Splitless Injectors

In capillary and micropacked gas chromatography (GC) there are four primary techniques for vaporizing a sample and transferring it onto the inlet of t...

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Technical Guide

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Operating Hints for Using Split/Splitless Injectors Inside: Overviews of split and splitless injection techniques Backpressure-regulated injection systems Headpressure-regulated injection systems Operating in the split injection mode Inlet liners for split injections Operating in the splitless injection Mode Inlet liners for splitless injections Septum purge optimization Problems associated with split and splitless injections Direct injection as an alternative to splitless injection Hints for analyzing dirty samples Hints for performing routine injection port maintenance Product listing

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Table of Contents Overview of Split/Splitless Injection Techniques ......................................2 Backpressure-Regulated Injection Systems ..2 Headpressure-Regulated Injection Systems..........................................3 Operating in the Split Injection Mode ......4 Inlet Liners for Split Injectors ................6 Operating in the Splitless Injection Mode ..7 Solvent Focusing and Analyte Focusing ......9 Inlet Liners for Splitless Injections ........11 Septum Purge Optimization ..................12 Problems Associated with Split and Splitless Injections ......................................13 Thermal Decomposition . . . . . . . . . . . . . .13 Active Compounds . . . . . . . . . . . . . . . . . .13 Molecular Weight Discrimination . . . . . . .13 Needle Discrimination . . . . . . . . . . . . . . .14 Backflash . . . . . . . . . . . . . . . . . . . . . . . . .15 Sample Size and Injection Port Temperature . . . . . . . . . . . . . . . . . . . . .15 Optimizing the Rate of Injection . . . . . . . .16 Pressure Programming . . . . . . . . . . . . . .16 Direct Injection as an Alternative to Splitless Injection ........................................16 Hints for Analyzing Dirty Samples ..........18 Hints for Performing Routing Injection Port Maintenance ..................................19 Cleaning and Deactivating Injector Liners . .19 Replacing Critical Seals . . . . . . . . . . . . . .19 Changing Septa . . . . . . . . . . . . . . . . . . . .19 Product Listing ........4, 5, 9, 18, 19, 20–35 Restek Flowmeter 6000 . . . . . . . . . . . . . . .4 Soap Film Bubble Flowmeters . . . . . . . . . . .4 Split Vent Trap . . . . . . . . . . . . . . . . . . . . . .5 Methane Cylinder . . . . . . . . . . . . . . . . . . . .5 Split and Splitless Injection in Capillary GC, 4th Ed. book . . . . . . . . . . . . . . . . . . .9 Mini Wool Puller/Inserter . . . . . . . . . . . . .18 Nylon Tube Brushes and Pipe Cleaner . . . .19 Leak Detective II Leak Detector . . . . . . . . .19 Siltek™ Inlet Liners . . . . . . . . . . . . . . . . . .20 Base-Deactivated Inlet Liners . . . . . . . . . .20 Prepacked Liners . . . . . . . . . . . . . . . . . . .20 Liners for Agilent/Finnigan GCs . . . . . .21–22 O-rings . . . . . . . . . . . . . . . . . . . . . . . . . .23 Inlet & FID Maintenance Kits . . . . . . . . . .23 Vespel® Ring Inlet Seals for Agilent 5890/6890 and 6850 GCs . . . . . . . . . . .24 Rethreading Tool . . . . . . . . . . . . . . . . . . .24 Replacement Inlet Seals . . . . . . . . . . . . . .25 Replacement Inlet Cross-Disk Seal for Agilent GCs . . . . . . . . . . . . . . . . . . .25 Liners for Varian GCs . . . . . . . . . . . . .26–27 Varian Inlet Liner Seals . . . . . . . . . . . . . .27 Inlet Liner Removal Tool . . . . . . . . . . . . .27 Liners for PerkinElmer GCs . . . . . . . . . . .28 Liners for Shimadzu GCs . . . . . . . . . . . . .29 Liners for Thermo Finnigan GCs . . . . .30–31 Inlet Liner Seal for TRACE™ 2000 GCs . . . .31 Graphite Sealing Ring and Washer for 8000 Series and TRACE™ GC Inlet Liners . . . . .31 Septa . . . . . . . . . . . . . . . . . . . . . . . . . . . .32 Press-Tight® Connectors . . . . . . . . . . . . .33 Polyimide Resin . . . . . . . . . . . . . . . . . . . .33 MXT®-Union Connector Kits . . . . . . . . . . .34 Valco® Connectors . . . . . . . . . . . . . . . . . .34 Gerstel GRAPHPACK® 3D/2 Connectors . .34 Guard Columns and Transfer Lines . . . . . .35

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Overview of Split/Splitless Injection Techniques In capillary and micropacked gas chromatography (GC) there are four primary techniques for vaporizing a sample and transferring it onto the inlet of the analytical column: split, splitless, direct, and on-column injections. Of these, split and splitless injections are the most commonly used techniques. This technical guide focuses on split and splitless injections— their optimization, troubleshooting, and system maintenance. Split and splitless injections are techniques that introduce the sample into a heated injection port as a liquid, and then rapidly and completely vaporize the sample solvent as well as all of the analytes in the sample. The vaporized sample is transferred to the head of the column. In the split injection mode, only a fraction of the vaporized sample is transferred onto the head of the column. The remainder of the vaporized sample is removed from the injection port via the split vent line. Split injections should be used only when sample concentrations are high enough to allow a portion of the sample to be discarded during the injection process, while still maintaining a sufficient concentration of analytes at the detector to produce a signal. When target analyte concentrations are so low that splitting the sample in the injection port will not allow an adequate signal from the detector, the injector should be operated in the splitless injection mode. In the splitless injection mode, most of the vaporized sample is transferred to the head of the column. The process of performing either a split or splitless injection is controlled by changing the flow path and flow rate of carrier gas through the injection port. The position of a switching valve in the injection port determines the flow path. In split injections, a high carrier gas flow rate rapidly moves the vaporized sample through the injection port liner, past the column (with only a minimal amount directed to the head of the column), and out the split vent. In splitless injections, a relatively slow carrier gas flow rate directs most of the vaporized sample into the head of the column. Split/splitless injection ports can be either backpressure-regulated or headpressure-regulated systems. Most modern GCs are backpressure regulated. However, some GC manufacturers still find headpressure regulation advantageous and use this design in their split/splitless injectors. It is important for analysts to be familiar with their injection port hardware and the operating principles of their instruments, so that they factor in the variables affecting the accuracy and reproducibility of their results.

Backpressure-Regulated Injection Systems Figure 1 illustrates the components of a typical backpressure-regulated split/splitless injection system (e.g., Agilent 5890, 6850, 6890 GCs; Varian 3300, 3400, 3500, 3600, 3800 GCs; Shimadzu 17A GCs). A flow controller, positioned upstream from the injection port, controls the total amount of carrier gas that enters the injection port. A backpressure regulator, located downstream from the injection port body, regulates the pressure inside the injection port. Carrier gas flow rate in the column is determined by the pressure that is maintained in the injection port. The outlet of the backpressure regulator is the outlet of the split vent line. The split vent line outlet is at the ambient pressure of the laboratory. The flow controller and the backpressure regulator work together to determine the column flow rate, septum purge flow rate, and split vent flow rate. Split and splitless injections in backpressure-regulated systems are controlled by the position of the 3-way solenoid valve. In the split injection mode, the flow path is always open from the injection port body through the 3-way solenoid valve to the split vent line. In the splitless injection mode, the flow path is temporarily closed from the injection port body to the split vent line. The carrier gas flow rate through the injection port liner is simply the column flow rate. Any excess flow is directed through the septum purge line, into the 3-way solenoid valve, and out the split vent line. In backpressure-regulated systems, the split vent flow rate is changed by adjusting the flow controller. An increase in the total flow being delivered to the injection port will result in a higher split vent flow rate and a higher split ratio. Column flow rate is not affected by changes in the total flow being delivered to the injection port, but by the backpressure regulator. To maintain the same pressure at all times, use the backpressure regulator to compensate for a change in the total flow delivered to the injection port.

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A flow-controlled, backpressure-regulated system is beneficial as it gives some measure of protection against a catastrophic loss of carrier gas. If there is a leak at an injection port fitting or a column fitting, the maximum rate of carrier gas loss would be the total flow rate into the injection port as determined by the flow controller. Unlimited flow of carrier gas into the injection port is prevented by having the flow controller at the inlet of the injection port. Leaks are indicated by a failure to maintain split vent flow rate. A common mistake analysts make when they observe a reduced split vent flow is to increase the total system flow, rather than check for leaks at the injector and column fittings. By understanding the characteristics of backpressure regulated pneumatics, analysts can detect and correct a leak, to avoid poor chromatography. Figure 1. Split injection flowpaths in a typical flow-controlled/backpressure-regulated system. needle valve

injection port

flow controller carrier gas inlet

septum purge vent

closed o-ring or ferrule

split vent 3-way solenoid valve

injector liner

backpressure regulator

Figure 1. • All carrier gas except septum purge flow directed through injector. • Column flow (established by backpressure regulator) enters column. • Solenoid valve open from injector to split vent. Bulk of gas flows out of injector liner, through solenoid valve, out split vent. • Sample vapor is directed onto column or vented through split vent and is split in the same proportions as for carrier gas. • Split ratio = portion of sample vented from split vent/portion of sample that enters column.

analytical column to detector

Headpressure-Regulated Injection Systems Figure 2 illustrates the components of a typical headpressure-regulated split/splitless injection system (e.g., PE Autosystem; Shimadzu 9A & 14A; Thermo Finnigan Trace 2000 GCs). A pressure regulator upstream from the injection port regulates or maintains the pressure inside the injection port. The pressure regulator supplies an unlimited flow of carrier gas until the desired pressure is reached. The pressure inside the injection port establishes the carrier gas flow in the column and determines the column flow rate. Flows through the split vent line and the septum purge line are controlled by needle valves or restrictors downstream from the injection port. The outlet pressure of the septum purge and split vent lines is ambient pressure. As long as constant pressure is maintained in the injection port, needle valves and restrictors will give constant flows. Figure 2. Split injection flowpaths in a typical headpressure-regulated system. throttling valve (optional safety device)

pressure regulator

needle valve

injection port

septum purge vent

carrier inlet open

Figure 2. • Solenoid valve open: column flow passes into column, split flow exits through split vent. • Throttling valve guards against loss of carrier gas caused by leaks in injection system.

split vent o-ring or ferrule

solenoid valve

needle valve

injector liner column to detector

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An on/off solenoid valve is used in headpressure-regulated systems instead of the 3-way solenoid valve used in backpressure-regulated systems. The position of the solenoid valve determines whether the injection port is operated in the split or splitless injection mode. In the split injection mode, the solenoid valve is always in the open position and the carrier gas is allowed to flow through the injection port liner and out the split vent line. In the splitless injection mode, the solenoid valve is closed and the only flow through the injection port liner is the column flow. The pressure regulator compensates for excess carrier gas flow available when the solenoid valve closes.

Restek Flowmeter 6000

The throttling valve upstream from the pressure regulator (Figure 2) is an optional component not typically included by the chromatograph manufacturer. We recommend installing a throttling valve (flow controller or needle valve) to guard against catastrophic loss of carrier gas if a leak occurs at an injection port fitting or a column fitting. To adjust the throttling valve, gradually close the valve, reducing the gas flow until it matches the requirements of the injection system. When the column headpressure begins to decrease, the throttling valve is closed too far.

Operating in the Split Injection Mode • Calculates linear velocity based on column ID. • Useful for measuring flows for N2, air, He, H2, CO2, O2, Ar, 7.5% CH4/Ar. • Reads flow accurately from 0 to 500mL/min. (0–300mL/min. for CO ). • Accuracy is 0.2mL/min. or +/- 2.5%. • Usable with inlet pressures up to 25psi. • Measures split flow and calculates split ratio. • Automatic shut-off. 2

Description

qty.

cat.#

Restek Flowmeter 6000 (9-volt battery-operated)

ea.

21622

Recalibration Service for Restek Flowmeter 6000

ea.

24618

Soap Film Bubble Flowmeters • 1mL flowmeter measures flows between 0.1 and 10cc/min. • 50mL flowmeter designed for flows between 10 and 300cc/min. • Both flowmeters come with a reservoir bulb, twenty-four inches of 1 /4-inch ID tubing, adaptor tubes for 1 /8-inch tubing and 0.53mm ID capillary columns, and Velcro® fasteners.

When operating in the split injection mode (Figures 1 and 2), the solenoid valve is always open along the flowpath from the injection port body to the split vent. With the exception of the septum purge flow, all of the carrier gas entering the injection port flows through the injection port liner and toward the head of the column. At the head of the column, the carrier gas flow is split between two flow paths: a portion of the flow enters the column as the column flow rate, and the remaining carrier gas flow is allowed to escape from the injection port, out the split vent line via the solenoid valve. The amount of flow entering the column is determined by the pressure of the carrier gas inside the injection port and the dimensions of the analytical column. The relative proportions of the split vent flow and the column flow determine the split vent ratio. Samples completely vaporized in the injection port liner behave in the same fashion as the carrier gas; sample vapors are split in the same proportions as the carrier gas, thereby allowing only a fraction of the sample to be introduced into the head of the column. A 50-to-1 split ratio can be used as a starting point when developing split injection methods. Table I shows the appropriate split vent flow rates for helium and hydrogen carrier gases when using common capillary column IDs. Table I. Typical split vent flow rates for 50-to-1 split ratio at optimum linear velocity when using a 30-meter column at 40°C. Column ID (mm)/Split Vent Flow Rate Carrier Gas

0.18

0.25

0.32

0.53

helium*

25cc/min.

37.5cc/min.

55cc/min.

135cc/min.

110cc/min.

270cc/min.

hydrogen** 50cc/min. 75cc/min. *optimum carrier gas linear velocity=20cm/sec. **optimum carrier gas linear velocity=40cm/sec.

Equation 1 shows how the split ratio is calculated. Split vent flow rates easily can be measured using a standard electronic flowmeter (cat.# 21622). However, measuring low flow rates (from 0.3 to 5cc/min.) exiting a capillary column can be difficult unless a special low-volume bubblemeter (cat.# 20135) or a sensitive electronic flowmeter is used. If a low flow-measuring device is not available, Equation 2 can be used to determine the approximate column flow.

