the HP 6890, verify that the NPD to be evaluated has its gas type set to heliumby pressing the [Configure] [Front Detector] {or [Back Detector]}. If necessary,change the gas type to helium by pressing the [Mode/type] key and choosinghelium from the menu.

3. After choosing one data handling device for the test, set up the data path betweenthe HP 6890 and the data handling device by choosing the appropriatecombination.


• Install the analog signal cable from the Signal 1 output receptacle on theHP 6890 to the integrator.

• Install the remote start cable from the Remote receptacle on the HP 6890 tothe integrator.

• At the HP 6890, assign Signal 1 to the NPD to be evaluated:[Signal 1] [Front Detector] {or [Back Detector]}








• Once the ChemStation is properly installed and configured, bring up theproper on-line instrument for the HP 6890 to be tested. Then at the Chem-Station under the View menu, choose Run Method and Control View. On theRun Method and Control View, choose Instrument. From the Instrumentmenu, choose Edit Parameters. On the Edit Parameters screen, click onOptions. On the Options screen, choose the radio button labeled “No” for thequestion “Keep instrument keyboard locked after method is loaded?” Click on



143

[OK] to leave the screen. This will allow you to enter setpoints from the key-board. You may remain in the Edit Parameters screen, and enter the setpointsdirectly from the ChemStation.



a. For an instrument with electronic pressure and flow control, enter the followingvalue :


Verify that the column is operating in constant flow mode by pressing the[Column 1] or [Column 2] key. Toggle down to the Mode line to check themode. If necessary, change to constant pressure using the [Mode/Type] key andselecting Constant Flow.


• Set the pressure of the inlet to 25 psi. Connect the flowmeter to the exit tubeof the detector. The flow should be between 5.5 and 7.0 mL/min at an oventemperature of 40°C. (The detector leaks so that all the flow does not gothrough the exit tube.)

• Connect the flowmeter to the inlet split flow vent and adjust the flow rate60 ± 10 mL/min

5. After thermal stabilization, set the following flow rate values:

a. For an electron pressure and flow controlled NPD, set mode to ConstantColumn plus Makeup, and input the following values.

Hydrogen at 3 (± 1) mL/minAir at 60 (± 5) mL/minColumn plus Make-Up (Helium) at 10 (± 1) mL/min

b. To measure flows properly for the manual NPD, the bead must be removed andthe NPD flow measurement adapter inserted. Connect the flowmeter. Set thefollowing:

Hydrogen flow = 3 mL/min (± 1) mL/minAir flow = 60 mL/min (± 5) mL/minMakeup plus column flow = 10 (± 1) mL/min




144

After all flow rates are set, remove the flowmeter and flow-measurementadapter, then turn on all gas flows.


Inlet Temperature: 250°CDetector Temperature: 300°COven Temperature: 250°C

Wait 30 minutes, then reset values as shown:

Inlet Temperature: 200°C



7. At the HP 6890, turn on the NPD electrometer by pressing [Configure] [FrontDetector] {or [Back Detector]}. Turn the electrometer on by scrolling to theElectrometer line and pressing [ON]. Press [Signal 1] to display its backgroundoffset. A stable value, < 3.0 display units, is acceptable criteria to continue. If notmet, stop here, and consult your HP 6890 service and user documentation foradditional information. If necessary, contact your local Hewlett-Packard servicerepresentative.

8. When powering up the NPD, use the Auto Adjust feature of the NPD to bring thebaseline(offset) up.

[Front Detector] {or [Back Detector]} [Det Control] [ON](If the default baseline setting is not 50, key in 50 now,)

[5] [0] [ENTER]

a. If no increase in signal output has been observed even though the bead voltageline reads 4.095, consult your HP 6890 service and user documentation foradditional information. If necessary, contact your local Hewlett-Packard servicerepresentative.

a. If after an extended time period no stable offset can be achieved, gas flow ratesmay be incorrect, a new bead/source may be required, or service is required.Turn off the auto adjusting process (press the [OFF] key while the cursor is onthe Adjust offset line), recheck gas flow rates and replace the bead/source. If




145

necessary, consult your HP 6890 service and user documentation for additionalinformation. If still necessary, contact your local Hewlett-Packard servicerepresentative.

