Split Splitless Nection
Split Splitless Nection
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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, 2035 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 . . . . . .2122 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 . . . . . . . . . . . . .2627 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 . . . . .3031 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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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.
flow controller carrier gas inlet o-ring or ferrule injector liner 3-way solenoid valve backpressure regulator analytical column to detector injection port needle valve septum purge vent split vent
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.
closed
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.
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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. 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.
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 40C.
Column ID (mm)/Split Vent Flow Rate Carrier Gas helium* 0.18 25cc/min. 0.25 37.5cc/min. 0.32 55cc/min. 110cc/min. 0.53 135cc/min. 270cc/min.
Description Restek Flowmeter 6000 (9-volt battery-operated) Recalibration Service for Restek Flowmeter 6000
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. 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. () (column radius in cm)2 (column length in cm) Flow = dead volume time (min.) where = 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.: Flow = (3.14159) (0.0265cm) (3000cm) = 2.65cm3/min. 2.50 min.
2
Equation 3. Calculating the approximate on-column concentration for split injections. Concentration = concentration in sample (g/L) sample vol. injected (L) split ratio
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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
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).
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D) Cup Splitter
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.
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.
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.
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.
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Figure 3. Splitless injection flowpaths (injector purge off) in a typical flow-controlled/backpressure-regulated system.
flow controller injection port needle valve septum purge vent o-ring or ferrule injector liner 3-way solenoid valve closed backpressure regulator split vent
Figure 3. Solenoid valve closed between injector and split vent: only column flow enters injector; column flow passes into column. 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. 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. 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.
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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*2L of liquid methylene chloride expanded to 0.8mL vapor at 250C (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 L at various column headpressures Solvent Heptane Hexane Pentane Toluene Ethyl acetate Chloroform Methylene chloride Density (g/mL) 0.68 0.66 0.63 0.87 0.90 1.49 1.33 0.79 1.00 MW 100 86 72 92 88 119 85 32 18 5psig 219 245 280 303 328 400 500 792 1776 l0psig 174 196 224 242 261 319 399 629 1418 15psig 145 163 186 201 217 266 332 525 1179
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Methanol H2O
The expansion volumes were determined using a 1.0L 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 2L injections, double the expansion volumes. Use these formulas to calculate values not listed in Table III:
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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). 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. A typical sequence of events for performing a splitless injection using solvent focusing is as follows: 1. Set the initial oven temperature approximately 20C 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 30C/min.) until the first analyte of interest elutes. 5. Slow the oven program rate to enhance resolution of the remaining analytes of interest.
area
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Figure 6. Initial oven temperature too high for improper solvent focusing: solvent peak and early eluting compounds are tailing.
The sequence of events for analyte focusing is the same, except for the initial oven temperature; instead of starting 20C below the boiling point of the solvent, the oven temperature is started 6080C 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 69C. The initial oven temperature is 150C, or 80C 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, 40C, 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 20C 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 40C) is frequently used for splitless work because of sample preparation techniques. Analyses performed with an initial oven temperature of 40C 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 20C 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 6080C below the boiling point of the earliest eluting compound, instead of 20C below the boiling point of the solvent, as with solvent focusing.
30m, 0.25mm ID, 0.25m Rtx-5 (cat.# 10223) 1.0L splitless injection of a pesticide mix in hexane (5ng/L); Oven temp.: 150C to 275C @ 4C/min.
Figure 7. Initial oven temperature at least 20C below boiling point of earliest eluting analyte: early eluting compounds are symmetrical.
30m, 0.25mm ID, 0.25m Rtx-5 (cat.# 10223) 1.0L splitless injection of a pesticide mix in hexane (5ng/L); Oven temp.: 40C to 150C @ 25C/min. then to 275C @ 4C/min.
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
Endrin Breakdown Liner Type Splitless with Wool Double Gooseneck Clean Seal 6.0% 2.0% Dirty Seal 12.8% 2.4%
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100%
deactivated
See page 17.
All Restek liners are deactivated to prevent adsorption of active compounds. Call for information on custom deactivations.
A) Straight Tube
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.
F) Drilled Uniliner
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.