Description 1mL Bubble Flowmeter 50mL Bubble Flowmeter

qty. ea. ea.

www.restekcorp.com

cat.# 20135 20136

Calculating the on-column concentration of analytes is necessary to ensure that the column is not overloaded and is operating within its capacity limits. Although quantitative analysis does not require that the on-column concentration be known, exceeding column capacity decreases resolution and reduces quantitative accuracy. Equation 3 illustrates how to calculate the approximate on-column concentration in the split mode. Setting the injection port temperature properly is critical for obtaining good peak shape and response. Injection port temperature must be hot enough to provide rapid vaporization of all

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Equation 1. Calculating the split ratio. column flow + split vent flow Split ratio = column flow Equation 2. Calculating the approximate column flow rate. (π) (column radius in cm)2 (column length in cm) Flow = dead volume time (min.)

High-Capacity Split Vent Trap • Reduces the release of hazardous materials from the capillary split vent into the lab. • Lasts one month or 1,500 injections. • Includes connecting lines and mounting kit.

where π = 3.14159 For example, a 30m x 0.53mm ID column operated at 20cm/sec. linear velocity (helium) retains methane for 2.50 min., and therefore has a flow rate of 2.65cm3/min.: (3.14159) (0.0265cm) (3000cm) = 2.65cm3/min. 2.50 min. 2

Flow =

Equation 3. Calculating the approximate on-column concentration for split injections. Concentration = concentration in sample (µg/µL) × sample vol. injected (µL) split ratio

Description

qty.

cat.#

High-Capacity Split Vent Trap

ea.

20698

High-Capacity Split Vent Trap

5-pk.

20699



For customer service, call sample components. In the split injection mode, the residence time of the sample in the injection port is very short because of the high carrier gas flow rate through the injection port liner and out the split vent. As a result, vaporization must be completed as rapidly as possible. However, injection port temperatures must not be so high that they cause sample degradation.

800-356-1688, ext. 3 (814-353-1300, ext. 3)

or call your local Restek representative.

When set up properly, split injections are very reproducible. Samples introduced under constant temperature, pressure, and flow conditions will vaporize and split consistently. Split injections can be used for both qualitative and quantitative work. Internal or external reference compounds are split under identical conditions compared to analytes in samples. Any variations experienced by the sample also are experienced by the reference compounds when the sample matrix and standard matrix match exactly. In general, split inlet liners are designed to have added surface area to help with sample vaporization. Improved vaporization can be acheived with changes in liner geometry that increase the surface area. Examples include incorporating fused silica or glass wool, CarboFrit™ packing, or using a laminar cup.

Caution! When analyzing hazardous compounds in the split mode, make sure they do not enter the lab atmosphere through the split vent. A small, charcoal-filled split vent trap connected to the split vent protects you from breathing contaminated air (cat. # 20698).

Methane Cylinder Setting the column flow rate by injecting methane and optimizing linear velocity is a preferred method for establishing reproducible retention times (ASTM Method E1510-93). Measuring the linear velocity of your carrier gas is made easy by using the Scotty® 14 cylinder containing 1% methane in helium. The complete kit includes the Scotty® 14 cylinder, a MINICYL regulator, a syringe adaptor, and a package of twenty septa for the adaptor. Description Complete Kit Replacement Septa Replacement Cylinder

qty. kit 20-pk. ea.

cat.# 20197 20198 20199

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Inlet Liners for Split Injections

A

Split liners are designed with mixing chambers and tortuous flow paths, to fully vaporize the sample into a homogeneous vapor cloud before it reaches the split point. All Restek split liners are fully deactivated using a high-temperature silanizing reagent. This caps surface silanol groups so active compounds in the sample do not degrade or adsorb onto the hot glass surface. To trap non-volatile residue and prevent column contamination when analyzing dirty samples, pack split liners with wool, CarboFrit™ packing, or fused silica beads. Some of the more commonly used inlet liners are described below.

B

A) Split Liner with Wool

D) Cup Splitter

C

The wool provides a large surface area to allow rapid vaporization of the sample and deliver a uniform vapor cloud to the split point. The low mass of the wool fiber promotes complete vaporization. Benefits: • Low cost. • Reproducible performance. Drawbacks: • Wool can be adsorptive, especially if fibers are broken. • High maintenance requirements.

The sample flows through a mini funnel and encounters a glass cup. The flow path then inverts twice before reaching the split point. Benefits: • Tortuous flow path aids in sample vaporization. • Minimizes molecular weight discrimination. • Can be packed with wool to trap particles. Drawbacks: • Difficult to clean.

D

B) Laminar Cup Splitter

E

F

The sample flows through a small opening and encounters the head of the elongated glass cup. It then travels around the outside of the elongated cup before the flow is inverted twice. Larger volume injections are possible because the liquid is trapped at the inner base and cannot escape until vaporized. Benefits: • Recommended by chromatography expert Dr. Konrad Grob1. • Best splitter liner for high molecular weight compounds. • Laminar flow profile provides highest resolution. Drawbacks: • Costly.

C) Frit Splitter The sample must pass through the porous ceramic frit. The high surface area and tortuous flow path ensure complete vaporization. Benefits: • Traps septum particles and residue. Drawbacks: • Ceramic frit can be active. • Difficult to clean.

E) Cyclosplitter® (Patent #: 5,119,669) This patented design incorporates a cylindrical glass spiral in the sample pathway, providing a large area for sample vaporization. Benefits: • Ideal for dirty samples. • Allows many injections of dirty samples before cleaning is required. • Easy to clean. Drawbacks: • Not recommended for large volume injections.

F) Baffle Splitter The baffle induces turbulent flow that directs the sample against the wall of the glass liner. Benefits: • Reproducible performance. Drawbacks: • Prone to molecular weight discrimination. • Septum particles and residue can enter column. • Subject to incomplete vaporization.

all liners are

100% deactivated

See page 17.

All Restek liners are deactivated to prevent adsorption of active compounds. Call for information on custom deactivations.

“Injectors Providing Complete Sample Evaporation Above the Column Entrance in Vaporizing GC Injections,” K. Grob and C. Wagner, HRC & CC, Vol. 16, p. 429. 1

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Operating in the Splitless Injection Mode When operating in the splitless injection mode (Figures 3 and 4), the solenoid valve is switched, changing the flow path of the carrier gas. At the beginning of a splitless injection, the solenoid valve is set to prevent the flow of carrier gas from the injection port body through the solenoid valve. When the solenoid valve is in this position, only the column flow moves through the injection port liner. Column flow rate is determined by the pressure of the carrier gas in the injection port as set by the pressure regulator and the analytical column dimensions.

Figure 3. Splitless injection flowpaths (injector purge off) in a typical flow-controlled/backpressure-regulated system. flow controller

Figure 3. • Solenoid valve closed between injector and split vent: only column flow enters injector; column flow passes into column.

needle valve

injection port

carrier gas inlet

septum purge vent o-ring or ferrule

split vent closed

3-way solenoid valve

injector liner

backpressure regulator

analytical column to detector

pressure regulator

needle valve

injection port

• Sample vapor in injector liner can exit only to column, mixed with column flow of carrier gas. • Solenoid valve switched to establish flowpaths as in split injection: sample vapor remaining in injection port swept out of split vent. • Splitless hold time determined by sample composition.

Figure 4. Splitless injection flowpaths in a typical headpressure-regulated system. throttling valve

• Needle valve at septum purge vent allows only septum purge flow to exit septum purge vent: most of carrier gas diverted through solenoid valve, out through split vent.

carrier inlet

septum purge vent

Figure 4. • Solenoid valve closed: entire carrier gas flow and entire sample directed onto analytical column. • Carrier gas flow rate into system reduced to enable entire flow to pass through analytical column.

closed split vent

o-ring or ferrule injector liner

solenoid valve

needle valve

column to detector

After a carefully determined time (the splitless hold time) the solenoid valve is switched to re-establish the flow paths as used in the split injection mode. This allows any vaporized sample remaining in the injection port to be quickly swept out of the injection port liner through the split vent. A typical splitless hold time is between 60 and 90 seconds. The ideal splitless hold time is long enough to allow most of the vaporized sample in the injection port liner to be transferred to the analytical column. Excessively long splitless hold times can produce tailing peaks and broad peaks. The splitless hold time must be determined through experimentation, and will vary according to sample composition, column length and

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Table II. Typical splitless hold times. Column ID

Hold Time

0.18mm

2 min.

Column Flow Rate He H2 0.3cc/min.

Sample Transfer Time* He H2

0.6cc/min.

2.7 min.

1.4 min.

0.25mm

1 min.

0.7cc/min.

1.4cc/min.

1.2 min.

0.6 min.

0.32mm

0.75 min.

1.2cc/min.

2.4cc/min.

0.7 min.

0.4 min.

0.53mm

0.5 min.

2.6cc/min.

5.2cc/min.

0.3 min.

0.2 min.

*2µL of liquid methylene chloride expanded to 0.8mL vapor at 250°C (10psig headpressure).

ID, carrier gas flow rate, and injection port liner configuration. Table II lists approximate splitless hold times for various column IDs when operated with helium or hydrogen. The splitless hold time will decrease as either the column ID or column flow rate increases. Setting an optimal splitless hold time also is dependent on the choice of sample solvent and the sample size. Use Table III to estimate the volume of vapor produced when using different solvents at different pressures. The volume of vapor cloud formed should be divided by the column flow rate to determine the approximate time needed to keep the solenoid valve closed for complete sample transfer. The calculated splitless hold time also should be evaluated to provide the optimum response for the sample analytes. If the solenoid valve is Table III. Solvent expansion volumes. Expansion Volume in µL at various column headpressures



For customer service, call

800-356-1688, ext. 3 (814-353-1300, ext. 3)

or call your local Restek representative.

Solvent

Density (g/mL)

MW

5psig

l0psig

15psig

Heptane

0.68

100

219

174

145

Hexane

0.66

86

245

196

163

Pentane

0.63

72

280

224

186

Toluene

0.87

92

303

242

201

Ethyl acetate

0.90

88

328

261

217

Chloroform

1.49

119

400

319

266

Methylene chloride

1.33

85

500

399

332

Methanol

0.79

32

792

629

525

H2O

1.00

18

1776

1418

1179

The expansion volumes were determined using a 1.0µL injection volume, a 250° C injection port temperature, and a headpressure of 5, 10, or 15psig (common operating pressures for 30m columns having IDs of 0.53, 0.32, or 0.25mm, respectively). For 2µL injections, double the expansion volumes. Use these formulas to calculate values not listed in Table III:

Expansion volume = nRT / P n= = R= = T=

number of moles of solvent and sample. [volume (mL) × density (g/mL)] / mol. wt. (g/mole) gas law constant 82.06cc atm/mole °K absolute temperature of injector (°K) (°K = °C + 273) P = absolute column headpressure = gauge pressure (atm) + 1 atm atm = psig × 0.06804 atm / psig

Online Backflash Calculator: http://www.restekcorp.com/calculators/backflash.htm

injector liner volume* = πr2L π = 3.14 r = liner internal radius (cm) L = liner length (cm) *Also use this formula to determine capillary column internal volume.

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Setting the injection port temperature for splitless injections is critical, just as it is for split injections. The injection port temperature must be high enough to completely vaporize the sample, yet not so high that it causes sample degradation. This is especially important because the residence time for a sample in the injection port during splitless injections is longer, compared to split injections. Solvent Focusing and Analyte Focusing The long residence time for samples in the injection port also affects peak shape. In splitless injections, samples are transferred to the head of the column over a longer period of time than in split injections. As a result, initial peak bandwidths can be very broad unless vaporized samples are refocused at the head of the column. Two techniques can be used to refocus vaporized samples at the head of the column: solvent focusing and analyte focusing. The difference between the two methods is the initial temperature of the column oven. For solvent focusing, the initial oven temperature is low enough to allow the solvent to recondense at the head of the column. This forms a zone of liquid solvent that traps all of the vaporized sample analytes in a narrow band at the head of the column. Analyte focusing requires an initial oven temperature that allows the solvent to move through the column as a vapor immediately after injection. Analytes that have a significantly higher boiling point than the solvent are recondensed at the head of the column because of the lower oven termperature.

Figure 5. Optimization of splitless hold time. The splitless hold time is optimized when further increases do not increase analyte response but result in solvent tailing.

area

opened too quickly, responses will be low. However, if the solenoid valve remains closed too long, the solvent peak will tail and peak resolution will suffer. To help determine the optimal splitless hold time, a series of injections should be made using increasingly longer splitless hold times. When the response for the analytes of interest plateaus, the sample transfer process has been optimized (Figure 5).

hold time (sec.)

A typical sequence of events for performing a splitless injection using solvent focusing is as follows: 1. Set the initial oven temperature approximately 20°C below the boiling point of the sample solvent. 2. Close the solenoid valve to divert the entire sample onto the head of the column. 3. Inject the sample and hold the oven temperature at the initial temperature to recondense the solvent and focus the sample at the head of the column. The initial oven temperature is typically held for the same amount of time that the solenoid valve is closed. 4. Switch the solenoid valve to open the flow path to the split vent line and rapidly program the oven temperature (10 to 30°C/min.) until the first analyte of interest elutes.

Split and Splitless Injection in Capillary GC, 4th Ed.

5. Slow the oven program rate to enhance resolution of the remaining analytes of interest.

This comprehensive handbook of split and splitless injection techniques has been totally revised and updated, containing information on sample evaporation in the injector, matrix effects, and a new chapter on injector design. It also includes a CD-ROM containing visualization of the evaporation process during split and splitless injection. K. Grob, Wiley-VCH, 2001, 460pp., ISBN 3-527-29879-7 cat.# 20451 (ea.)

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Figure 6. Initial oven temperature too high for improper solvent focusing: solvent peak and early eluting compounds are tailing.

30m, 0.25mm ID, 0.25µm Rtx®-5 (cat.# 10223) 1.0µL splitless injection of a pesticide mix in hexane (5ng/µL); Oven temp.: 150°C to 275°C @ 4°C/min.

Figure 7. Initial oven temperature at least 20°C below boiling point of earliest eluting analyte: early eluting compounds are symmetrical.