9. Bakeout may be required to improve baseline quality after extended storage,service, or part replacement. If necessary, perform bakeout of the NPD in thefollowing manner.


b. For an electronic pressure and flow controlled NPD, set the mode to ConstantMakeup, and set Makeup to 10 mL/min. For a manual pressure and flowcontrolled NPD, attach the flowmeter to the NPD vent, and adjust Makeup toapproximately 9 mL/min.

c. Use the Auto Adjust feature of the NPD to bring the offset up. When itapproximates the target value, press [Delete] to abort the adjustment process.

d. Reset the detector, oven, and inlet temperatures to the flowing values using theappropriate Inlet and Detector Control tables on the HP 6890.


e. Monitor the displayed detector signal. It should rise quickly to some highervalue as the NPD heats to the higher temperature. Then oven a longer time(typically 1 hour or more), the signal should decrease to some reasonableconstant value.

f. Restore the original setpoints, and allow at least 30 minutes for thermalstabilization.

g. Proceed to step 10 to check signal noise, wander and drift with no columninstalled. If results are acceptable, turn the detector off, reinstall the column,and restore the original Makeup flow parameters. Then continue the processwith the column reinstalled starting with step 10.

h. If the results are not acceptable, repeat the bakeout process. If repeatedbakeout cycles fail to give acceptable results, install a new bead/source andrepeat the process starting with step 8. If neither bakeout nor bead/sourcereplacement is effective, consult your HP 6890 service and user documentationfor additional information. If necessary, contact your local Hewlett-Packardservice representative.



146


Page 7 of 14



147


• At the HP 6890, enter a Range value of 0 (zero) for Signal 1 (or Signal 2) bypressing [Signal 1] and scrolling down the control table to Range

• At the integrator, enter the following setpoint values:[ZERO] [5] [0] [ENTER][ATT 2^] [0] [ENTER][CHT SP] [1] [ENTER]

• Press [PLOT] to begin plotting the NPD signal. After approximately 2minutes, press [ATT 2^] [2] [ENTER].


− Noise of the plot (first 2 minutes only) should be < 12 mm in width.

− Wander over any given 2-minute period (after first 2 minutes) should be<15 mm in width

− Drift over any given 5-minute period (after first 2 minutes) should be<30 mm in width.

• If these criteria are not met, repeat the test. Some adjustments to hydrogenand air flow may be necessary for optimal results. If, after repeated testing,the criteria cannot be met, stop here and consult your 6890 service and userdocumentation for additional information. If necessary, contact your localHewlett-Packard Service representative.




[LIST] [OP#] [6]

This will give the HP 6890 method listing. At the bottom of the listing is therange value for signal 1 and 2. This is the range set at the MIO (INET) card.Normally this value is set to 5. The noise can be plotted with the integratorrange value (this range is designated as SIG1RANGE) set to 5. The nextbulleted step is to be used with a SIG1RANGE = 5. The attenuation valueshave been adjusted to give the same amplitude plot as the analog. It ispermissible for the user to change the SIG1RANGE value to 0 (zero) and usethe same integrator settings as in step 10a. The user is referred to the HP 3396

Page 8 of 14



148

manual for further details in how to change the SIG1RANGE value.

• At the integrator, enter the following setpoi nt values:[ZERO] [5] [0] [ENTER][ATT 2^] [5] [ENTER][CHT SP] [1] [ENTER]

• Press [PLOT] to begin plotting the NPD signal. After approximately 2 minutes,press [ATT 2^] [-] [3] [Enter].


− Noise of the plot (first 2 min only) should be < 15 mm in width.

− Wander over any given 2-minute period (after first 2 min) should be<18.75 mm in width.

− Drift over any given 5-minute period (after first 2 min) should be < 37.5 mmin width.

• If these criteria are not met, repeat the test. Some adjustments to hydrogenand air flow may be necessary for optimal results. If after repeated testingthe criteria cannot be met, stop here, and consult your HP 6890 service anduser documentation for additional information. If necessary, contact yourlocal Hewlett-Packard service representative.