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carrier gas in
split liner
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.
split point
spring 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
GC_EX00600
GC_EX00601
Rtx -5 15m, 0.32mm ID, 1.50m (cat.# 10266) Sample: 50g/mL PAH standard (cat.#31011 ) in hexane Inj.: 1.0L splitless (hold 2 min.), 4mm single gooseneck inlet liner w/FSwool (cat.# 22405) Inj. temp.: 200C Carrier gas: helium, constant pressure Linear velocity: 76cm/sec. @ 40C Oven temp.: 40C(hold 4min.) to 325C @10C/min. (hold 5 min.) Det.: FID @350C
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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 0.25m bonded methyl silicone Sample: 1L each of TMS n-tetracosanoate, TMS n-hexacosanoate, and n-triacontane in nnonane at 2ng/L each component. 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 200C Carrier gas: helium at 47cm/sec. Oven: 130 to 280C 20C/min. (hold 2 min.) FID: 300C, 32 x 10-12
2 1 2 3
1 3
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C6 C44
C44
min. 4
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28
36
44
52
min. 4
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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. 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
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 evaporating solvent and volatile solutes residual layer of high-boiling point materials high boiling materials (aerosols) volatile solutes (vapor state)
vaporizing chamber
column inlet
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Figure 13. Always pack splitless inlet liners with wool when using rapid injection autosamplers.
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36
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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 (35 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 1L injections of a variety of solvents. When using an injection port temperature of 250C 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 240L, 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.
*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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Figure 14. The injection rate must be slower for large volume splitless injections. 5L/sec. injection rate
1 2 3 4 5
Solvent: Isooctane 1. n-C12 5L 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 5L sample. When a rapid injection (5L/sec.) is made, the solvent peak tails and the responses for equal concentrations of each analyte are not reproducible. A 1L/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 0.2L/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.
800-356-1688, ext. 3
or call your local Restek representative.
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.
www.restekcorp.com
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 Resteks 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 RtxTNT columns.
800-356-1688, 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.
www.restekcorp.com
18
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. 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).
4 2
6 3 5 7 9 10 8 11
1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11.
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
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 samples interaction with non-volatile residue in the inlet liner.
5 6 7 8
9 10 11
min. 4
12
16
min. 4
12
16
15m, 0.32mm ID, 1.0m Rtx-5 (cat.# 10251) 0.2L split injection of phenols (604 Phenol Mix, cat.# 31029) Oven temp.: 80C to 290C @ 8C/min. lnj.& det: temp.: 310C 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. 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.
qty. 2-pk.
cat.# 20114
www.restekcorp.com
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.
qty. set
cat.# 20108
Table V. Deactivated inlet liners show higher response factors for active components.
Compound 2,4-dinitrophenol pentachlorophenol benzidine RF Deactivated Liner 0.248 0.240 0.327 RF Undeactivated Liner 0.185 0.188 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. 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. Resteks high quality, lowbleed Thermolite septa are available for most common models of capillary GCs. For more information, request a copy of Resteks Guide to Minimizing Septa Problems (lit. cat.# 59886). For additional hints for analyzing dirty samples, request a copy of Resteks A Guide When Injecting Dirty Samples (lit. cat.# 59881).
*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
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. 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 Siltek with CarboFrit -216.1 addl. cost -216.5 addl. cost -216.25 addl. cost
5-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
25-pk.
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 -209.1 -209.5 -209.25
800-356-1688, ext. 3
or call your local Restek representative.