The sequence of events for analyte focusing is the same, except for the initial oven temperature; instead of starting 20°C below the boiling point of the solvent, the oven temperature is started 60–80°C below the boiling point of the earliest eluting compound. Figure 6 shows an example of improper solvent focusing. The sample solvent is hexane, which has a boiling point of 69°C. The initial oven temperature is 150°C, or 80°C above the boiling point of hexane. The solvent peak is tailing, and the early-eluting compounds have broad peak shapes and are poorly resolved from one another. Figure 7 illustrates proper solvent focusing. The initial oven temperature, 40°C, is well below the boiling point of hexane. The square solvent peak is a good indicator of proper solvent focusing. Also notice the sharp peak shapes for both early- and late-eluting compounds. When the solvent is not detected or elicits a low response, such as hexane with electron capture detectors (ECDs), the only indication of proper solvent focusing is narrow peaks for early-eluting compounds. For optimal solvent focusing, choose a solvent that has a boiling point at least 20°C below the boiling point of the earliest eluting target analyte. In some cases, it is not possible to select the perfect solvent to achieve focusing. For example, methylene chloride (boiling point 40°C) is frequently used for splitless work because of sample preparation techniques. Analyses performed with an initial oven temperature of 40°C will not allow the solvent to recondense at the head of the column and will not refocus the sample analytes. Ideally, analysts would start the oven temperature at 20°C when using methylene chloride as the sample solvent, but because this is not practical, they must rely more on analyte focusing to refocus sample analytes at the head of the column. An important part of solvent focusing is the ability of the solvent to “wet” the stationary phase in the column. Non-polar solvents should be used for splitless injections on non-polar stationary phases (e.g., use hexane or isooctane for injections on Rtx®-1 and Rtx®-5 columns). Non-polar solvents are more soluble in non-polar stationary phases and will form a more efficient zone of recondensed solvent in the column. Polar solvents are not as soluble in non-polar stationary phases and will bead up on the stationary phase rather than forming an even layer of recondensed solvent at the head of the column. Mismatches between the polarity of the solvent and the polarity of the stationary phase can cause band broadening, peak splitting, and poor resolution. Once again, the same basic procedures are followed for analyte focusing, except the initial oven temperature is 60–80°C below the boiling point of the earliest eluting compound, instead of 20°C below the boiling point of the solvent, as with solvent focusing.

30m, 0.25mm ID, 0.25µm Rtx®-5 (cat.# 10223) 1.0µL splitless injection of a pesticide mix in hexane (5ng/µL); Oven temp.: 40°C to 150°C @ 25°C/min. then to 275°C @ 4°C/min.

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A unique situation with Agilent 5890 and 6890/6850 split/splitless inlets makes a double gooseneck liner highly desirable for samples that contain compounds prone to catalytic degradation through contact with hot metal surfaces. Agilent splitless inlets contain a metal seal at the base of the inlet (just under the liner outlet). Because the column is installed only a few millimeters above the seal surface, the sample contacts the seal while it is being slowly drawn into the column. A double gooseneck inlet liner minimizes contact between the sample and the metal seal. A dirty seal increases the breakdown of endrin (a pesticide prone to decomposition) from 6% to 12.8% in an Agilent 5890 inlet when a 4mm straight inlet liner is installed. However, when a double gooseneck inlet liner is used, the breakdown remains at 2% regardless of whether the seal is clean or dirty. (For more information, see page 24 of this guide for a description of our Vespel® Ring Inlet Seal.)

Double gooseneck inlet liner minimizes the catalytic effects of sample contact with the metal disk in an Agilent inlet.

splitless liner

double gooseneck liner inlet seal

Endrin Breakdown Liner Type

Clean Seal

Dirty Seal

Splitless with Wool

6.0%

12.8%

Double Gooseneck

2.0%

2.4%

11

Inlet Liners for Splitless Injections

all liners are

The residence time of the sample in a splitless liner is between 0.5 and 2 minutes, so splitless inlet liners do not require large surface areas for efficient vaporization (unless you are using a rapid-injecting autosampler). Splitless liners usually are designed as straight tubes. Alternative splitless liner designs, such as gooseneck restrictions, help contain the sample cloud in the injector and minimize the breakdown of compounds sensitive to catalytic decomposition on metal inlet parts. Splitless liners should be packed with wool or fused silica beads to help with vaporization, trap non-volatile residue, and prevent column contamination when analyzing dirty samples. Some of the more commonly used splitless liners are described below.

All Restek liners are deactivated to prevent adsorption of active compounds. Call for information on custom deactivations.

A) Straight Tube

F) Drilled Uniliner®

Use for samples containing a narrow molecular weight distribution and for those not prone to thermal decomposition. Packing with wool is recommended. Wool aids in vaporization of high molecular weight compounds and minimizes discrimination. Benefits: • Low cost. Drawbacks: • Potential decomposition of active compounds such as endrin and phenols when packed with wool. • Prone to high molecular weight discrimination. • Sample exposed to metal surface below liner.

This direct injection liner features a hole drilled into the inlet end that reduces sample discrimination, compared to typical splitless injections. Benefits: • Excellent transfer of analytes to column. • Decreases injection port discrimination. • Removes excess solvent vapor. • Eliminates the need for wool. • No sample contact with metal parts below liner, less adsorption. Drawbacks: • Higher amounts of non-volatile materials transferred to column.

A

B) Gooseneck C) Recessed Gooseneck Benefits: • Increases splitless efficiency. • Decreases breakdown of active compounds such as endrin and DDT. • Chamber contains sample vaporization cloud. • Can be packed with wool. Drawbacks: • No known drawbacks.

D) Double Gooseneck

100% deactivated

See page 17.

B

C

G) 4mm Splitless with Fused Silica Wool The wool provides a large surface area to allow rapid vaporization of the sample and deliver a uniform vapor cloud to the split point. The low mass of the wool fiber promotes complete vaporization. Benefits: • Low cost. • Reproducible performance. Drawbacks: • Wool can be adsorptive, especially if fibers are broken. • High maintenance requirements.

D

E

F

E) Recessed Double Gooseneck Best liner for catalytically labile or high molecular weight compounds. Isolates sample from metal injection port parts. Use the cyclo-version for dirty samples. Benefits: • Highest splitless efficiency. • Breakdown of active compounds decreased. • Chamber contains vaporization cloud. Drawbacks: • Higher cost than straight splitless liners. • Only recessed double goosenecks can be packed with wool.

G

Note: Recessed gooseneck liners offer the same benefits as single or double gooseneck liners, but the base of the recessed gooseneck can be packed with wool and the liner can be used for dual-column analysis with a two-hole ferrule.

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12

Septum Purge Optimization Figure 8. Typical carrier gas flowpath in a Varian split injector. septum purge out ferrule

carrier gas in

split vent out

split liner

split point

spring

The septum purge (Figure 8) serves two functions: to sweep septum bleed volatiles out of the system and to reduce the potential for sample backflash contaminating the carrier gas inlet line. Optimization of the septum purge flow rate is important, especially when the inlet is operated in the splitless mode. Most GC manufacturers recommend that the septum purge flow rate be set between 3 and 5cc/min. Flow rates exceeding 5cc/min. should not be used because highly volatile sample components could be preferentially purged from the inlet liner buffer volume after vaporization. Flow rates lower than 3cc/min. can allow septum bleed to enter the inlet liner and cause ghost peaks to appear on the chromatogram. The septum purge flow rate must be readjusted each time the injection pressure is changed by more than 5psig. Most GCs have a lowflow needle valve that makes septum purge adjustments easy.

column

Figure 9. Injector temperature affects the recovery of higher molecular weight compounds. 1. naphthalene 2. acenaphthylene 3. acenaphthene 4. fluorene 5. phenanthrene 6. anthracene 7. fluoranthene 8. pyrene 9. benzo(a)anthracene 10. chrysene 11. benzo(b)fluoranthene 12. benzo(k)fluoranthene 13. benzo(a)pyrene 14. indeno(1,2,3-cd)pyrene 15. dibenzo(a,h)anthracene 16. benzo(ghi)perylene

Injector temp: 200°C

GC_EX00600

Injector temp: 300°C

GC_EX00601 ®

Rtx -5 15m, 0.32mm ID, 1.50µm (cat.# 10266) Sample: 50µg/mL PAH standard (cat.#31011 ) in hexane Inj.: 1.0µL splitless (hold 2 min.), 4mm single gooseneck inlet liner w/FSwool (cat.# 22405) Inj. temp.: 200°C Carrier gas: helium, constant pressure Linear velocity: 76cm/sec. @ 40°C Oven temp.: 40°C(hold 4min.) to 325°C @10°C/min. (hold 5 min.) Det.: FID @350°C

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13

Figure 10. The Donike Test illustrates the importance of injector temperature when a sample contains thermally labile compounds. 1. TMS tetracosanoate (thermolabile) 2. n-triacontane (stable) 3. TMS hexacosanoate (thermolabile) 15m x 0.32mm ID fused silica coated with 0.25µm bonded methyl silicone Sample: 1µL each of TMS n-tetracosanoate, TMS n-hexacosanoate, and n-triacontane in nnonane at 2ng/µL each component.

1

2

2

3

1 3

GC: 3000 Series Varian gas chromatograph with 1077 split/splitless injector, FID and autosampler. Split/splitless injector: Run 1: SPI held at 280° C Run 2: SPI held at 200°C Carrier gas: helium at 47cm/sec. Oven: 130° to 280°C 20°C/min. (hold 2 min.) FID: 300°C, 32 x 10-12

Chromatograms courtesy of Varian Instrument Co.

280°C: Injector too hot, thermal degradation evident

200°C: Injector temperature appropriate, breakdown minimized

Problems Associated with Split and Splitless Injections When performed properly, split and splitless injections are easy to automate, produce narrow peaks, and yield consistent run-to-run peak areas. However, split and splitless injections have inherent limitations associated with vaporizing the sample in a hot injection port. Thermal Decomposition: The injection port temperature is a critical factor in optimizing hot vaporization injection techniques. If the injection port temperature is too low, high molecular weight analytes will not vaporize completely and will not be transferred to the head of the column efficiently (as shown by peaks 14, 15 and 16 in Figure 9). If the injection port temperature is too high, thermally labile compounds can break down inside the injection port before reaching the column. Figure 10 shows the effect of temperature on thermally labile TMS derivatives of fatty acids. When the injection port temperature is set at 280°C, the response for the TMS derivatives is reduced. When the injection port temperature is lowered to 200°C, the response for the TMS derivatives is comparable to triacontane at equivalent sample concentrations. Careful optimization of injection port temperatures will maximize sample vaporization while minimizing sample decomposition. Active Compounds: Active compounds can be problematic in split or splitless injections. The high surface area and heat needed to uniformly vaporize the sample can cause these compounds to break down or be adsorbed onto the surface of the injection port liner. Deactivated inlet liners, and Silcosteel®-treated or gold-plated inlet seals can help minimize active sites in the injection port. If tailing peaks and poor response for active compounds cannot be corrected by using properly deactivated inlet liners and treated inlet seals, other injection techniques such as cold on-column or temperature-programmed injections should be considered.



For customer service, call

800-356-1688, ext. 3 (814-353-1300, ext. 3)

or call your local Restek representative.

Molecular Weight Discrimination: In hot vaporization injections, one injection port temperature is used to vaporize all of the analytes in one sample injection. Compounds spanning a range of molecular weights and boiling points will exhibit differences in response for equal concentrations of analyte. High molecular weight, high boiling point analytes will have a noticeably reduced response when compared to lower molecular weight, lower boiling point analytes. This effect is more pronounced when analyzing samples that have a broad range of molecular weights and boiling points. Samples containing analytes that are more closely grouped by molecular weight and boiling point show less molecular weight discrimination.

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14

Figure 11. Splitter discrimination typical of split and splitless injections. Splitter discrimination is evident from relatively enhanced peak heights for the early-eluting compounds and diminished peak heights for the later-eluting higher molecular weight compounds. The same sample analyzed by cold on-column injection shows no discrimination; the peak heights for low and high molecular weight compounds are truly representative of this sample. C6

C6

C44

C44

min. 4

12

20

28

36

44

52

Discrimination typical of a split or splitless injector. Injector temperature: 340°C 30m, 0.32mm ID, 0.25µm Rtx®-1 (cat.# 10124) Inj. volume: 0.2µL On-column conc.: 15ng. Oven temp.: 40°C to 340°C @ 5°C/min.

min. 4

12

20

28

36

44

52

Cold on-column injection provides accurate information. Injector temperature: 40°C. Det. (FID) temp.: 340°C Linear velocity: 50cm/sec., hydrogen Attenuation: 8x10-11AFS

Figure 11 demonstrates the molecular weight discrimination experienced when analyzing a series of hydrocarbons with a broad range of molecular weights (C6 through C44). Alternative injection techniques, such as cold on-column injection, can be used to minimize molecular weight discrimination.

Figure 12. Factors in discrimination: high molecular weight material clinging to the syringe needle and non-homogeneous vaporization of the sample in the inlet liner.

syringe sample liquid septum needle

vaporizing chamber

evaporating solvent and volatile solutes residual layer of high-boiling point materials high boiling materials (aerosols)

column inlet

volatile solutes (vapor state)

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Molecular weight discrimination is usually very repeatable. In split and splitless injections, if the same injection port temperature, carrier gas pressure, sample size and sample solvent are used for every injection, sample vaporization should be a reproducible process. Any molecular weight discrimination experienced should be the same from one injection to the next. Because of this consistency, many analysts choose to ignore molecular weight discrimination unless it compromises overall sensitivity. To help compensate for differences in response due to molecular weight discrimination, multiple internal standards can be used to mimic the range of molecular weights and boiling points for the analytes in the sample. Molecular weight discrimination can be minimized by choosing an injection port liner that ensures the sample is completely and uniformly vaporized. Inadequate vaporization causes the sample to approach the head of the column in both the aerosol and vapor states. Aerosol droplets, consisting predominantly of high molecular weight compounds, can be driven past the head of the column by the momentum of the carrier gas and will be preferentially swept out of the injection port and through the split vent. Injection port liners that are packed with glass wool or that incorporate a flow diverting device within their bore assist in vaporizing the sample and transferring a homogeneous representation to the head of the column. Needle Discrimination: During sample injections, the syringe needle undergoes some degree of heating in the injection port. The temperature reached by the needle can influence the relative response for low and high molecular weight analytes. During the process of expelling the sample from the syringe, the contents in the needle are not completely transferred to the injection port. As the needle begins to heat, low molecular weight analytes begin to vaporize from the needle while higher molecular weight analytes remain inside the needle. Therefore, the lower molecular weight analytes will show enhanced response compared to higher weight analytes (Figure 12). Three techniques can be used to minimize needle discrimination in split and splitless injections. The first technique is to inject the sample as rapidly as possible. Rapid injections minimize the amount of time the needle spends in the injection port and reduces the amount of heating the needle experiences. When making rapid injections in straight injection port liners for split or splitless analysis, the sample can be propelled beyond the inlet of the column and onto the injector base fitting. Always pack injection port liners with deactivated glass wool or CarboFrit™ packing, or use a flow diverting device like a laminar cup to assist in sample

15

Figure 13. Always pack splitless inlet liners with wool when using rapid injection autosamplers.