149

• Under View, choose Method and Run Control. Under the Method menu,choose Save Method As, which will allow a unique method name to be chosenfor the noise measurement. Once a method name has been assigned, go tothe Instrument menu, and choose Edit Parameters. On the Edit Parametersscreen, select the oven icon, and check that the oven temperature is 60°C. Setthe initial time to 12 minutes and rate 1 to 0°C/min. (This sets up a 12-minuteisothermal run.) Check the other parameters in steps 4 through 6 by choosingthe appropriate icon. Then click on OK to close the Edit Parameters screen.

• Under Run Control, choose Sample Information. Enter a directory name and,if you choose, a file name. (This will allow you to have the file as a uniquefile and not as the default.) Once this is completed, close the window. Pressstart at the HP 6890 keyboard. This will start the noise measurement once therun is completed. (If the method has not been set up to print the report, go toData Analysis View.) See the ChemStation manual for more instructions onData Analysis.

• Under View, choose Data Analysis. Load the data file for the blank run justcompleted. Under Report, choose Specify Report. Choose printer and screen.Under Integration, choose Integrate. After integration is completed, print thereport by choosing Print Report under Report. The report will list measure-ments for noise (peak to peak, 6 * sd, and ASTM) and for drift and wander.




min0 2 4 6 8 10

pA

46

48

50

52

54

NPD1 A, of NPDNOISE\NPDN0002.D



150




• At the integrator, enter the following setpoint values:[ZERO] [1] [0] [ENTER][ATT 2^] [7] [ENTER][CHT SP] [1] [ENTER][AR REJ] [1] [0] [0] [0] [ENTER][THRSH] [7] [ENTER][PK WD] [.] [0] [4] [ENTER][TIME] [1] [2] [STOP]

• Inject 1 µL of the checkout sample, and press [START] at the HP 6890 to beginthe checkout run.

• The resulting chromatogram should appear similar to that shown in thechromatogram figure. The following criteria indicate successful completion ofthe NPD chemical checkout:

− Area counts for the component labeled azobenzene should be >306,000

MDL (azobenzene) = 10,200*Noise/Area

MDL (azobenzene) should be <0.4 pg/s

− Area counts for the component labeled malathion should be 575,000

MDL (malathion) = 9,600*Noise/Area

MDL (malathion) should be <0.2 pg/s




• At the integrator, enter the following setpoint values:[ZERO] [1] [0] [ENTER][ATT 2^] [7] [ENTER]




151

[CHT SP] [1] [ENTER][AR REJ] [1] [0] [0] [0] [ENTER][THRSH] [7] [ENTER][PK WD] [.] [0] [4] [ENTER][TIME] [1] [2] [STOP]



− Area counts for the component labeled azobenzene should be >12,000.

MDL (azobenzene) = 319*Noise/Area


− Area counts for the component labeled malathion should be >22,500.

MDL (malathion) = 300*Noise/Area






− Area counts for the component labeled azobenzene should be >38.

MDL (azobenzene) = 200 * Noise/Area

MDL (azobenzene) should be <= 0.4 pg/s

− Area counts for the component labeled malathion should be >71.

MDL (malathion) = 188 * Noise/Area

MDL (malathion) should be <= 0.2 pg/s

Page 13 of 14



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min0 2.5 5 7.5 1 12

arbs

40

50

60

70

80

90

10

11

12

Azobenzene

Octadecane

Malathion

Page 14 of 14


153


Title: NPD (Nitrogen Phosphorus Detector) Checkout Using aSplit/Splitless Capillary Column Inlet


Revision Number: ____________________________________________________________________


Approved by: ________________________________________________________________________

Reviewed by: ________________________________________________________________________

Effective Date: _______________________________________________________________________

Company Stamp:


• __________________________________________________________________

• __________________________________________________________________

• __________________________________________________________________

• __________________________________________________________________

• __________________________________________________________________

Page 1 of 14

NPD (Nitrogen Phosphorus Detector), Split/Splitless


154

Scope

Use the following procedure to verify proper NPD operation with the split/splitlessinlet.