www.restekcorp.com
100%
deactivated
2mm Splitless
21
20772
20773
20774
4mm Splitless
featuring
Siltek deactivation
19251-60540
20772-214.1
20773-214.5
20774-214.25
22400
22401
22402
20914
20915
2mm Splitless (quartz) trace samples >2L 4mm Splitless (quartz) trace samples >2L 4mm Splitless (quartz) w/ FS Wool trace samples <2L Gooseneck Splitless (2mm)
featuring
20912
20913
22403
22404
20795
20796
20797
Siltek deactivation
5181-3316***
20795-214.1
20796-214.5
20797-214.25
5181-3316
20798
20799
20800
Siltek deactivation
5181-3316
20798-214.1
20799-214.5
20800-214.25
5062-3587
22405
22406
22407
Siltek deactivation
Siltek Gooseneck Splitless (4mm) w/ Siltek Glass Wool
5062-3587
22405-213.1
22406-213.5
22407-213.25
5181-3315
20784
20785
20786
5181-3315
20784-214.1
20785-214.5
20786-214.25
20907
20908
20895
20896
20997
Siltek deactivation
20895-214.1
20896-214.5
20997-214.25
base easily packs with wool for dirty samples <2L base easily packs with wool for dirty samples >2L
featuring
20980
20981
20982
20983
20984
20985
Siltek deactivation
base easily packs with wool for dirty samples >2L base easily packs with wool for dirty samples > 2L base easily packs with wool for dirty, active samples > 2L
20983-214.1
20984-214.5
20985-214.25
22408
22409
22410
20986
20987
20988
*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
100%
1mm Split
19251-60540
20781
20782
20783
Siltek
19251-60540
20781-213.1
20782-213.5
20783-213.25
18740-80190
20801
20802
20990
20991
mini-Lam Split
Cup Splitter
featuring
18740-80190
20709
20710
Siltek deactivation
high & low MW compounds dirty samples, many injections before cleaning required dirty samples, trace samples
18740-80190
20709-214.1
20710-214.5
20706
20707
20708
Cyclosplitter
21022
21023
20979
Siltek deactivation
Siltek 4mm Split Precision Liner w/ Siltek Glass Wool
21022-213.1
21023-213.5
20979-213.25
ID**/OD & Length (mm) 4.0 ID 6.3 OD x 78.5 ID**/OD & Length (mm) 1.0 ID 6.3 OD x 78.5 4.0 ID 6.3 OD x 78.5 4.0 ID 6.3 OD x 78.5 4.0 ID 6.3 OD x 78.5 4.0 ID 6.3 OD x 78.5 4.0 ID 6.3 OD x 78.5
A T
Low Pressure Drop Liner w/ Wool DI Liners for Agilent/Finnigan GCs (For 0.32/0.53mm ID Columns)
featuring
Benefits/Uses: trace, active samples, samples <1L trace, active samples, high recovery & linearity
Siltek deactivation
20335
20336
Uniliner***
featuring
Siltek deactivation
trace, active samples, high recovery & linearity 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
20335-214.1
20336-214.5
20337
20338
Cyclo-Uniliner ***
featuring
Siltek Cyclo-Uniliner***
Siltek deactivation
20337-214.1
20338-214.5
20843 ID**/OD & Length (mm) 4.0 ID 6.3 OD x 78.5 4.0 ID 6.3 OD x 78.5 1.0 ID 6.3 OD x 78.5 cat.# ea. 21054
Open-top Uniliner with Wool*** DI Liners for Agilent 5890 & 6890 GCs (For 0.25/0.32/0.53mm ID Columns)
Hole makes direct injection possible with EPCequipped Agilent 6890 GCs!
Drilled Uniliner
Siltek deactivation
featuring
allows direct injection when using an EPC-equipped GC allows direct injection when using an EPC-equipped GC
21054-214.1
21055-214.5
Siltek deactivation
21390-214.1
21391-214.5
www.restekcorp.com
*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. 350C Similar to Agilent part # 5180-4182 qty. 25-pk. Restek cat.# 20377
Graphite O-Rings
For Agilent and Varian 1177 GCs. Excellent thermal stability at injection port temperature up to 450C!
Description 6.35mm ID Graphite O-rings for split liners 6.5mm ID Graphite O-rings for splitless liners Max. temp. 450C 450C Similar to Agilent part # 5180-4168 5180-4173 Restek cat.# 10-pk. 50-pk. 20296 20297 20298 20299
High-Temperature O-Rings
Stable to 400C. Will not crack or melt. Softer and easier to use than graphite.
Description High-temperature O-rings Max. temp. 400C qty. 5-pk. cat.# 20437
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
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. 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
Figure 1 The Vespel Ring Inlet Seal achieves leak-tight seals even at low torque, reducing the chance of leaks.
0.01 1E-3 Leak Rate (Log10 atm cc/sec.) 1E-4 1E-5 1E-6 1E-7 1E-8 1E-9 1E-10 0 10 20 30 40 Torque (in. lbs.) 50 60
Our Vespel Ring Inlet Seal greatly improves injection port performanceit 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). Why trust a metal-to-metal seal when you can make leak-tight seals quickly and easily and more reliablywith 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.
Re-Threading Tool
Repair worn or damaged threads. Multiple uses (injection ports, fittings, etc.). Built-in guide to prevent cross-threading.
1
Achieve a better seal!