20

24

28

32

4mm ID splitless liner without wool may exhibit fronting peaks.

36

20

24

28

32

36

4mm ID splitless liner with wool eliminates fronting peaks by promoting sample vaporization.

vaporization. Figure 13 shows the improvement in peak shape when an HP autosampler is used with an injection port liner packed with wool, versus a liner without wool. The second technique is to use hot needle injection. Hot needle injections are performed by drawing the sample all the way into the syringe barrel, leaving the needle empty. When the needle is introduced into the injection port the injection in delayed for a short period of time (3–5 seconds, for example) to allow the needle to heat completely. Then the syringe plunger is depressed and the sample is expelled into the injection port liner. The third technique is to use a solvent flush with each injection. This technique involves drawing a small amount of solvent into the syringe, followed by a small amount of air, followed by the desired amount of sample. All of the solvent, air, and sample are then drawn into the barrel of the syringe, just as in a hot needle injection. The needle is preheated, as in the hot needle injection, and the contents of the syringe are expelled into the injection port liner. The solvent that was first drawn into the syringe acts to flush the syringe barrel and needle, and completely transfers all of the sample during the injection process. Backflash: Backflash occurs when the volume of the vaporized sample exceeds the volume inside the injection port liner. Most of the excess vaporized sample escapes out the top of the injection port liner. Some of it is swept down the septum purge line. Another portion of it can back up into the carrier gas supply line, and some of it can be re-introduced into the injection port. Backflash can cause poor peak area reproducibility, tailing peaks, split peaks, and poor resolution. Table III (page 8) shows the estimated expansion volumes for 1µL injections of a variety of solvents. When using an injection port temperature of 250°C and a carrier gas pressure of 10psig, most solvents will vaporize and expand to a volume that exceeds the capacity of a 2mm ID injection port liner (approximately 240µL, see Table IV). In order to minimize backflash, injection port parameters must be carefully optimized. Injection port temperature, carrier gas pressure, sample size, and rate of injection all should be adjusted to ensure the vaporized sample remains inside the liner prior to being transferred to the head of the column. Sample Size and Injection Port Temperature: As the equation in Table III shows, the volume of vaporized sample produced is directly related to the size of the liquid sample (n) and the temperature of the injection port (T). A decrease in either of these values will translate into a smaller vaporized sample volume. If the injection port temperature cannot be decreased because of vaporization problems and the sample size cannot be decreased because of sensitivity issues, backflash must be minimized by optimizing the rate of injection or by adjusting the carrier gas pressure.

Table IV. Liner Volumes. Theoretical*

Effective

1.0mm ID =

59µL

30µL

2.0mm ID =

236µL

118µL

3.0mm ID =

530µL

265µL

4.0mm ID =

942µL

471µL

*Liner volume actually available for vaporization with carrier gas present is ≤ 1/2 theoretical, due to the presence of carrier gas in the liner. From Split and Splitless Injection in Capillary GC, 3rd Ed., K. Grob, Wiley-VCH, 2001.

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16

Figure 14. The injection rate must be slower for large volume splitless injections. 5µL/sec. injection rate

1µL/sec. injection rate

0.2µL/sec. injection rate

1 2

3

4 5

Solvent: Isooctane 1. n-C12 5µL injection 2. n-C14 3. n-C16 Chromatograms courtesy of Varian Instrument Co. 4. n-C18 5. n-C20

Optimizing the Rate of Injection: Figure 14 shows the effect of varying rates of injection for a 5µL sample. When a rapid injection (5µL/sec.) is made, the solvent peak tails and the responses for equal concentrations of each analyte are not reproducible. A 1µL/sec. injection rate improves the solvent peak shape, but the response for each analyte still is not proportional to the concentration of each analyte. Only when the injection rate is slowed to 0.2µL/sec. does the response for each analyte become consistent with the amount injected. Some autosamplers are capable of slowing the injection rate to minimize backflash, but most autosamplers use a rapid injection sequence. If large-volume injections must be made rapidly, adjustments to the carrier gas pressure must be used to control sample expansion. Pressure Programming: Pressure (P) is in the denominator of the equation in Table III (page 8). Any increase in carrier gas pressure will help to reduce sample expansion volume. Most of the latest models of GCs incorporate electronic pressure control (EPC) of the carrier gas pressure. Pressure can be time-programmed so that the carrier gas pressure initially is very high, then is reduced after the injection to optimize carrier gas flow rate for best resolution. Setting the initial carrier gas pressure to a high value will reduce the amount of sample expansion that occurs at the point of injection and will speed up the transfer of the vaporized sample from the liner to the head of the column.



For customer service, call

800-356-1688, ext. 3 (814-353-1300, ext. 3)

or call your local Restek representative.

Direct Injection as an Alternative to Splitless Injection Figure 15. A Uniliner® liner forms a leak-tight seal with the column, preventing the sample from contacting metal parts at the base of a splitless injection port. Uniliner® with a Press-Tight® seal

splitless liner inlet seal

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Direct injections are an alternative approach for injecting samples with low concentrations of analytes. Direct injections vaporize the entire sample in a heated injection port, just like split and splitless injections. However, in direct injections, there is only one flow path through the injection port. All of the carrier gas is directed into the column and, hence, the entire vaporized sample is directed into the column as well. This can be accomplished by using a specially designed injection port liner. Unliner® injection port liners have an internal taper in one end that allows a direct connection between the liner and the capillary column. With this connection, the flow path from the injection port body through the split vent is blocked and all of the carrier gas flow is directed into the capillary column. Figure 15 illustrates how a Uniliner® injection port liner with a Press-Tight® seal forms a leak-free connection between the liner and the column.

17

Because all of the carrier gas flow and the entire vaporized sample is directed into the capillary column, direct injections give comparable performance to splitless injections. Faster carrier gas flow rates usually are used to speed up the sample transfer process, and improve peak shapes and resolution. Direct injections can be used as another option to minimize molecular weight discrimination and loss of active compounds. A Uniliner® inlet liner can be used as a direct replacement for a splitless liner. It can be installed in the same manner as a splitless liner, except that the system must be operated continuously with the solenoid valve closed. Uniliner® inlet liners are designed to accommodate 0.32 or 0.53mm ID columns. Request Restek’s Guide to Direct On-Column Vaporization Injection (lit. cat.# 59882) for more information on how to perform and optimize direct injections. Standard Gooseneck Uniliner® Inlet Liner The buffer volume chamber contains the sample vaporization cloud and prevents analyte contact with metal injector parts. Peak tailing is reduced and larger injections can be made. Cyclo-Uniliner® Inlet Liner The glass cyclo spiral provides an excellent vaporization surface for high and low molecular weight samples. Particles are trapped on the first turn of the spiral, reducing subsequent residue/sample interaction. In comparison to liners packed with wool, CycloUniliner® liners accept up to five times as many injections of dirty samples before calibration curves degrade. Because they are deactivated, they are ideal for active samples. Open-top Uniliner® Inlet Liner Open-top Uniliner® liners are ideal for extremely dirty samples because they can be packed with fused silica wool to trap dirt and sample residue. Contaminated wool is easily replaced and the liner can be cleaned with a nylon brush or pipe cleaner. Drilled Uniliner® Inlet Liner A specially modified injection port liner, developed by Restek chemists, reduces sample contact with active metal parts in split/splitless injection ports. The Drilled Uniliner® liner gives the benefits of both direct injection and splitless injection. The column is connected to the liner by a press-fit connection, thus preventing the sample from contacting the metal at the bottom of the injection port. The hole on the side of the liner allows the purge flow to escape from the liner when the injection mode is switched from splitless to split.

Deactivation Siltek Deactivation • Revolutionary deactivation lowers endrin breakdown to less than 1%. • Inertness retained over a wide range of sample pH. • Minimal bleed. • Recommended for difficult matrix and reactive compound analysis. • Ideal for chlorinated pesticide analysis. • Recommended for use with Rtx®-CLPesticides, Stx-CLPesticides, Stx-1HT, and Rtx®TNT columns. ™



For customer service, call

800-356-1688, ext. 3 (814-353-1300, ext. 3)

or call your local Restek representative.

Base-Deactivation • Provides excellent inertness for basic compounds. • Recommended for use with Rtx®-5 Amine, Rtx®-35 Amine, and Stabilwax®-DB columns. Intermediate Polarity (IP) Deactivation Our standard deactivation for liners. Phenylmethyl-deactivated surface provides optimum compatibility for both polar and non-polar compounds. In most cases, the standard IP deactivation should be chosen. The IP surface contains methyl groups, as well as phenyl groups, making this surface compatible with most common solvents.

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18

Hints for Analyzing Dirty Samples

Guard Columns Guard columns protect analytical columns in several ways: Guard columns trap non-volatile residues, preventing them from collecting at the analytical column inlet. These residues may be very high molecular weight organic compounds, inorganic salts, or particles. If these contaminants enter the analytical column, they can cause adsorption of active compounds, loss of resolution, and poor peak symmetry. When this contamination begins to affect sample analysis, a small section of the analytical column must be removed to restore proper performance. Each time a column section is removed, retention times change, and some resolution is lost. By using a guard column and removing contaminated loops from it instead of from the analytical column, analytical column length and inertness remain intact.

When injecting dirty samples, non-volatile contaminants such as high molecular weight compounds, septum particles, derivatization reagents, salts, and pyrolyzed samples adhere to the interior wall of the injection port liner after the sample solvent and sample analytes have been vaporized. As this layer of residue thickens, it can cause loss of response for active compounds. Figure 16 illustrates this effect when highly active phenols are analyzed on a clean and a dirty inlet liner. In this example, responses are reduced because of adsorptive effects in the liner. Figure 16. Phenols are adsorbed after several injections of a dirty sample. 1

1

1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11.

4 2

6 3 5

phenol 2-chlorophenol 2-nitrophenol 2,4-dimethylphenol 2,4-dichlorophenol 4-chloro-3-methylphenol 2,4,6-trichlorophenol 2,4-dinitrophenol 4-nitrophenol 2-methyl-4,6-dinitrophenol pentachlorophenol

2

4

9 7

3

10 8

Initially, phenols respond well on a clean, deactivated inlet liner. However, after several injections of Southern Louisiana crude oil, responses are greatly diminished due to the sample’s interaction with non-volatile residue in the inlet liner.

5 6

11 7

9 8

Guard columns also allow more injections to be made before contamination interferes with analytical results. Because there is no stationary phase coated on a guard column, the amount of time the sample spends in the guard column is minimal. This reduces the interaction between sample components and contamination from non-volatile residue in the guard column. For more information on selecting a guard column for your analysis, request our Fast Facts GC Capillary Column Guard Columns (lit. cat.# 59319).

Mini Wool Puller/Inserter Makes inserting and removing wool easy. Not recommended for double gooseneck liners.

min. 4

8

12

16

min. 4

8

12

10

11

16

15m, 0.32mm ID, 1.0µm Rtx®-5 (cat.# 10251) 0.2µL split injection of phenols (604 Phenol Mix, cat.# 31029) Oven temp.: 80°C to 290°C @ 8°C/min. lnj.& det: temp.: 310°C Carrier gas: hydrogen Linear velocity: 45cm/sec. FID sens.: 16x10-11 Split ratio: 9:1

Non-volatile contamination can be trapped in the injection port liner by using a small plug of deactivated fused silica or glass wool. Usually a 1cm plug of wool, positioned in the center of the injection port liner, is sufficient to provide a surface for non-volatile contamination to collect. Some instrument manufacturers provide specific instructions on packing injection port liners to maximize quantitative accuracy and minimize discrimination. If fused silica wool or glass wool is used in an injection port liner, it should be replaced as part of the routine maintenance schedule for the injection port. Regular replacement of the wool in the injection port liner will extend the lifetime of the injection port liner as well as prevent chromatographic problems from extensive non-volatile contaminant build up. When replacing the wool during routine maintenance, minimize handling of the wool by using a wool puller tool (cat.# 20114). If fused silica or glass wool is not an effective mode of trapping non-volatile contamination under your conditions, injection port liners with a “cyclo” or glass frit design can be used to trap non-volatile contamination. While these types of injection port liners may provide effective trapping of non-volatile contamination, they are harder to clean than straight injection port liners packed with wool.

Description Mini Wool Puller/Inserter

qty. 2-pk.

www.restekcorp.com

cat.# 20114

In the past, some instruments were supplied with injection port liners that were packed with a small amount of packed column packing material. We do not recommend using this type of injection port liner. Diatomites used in packed column GC packings often are active and contain impurities that increase adsorptive effects for active compounds. Also, the stationary phases that are used in these packings can produce significant bleed when used in injection ports at elevated temperatures.

19

In addition to using a clean and deactivated injection port liner, we recommend using a fivemeter deactivated guard column when analyzing dirty samples. Routine maintenance of the liner and the guard column will prevent dirty samples from contaminating the analytical column, and will help ensure reproducible and accurate analytical results.

Hints for Performing Routine Injection Port Maintenance Injection port maintenance should be performed prior to installing any capillary column. Maintenance of the injection port after a column is installed should be performed periodically, based on the number of injections made and the cleanliness of the samples. Maintenance includes cleaning, deactivating, or replacing injection port liners, and replacing critical inlet seals and the septum. Review the instrument manual inlet diagram prior to disassembling the inlet. Cleaning and Deactivating Injector Liners For optimum column performance, the injection port liner must be free of septum particles, sample residue, and ferrule fragments. Use a deactivated injection port liner when analyzing samples with compounds that are active or prone to decomposition or adsorption on untreated glass surfaces. Table V illustrates the importance of a deactivated injection port liner when analyzing active compounds. The response factors (RF) for all three of these active compounds were much lower with non-deactivated inlet liners.