• Deactivated splitless liner, HP part no. 5062-3587





• NPD Flow-Measurement Adapter, P/N G1534-60640

• Chromatographic-grade purity gases: air and hydrogen to support the NPD, heliumas carrier and as makeup


Analog Input





INET Input


Page 2 of 14



155



ChemStation Input



Related SOPs






Procedure



a. At the capillary column inlet, install a new septum, a new splitless liner, a newO-ring seal, and an HP 6890 evaluation column.

b. At the NPD, install an 0.011-inch jet, capillary column adapter (if the detector isnot capillary only), and remaining end of the HP 6890 evaluation column.

c. If needed, install a new NPD bead/source.

2. At the HP 6890, verify that the NPD to be evaluated has its gas type set to heliumby pressing the [Configure] [Front Detector] {or [Back Detector]}. If necessary,change the gas type to helium by pressing the [Mode/type] key and choosingnitrogen from the menu.

Page 3 of 14



156













• Once the ChemStation is properly installed and configured, bring up theproper on-line instrument for the HP 6890 to be tested. Then at the Chem-Station under the View menu, choose Run Method and Control View. On theRun Method and Control View, choose Instrument. From the Instrumentmenu, choose Edit Parameters. On the Edit Parameters screen, click onOptions. On the Options screen, choose the radio button labeled “No” for thequestion “Keep instrument keyboard locked after method is loaded?” Click on[OK] to leave the screen. This will allow you to enter setpoints from the key-board. You may remain in the Edit Parameters screen, and enter the setpointsdirectly from the ChemStation.

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4. Verify the inlet is operating in splitless mode by pressing the [Front Inlet] or [BackInlet] key. If not, change to the splitless mode by pressing the [Mode/Type] key andselecting Splitless.



Column pressure (He) = 25 psiPurge Flow = 60 mL/minPurge Time = 0.75 min

Verify that the column is operating in constant pressure mode by pressing the[Column 1] or [Column 2] key. Toggle down to the Mode line to check the mode.If necessary, change to constant pressure using the [Mode/Type] key and selectingConstant Pressure.


• Set the pressure of the inlet to 25 psi. Connect the flow meter to the exit tubeof the detector. The flow should be between 5.5 and 7.0 mL/min at an oventemperature of 60°C. (The detector leaks so that all the flow does not gothrough the exit tube.)

• Connect the flowmeter to the inlet split flow vent and adjust the flow rate60 ± 10 mL/min.

6. Set the following flow rates according to the appropriate instrument:

a. For an electronic pressure and flow controlled NPD, input the following valuesby pressing the appropriate detector key to open the control screen and thenentering the following flow values:

Hydrogen flow = 3 (± 1) mL/minAir flow = 60 (± 5) mL/minMakeup plus column flow (helium) = 10 mL/min


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Hydrogen flow = 3 (± 1) mL/minAir flow = 60 (± 5) mL/minMakeup plus column flow = 10 mL/min

After all flow rates are set, remove the flow meter and NPD flow measurementadapter, reinstall bead/source, and turn on all detector gases.


Inlet Temperature: 250°CDetector Temperature: 300°COven Temperature: 250°C

Wait 30 minutes; then reset the values as shown:Inlet Temperature: 200 C



8. Press [Signal 1] to display its background offset. A stable value < 3.0 display unitsshould be attained within 1 hour. If not, stop here and consult your HP 6890 serviceand user documentation for additional information. If necessary, contact your localHewlett-Packard service representative.