1) Worn & damaged threads can allow oxygen into the systemcompromising analytical results and destroying columns. 2) Screw the tool completely onto the injection port in a clockwise direction. 3) Unscrew the tool and inspect the threads, repeat as necessary, and, when done, wipe threads with methanol to remove any debris.
Description
qty. ea.
cat.# 23018
www.restekcorp.com
Re-threading Tool for 1/4" compression fitting for Agilent split/splitless injection ports
25
20392
20393
*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.
www.restekcorp.com
26
100%
deactivated
2mm Splitless
trace samples >2L 4mm Splitless trace, active samples up to 4L trace, dirty, active samples up to 4L
01-900109-05
20904
20905
20906
20847
20848
20849
Double Gooseneck
20897
20898
Benefits/Uses: purge & trap inlet splitting or samples <1L universal, use with rapid autosamplers high MW compounds
ID**/OD & Length (mm) 1.0 ID 6.3 OD x 72 4.0 ID 6.3 OD x 72 4.0 ID 6.3 OD x 72 4.0 ID 6.3 OD x 72 4.0 ID 6.3 OD x 72 4.0 ID 6.3 OD x 72 4.0 ID 6.3 OD x 72 4.0 ID 6.3 OD x 72
ea. 20970
25-pk.
I
1mm Split
01-900109-01
20792
20793
20794
01-900109-02
20803
20804
high & low MW compounds Cup Splitter dirty samples, many injections before cleaning required dirty samples, non-active compounds close boiling compounds
20724
20725
20727
20728
Cyclosplitter
01-900109-03
20715
20716
20717
Frit Splitter
01-900109-04
20718
20719
20720
Baffle Splitter dirty samples, active samples Split Precision Liner DI Liners for Varian 1075/1077 GCs (0.32/0.53mm ID)
21030
21031
Benefits/Uses: trace, active samples, high recovery & linearity trace, dirty, high MW, active samples, linearity trace, dirty, active samples, high recovery & linearity
ID**/OD & Length (mm) 4.0 ID 6.3 OD x 72 4.0 ID 6.3 OD x 72 4.0 ID 6.3 OD x 72
ea. 20345
25-pk.
I
Uniliner
20347
20348
Cyclo-Uniliner
20845
20846
ID**/OD & Length (mm) 0.53 ID 4.6 OD x 54 0.53 ID 4.6 OD x 54 0.80 ID 4.6 OD x 54 2.4 ID 4.6 OD x 54
ea. 20775
25-pk. 20777
0.5mm SPI
Siltek deactivation
high linearity for 0.25 & 0.32mm ID columns high linearity for 0.53mm ID columns dirty samples >1L, fits 0.25, 0.32 & 0.53mm ID columns
01-900109-06
01-900109-07
0.8mm SPI
01-900109-08
20850
20851
20852
www.restekcorp.com
*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.
100%
deactivated
4mm Split
27
EN D
39-26119-38
21077
TH IS
2mm Splitless w/wool* universal 4mm Split w/wool* 1078/1079 Liners for Varian GCs Benefits/Uses: dirty samples, non-active compounds trace samples <2L 1078/1079 Splitless
featuring
ea. 21708
25-pk.
I N S TALLS
1078/1079 Split
03-918466-00
21711
21712
Siltek deactivation
03-918466-00
trace samples <1L Open 0.5mm ID active samples 1078/1079 SplitNo Frit
featuring
03-925331-00
C O L U M N
03-918464-00
20859
20901
20909
Siltek deactivation
active samples
03-918464-00
trace, low volume samples Open 0.75mm ID trace samples, dirty samples 1078/1079 Split Precision Liner
03-925330-00
21024
21025
*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
28
100%
deactivated
Baffle Splitter
20739
20740
Cup Splitter
20745
20746
Cyclosplitter
20805
20806
N6101052
20832
20833
20834
Siltek deactivation
universal for most common analyses high & low MW compounds dirty samples, max. injections before cleaning required high MW compounds
N6101052
20832-213.1
20833-213.5
20834-213.25
20835
20836
20910
20911
20827
20828
21026
Auto SYS Split Precision Liner Splitless Liners for PerkinElmer GCs
ea. 20730
25-pk. 20732
T S
Splitless (2mm ID) trace samples Auto SYS Splitless w/Wool (2mm ID)*
featuring
N6101372
20829
20830
20831
Siltek deactivation
N6101372
20829-213.1
20830-213.5
20831-213.25
20853
20854
Similar to PE part#
20899
Auto SYS Cyclo Double Gooseneck DI Liners for PerkinElmer GCs (0.32/0.53mm ID)
Uniliner
Cyclo-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
ea. 20855
25-pk.