Table V. Deactivated inlet liners show higher response factors for active components. Compound

RF Deactivated Liner

RF Undeactivated Liner

2,4-dinitrophenol

0.248

0.185

pentachlorophenol

0.240

0.188

benzidine

0.327

0.234

RF relative to naphthalene; N=3

If the injection port liner is deactivated and is not excessively dirty, cleaning with organic solvents usually is enough to restore original performance. Most organic solvents will not affect the integrity of the surface deactivation. First, remove septum particles that adhere to the inside wall of the injection port liner by rinsing with methanol or isopropanol. Next, use pentane, methylene chloride or toluene to remove sample residue. Do not use laboratory detergents, acids, or bases to clean injection port liners. Harsh cleaning agents will remove or damage the deactivation layer and the liner will require re-deactivation. Nylon brushes and pipe cleaners (cat.# 20108) can be used for mild abrasive cleaning of injection port liners.

Nylon Tube Brushes and Pipe Cleaner Use to remove small septum fragments and residue from dirty glass inlet liners. Brushes are 1/8-, 3/16-, and 1/4-inch in diameter; pipe cleaner is one foot long.

Description

qty.

cat.#

Nylon Tube Brushes and Pipe Cleaner

set

20108

Leak Detective™ II Leak Detector • Affordable thermal conductivity leak detector—every analyst can have one.* • Compact, ergonomic design is easy to hold and operate with one hand. • Helium, hydrogen, and nitrogen can be detected at 1x10-4cc/sec. or at an absolute concentration as low as 100ppm.** • Fast results—responds in less than 2 seconds to trace leaks of gases with thermal conductivities different than air. • Micro-chip design improves sensitivity and response time over previous models. • Auto zeroing with the touch of a button. • Battery-operated for increased portability (one 9-volt).

Replacing Critical Seals Replace critical seals prior to installing an injection port liner (see the instrument manual for seal locations). In most capillary injection ports, an o-ring or ferrule made of rubber or graphite is used to seal the injection port liner into the injection port body. It is critical that the seal fits tightly around the liner, to prevent the carrier gas from leaking around the outside of the liner. Check for leaks with a thermal conductivity-type leak detector (e.g., Leak Detective™ II, cat.# 20413). Changing Septa Always use a high-quality, low-bleed septum. We recommend replacing the septum frequently, to prevent leaks and fragmentation. Multiple injections and continuous exposure to hot injection port surfaces will decompose the septum and cause particles to fall into the injection port liner. Septum particles are a potential source of ghost peaks, loss of inertness, and carrier gas flow occlusion. It is best to install a new septum at the end of an analytical sequence so that it can condition in the injector and reduce the incidence of ghost peaks. To avoid contamination, always use forceps when handling septa. Restek’s high quality, lowbleed Thermolite® septa are available for most common models of capillary GCs. For more information, request a copy of Restek’s Guide to Minimizing Septa Problems (lit. cat.# 59886). For additional hints for analyzing dirty samples, request a copy of Restek’s A Guide When Injecting Dirty Samples (lit. cat.# 59881).

Description

qty. cat.#

Leak Detective™ II Leak Detector (9 volt, Battery-Operated)

ea. 20413

*Never use liquid leak detectors on a capillary system because liquids can be drawn into the column. **Caution: NOT designed for determining leaks of combustible gases. A combustible gas detector should be used for determining combustible gas leaks in possibly hazardous conditions.

www.restekcorp.com

20

featuring

20



Siltek deactivation

Siltek™ Deactivation—The Next Generation • • • • •

Maximizes the inertness of the sample pathway. Minimizes breakdown. Low bleed. Thermally stable. “Clean and green”—manufactured without the use of harmful organic solvents.

Restek offers the next generation of deactivation. The Siltek™ deactivation process (patent pending) produces a highly-inert glass surface, which features high temperature stability, extreme durability, and low bleed. Try Siltek™ liners, guard columns, wool, and connectors for better recovery of sample analytes.

For Siltek™ inlet liners, add the corresponding suffix number to your liner catalog number. qty. each 5-pk. 25-pk.

Deactivation—Which Should You Choose? Siltek™ Deactivation • Revolutionary deactivation lowers endrin breakdown to less than 1%. • Inertness retained over a wide range of sample pH. • Minimal bleed. • Recommended for difficult matrix and reactive compound analysis. • Ideal for chlorinated pesticide analysis. • Recommended for use with Rtx®CLPesticides, Stx-CLPesticides, Stx-1HT, and Rtx®-TNT columns. Base-Deactivation • Provides excellent inertness for basic compounds. • Recommended for use with Rtx®-5 Amine, Rtx®-35 Amine, and Stabilwax®-DB columns.

Siltek™ -214.1 addl. cost -214.5 addl. cost -214.25 addl. cost

Siltek™ with Siltek™ wool -213.1 addl. cost -213.5 addl. cost -213.25 addl. cost

Base-Deactivated Inlet Liners for Agilent GCs If you do not see the deactivated liner you need, you can order it on a custom basis by adding the appropriate suffix number to the liner catalog number. For base deactivation: each (-210.1), 5-pack (-210.5), 25-pack (-210.25). For base-deactivated liners packed with base-deactivated wool: each (-211.1), 5-pack (-211.5), 25-pack (-211.25). ea. 20781-211.1 20706-210.1 20772-210.1 20795-210.1 20798-210.1

5-pk.

25-pk.

4mm Split Straight w/ Wool 20782-211.5 Cyclosplitter® 20707-210.5 4mm Splitless Straight 20773-210.5 2mm Gooseneck 20796-210.5 4mm Gooseneck 20799-210.5

20783-211.25 — 20774-210.25 20797-210.25 20800-210.25

Prepacked Liners Let Restek do the work! Just add the appropriate suffix to the liner catalog number. qty. ea. 5-pk. 25-pk.

Prepacked Inlet Liners Suffix Numbers FS Wool FS Beads Glass Wool -200.1 -201.1 -202.1 -200.5 -201.5 -202.5 -200.25 -201.25 -202.25

†CarboFrit™ inserts require a neck greater than 2mm.



For customer service, call

800-356-1688, ext. 3 (814-353-1300, ext. 3)

or call your local Restek representative.

www.restekcorp.com

Siltek™ with CarboFrit™ -216.1 addl. cost -216.5 addl. cost -216.25 addl. cost

CarboFrit™† -209.1 -209.5 -209.25

21

all liners are

100% deactivated

Liners for Agilent/Finnigan GCs

Splitless Liners for Agilent/Finnigan GCs

ID**/OD & Length (mm)

Similar to Agilent part #

ea.

cat.# 5-pk.

25-pk.

trace samples <2µL

2.0 ID 6.5 OD x 78.5

18740-80220 5181-8818

20712

20713

20714

trace samples >2µL

4.0 ID 6.5 OD x 78.5

19251-60540

20772

20773

20774

trace samples >2µL

4.0 ID 6.5 OD x 78.5

19251-60540

20772-214.1

20773-214.5

20774-214.25

trace samples >2µL

4.0 ID 6.5 OD x 78.5

19251-60540

22400

22401

22402

trace samples <2µL

2.0 ID 6.5 OD x 78.5

18740-80220 5181-8818

20914

20915



trace samples >2µL

4.0 ID 6.5 OD x 78.5

18740-80220 5181-8818

20912

20913



trace samples >2µL

4.0 ID 6.5 OD x 78.5

18740-80220 5181-8818

22403

22404



trace samples <2µL

2.0 ID 6.5 OD x 78.5

5181-3316***

20795

20796

20797

trace samples <2µL

2.0 ID 6.5 OD x 78.5

5181-3316***

20795-214.1

20796-214.5

20797-214.25

trace samples >2µL

4.0 ID 6.5 OD x 78.5

5181-3316

20798

20799

20800

trace samples >2µL

4.0 ID 6.5 OD x 78.5

5181-3316

20798-214.1

20799-214.5

20800-214.25

trace samples >2µL

4.0 ID 6.5 OD x 78.5

5062-3587

22405

22406

22407

trace samples >2µL

4.0 ID 6.5 OD x 78.5

5062-3587

22405-213.1

22406-213.5

22407-213.25

trace, active samples >2µL

4.0 ID 6.5 OD x 78.5

5181-3315

20784

20785

20786

™ trace, active samples >2µL Siltek deactivation

4.0 ID 6.5 OD x 78.5

5181-3315

20784-214.1

20785-214.5

20786-214.25

trace, active, dirty samples <2µL

2.0 ID 6.5 OD x 78.5



20907

20908

trace, active, dirty samples >2µL

4.0 ID 6.5 OD x 78.5



20895

20896

20997

trace, active, dirty samples >2µL

4.0 ID 6.5 OD x 78.5



20895-214.1

20896-214.5

20997-214.25

base easily packs with wool for dirty samples <2µL

2.0 ID 6.5 OD x 78.5



20980

20981

20982

base easily packs with wool for dirty samples >2µL

4.0 ID 6.5 OD x 78.5



20983

20984

20985

base easily packs with wool for dirty samples >2µL

4.0 ID 6.5 OD x 78.5



20983-214.1

20984-214.5

20985-214.25

base easily packs with wool for dirty samples > 2µL

4.0 ID 6.5 OD x 78.5



22408

22409

22410

base easily packs with wool for dirty, active samples > 2µL

4.0 ID 6.5 OD x 78.5



20986

20987

20988

Benefits/Uses:

D

2mm Splitless

4mm Splitless ™ Siltek deactivation

Siltek™ 4mm Splitless

4mm Splitless w/ FS Wool

2mm Splitless (quartz)

4mm Splitless (quartz)

4mm Splitless (quartz) w/ FS Wool

T

H

I

S

E

N

featuring

Gooseneck Splitless (2mm)

L

S

featuring ™ Siltek deactivation

Siltek Gooseneck Splitless (2mm) ™

Gooseneck Splitless (4mm)† featuring

L

™ Siltek deactivation

A

Siltek™ Gooseneck Splitless (4mm)†

T

Gooseneck Splitless (4mm) w/ FS Wool† featuring ™ Siltek deactivation

Siltek Gooseneck Splitless (4mm) w/ Siltek Glass Wool†

N

S





Double Gooseneck Splitless (4mm)

I

featuring

Cyclo Double Gooseneck (2mm)

Cyclo Double Gooseneck (4mm)

Siltek Cyclo Double Gooseneck (4mm)

Recessed Gooseneck (2mm)*



™ Siltek deactivation

Recessed Gooseneck (4mm)* featuring

C

O

U

featuring

L

M

N

Siltek™ Double Gooseneck Splitless (4mm)



Siltek Recessed Gooseneck (4mm)*

™ Siltek deactivation

Recessed Gooseneck (4mm)* w/ FS Wool

Recessed Double Gooseneck (4mm)*

*Use with two-hole ferrule for dual-column analysis. **Nominal ID at syringe needle expulsion point.

***Restek design changes improve performance over the original Agilent liner. †Use this liner for increased sensitivity.



www.restekcorp.com

22

all liners are

100%

Liners for Agilent/Finnigan GCs

Split Liners deactivated for Agilent/Finnigan GCs

Benefits/Uses: for purge & trap inlet splitting or sample <1µL universal, use with Agilent 7673 autosampler featuring universal, use with ™ Agilent 7673 deactivation autosampler

D

Siltek™ 4mm Split w/ Siltek™ Glass Wool

E

4mm Split with Wool*

N

1mm Split†

S I H T

®

4mm Split Precision Liner



20783

4.0 ID 6.3 OD x 78.5

19251-60540

20781-213.1

20782-213.5

20783-213.25

high MW compounds

4.0 ID 6.3 OD x 78.5

18740-80190

20801

20802

high MW compounds

4.0 ID 6.3 OD x 78.5

high & low MW compounds

4.0 ID 6.3 OD x 78.5

18740-80190

20709

20710



high & low MW compounds

4.0 ID 6.3 OD x 78.5

18740-80190

20709-214.1

20710-214.5



dirty samples, many injections before cleaning required

4.0 ID 6.3 OD x 78.5



20706

20707

20708

dirty samples, trace samples

4.0 ID 6.3 OD x 78.5



21022

21023

20979

dirty samples, trace samples

4.0 ID 6.3 OD x 78.5



21022-213.1

21023-213.5

20979-213.25



20990



20991



featuring ™ Siltek deactivation

L

S

Cyclosplitter

20973

20782

mini-Lam Split

™ Siltek deactivation

20972

25-pk.

20781



Siltek™ Cup Splitter



cat.# 5-pk.

ea.

19251-60540

Laminar Cup Splitter

featuring

1.0 ID 6.3 OD x 78.5

Similar to Agilent part#

4.0 ID 6.3 OD x 78.5

Siltek

Cup Splitter

ID**/OD & Length (mm)



Siltek 4mm Split Precision Liner w/ Siltek Glass Wool

L



Similar to Agilent part #

cat.# ea.

cat.# 5-pk.

universal, use with Agilent 6890 GCs

4.0 ID 6.3 OD x 78.5

5183-4647

21032

21033

Benefits/Uses:

ID**/OD & Length (mm)

cat.# ea.

cat.# 5-pk.

trace, active samples, samples <1µL

1.0 ID 6.3 OD x 78.5

21052-214.1

21053-214.5

trace, active samples, high recovery & linearity

4.0 ID 6.3 OD x 78.5

20335

20336

trace, active samples, high recovery & linearity

4.0 ID 6.3 OD x 78.5

20335-214.1

20336-214.5

4.0 ID 6.3 OD x 78.5

20337

20338

4.0 ID 6.3 OD x 78.5

20337-214.1

20338-214.5

4.0 ID 6.3 OD x 78.5

20843

20844

A N I

featuring

Uniliner®***

™ Siltek deactivation

featuring ™ Siltek deactivation

Siltek Uniliner *** ®

N



®

Cyclo-Uniliner *** featuring

U

™ Siltek deactivation

Siltek™ Cyclo-Uniliner®***

L

M

ID**/OD & Length (mm)

DI Liners for Agilent/Finnigan GCs (For 0.32/0.53mm ID Columns)

S

T

Low Pressure Drop Liner w/ Wool

Siltek™ 1mm Uniliner®***

Open-top Uniliner® with Wool***

trace, dirty, high MW active samples, high recovery & linearity trace, dirty, high MW active samples, high recovery & linearity trace, dirty, active samples, high recovery & linearity

DI Liners for Agilent 5890 & 6890 GCs (For 0.25/0.32/0.53mm ID Columns)

O C

Benefits/Uses

Split/Splitless Liners for Agilent 6890 GCs

Hole makes direct injection possible with EPCequipped Agilent 6890 GCs!