9. When powering up the NPD, use the Auto Adjust feature of the NPD to bring thebaseline (offset) up.

[Front Detector] {or [Back Detector]} [Det Control] [ON]

(If the default baseline setting is not 50, key in 50 now.)[5] [0] [ENTER ]

a. If no increase in signal output has been observed even though the Bead voltageline reads 4.095, consult your HP 6890 service and user documentation foradditional information. If necessary, contact your local Hewlett-Packard servicerepresentative.

b. If after an extended time period no stable offset can be achieved, gas flow ratesmay be incorrect, a new bead/source may be required or service is required.Turn off the auto adjusting process (press the [OFF] key while the cursor is onthe Adjust offset line), recheck gas flow rates, and replace the bead/source. If

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159

necessary, consult your HP 6890 service and user documentation for additionalinformation. If still necessary, contact your local Hewlett-Packard servicerepresentative.







e. Monitor the displayed detector signal. It should rise quickly to some highervalue as the NPD heats to the higher temperature. Then oven a longer time(typically 1 hour or more), the signal should decrease to some reasonableconstant value.



e. If the results are not acceptable, repeat the bakeout process. If repeatedbakeout cycles fail to give acceptable results, install a new bead/source andrepeat the process starting with step 9. If neither bakeout nor bead/sourcereplacement is effective, consult your HP 6890 service and user documentationfor additional information. If necessary, contact your local Hewlett-Packardservice representative.


Page 7 of 14



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• Press [PLOT] to begin plotting the NPD signal. After approximately 2 minutes,press [ATT 2^] [2] [Enter]



− Wander over any given 2-minute period (after first 2 minutes) should be <15 mm in width


• If these criteria are not met, repeat the test. Some adjustments to hydrogenand air flow may be necessary for optimal results. If after repeated testingthe criteria cannot be met, stop here, and consult your HP 6890 service anduser documentation for additional information. If necessary, contact yourlocal Hewlett-Packard service representative.




[LIST] [OP#] [6]


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− Wander over any given 2-minute period (after first 2 min) should be < 18.75mm in width.







• On the Specify Report menu, choose the “performance + noise” Report Stylefor the report format. Close the window by clicking OK.


• Under View, choose Method and Run Control. Under the Method menu,choose Save Method As, which will allow a unique method name to be chosen

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for the noise measurement. Once a method name has been assigned, go tothe Instrument menu, and choose Edit Parameters. On the Edit Parametersscreen, select the oven icon, and check that the oven temperature is 60°C. Setthe initial time to 12 minutes and rate 1 to 0°C/min. (This sets up a 12-minuteisothermal run.) Check the other parameters in steps 4 through 6 by choosingthe appropriate icon. Then click on OK to close the Edit Parameters screen.






min0 2 4 6 8 10

pA

46

48

50

52

54


12. To perform chemical checkout, choose the appropriate data handling device:Page 10 of 14



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• Press [Prep Run] at the HP 6890 to prepare the inlet for split less injection.Press [Status], and wait for the message “Ready for Injection.” Then inject1 µL of the checkout sample, and press [Start] at the HP 6890 to begin thecheckout run.


− Area counts for the component labeled azobenzene should be >306,000



− Area counts for the component labeled malathion should be >575,000







Page 11 of 14



164

[ZERO] [1] [0] [ENTER][ATT 2^] [7] [ENTER][CHT SP] [1] [ENTER][AR REJ] [1] [0] [0] [0] [ENTER][THRSH] [7] [ENTER][PK WD] [.] [0] [4] [ENTER][TIME] [1] [2] [STOP]















MDL (azobenzene) should be <= 0.4 pg/sPage 12 of 14



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min0 2.5 5 7.5 1 12.

arbs

40

50

60

70

80

90

10

11

12

Azobenzene

Octadecane

Malathion




166

NPD (Nitrogen Phosphorus Detector), Cool On-Column


167


Title: NPD (Nitrogen Phosphorus Detector) Checkout Using a CoolOn-Column Capillary Column Inlet


Revision Number: ____________________________________________________________________


Approved by: ________________________________________________________________________

Reviewed by: ________________________________________________________________________

Effective Date: _______________________________________________________________________

Company Stamp:


• __________________________________________________________________

• __________________________________________________________________

• __________________________________________________________________

• __________________________________________________________________

• __________________________________________________________________

Page 1 of 14



168

Scope

Use the following procedure to verify proper NPD operation with the cool on-columninlet.