20857
20858
20837
20838
20839
20840
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
100%
deactivated
17A 1mm Split 128mm Split
29
221-25822-01
20751
20752
20753
20754
20755
128mm Cyclosplitter
20757
20758
20807
20808
99mm Split
universal, for most common analyses dirty samples, many injections before cleaning required high MW compounds
221-32544-01
20860
20861
20862
20870
20871
99mm Cyclosplitter
20866
20867
20868
20869
21020
ea. 20748
25-pk. 20750
128mm Splitless (3mm ID) trace samples 99mm Splitless (3mm ID) reduces backflash and catalytic decomposition reduces backflash, also operates in DI mode
221-32544-00
20863
20864
20865
20958
20959
20960
20961
20963
Siltek deactivation
Siltek 95mm Split/Splitless w/ Siltek Glass Wool DI Liners for Shimadzu GCs (0.32/0.53mm ID) Benefits/Uses: trace, active samples, high recovery & linearity trace, dirty, high MW active samples, high linearity trace, active samples, high recovery & linearity trace, dirty, high MW active samples, high recovery & linearity trace, dirty, high MW active samples, high recovery & linearity
ea. 20872
25-pk.
L
128mm Uniliner
20874
20875
128mm Cyclo-Uniliner
20876
20877
99mm Uniliner
20893
20894
99mm Cyclo-Uniliner
21713
21719
*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.
30
100%
deactivated D N E
Cyclosplitter
Laminar Cup Splitter dirty samples, many injections before cleaning required high & low MW compounds
20817
20818
Similar to TF part #
20885
ea. 20811
25-pk. 20813
I H
Splitless (2mm ID) trace samples
20814
20816
Splitless (4mm ID) DI Liners for 5000-6000 Series GCs (0.32/0.53 ID) Benefits/Uses: trace, dirty, active samples, high recovery & linearity Benefits/Uses: purge & trap & fast GC 1mm Split universal
ea. 20841
25-pk.
S
Open-top Uniliner w/Wool*
ea. 20916
25-pk.
453 20031
20936
20937
20938
3mm Split universal 5mm Split high MW compounds Laminar Cup Splitter high & low MW compounds trace samples, dirty samples
453 20030
20939
20940
20941
20948
20949
20950
20951
Cup Splitter
21028
5mm Split Precision Liner Splitless Liners for 8000 & TRACE Series GCs
ea. 20942
25-pk. 20944
Siltek deactivation
trace samples
453 20032
20942-214.1
20943-214.5
20944-214.25
453 20033
20945
20946
20947
20952
20953
Double Gooseneck
*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.
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100%
deactivated
Uniliner w/Wool
31
ea. 21114
25-pk.
21116
21117
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 for QCQ Thermo Finnigan 8000 & TRACE 2000
Ferrule ID 0.4mm* 0.5mm* 0.8mm* Fits Column ID 0.180.25mm 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.
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32
Thermolite Septa
Usable to 340C 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 325C inlet temperatures. Preconditioned and ready to use. Excellent puncturability. Do not adhere to hot metal surfaces. Low bleed. Packaged in non-contaminating glass jars.
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
Septum Diameter 9mm 9.5mm (3/8") 10mm 11mm (7/16") 11.5mm 12.5mm (1/2") 17mm Shimadzu Plug
IceBlue Septa
Usable to 250C 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.
50-pk. 22381 22388 22390 22392 22383 22394 22396 22398 100-pk. 22382 22389 22391 22393 22384 22395 22397 22399
Septum Diameter 9mm 9.5mm (3/8") 10mm 11mm (7/16") 11.5mm 12.5mm (1/2") 17mm Shimadzu plug
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33
Polyimide Resin
Permanently connects a PressTight connector to a fused silica column. 350C maximum operating temperature.
qty. 5 grams
cat.# 20445
www.restekcorp.com
34
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.
www.restekcorp.com
35
Example:
A 5m, 0.32mm ID Siltek guard column connected to a 30m, 0.32mm ID, 1.0m Rtx-5 column is cat.# 10254-365.
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.).
*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.
www.restekcorp.com
814-353-1309
www.restekcorp.com