Drilled Uniliner®

Siltek™ Drilled Uniliner®



Siltek 1mm Drilled Uniliner

www.restekcorp.com

®

featuring ™ Siltek deactivation featuring ™ Siltek deactivation

Benefits/Uses:

ID**/OD & Length (mm)

cat.# ea.

cat.# 5-pk.

allows direct injection when using an EPC-equipped GC

4.0 ID 6.3 OD x 78.5

21054

21055

allows direct injection when using an EPC-equipped GC

4.0 ID 6.3 OD x 78.5

21054-214.1

21055-214.5

allows direct injection when using an EPC-equipped GC

1.0 ID 6.3 OD x 78.5

21390-214.1

21391-214.5

*Use with two-hole ferrule for dual-column analysis. **Nominal ID at syringe needle expulsion point.

***Restek design changes improve performance over the original Agilent liner. †Use this liner for increased sensitivity.

23

O-Rings Viton® O-Rings • For Agilent and PE AutoSys GCs. • Viton® O-rings fit split (6.3mm OD) or splitless (6.5mm OD) liners. • Graphite O-rings have excellent thermal stability. Description Viton® (fluorocarbon) O-rings

Max. temp. 350°C

Similar to Agilent part # 5180-4182

Restek cat.# 20377

qty. 25-pk.

Graphite O-Rings • For Agilent and Varian 1177 GCs. • Excellent thermal stability at injection port temperature up to 450°C! Description 6.35mm ID Graphite O-rings for split liners 6.5mm ID Graphite O-rings for splitless liners

Max. temp. 450°C 450°C

Similar to Agilent part # 5180-4168 5180-4173

Restek cat.# 10-pk. 50-pk. 20296 20297 20298 20299

High-Temperature O-Rings • Stable to 400°C. • Will not crack or melt. • Softer and easier to use than graphite. Description High-temperature O-rings

Max. temp. 400°C

qty. 5-pk.

cat.# 20437

Inlet and FID Maintenance Kits for Agilent GCs • Kits include the most common consumable supplies. • All parts meet or exceed instrument manufacturer’s specifications. • Includes parts list that makes reordering easy. Inlet kits include: • 0.4, 0.5, and 0.8mm ID graphite ferrules. • Viton® o-rings. • Capillary nuts. • Inlet seals. • Reducing nut. • Scoring wafer. • 11mm Thermolite® septa. • 4.0mm single gooseneck liner. • 4.0mm split liner with wool. • Capillary column caps. • 1/4- to 5/16-inch wrench. • Septum puller. • Installation gauge. • Wire cleaning brush. • Jet reamers/ferrule removers. • Inlet liner removal tool.

FID kits include: • 1/4-Inch, 0.4, 0.5, and 0.8mm ID graphite ferrules. • FID/NPD capillary adaptor. • Capillary nuts. • Jet reamers/ferrule removers. • 1/4-Inch nut. • Scoring wafer. • Capillary column caps. • Ignitor for either Agilent 5890 or 6890/6850 GCs. • FID flow measuring adaptor. • 1/4- to 5/16-inch wrench. • Installation gauge. • Wire cleaning brush. • High-performance Silcosteel®-treated FID jet for either Agilent 5890 or 6890/6850 GCs. • 1/4-Inch nut driver for jet removal.

Description Inlet Maintenance Kit for Agilent 5890/6890/6850 GCs FID Maintenance Kit for Agilent 5890 GCs FID Maintenance Kit for Agilent 6890/6850 GCs

qty. kit kit kit

cat.# 21069 21070 21071

www.restekcorp.com

24

Vespel® Ring Inlet Seals for Agilent 5890/6890 and 6850 GCs • Easy-to-use, patent-pending design makes a better seal, easily. • Prevents oxygen from damaging your columns. • Reduces wear on the injection port body.

Figure 1 The Vespel® Ring Inlet Seal achieves leak-tight seals even at low torque, reducing the chance of leaks. 0.01

Leak Rate (Log10 atm cc/sec.)

1E-3

stainless steel original equipment inlet seal

1E-4 1E-5 1E-6 1E-7

In Agilent split/splitless injection ports, it can be difficult to make and maintain a good seal with a conventional metal inlet disk. The metal-to-metal seal dictates that the analyst apply considerable torque to the reducing nut, and, based on our testing, this does not ensure a leak-tight seal. Over the course of oven temperature cycling, metal seals are prone to leaks, which ultimately can degrade the capillary column, and cause other analytical difficulties.

Vespel® ring minimizes leaks

Our Vespel® Ring Inlet Seal greatly improves injection port performance—it seals even after repeated temperature cycles and without retightening the reducing nut! This seal features a Vespel® ring embedded into its face. This soft Vespel® ring will not harm the critical seal on the injector body, and is outside the sample flow path. Tests using a high sensitivity helium leak detector indicate the Vespel® Ring Inlet Seal seals equally effectively at torques of 5lb. or 60lb. (Figure 1).

Vespel® Ring Inlet Seal

1E-8 1E-9

1E-10 0

10

20

30 40 Torque (in. lbs.)

50

60

Why trust a metal-to-metal seal when you can make leak-tight seals quickly and easily— and more reliably—with the Restek Vespel® Ring Inlet Seal? Use the stainless steel seal for analysis of unreactive compounds. To reduce breakdown and adsorption of active compounds, use the gold-plated or Silcosteel®-treated seals. The gold surface offers better inertness than standard stainless steel; Silcosteel® treatment provides inertness similar to that of fused silica capillary columns.

Vespel® Ring Inlet Seals for Agilent 5890/6890/6850 GCs 0.8mm ID Vespel® Ring Inlet Seal (washers included) Gold-Plated Silcosteel® Stainless Steel 1.2mm ID Vespel® Ring Inlet Seal (washers included) Gold-Plated Silcosteel® Stainless Steel

2-pk. 21562 21564 21560 2-pk. 21568 21570 21566

10-pk. 21563 21565 21561 10-pk. 21569 21571 21567

Re-Threading Tool • Repair worn or damaged threads. • Multiple uses (injection ports, fittings, etc.). • Built-in guide to prevent cross-threading.

1

2

3

1) Worn & damaged threads can allow oxygen into the system—compromising analytical results and destroying columns. 2) Screw the tool completely onto the injection port in a clockwise direction.

Achieve a better seal!

3) Unscrew the tool and inspect the threads, repeat as necessary, and, when done, wipe threads with methanol to remove any debris.

www.restekcorp.com

Description

qty.

cat.#

Re-threading Tool for 1/4" compression fitting for Agilent split/splitless injection ports

ea.

23018

25

Replacement Inlet Seals • Special grade of stainless steel that is softer and deforms more easily, ensuring a completely leak-free seal. • Increases column lifetime because oxygen cannot permeate into the carrier gas. • Reduced noise benefits high-sensitivity detectors (e.g., ECDs, MSDs). • Silcosteel® seal offers the inertness of glass. • All seals include washers.

Replacement Inlet Seals for Agilent 5890/6890/6850 Split/Splitless Injection Ports The inlet seal at the base of the Agilent 5890/6890 GC injection port contacts the sample and must be changed frequently to prevent adsorption of active compounds. In addition, septum fragments and sample residue accumulate on the disk surface, requiring disk replacement. The inlet seal design increases column lifetime because oxygen cannot permeate into the carrier gas. Detector noise also is reduced with high-sensitivity detectors (e.g., ECDs or MSDs). To reduce breakdown and adsorption of active compounds, use the gold-plated or Silcosteel® seals. The gold surface offers better inertness than standard stainless steel, and the Silcosteel® treatment offers inertness similar to that of fused silica capillary columns. Single-Column Installation, Opening Size 0.8mm ID* 2-pk. 10-pk. 21315 21317

0.25/0.32mm ID Dual-Column 0.53mm ID Dual-Column Installation Installation, Opening Size 1.2mm ID Opening Size (1/16-inch hole) 2-pk. 10-pk. 2-pk. 10-pk.

21316

Stainless Steel Inlet Seal 20390 20391

20392

20393

21318

Gold-Plated Inlet Seal 21305 21306





21320

Silcosteel Inlet Seal 21307 21308





®

21319

*0.8mm ID stainless steel inlet seal is equivalent to Agilent part #18740-20880, 0.8mm ID gold-plated inlet seal is equivalent to Agilent part #18740-20885.

Replacement Inlet Cross-Disk Seal for Agilent GCs • Ideal for high-flow split applications on Agilent 5890 GCs. • All seals include washers. (Similar to Agilent part # 5182-9652.) 0.8mm ID Cross-Disk Inlet Seal for Agilent GCs Gold-Plated Silcosteel® 1.2mm ID Cross-Disk Inlet Seal for Agilent GCs Gold-Plated Silcosteel®

2-pk. 20477 20475 2-pk. 21009 21011

10-pk. 20476 20474 10-pk. 21010 21012

www.restekcorp.com

26

all liners are

100% deactivated

Liners for Varian GCs Splitless Liners for Varian 1075/1077 GCs

ID**/OD & Length (mm)

Similar to Varian part #

ea.

cat.# 5-pk.

25-pk.

trace samples <2µL

2.0 ID 6.3 OD x 74

01-900109-05

20721

20722

20723

trace samples >2µL

4.0 ID 6.3 OD x 74

01-900109-05

20904

20905

20906

trace, active samples up to 4µL

4.0 ID 6.3 OD x 74



20847

20848

trace, dirty, active samples up to 4µL

4.0 ID 6.3 OD x 74



20897

20898

Benefits/Uses:

ID**/OD & Length (mm)

purge & trap inlet splitting or samples <1µL

1.0 ID 6.3 OD x 72

universal, use with rapid autosamplers

4.0 ID 6.3 OD x 72

01-900109-01

20792

20793

high MW compounds

4.0 ID 6.3 OD x 72

01-900109-02

20803

20804

high & low MW compounds

4.0 ID 6.3 OD x 72



20724

20725



dirty samples, many injections before cleaning required

4.0 ID 6.3 OD x 72



20727

20728



dirty samples, non-active compounds

4.0 ID 6.3 OD x 72

01-900109-03

20715

20716

20717

close boiling compounds

4.0 ID 6.3 OD x 72

01-900109-04

20718

20719

20720

dirty samples, active samples

4.0 ID 6.3 OD x 72

Benefits/Uses:

4mm Splitless

Double Gooseneck

E

N

D

2mm Splitless

Cyclo Double Gooseneck

I

S

Split Liners for 1075/1077 Varian GCs

T

H

1mm Split

Splitter with Wool*

Cup Splitter

L

S

Laminar Cup Splitter

®

Frit Splitter

Baffle Splitter

Split Precision™ Liner

N

S

T

A

L

Cyclosplitter





Similar to Varian part #

ea. 20970

21030

cat.# 5-pk. 20971

21031

25-pk. —

20794





Benefits/Uses:

ID**/OD & Length (mm)

trace, active samples, high recovery & linearity

4.0 ID 6.3 OD x 72



20345

20346



trace, dirty, high MW, active samples, linearity

4.0 ID 6.3 OD x 72



20347

20348



trace, dirty, active samples, high recovery & linearity

4.0 ID 6.3 OD x 72



20845

20846



Benefits/Uses:

ID**/OD & Length (mm)

Similar to Varian part #

ea.

cat.# 5-pk.

25-pk.

high linearity for 0.25 & 0.32mm ID columns

0.53 ID 4.6 OD x 54

01-900109-06

20775

20776

20777

high linearity for 0.25 & 0.32mm ID columns

0.53 ID 4.6 OD x 54

01-900109-06

207752077720776-214.5 214.1 214.25

high linearity for 0.53mm ID columns

0.80 ID 4.6 OD x 54

01-900109-07

20778

20779

20780

dirty samples >1µL, fits 0.25, 0.32 & 0.53mm ID columns

2.4 ID 4.6 OD x 54

01-900109-08

20850

20851

20852

ea.

cat.# 5-pk.



25-pk.

I

DI Liners for Varian 1075/1077 GCs (0.32/0.53mm ID)

Similar to Varian part #

20849

Cyclo-Uniliner®

M

N

Uniliner®

U

Open-top Uniliner® with Wool*

O

L

SPI Liners for Varian GCs

0.5mm SPI

C

featuring ™

Siltek 0.5mm SPI

0.8mm SPI

SPI with Buffer

www.restekcorp.com

™ Siltek deactivation

*Prepacked with fused silica wool. For glass wool instead, add the suffix “-202” to the liner catalog number. **Nominal ID at syringe needle expulsion point.

27

all liners are

100%

C O L U M N

I N S TALLS

TH IS

EN D

deactivated

Liners for Varian GCs Liners for Varian 1177 GCs

ID**/OD & Length (mm)

Similar to Varian part #

ea.

cat.# 5-pk.

universal

4.0 ID 6.3 OD x 78.5

39-26119-36

21045

21046

trace samples <2µL

2.0 ID 6.5 OD x 78.5

39-26119-38



21077



universal

4.0 ID 6.3 OD x 78.5

39-26119-37



21079



Benefits/Uses:

ID**/OD & Length (mm)

Similar to Varian part #

ea.

cat.# 5-pk.

dirty samples, non-active compounds

3.4 ID 5.0 OD x 54

03-918464-00

21708

21709



trace samples <2µL

2.0 ID 5.0 OD x 54

03-918466-00

21711

21712



trace samples <2µL

2.0 ID 5.0 OD x 54

03-918466-00

2171121712-214.5 214.1



trace samples <1µL

0.5 ID 5.0 OD x 54

03-925331-00

20992

20993



active samples

3.4 ID 5.0 OD x 54

03-918464-00

20859

20901

active samples

3.4 ID 5.0 OD x 54

03-918464-00

208592090920901-214.5 214.1 214.25

trace, low volume samples

0.75 ID 5.0 OD x 54

03-925330-00

21714

trace samples, dirty samples

3.4 ID 5.0 OD x 54

Benefits/Uses:

4mm Split

2mm Splitless w/wool*

4mm Split w/wool* 1078/1079 Liners for Varian GCs

1078/1079 Split

1078/1079 Splitless featuring

™ Siltek deactivation



Siltek 1078/1079 Splitless

Open 0.5mm ID

1078/1079 Split–No Frit featuring

™ Siltek deactivation



Siltek 1078/1079 Split–No Frit

Open 0.75mm ID



1078/1079 Split Precision Liner



21024

21715

21025

25-pk. —

25-pk.