• 5-µl syringe, HP part no. 5182-0836 (barrel), 5182-0831 (needle)


• Plunger button (10/pk) converts HP 7673 syringes for manual use, HP part no.5181-8866


• NPD flow measurement adapter, HP part no. G1534-60640

• Chromatographic-grade purity gases: air and hydrogen to support the NPD, helium ascarrier and as makeup

• 320-µm capillary column on-column insert (HP part no. 19245-20525


Analog Input

• HP 3395B, HP 3396 Series II (HP 3396B), HP 3396 Series III (HP 3396C), and HP 6890Series (HP 3397A) integrator






169

INET Input

• HP 3396 Series II (HP 3396B), HP 3396 Series III (HP 3396C), or HP 6890 Series(HP 3397A integrator



ChemStation Input



Related SOPs





Procedure




b. At the NPD, install a 0.011-inch jet, capillary column adapter, if needed, and theremaining end of the HP 6890 Evaluation Column.

c. If needed, install a new NPD bead/source.

Page 2 of 14



170

2. At the HP 6890, verify that the NPD to be evaluated has its gas type set to heliumby pressing the [Configure] [Front Detector] {or [Back Detector]}. If necessary,change the gas type to helium by pressing the [Mode/type] key and choosinghelium from the menu.













• Once the ChemStation is properly installed and configured, bring up theproper on-line instrument for the HP 6890 to be tested. Then at the Chem-Station under the View menu, choose Run Method and Control View. On theRun Method and Control View, choose Instrument. From the Instrumentmenu, choose Edit Parameters. On the Edit Parameters screen, click onOptions. On the Options screen, choose the radio button labeled “No” for the




171

question “Keep instrument keyboard locked after method is loaded?” Click on[OK] to leave the screen. This will allow you to enter setpoints from the key-board. You may remain in the Edit Parameters screen, and enter the setpointsdirectly from the ChemStation.



a. For an instrument with electronic pressure and flow control, enter the followingvalue :


Verify that the column is operating in constant flow mode by pressing the[Column 1] or [Column 2] key. Toggle down to the Mode line to check themode. If necessary, change to constant flow by pressing the [Mode/Type] keyand selecting Constant Flow.


• Set the pressure of the inlet to 25 psi. Connect the flowmeter to the exit tubeof the detector. The flow should be between 5.5 and 7.0 mL/min at an oventemperature of 40°C. (The detector leaks so that all the flow does not gothrough the exit tube.

5. Set the following flow rate values:

a. For an electronic pressure and flow controlled NPD, set the mode to ConstantColumn plus Makeup, and input the following values.

Hydrogen at 3 (± 1) mL/minAir at 60 (± 5) mL/minColumn plus Make-Up (Helium) at 10 mL/min


Hydrogen at 3 (± 1) mL/minAir at 60 (± 5) mL/minColumn plus Make-Up (Helium) at 10 (± 1) mL/min

After all flow rates are set, remove the flowmeter and flow-measurementadapter, reinstall bead/source, then turn on all gas flows.



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Inlet Temperature: Oven TrackDetector Temperature: 300°COven Temperature: 250°C

Wait 30 minutes, then reset the values as shown:



7. At the HP 6890, turn on the NPD electrometer by pressing [Configure] [FrontDetector] {or [Back Detector]}. Turn the electrometer on by scrolling to theElectrometer line and pressing [ON]. Press [Signal 1] to display its backgroundoffset. A stable value, < 3.0 display units, is acceptable criteria to continue. If notmet, stop here, and consult your HP 6890 service and user documentation foradditional information. If necessary, contact your local Hewlett-Packard servicerepresentative.

8. When powering up the NPD, use the Auto Adjust feature of the NPD to bring thebaseline(offset) up.

[Front Detector] {or [Back Detector]} [Det Control] [ON](If the default baseline setting is not 50, key in 50 now.)

[5] [0] [ENTER]

a. If no increase in signal output has been observed even though the bead voltageline reads 4.095, consult your HP 6890 service and user documentation foradditional information. If necessary, contact your local Hewlett-Packard servicerepresentative.

b. If after an extended time period no stable offset can be achieved, gas flow ratesmay be incorrect, a new bead/source may be required, or service is required.Turn off the auto adjusting process (press the [OFF] key while the cursor is onthe Adjust offset line), recheck gas flow rates and replace the bead/source. Ifnecessary, consult your HP 6890 service and user documentation for additionalinformation. If still necessary, contact your local Hewlett-Packard servicerepresentative.