20909

21716



*Prepacked with fused silica wool. For glass wool instead, add the suffix “-202” to the liner catalog number. **Nominal ID at syringe needle expulsion point.

Inlet Liner Seals for Varian 1177 Injectors Meets original equipment specifications. (Similar to Varian part # 39-26119-40.) Description Inlet Liner Seals for Varian 1177 Injectors

qty. 10-pk.

cat.# 20298

5mm Liner Seals for Varian 1078/1079 GCs Description 5mm Liner Seals for Varian 1078/1079 GCs

qty. 10-pk.

cat.# 22683

Inlet Liner Removal Tool • • •

Easily remove liners from injectors. Made from high-temperature silicone. Won’t chip or crack the liner.

Description Inlet Liner Removal Tool

qty. 3-pk.

cat.# 20181

No more burned fingers!

www.restekcorp.com

28

all liners are

100% deactivated

Liners for PerkinElmer GCs Split Liners for PerkinElmer GCs

E

N

D

Baffle Splitter

Cup Splitter

Cyclosplitter®

Benefits/Uses:

ID**/OD & Length (mm)

Similar to PE part #

ea.

cat.# 5-pk.

universal, for most common analyses

3.5 ID 5.0 OD x 100

0330-5181

20736

20737

high & low MW compounds

3.5 ID 5.0 OD x 100



20739

20740



dirty samples, max. injections before cleaning required

3.5 ID 5.0 OD x 100



20745

20746



high MW compounds

3.5 ID 5.0 OD x 100



20805

20806



universal for most common analyses

4.0 ID 6.2 OD x 92.1

N6101052

20832

20833

20834

universal for most common analyses

4.0 ID 6.2 OD x 92.1

N6101052

20832-213.1

20833-213.5

20834-213.25

high & low MW compounds

4.0 ID 6.2 OD x 92.1



20835

20836



dirty samples, max. injections before cleaning required

4.0 ID 6.2 OD x 92.1



20910

20911



high MW compounds

4.0 ID 6.2 OD x 92.1



20827

20828



dirty samples, trace samples

4.0 ID 6.2 OD x 92.1



21026

21027



Benefits/Uses:

ID**/OD & Length (mm)

Similar to PE part #

ea.

cat.# 5-pk.

25-pk.

trace samples

2.0 ID 5.0 OD x 100

0330-5180

20730

20731

20732

trace samples

2.0 ID 6.2 OD x 92.1

N6101372

20829

20830

20831

trace samples

2.0 ID 6.2 OD x 92.1

N6101372

20829-213.1

20830-213.5

20831-213.25

trace, active samples up to 4µL

4.0 ID 6.2 OD x 92.1



20853

20854



trace, dirty, active samples, up to 4µL

4.0 ID 6.2 OD x 92.1



20899

20900



S

Laminar Cup Splitter

I

Auto SYS Splitter with Wool* featuring

H



™ Siltek deactivation

Siltek Auto SYS Splitter w/ Siltek Glass Wool

T



Auto SYS Cup Splitter

®

Auto SYS Laminar Cup Splitter



Auto SYS Split Precision Liner Splitless Liners for PerkinElmer GCs

Splitless (2mm ID)

S

T

A

L

L

S

Auto SYS Cyclosplitter

Auto SYS Splitless w/Wool (2mm ID)*

N

™ Siltek deactivation

I Auto SYS Cyclo Double Gooseneck DI Liners for PerkinElmer GCs (0.32/0.53mm ID)

M

N

Auto SYS Double Gooseneck

Uniliner®

L

U



featuring

Siltek™ Auto SYS Splitless w/Siltek Glass Wool (2mm ID)

O

Cyclo-Uniliner®

®

C

25-pk.

Auto SYS Open-top Uniliner w/Wool*

Auto SYS Cyclo-Uniliner

®

Auto SYS Drilled Uniliner®

Benefits/Uses: trace, active samples, high recovery & linearity trace, dirty, active samples, high linearity trace, dirty, active samples, high recovery & linearity trace, dirty, high MW active samples, high linearity allows direct injection when using an EPC-equipped GC

ID**/OD & Length (mm)

Similar to PE part#

ea.

25-pk.

3.5 ID 5.0 OD x 100



20855

20856



3.5 ID 5.0 OD x 100



20857

20858



4.0 ID 6.2 OD x 92.1



20837

20838



4.0 ID 6.2 OD x 92.1



20839

20840



4.0 ID 6.2 OD x 92.1



20819

20822



*Prepacked with fused silica wool. For glass wool instead, add the suffix “-202” to the liner catalog number. **Nominal ID at syringe needle expulsion point.

www.restekcorp.com

cat.# 5-pk.

29

all liners are

100%

Liners for Shimadzu GCs Split Liners for Shimadzu GCs

deactivated

Benefits/Uses:

E

D N

128mm Cyclosplitter®

128mm Cup Splitter

S

cat.# 5-pk.

ea.

25-pk.

purge & trap & fast GC universal, for most common analyses

3.5 ID 5.0 OD x 128

dirty samples, many injections before cleaning required

3.5 ID 5.0 OD x 128



20754

20755



high & low MW compounds

3.5 ID 5.0 OD x 128



20757

20758



high MW compounds

3.5 ID 5.0 OD x 128



20807

20808



universal, for most common analyses

3.5 ID 5.0 OD x 99

dirty samples, many injections before cleaning required

3.5 ID 5.0 OD x 99



20870

20871



high MW compounds

3.5 ID 5.0 OD x 99



20866

20867



high MW compounds

3.5 ID 5.0 OD x 99



20868

20869



trace samples, dirty samples

3.5 ID 5.0 OD x 95



21020

21021



Benefits/Uses:

ID**/OD & Length (mm)

Similar to Shimadzu part #

ea.

cat.# 5-pk.

25-pk.

trace samples

3.5 ID 5.0 OD x 128

221-25440-03

20748

20749

20750

trace samples

3.5 ID 5.0 OD x 99

221-32544-00

20863

20864

20865

reduces backflash and catalytic decomposition

3.5 ID 5.0 OD x 95

reduces backflash, also operates in DI mode

3.5 ID 5.0 OD x 95

221-41599-00

20961

20962

20963

Benefits/Uses:

ID**/OD & Length (mm)

Similar to Shimadzu part #

ea.

cat.# 5-pk.

25-pk.

universal, for most common analyses

3.5 ID 5.0 OD x 95

221-41444-00

20955

20956

20957

universal, for most common analyses

3.5 ID 5.0 OD x 95

221-41444-00

20955213.1

20956-213.5

20957213.25

Benefits/Uses:

ID**/OD & Length (mm)

Similar to Shimadzu part #

trace, active samples, high recovery & linearity

3.5 ID 5.0 OD x 128



20872

20873



trace, dirty, high MW active samples, high linearity

3.5 ID 5.0 OD x 128



20874

20875



trace, active samples, high recovery & linearity

3.5 ID 5.0 OD x 99



20876

20877



trace, dirty, high MW active samples, high recovery & linearity

3.5 ID 5.0 OD x 99



20893

20894



trace, dirty, high MW active samples, high recovery & linearity

3.5 ID 5.0 OD x 95



21713

21719



128mm Laminar Cup Splitter



221-25822-01

221-32544-01

20976

20977

20751

20978

20752

20860

20861

20753

20862

H

99mm Cyclosplitter®

T

I

99mm Split

Similar to Shimadzu part #

1.0 ID 5.0 OD x 95

17A 1mm Split

128mm Split

ID**/OD & Length (mm)

99mm Cup Splitter

17A Split Precision™ Liner Splitless Liners for Shimadzu GCs

128mm Splitless (3mm ID)

99mm Splitless (3mm ID)

S

T

A

L

L

S

99mm Laminar Cup Splitter

N

17A 95mm Double Gooseneck

20958

20959

20960

I

17A 95mm Single Gooseneck



N

Split/Splitless Liners for Shimadzu GCs

17A 95mm Split/Splitless with Wool* ™ Siltek deactivation

Siltek™ 95mm Split/Splitless w/ Siltek™ Glass Wool DI Liners for Shimadzu GCs (0.32/0.53mm ID)

L

U

M

featuring

O

128mm Uniliner®

C

128mm Cyclo-Uniliner®

99mm Uniliner®

99mm Cyclo-Uniliner®

®

95mm Uniliner with Wool*

ea.

*This liner is prepacked with fused silica wool. To order glass wool instead, add the suffix “-202” to the liner catalog number. **Nominal ID at syringe needle expulsion point.

cat.# 5-pk.

25-pk.

30

all liners are

100% E

N

D

deactivated

Liners for Thermo Finnigan Split Liners for 5000-6000 Series GCs

Benefits/Uses:

Cyclosplitter

S

Cup Splitter Gooseneck

H

Splitless (2mm ID)

T

Splitless (4mm ID)

S

DI Liners for 5000-6000 Series GCs (0.32/0.53 ID)

L

Open-top Uniliner® w/Wool* Split Liners for 8000 & TRACE™ Series GCs

20810



dirty samples, many injections before cleaning required

4.0 ID 5.4 OD x 79.5



20817

20818



high & low MW compounds

4.0 ID 5.4 OD x 79.5



20885

20886



Benefits/Uses:

ID**/OD & Length (mm)

L A T S N I N M U

20812

20813

trace samples

4.0 ID 5.4 OD x 79.5



20814

20815

20816

Benefits/Uses: trace, dirty, active samples, high recovery & linearity

L O

4.0 ID 5.4 OD x 79.5

Similar to TF part # —

ea. 20841

20842

25-pk. —

ea.

cat.# 5-pk.

purge & trap & fast GC

1.0 ID 8.0 OD x 105

453 20075

20916

20917

universal

3.0 ID 8.0 OD x 105

453 20031

20936

20937

20938

universal

5.0 ID 8.0 OD x 105

453 20030

20939

20940

20941

high MW compounds

4.0 ID 8.0 OD x 105



20948

20949



high & low MW compounds

4.0 ID 8.0 OD x 105



20950

20951



trace samples, dirty samples

5.0 ID 8.0 OD x 105



21028

21029



Benefits/Uses:

ID**/OD & Length (mm)

Similar to TF part #

ea.

cat.# 5-pk.

25-pk.

trace samples

3.0 ID 8.0 OD x 105

453 20032

20942

20943

20944

trace samples

3.0 ID 8.0 OD x 105

453 20032

20942-214.1

20943-214.5

20944-214.25

trace samples

5.0 ID 8.0 OD x 105

453 20033

20945

20946

20947

trace active samples up to 4µL

4.0 ID 8.0 OD x 105



20952

*Prepacked with fused silica wool. For glass wool instead, add the suffix “-202” to the liner catalog number. **Nominal ID at syringe needle expulsion point.

www.restekcorp.com

cat.# 5-pk.

Similar to TF part #

Splitless (5mm ID)

C

ID**/OD & Length (mm)

ID**/OD & Length (mm)

featuring

Double Gooseneck

25-pk.

20811

Splitless (3mm ID) ™ Siltek deactivation

cat.# 5-pk.



Laminar Cup Splitter

Siltek Splitless (3mm ID)

ea.

trace samples

5mm Split



Similar to TF part #

2.0 ID 5.4 OD x 79.5

3mm Split

Splitless Liners for 8000 & TRACE™ Series GCs

25-pk.

20809

1mm Split

5mm Split Precision™ Liner

cat.# 5-pk.



Benefits/Uses:

Cup Splitter

ea.

high MW compounds

I

Splitless Liners for 5000-6000 Series GCs

Similar to TF part #

4.0 ID 5.4 OD x 79.5

Laminar Cup Splitter

®

ID**/OD & Length (mm)

20953

25-pk. —



31

all liners are

COLUMN INSTALLS THIS END

100%

Liners for Thermo Finnigan

DI Liners for 8000 & TRACE™ Series GCs

deactivated

Benefits/Uses: trace, active samples, high recovery, & linearity

Uniliner® w/Wool Split Liners for TRACE™ 2000 GCs

1mm ID Trace 2000 Glass Liner

ID**/OD & Length (mm)

Similar to TF part #

5.0 ID 8.0 OD x 105



21005

cat.# 5-pk. 21006



ID**/OD & Length (mm)

trace samples, high recovery & linearity

1mm ID 2.95 OD x 120



21114

21115



universal

2mm ID 2.95 OD x 120



21116

21117



ea.

cat.# 5-pk.

25-pk.

Benefits/Uses:

2mm ID Trace 2000 Glass Liner

Similar to TF part #

ea.

25-pk.

**Nominal ID at syringe needle expulsion point.

Inlet Liner Seal for TRACE™ 2000 GCs Description Inlet Liner Seal

qty. 2-pk.

cat.# 21392

Graphite Sealing Ring and Washer for 8000 Series and TRACE™ GC Inlet Liners (Similar to Thermo Finnigan part # 290-03406) Description Graphite Sealing Ring and Washer Graphite Sealing Rings and Washers

qty. ea. 2-pk.

cat.# 21898 21899

Graphite Ferrules for M4 Fittings • • • •

High-purity, high-density graphite. Smoother surface and cleaner edges than conventional graphite ferrules. Contain no binders that can off-gas or adsorb analytes. Stable to 450°C.

Graphite Ferrules for M4 Fittings for QCQ Thermo Finnigan 8000 & TRACE™ 2000 Ferrule ID 0.4mm* 0.5mm* 0.8mm*

Fits Column ID 0.18–0.25mm 0.28/0.32mm 0.45/0.50 & 0.53mm

Graphite 2-pk. 20280 20282 20284

Graphite 10-pk. 20281 20283 20285

*0.4mm ID ferrule is similar to Thermo Finnigan part #290-13488, 0.5mm ID ferrule is similar to Thermo Finnigan part #290-13487, and 0.8mm ID ferrule is similar to Thermo Finnigan part #29013486.

www.restekcorp.com

32

handy Septum Size Chart Instrument Septum Size Agilent (HP) 5880A, 5890, 6890,6850 11mm 5700, 5880 9.5/10mm On-Column Injection 5mm CE Instruments (TMQ) TRACE GC 17mm Finnigan (TMQ) GC 9001 9.5mm GCQ 9.5mm GCQ w/TRACE 17mm QCQ™ 9.5mm TRACE 2000 9.5mm Fisons/Carlo Erba (TMQ) 8000 series 17mm Gow-Mac 6890 series 11mm All other models 9.5mm PerkinElmer Sigma series 11mm 900,990 11mm 8000 series 11mm Auto SYS 11mm Auto SYS XL 11mm Pye/Unicam All models 7mm Shimadzu All models Plug SRI All models Plug Tracor 540 11.5mm 550,560 9.5mm 220,222 12.5mm Varian Injector type: Packed column 9.5/10mm Split/splitless 1078/1079 10/11mm 1177 9mm 1075/1077 11mm

Thermolite® Septa • Usable to 340°C inlet temperatures. • Each batch tested on FIDs, ECDs, and MSDs to ensure lowest bleed. • Excellent puncturability. • Preconditioned and ready to use. • Do not adhere to hot metal surfaces. • Packaged in non-contaminating glass jars. Septum Diameter 5mm (3/16") 6mm (1/4") 7mm 8mm 9mm 9.5mm (3/8") 10mm 11mm (7/16") 11.5mm 12.5mm (1/2") 17mm Shimadzu Plug

25-pk. 20351 20355 20381 20370 20354 20359 20378 20363 22385 20367 20384 20372

50-pk. 20352 20356 20382 20371 20358 20360 20379 20364 22386 20368 20385 20373

100-pk. 20353 20357 20383 — 20362 20361 20380 20365 22387 20369 20386 20374

InfraRed™ Septa • • • • • •

Usable to 325°C inlet temperatures. Preconditioned and ready to use. Excellent puncturability. Do not adhere to hot metal surfaces. Low bleed. Packaged in non-contaminating glass jars.

Septum Diameter 9mm 9.5mm (3/8") 10mm 11mm (7/16") 11.5mm 12.5mm (1/2") 17mm Shimadzu Plug

25-pk. 21417 21421 21424 21427 21430 21433 21436 21439

50-pk. 21418 21422 21425 21428 21431 21434 21437 21440

100-pk. 21419 21423 21426 21429 21432 21435 21438 21441

IceBlue™ Septa • • • • • • •

Usable to 250°C inlet temperatures. General-purpose septa. Excellent puncturability. Preconditioned and ready to use. Do not adhere to hot metal surfaces. Packaged in non-contaminating glass jars. Ideal for SPME.

Septum Diameter 9mm 9.5mm (3/8") 10mm 11mm (7/16") 11.5mm 12.5mm (1/2") 17mm Shimadzu plug

www.restekcorp.com

50-pk. 22381 22388 22390 22392 22383 22394 22396 22398

100-pk. 22382 22389 22391 22393 22384 22395 22397 22399

33

Siltek™ Press-Tight® Connectors • Siltek™ deactivation for inert pathways to maintain sample integrity. • Ideal for connecting guard columns to analytical columns. • Angled Press-Tight® connector designed at an angle approximating the curvature of a capillary column to reduce strain on column-end connections. • Fits 0.18, 0.25, 0.32, & 0.53mm ID columns.

Siltek™ Press-Tight™ Connectors Press-Tight® Connector Universal Press-Tight® Connector Universal Angled Press-Tight® Connector Universal “Y” Press-Tight® Connector Universal Angled “Y” Press-Tight® Connector

ea. — — 20485 20487

3-pk. — — 20486 20469

5-pk. 20480 20482 — —

25-pk. 100-pk. 20449 20481 20483 20484 — — — —

Siltek™—the most inert deactivation available!

Universal Angled Press-Tight® Connectors • • • •

Designed at an angle approximating the curvature of a capillary column. Reduces strain on column-end connections. Ideal for connecting guard columns to analytical columns. Seals all common sizes of fused silica tubing (0.18 to 0.53mm ID, outside diameters from 0.3 to 0.75mm). • Made from inert fused silica. Description Universal Angled Press-Tight® Connectors Universal Angled Press-Tight® Connectors Universal Angled Press-Tight® Connectors

qty. 5-pk. 25-pk. 100-pk.

cat.# 20446 20447 20448

Universal Press-Tight® Connectors • Connect guard columns to analytical columns. • Repair broken columns. • Connect column outlets to transfer lines. Description Universal Press-Tight® Connectors Universal Press-Tight® Connectors Universal Press-Tight® Connectors

qty. 5-pk. 25-pk. 100-pk.

cat.# 20400 20401 20402

Deactivated, Universal Press-Tight® Connectors • High-temperature silanization for excellent inertness. • Ideal for trace analysis of active compounds. • Ideal for analysis of pesticides, semivolatile pollutants, or clinical/forensic samples. Description Deactivated, Universal Press-Tight® Connectors Deactivated, Universal Press-Tight® Connectors Deactivated, Universal Press-Tight® Connectors

qty. 5-pk. 25-pk. 100-pk.

cat.# 20429 20430 20431

qty. ea. 3-pk.

cat.# 20405 20406

Polyimide Resin • Permanently connects a PressTight® connector to a fused silica column. • 350°C maximum operating temperature.

Universal “Y” Press-Tight® Connectors • Split sample flow onto two columns. • Split a single column flow into two detectors— perform confirmational analysis with a single injection. • Fit 0.18, 0.25, 0.32, & 0.53mm ID columns. Description Universal “Y” Press-Tight® Connector Universal “Y” Press-Tight® Connectors

Description Polyimide Resin

qty.

cat.#

5 grams

20445

www.restekcorp.com

34

MXT®-Union Connector Kits—For Fused Silica Columns Use for fused silica-to-fused silica or fused silica-to-metal connections!

• • • • • •

Low-dead-volume, leak-free connection. Reusable. Silcosteel® treatment ensures maximum inertness. Ideal for connecting guard columns and transfer lines. Use to oven temperatures of 350°C. Available in union and “Y” configurations.

Previously, easy-to-use MXT® connectors could only be used with metal tubing. Now MXT® connectors can be used with fused silica capillary columns, because of a Valcon polyimide 1/32-inch one-piece fused silica adaptor. This unique graphite-reinforced composite allows capillary columns to slide into and be locked in place simply by loosening and tightening the MXT® union 1/32-inch fitting.

MXT®-Union Connector Kits—For Fused Silica Columns Each kit contains the MXT® union, two 1/32-inch nuts and two one-piece fused silica adaptors. Description For 0.25mm ID Fused Silica Columns For 0.32mm ID Fused Silica Columns For 0.53mm ID Fused Silica Columns

qty. kit kit kit

cat.# 21386 21385 21384

MXT® “Y”-Union Connector Kits—For Fused Silica Columns Each kit contains the MXT® union, three 1/32" nuts and three one-piece fused silica adaptors. Description For 0.25mm ID Fused Silica Columns For 0.32mm ID Fused Silica Columns For 0.53mm ID Fused Silica Columns

qty. kit kit kit

cat.# 21389 21388 21387

qty. 5-pk.

cat.# 20389

/32-Inch Replacement Nut

1

Description 1 /32" Replacement Nut

Valco® Connectors—One-Piece Fused Silica Adaptor Ferrule We recommend a one-piece adaptor ferrule for use in fittings where the ferrule will not be removed. Connections are made and disconnected by loosening the fitting nut and sliding the tube out. Fused silica adaptor ferrules are available in Valcon polyimide for use up to 350°C. Valcon polyimide is a unique graphite-reinforced composite, specially prepared to maximize mechanical stability at high temperatures. The determining factor in adaptor ferrule size selection is the fused silica tubing outer diameter (OD).

/32-Inch Adaptor Ferrule

1

Tubing OD <0.25–0.4mm 0.4–0.5mm 0.5–0.8mm

Tubing ID 0.25mm 0.32mm 0.53mm 1 /32" Replacement Nut

Valco® # FS.4-5 FS.5-5 FS.5V-5

Valcon Polyimide qty. cat.# 5-pk. 20137 5-pk. 20140 5-pk. 20141 5-pk. 20389

Gerstel GRAPHPACK® 3D/2 Connectors Ideal for MXT® stainless steel to fused silica capillary connections!

GRAPHPACK® technology provides a complete system that quickly and reliably makes leak-free, low-dead-volume connections. The central component is a metal-jacketed graphite ferrule—the ideal seal for GC applications. GRAPHPACK® ferrules eliminate all the disadvantages and shortcomings associated with previous sealing systems. Description

qty.

cat.#

GRAPHPACK 3D/2 Connector** (0.25mm to 0.32mm ID)

ea.

20272

GRAPHPACK® 3D/2 Connector** (0.45mm to 0.7mm ID)

ea.

20273

®

www.restekcorp.com

**Use only with GRAPHPACK® 3D/2 ferrules.

GRAPHPACK® 3D/2 Ferrules Ferrule ID 0.4mm 0.5mm 0.8mm

Fits Column ID 0.25mm 0.32mm 0.45/0.53mm

qty. cat.# 10-pk. 20271 10-pk. 20270 10-pk. 20274

35

Intermediate-Polarity Deactivated Guard Columns & Transfer Lines • Useful for a wide range of applications. • Compatible with most common solvents.

Fused Silica Guard Columns/Transfer Lines Nominal ID 0.025mm* 0.05mm 0.075mm* 0.10mm 0.15mm 0.18mm 0.25mm 0.28mm 0.32mm 0.45mm 0.53mm

Nominal OD 0.363 ± 0.012mm 0.363 ± 0.012mm 0.363 ± 0.012mm 0.363 ± 0.012mm 0.363 ± 0.012mm 0.37 ± 0.04mm 0.37 ± 0.04mm 0.37 ± 0.04mm 0.45 ± 0.04mm 0.69 ± 0.04mm 0.69 ± 0.05mm

Nominal ID 0.25mm 0.32mm 0.53mm

Nominal OD 0.37 ± 0.04mm 0.45 ± 0.04mm 0.69 ± 0.05mm

1-Meter 10097 10098 10099 10100 10101 10102

10-Meter 10049 10048 10047

5-Meter

5-Meter/6-pk.

10040

10040-600

10041 10042 10046 10043 10003 10044 10005 10045

10043-600 10003-600 10044-600 10005-600 10045-600

10-Meter/6-pk. 10049-600 10048-600

30-Meter** 10012 10022 10032

60-Meter**† 10013 10023 10033

MXT® Guard Columns/Transfer Lines Nominal ID 0.28mm 0.53mm

Nominal OD 0.53 ± 0.025mm 0.74 ± 0.025mm

5-Meter 70044 70045

5-Meter/6-pk. 70044-600 70045-600

10-Meter 70046 70047

Siltek™-Deactivated Guard Columns • • • • •

Revolutionary deactivation process lowers analyte breakdown to less than 1%. Minimizes bleed. Ideal for chlorinated pesticide analysis. Analyze tough samples quickly and accurately. Maximum temperature of 380°C.

Siltek™-Deactivated Guard Columns Nominal ID 0.25mm 0.32mm 0.53mm

Nominal OD 0.37 ± 0.04mm 0.45 ± 0.04mm 0.69 ± 0.05mm

5-Meter 10026 10027 10028

10-Meter 10036 10037 10038

Let Restek Make the Connection for You! Restek will connect a Siltek™ guard column to any analytical column using a universal Siltek™ Press-Tight® connector and polyimide sealing resin. To order a preconnected guard column, add the three-digit suffix from the chart below to any analytical column catalog number when ordering.

5m Siltek™ Guard Column/Transfer Line ID 0.25mm 0.32mm 0.53mm

cat.# suffix -364 -365 -366

Example: A 5m, 0.32mm ID Siltek™ guard column connected to a 30m, 0.32mm ID, 1.0µm Rtx®-5 column is cat.# 10254-365.

*Not tested with the Grob test mix because of a high pressure drop. **30- and 60-meter lengths are banded in 5-meter sections. †Recommendation: Cut 60m guard columns into shorter lengths. Using full length may cause peak distortion.

Restek Trademarks: Siltek, Press-Tight, MXT, CarboFrit, Rtx, Uniliner, Silcosteel, Stx, Leak Detective, Stabilwax, Cyclosplitter, mini-Lam, Precision, InfraRed, IceBlue, Plus 1. Other Trademarks: Valco (Valco Instruments Co., Inc.), GRAPHPACK (Gerstel GmbH), Carbowax (Union Carbide Corp.), TRACE (ThermQuest Corp.), Velcro (Velcro Industries BV), Scotty (Scott Specialty Gases, Inc.), Viton & VESPEL (E.I du Pont de Nemours & Co., Inc.).

www.restekcorp.com

Plus 1Restek’s Customer Commitment Plus 1™ Service means we will surpass your expectations every time you contact us! You’ll get Plus 1™ service when you ask our experienced Technical Service team to help solve a difficult analytical problem. Our efficient Customer Service Team will provide Plus 1™ service even when you place a late-day order. Keep reaching for Restek products and service, and we will provide you with Plus 1™ quality and attention.

Orders & Customer Service (in the U.S.) PHONE:

FAX:

Restek Corporation

800-356-1688 (ext. 3) or 814-353-1300 (ext. 3)

814-353-1309

110 Benner Circle Bellefonte, PA 16823

Monday–Friday, 8:00 a.m.–6:00 p.m. EST

www.restekcorp.com

For customer and technical service outside the U.S.… please contact your local Restek International location or distributor. Germany: Schaberweg 23, 61348 Bad Homburg • phone: 49 06172 2797 0 • fax: 49 06172 2797 77 France: 1, rue Montespan, 91024 Evry • phone: 01 60 78 32 10 • fax: 01 60 78 70 90 Ireland: 8 Baronscourt Lane, Belfast, BT8 8RR • phone: 44 28 9081 4576 • fax: 44 28 9081 4576 Thames Restek UK Ltd.: Units 8-16 Ministry Wharf, Wycombe Road, Saunderton, Buckinghamshire, HP14 4HW phone: 01494 563377 • fax: 01494 564990 ©Copyright 2002, Restek Corporation For permission to reproduce any portion of this technical guide, please contact Restek’s publications/graphics department by phone (ext. 2128) or fax (814) 353-9278.

Lit. Cat. #59880A