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a. Turn the detector off, remove the column for the detector, and cap the detectorfitting.





e. Monitor the displayed detector signal. It should rise quickly to some highervalue as the NPD heats to the higher temperature. Then oven a longer time(typically 1 hours or more), the signal should decrease to some reasonableconstant value.



h. If the results are not acceptable, repeat the bakeout process. If repeatedbakeout cycles fail to give acceptable results, install a new bead/source andrepeat the process starting with step 8. If neither bakeout nor bead/sourcereplacement is effective, consult your HP 6890 service and user documentationfor additional information. If necessary, contact your local Hewlett-Packardservice representative.

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• At the HP 6890, enter a Range value of 0 (zero) for Signal 1 (or Signal 2) bypressing [Signal 1] and scrolling down the control table to Range.


• Press [PLOT] to begin plotting the NPD signal. After approximately 2minutes, press [ATT 2^] [2] [ENTER].



− Wander over any given 2-minute period (after first 2 minutes) should be<15 mm in width


• If these criteria are not met, repeat the test. Some adjustments to hydrogenand air flow may be necessary for optimal results. If, after repeated testing,the criteria cannot be met, stop here and consult your 6890 service and userdocumentation for additional information. If necessary, contact your localHewlett-Packard




[LIST] [OP#] [6]

This will give the HP 6890 method listing. At the bottom of the listing is therange value for signal 1 and 2. This is the range set at the MIO (INET) card.Normally this value is set to 5. The noise can be plotted with the integratorrange value (this range is designated as SIG1RANGE) set to 5. The nextbulleted step is to be used with a SIG1RANGE = 5. The attenuation valueshave been adjusted to give the same amplitude plot as the analog. It is

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permissible for the user to change the SIG1RANGE value to 0 (zero) and usethe same integrator settings as in step 10a. The user is referred to the HP 3396manual for further details in how to change the SIG1RANGE value.





− Wander over any given 2-minute period (after first 2 min) should be<18.75 mm in width


• If these criteria are not met, repeat the test. Some adjustments to hydorgenand air flow may be necessary for optimal results. If after repeated testingthe criteria cannot be met, stop here, and consult your HP 6890 service anduser documentation for additional information. If necessary, contact yourlocal Hewlett-Packard service representative.






• From the Report menu, choose System Suitability, which will bring up asecond menu. On the second menu, choose Edit Noise Ranges. (If SystemSuitability does not appear under the Report menu, go to the View menu, andchoose Full Menu.) Once Edit Noise Ranges has been chosen, a window willappear that allows time ranges to be entered. The ChemStation calculatesseveral different noise calculations. The ASTM noise will be used in the MDLcalculation later. The ASTM noise measurement requires that the noise rangebe ≥1.01 minutes. Enter several time ranges that are ≥1.01 minutes. A time

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range of 5.0 minutes should also be entered. These ranges can overlap withthe other ranges. Close the window by choosing OK.

• Under View, choose Method and Run Control. Under the Method menu,choose Save Method As, which will allow a unique method name to be chosenfor the noise measurement. Once a method name has been assigned, go tothe Instrument menu, and choose Edit Parameters. On the Edit Parametersscreen, select the oven icon, and check that the oven temperature is 60°C. Setthe initial time to 12 minutes and rate 1 to 0°C/min. (This sets up a 12-minuteisothermal run.) Check the other parameters in steps 4 through 6 by choosingthe appropriate icon. Then click on OK to close the Edit Parameters screen.






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min0 2 4 6 8 10

pA

46

48

50

52

54











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c. HP 6890 HP-IB output to the HP GC ChemStationPage 12 of 14



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MDL (azobenzene) should be <= 0.4 pg/s





min0 2.5 5 7.5 10 12.5

arbs

40

50

60

70

80

90

100

110

120

Azobenzene

Octadecane

Malathion

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6890 Standard Operating Procedures G1530-90380

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Transcript of 6890 Standard Operating Procedures G1530-90380